UNIVERSITY OF CALIFORNIA DEPARTMENT OF EDUCATION GIFT OF THE PUBLISHER No./<f<? Received /#4 LIBRARY OF THE UNIVERSITY OF CALIFORNIA. GIFT OF Class From the collection of the n i-k -r m Prelinger a JJibrary p San Francisco, California 2006 ELEMENTARY CHEMISTRY A LAB OR A TOR Y MA NUA L ELEMENTARY CHEMISTRY A LABORATORY MANUAL By C. E. LINEBARGER Instructor in Chemistry in the Lake View High School, Chicago, and Editor of " School Science" RAND, McNALLY & COMPANY CHICAGO NEW YORK LONDON vi Elementary Chemistry the general work, the last few months of the course being given to the simpler parts of it. This Manual represents an attempt to fulfill the above requirements. It contains more experiments than can be performed in the usual course so as to offer a considerable range and option. The Qualitative Analysis is confined to the Appendix, and may well serve as the basis for an advanced course. The author takes pleasure in thanking the following teachers for valuable criticisms on the manuscript : Mr. Harry D. Abells, Morgan Park Academy, Morgan Park, III.; Dr. C. E. Boynton, Robert Waller High School, Chicago ; Miss Louella Chapin, South Division High School, Chicago; Mr. Harry Clifford Doane, Central High School, Grand Rapids, Midi.; Mr. Oscar R. Flynn, Hyde Park High School, Chicago; Mr. Albert C. Hale, Boys' High School, Brooklyn, N. Y.; Prof. Alexander Smith, the University of Chicago; Mr. Charles M. Turton, South Chicago High Scliool, Chicago; Prof. Theodore Whittelsey, Northwestern University ; Mr. C. M. Wirick, R. T. Crane Manual Training High School, Chicago ; Mr. E. C. Woodruff, Lake View High School, Chicago; and Mr. F. J. Watson, William McKinley High Scliool, Chicago. He also wishes to acknowledge his indebtedness to the following teachers who have read the proofs of the book and offered many helpful suggestions : Prof. Alexander Smith, the University of Chicago; Prof. G. C. Caklwell, Cornell University, Ithaca, N. Y.; Mr. Charles M. Turton, South Chicago High School, Chicago; Mr. E. C. Woodruff, Lake Vievv High School, Chicago. His thanks are also due Mr. W. E. Davis and Mr. E. C. Woodruff for the preparation of the illustrations. C. E. LlNEBARGER. Chicago, April, 1904.. THE TABLE OF CONTENTS (Numbers of Experiments follow the Titles) PAGE Introductory i Some Physical Properties of a Few Familiar Sub- stances, i Chemical Properties of a Few Familiar Sub- stances, 2 Physical and Chemical Changes, 3 Dry and Wet Reactions, 4 Reactions in Gases, 5 Reaction Due to Light, 6 Mixtures and Compounds, 7 Law of Con- servation of Matter (Persistence of Mass), 8. Oxygen ... 14 Oxygen from Silver Oxid, 9 Oxygen from Mercuric Oxid, 10 Oxygen from Potassium Chlorate, from a Mix- ture of Potassium Chlorate and Manganese Dioxid, n Preparation of Oxygen from a Mixture of Potassium Chlo- rate and Manganese Dioxid, 12 Oxygen from Sodium Peroxid by Action of Water, 13 Properties of Oxygen, 14. Ozone 21 Preparation of Ozone, 15 To Find the Weight of One Liter of Oxygen, 16 To Find the Percentage of Oxygen in Potassium Chlorate, 17. Hydrogen 26 Hydrogen from Acids by Action of Zinc, 18 Proper- ties of Hydrogen, 19 Transpiration of Hydrogen, 20 Combustion of Hydrogen, 21 Oxidation and Reduction, 22 Hydrogen from Water by Action of Sodium, 23 Hydrogen from Steam by Action of Magnesium, 24 Hydrogen from Steam by Action of Iron, 25 Hydrogen from Solutions of Caustic Alkalis by Action of Aluminum, 26 Hydrogen from Sodium Hydroxid by Heating with Iron Powder, 27 Hydrogen from Calcium Hydroxid by Action of Iron Powder or Zinc Dust, 28. Water 34 Dissolved Matter in Different Waters, 29 Distillation, 30 Coagulation Filters, 31 Conditions Effecting Solu- tions, 32 To Determine the Solubility of Potassium [vii] viii Elementary Chemistry PAGE Dichromate in Water, 33 To determine the Solubility of Air in Water, 34 Heat Effects of Solution, 35 Super- saturation, 36 Water of Crystallization, 37 To Find the Percentage of Water of Crystallization in Gypsum, 38 Deliquescence, 39 Efflorescence, 40 Test for Water, 41 - To'Ascertain the Volumetric Composition of Water, 42. Hydrogen Dioxid 43 Hydrogen Dioxid by Action of Sodium Peroxid on Water, 43 Hydrogen Dioxid by Action of Sulfuric Acid on Barium Dioxid, 44 Properties of Hydrogen Dioxid, 45 - To Verify the Law of Definite Proportions by Weight, 46 To Verify the Law of Definite Proportions by Vol- ume, 47 To Verify the Law of Multiple Proportions, 48. Nitrogen and Its Hydrogen Compounds 47 Separation of Nitrogen from the Air, 49 Nitrogen by the Decomposition of Ammonium Nitrate, 50 Nitrogen from Potassium Nitrate by Action of Iron Powder, 51 Ammonia from Ammonium Salts by Action of Caustic Alkalis or Lime, 52 Ammonia from the Destructive Distillation of Some Animal Substances, 53 Preparation and Properties of Ammonia, 54 Ammonia by the Inter- action of Potassium Nitrate, Potassium Hydroxid, and Iron Powder, 55. Carbon 51 Formation of Charcoal, 56 Graphite from Pig Iron, 57 Preparation of Lampblack, 58 Density and Porosity of Charcoal, 59 Adsorption of Gases by Charcoal, 60 Reduction by Charcoal, 61 Decolorizing Action of Bone- black, 62 Combustibility of Different Forms of Carbon, 63. The Compounds of Carbon with Oxygen 54 Carbon Dioxid a Product of Combustion, 64 Carbon Dioxid Given Off in Respiration, 65 Carbon Dioxid Pro- duced by Fermentation, 66 Carbon Dioxid from a Car- bonate by Action of an Acid, 67 Properties of Carbon Dioxid, 68 Action of Carbon Dioxid on Litmus, 69 Carbon Dioxid Absorbed by Sodium or Potassium Hydroxid Solutions, 70 Carbon Dioxid in Solution Dissolves Cal- cium Carbonate, 71 Carbon Monoxid by Action of Sul- furic Acid on Sodium Formate, 72 Carbon Monoxid by The Table of Contents ix PAGE the Action of Sulfuric Acid on Potassium Ferrocyanid, 73 Oxids of Carbon from Oxalic Acid, 74 To Find the Weight of a Liter of Carbon Dioxid, 75. Nitrogen and Hydrogen Compounds of Carbon .... 60 Methane from Sodium Acetate by Action of Soda-lime., 76 Ethylene from Alcohol by Action of Sulfuric Acid, 77 Acetylene by Action of Water on Calcium Carbid, 78 Destructive Distillation, 79 A Simple Gas Factory, 80 A Candle as a Gas Factory, 81. The Atmosphere 62 To Determine the Percentage of Oxygen in the Air, 82 Volume of Oxygen in Air, 83 Action of Dust on the Precipitation of Water Vapor, 84 To Find the Weight of a Liter of Air, 85. Fire and Flame 66 Kindling Temperature, 86 Structure of Flame, 87 Luminosity of Flame, 88 Speed of Propagation of Flame, 89 Oxidizing and Reducing Flames, 90. Salts, Acids, and Bases 68 General Properties of Acids, 91 General Properties of Bases, 92 Neutralization, 93. Oxids of Nitrogen ; Nitric Acid 69 Preparation and Properties of Nitrous Oxid, 94 Nitric Oxid ; Its Preparation and Properties, 95 Volumetric Composition of Nitric Oxid, 96 Nitrogen Dioxid, 97 Illustration of the Law of Volumetric Proportions, 98 Preparation and Properties of Nitric Acid, 99 Decompo- sition of Nitric Acid by Heat, 100 Reduction of Nitric Acid to Ammonia, 101 Reduction of a Nitrate to a Nitrite, 102. Preparation and Properties of Acids, Bases, and Salts . . 75 Preparation of a Salt by Direct Union of the Elements, IO 3 Preparation of a Salt by the Solution of a Metal in an Acid, 104 Preparation of a Salt by Neutralization of Ammonium Hydroxid by Hydrochloric Acid, 105 The Solubility Product, 106. x Elementary Chemistry PAGE The Halogens and Their Hydrogen Compounds 78 Chlorin by Oxidization of Hydrochloric Acid, 107 Preparation of Chlorin, 108-109 Properties of Chlorin, no Chlorin Water, in Preparation and Properties of Bromin, 112 Preparation and Properties of lodin, 113 Tests for Free Bromin and lodin, 114 Action of Concen- trated Sulfuric Acid on Halid Salts, 115 Preparation and Properties of Hydrochloric Acid, 116 Analysis of Hy- drogen Chlorid, 117 Tests for Chlorids, Bromids, and lodids, 118 To find the Atomic Weight of Chlorin, 119 To Ascertain the Strength of a Given Sample of Hydro- chloric Acid, 120 To find the Strength of a Given Sample of Nitric Acid, 121. The Alkali Metals 89 Properties of Sodium and Potassium, 122 Preparation and Properties of Potassium Carbonate, 123 Preparation and Properties of Sodium and Potassium Hydroxids, 124 Preparation and Properties of Ammonium Amalgam, 125 Solvay Process of Sodium Carbonate Manufacture, 126 Flame Tests, 127 Preparation and Properties of the Nitrates_of the Alkali Metals, 128 Test for a Nitrate, 129. Equivalent Weights 93 Equivalent of Sodium, 130 Equivalent of Zinc, 131 Equivalent of Magnesium, 132 Equivalent of Zinc, 133 To Determine the Vapor Density of Alcohol by Dumas' Method, 134. Sulfur and Its Compounds 97 Properties of Sulfur, 135 Preparation and Properties of Hydrogen Sulfid, 136 Preparation of Sulfur Dioxid, 137 Properties of Sulfur Dioxid, 138 Properties of Sulfurous Acid, 139 Properties of Sulfuric Acid, 140. Phosphorus 100 Physical Properties of Phosphorus, 141 Conversion of Red Phosphorus into Yellow Phosphorus, 142 Prepa- ration and Properties of Phosphin, 143 Preparation of Metaphosphoric Acid, 144 Preparation of Orthophos- phoric Acid, 145 Reactions of Phosphates, 146. The Table of Contents xi PAGE Arsenic and Antimony 103 Properties of Arsenic, 147 Arsin, 148 Arsenic Tri- oxid, Trichlorid, and Trisulfid, 149 Arsenic Acid, 150 Properties of Antimony, 151 Stibin, 152 Antimony Trioxid, Trichlorid, and Trisulfid, 153. Bismuth 105 Properties of Bismuth, 154 Reactions of Salts of Bis- muth, 155. Magnesium 106 Properties of Magnesium, 156 Reactions of Mag- nesium Salts, 157 Preparation of Magnesium Sulfate, 158 Preparation and Properties of Calcium Oxid and Hydroxid, 159 Properties of Calcium Compounds, 160 Reactions of Strontium and Barium Salts, 161. Boron and Silicon , 108 Preparation of Boric Acid, 162 Characteristic Reac- tion of Boron Compounds, 163 Borax Bead, 164 Prep- aration of Magnesium Silicid and of Silicon Hydrid, 165 Preparation of Silicic Acids, 166. Zinc no Properties of Zinc, 167 Reactions of Zinc Salts, 168 Blowpipe Reactions, 169. Cadmium no Properties and Reactions, 170. Mercury in Preparation of Mercury, 171 Mercurous Nitrate, 172 Mercuric Nitrate, 173 Reactions of Mercurous Salts, 174 Reactions of Mercuric Salts, 175. Aluminum 112 Properties of Aluminum, 176 Action of Acids and Alkalis on Aluminum, 177 Action of Mordants, 178 Alums, 179 Reactions of Aluminum Compounds, 180. Tin 114 Physical Properties, 181 Crystallization of Tin, 182 Action of Acids on Tin, 183 Preparation of a Solution of Stannic Chlorid, 184 Distinction Between Stannous and Stannic Salts, 185 Replacement of Tin by Zinc, 186 To Determine the Equivalent of Tin, 187. xii Elementary Chemistry PAGE Lead 116 Physical Properties of Lead, 188 Deposition of Lead by Zinc, 189 Action of Acids on Lead, 190 Prepara- tion and Properties of Lead Monoxid, 191 Preparation and Properties of Red Lead, 192 Preparation and Properties of Lead Dioxid, 193 Reactions of Lead Salts, 194 Action of Water on Lead, 195. Copper 118 Properties of Copper, 196 Precipitate of Copper, 197 Preparation of Cuprous Oxid, 198 Reactions of Cop- per Salts, 199 To Find the Equivalent of Copper, 200. Silver 120 Preparation and Properties of Silver, 201 Reactions of Silver Salts, 202. Iron 121 Properties of Iron, 203 Reactions of Ferrous Salts, 204 Reactions of Ferric Salts, 205 Oxidation of Fer- rous Salts, 206 Reduction of Ferric Salts, 207 Manu- facture of Ink, 208 Borax Bead Test for Iron, 209. Nickel 124 Reactions of Nickel Salts, 210. Cobalt 124 Reactions of Cobalt Salts, 211 Analysis of a Nickel Coin, 212. Chromium and Manganese 125 Reactions of Chromic Salts, 213 Borax Bead Test for Chromium, 214 Reduction of Chromates to Chromic Compounds, 215 Properties of Chromates, 216 Reac- tions of Manganous Salts, 217 Borax Bead Test for Manganese, 218 Oxidation with Potassium Perman- ganate, 219. Some Organic Compounds 127 Preparation of Aldehydes, 220 Preparation of Ethyl Acetate, 221 Preparation of Soap, 222 Fehling's Test for Sugar, 223 Preparation of Oxalic Acid, 224 Prepa- ration of Nitrobenzene, 225 Preparation of Aniline, 226. The Table of Contents xiii PAGE APPENDIX A Qualitative Analysis i Introductory Hydrochloric Acid Group Hydrogen Sulfid Group Ammonium Sulfid Group Ammonium Carbonate Group The Alkali Metals : Ammonium, Sodium, Potassium. APPENDIX B The Metric System of Weights and Measures .... xvii APPENDIX C Instruments for Weighing and Measuring xix The Thermometer The Barometer Balances Grad- uated Vessels. APPENDIX D Tables xxvi Physical Constants of some of the Elements Tension of Water Vapor Solutions to be Prepared. APPENDIX E Significant Figures and Forms of Record in Quantitative Work xxxi APPENDIX F Laboratory Equipment xxxvi List A, Individual Apparatus List B, Table Appa- ratus List C, Demonstration Apparatus List D, Chemicals. EXPERIMENTS INTRODUCTORY EXPERIMENT i. Some Physical Properties of a Few Familiar Substances. What information do your senses of sight, of smell, of taste, of hearing, and of feeling give you in regard to the following sub- stances : Charcoal, sulfur, paraffin, common salt (sodium chlorid), sugar, naphthalene (moth balls), borax, salt- peter (potassium nitrate), alcohol ? Tabulate the results of your observations in the form outlined below. Put some (S mm - or i cm - circle 1 ) of each of the sub- stances examined above in a test tube (a separate tube for each substance), fill the tube a third full of water, and note whether the substance sinks or swims. Shake the substance and water well together 2 and see if it dissolves. Heat the water to boiling 3 in the flame of a Bunsen burner 4 and note anything that happens. Set the tubes aside until cold (leave the one containing the charcoal for several hours) and note any changes. Tabulate your observations in the form outlined below: Behavior in Water SUBSTANCE Sight Smell Taste Hear- Feeling Specific gravity, solubility, etc. ing Cold Hot color odor sweet ring hard opacity sonr thud soft etc. etc. etc. [I] Elementary Chemistry Fig. I ONE WAY OF SHAKING THE CONTENTS OF A TEST TUBE Which of your senses gives you the most information ? What tests serve to identify each of the substances? NOTE i. Estimation of Amounts of Substances. Many chem- icals come in powdered form or may be easily reduced to a powder. If a circle of given diameter be drawn on a piece of paper and as much of the powder as possible placed upon it so as to form a conical heap whose base is the circle, fairly definite amounts of the powder are obtained. In the directions the diameter in centimeters is given right after the weight in case the sub- stance in use is a powder; as, (s cm - circle). If the substance is not powdered and it is not convenient to reduce it to a powder, the amount may be expressed in terms of the size of a single piece; this is given in millimeters. Thus, bim. means that a piece should be selected or prepared that is equivalent in size to one of spherical shape &mm. \\\ diameter. Such estimations need not be made very accurately, as even rather wide deviations will not essentially affect the experiment. Note that the unit employed in designating amounts of powders is centimeters, while that used in denoting the size of single pieces is millimeters. NOTE 2. To Shake a Liquid and Solid Together in a Test Tube, (i) Gently tap the rounded end of the tube held as horizontally as possible in the palm of the hand (Fig. i). (2) Close the tube with the thumb and invert it. The first method is to be used when the liquid is hot or corrosive. NOTE 3. Handling Test Tubes. Test tubes may be held by the upper end in the lingers (Fig. 2) generally without inconvenience, but if the liquid is to be boiled for some time or the substance is to be heated to a high temperature in the test tube, it may be grasped and held with a test tube holder, several forms of which are on the market. A serviceable Fig. 2 TEST TUBE-HEED IN THE- FINGERS Experiments test tube holder may readily be made of rather stout wire, the ends of which are twisted into coils into which the tube just fits, while the middle part is twisted together and inserted in a handle of wood or cork (Fig. 3). A substitute for a test Fig. 3 TEST TUBE HOLDER tube holder is a strip of paper folded and passed around the test tube just below its mouth so that the two ends of the paper may be held between the thumb and forefinger (Fig. 4) or by tongs (Fig. 5). In heating test tubes containing a liquid, the outside of the tube must be dry and the glass heated uniformly and gradually. It should be held in the upper part of the flame and should at first be passed to and fro through it. The flame should never be allowed to touch any part of the tube which is not covered on the inside with the liquid, as the bare glass may become so high- ly heated that if the compara- tively cold liquid touches it, it may break. When a liquid is being boiled vigorously in a test tube, it sometimes happens that portions of the hot liquid are thrown out of the tube with considerable force. This may be avoided by holding the tube in an inclined position and continually rolling it to and fro and moving it around in the flame. Be very careful always to hold the mouth of the tube away from yourself as well as your neigh- bors, so that in case the liquid does spurt out, it will not harm any one. Test tubes should always be cleaned as soon as possible after using. A test tube swab or cleaner which compares favorably with the bristle ones sold by the dealers may be made out of a wooden stick with a bit of sponge or rag tied over its end. NOTE 4. Bunsen Burners. Bunsen burners are not only an indispensable source of heat in all laboratories provided with gas, but are also used in slightly modified form in gas stove and "Welsbach" burners. The construction of a Bunsen burner is shown in Fig. 6. The gas enters at e and passes up through the opening at in into the tube n. Air is drawn in through the holes at the base of n, and mixes with the gas. These holes can be more or less closed by means of a ring 0, perforated with two corresponding holes a. The mixture of gas and air issuing from Fig. 4 TEST TUBE HELD BY STRIP OF PAPER Elementary Chemistry 1 Fitf. 5 TEST TUBE HELD BY STRIP OF PAPER GRASPED BY TONGS the top of the tube burns with an almost non-luminous flame. When the supply of air is cut off by turning the ring b, the flame becomes luminous and smoky. To put a Bunsen burner in good condition, unscrew the tube , and clean, if necessary, the gas tip at m. The ring should move freely around the tube. Put the burner together again and, connecting e with the gas supply by means of rubber hose of suitable length, open wide the gas cock. As soon as the gas seems to be escap- ing freely, light it. If the burner is in order and the airholes at in are wide open, the flame should be blue, with the exception of a minute yellow spot near the top of the flame. If this spot does not appear in the ^ flame, partially close the airholes until it is seen. If the flame is at all luminous, even when the airholes are wide open, the supply of gas is too great for the supply of air. So unscrew the tube n, and make ;;/ a little smaller by pinching or hammering it together somewhat. If the flame is too small and burns with a hissing noise, open ;;/ a little. Never use a burner unless it is in perfect work- ing condition. If the gas supply is insufficient, the flame will often "strike back," /. e., the gas will burn at m instead of d. When this occurs the tube n soon becomes so hot that it cannot be handled, and the flame appears green and smoky, and emits an unpleasant odor. As soon as you find that a flame has " struck back," cut off the supply of gas, and after a minute or so relight. EXPERIMENT 2. Some Chemical Properties of a Few Familiar Substances. Put a piece (3 mm.^ o f charcoal in a clean iron spoon and hold it in a Bunsen flame (Fig. 7). Observe carefully Fig. 6 BUNSEN BURNER Experiments the behavior of the charcoal. Heat as hot as possible until no further change is manifest. Go through similar operations with the substances used in Experiment i, taking a piece not larger than 3 mm -, and noting the appearance of flame, color, and odor of fumes, appear- ance and relative amount of ash, and in case the sub- stance does not seem to burn, whether it swells up or melts. Which of the substances are not changed chemically ? What tests can you add to those you found in Experiment i ? EXPERIMENT 3. Physical and Chem- ical Changes, (a) Hold a piece of plati- num wire in a Bunsen flame for a minute or so, and note what occurs. Let the wire cool and see if it has been per- manently changed. (b) Go through the same operations as in (#), using magnesium Wire Or ribbon instead Fig - T-HEATING A SUBSTANCE IN A SPOON of platinum. Compare restilt with that obtained in (a). Compare the nature of the changes in (a) and (b). (c) Wind tightly around one of the ends of each of two electric light carbons (not "coppered") about 10 cm - of pieces of copper wire about \$cm. long. Con- nect the other ends of the wires with a source of elec- tricity and immerse the lower halves of the carbons in a strong solution of copper sulfate (blue vitriol) Elementary Chemistry contained in a beaker or tumbler (Fig-. 8). Keeping the carbons about a centimeter apart, let the current pass for a few minutes. Then remove and examine the carbons. Is there any evidence that a chemical change has taken place ? Are both carbons affected in the same way ? Compare this result with that obtained by causing a current of electricity to pass through a wire (incandescent bulb). (d) Place a little (2 cm - circle) table salt in a test tube and half fill the tube with water. Close the tube with the thumb and shake until most of the salt has disappeared. Filter 5 , catching the filtrate (the liquid which passes through the paper) in a clean evaporating dish. Does the filtrate taste salty ? Set the dish on a ring of a retort stand (Fig. 9) and heat, using a large flame and play- ing it around so that the dish is heated uni- formly and the bottom not more than the sides. Conduct all Fig. 8 ELECTRIC LIGHT CARBONS CONNECTED WITH A BATTERY BY MEANS OF COPPER WIRES AND IMMERSED IN A COPPER SUL- WITH A BATTERY BY MEANS OF COPPER r ~ rp ,f ,-, 11 -rr Qn fV, p f n nn A ^ S FATE SOLUTION o f t ft Q liquid may spatter out of the dish and be lost. As the water boils away a white substance is deposited, w^hich, when most of the water has been driven off, crackles or decrepitates. The decrepitation is due to particles of the solid enclos- ing minute amounts of water, which are expelled with explosive violence when the solid is heated. When the decrepitation ceases let the dish cool and examine its contents. Give all your reasons for thinking it to be the substance you take it to be. Are the changes phys- ical or chemical ? Experiments (c) Put some (2 cm - circle) powdered marble in a test tube about a third full of water. Close the tube with the thumb and shake well. Does any of the marble seem to dissolve ? Decant the liquid, i. e., pour it off from the solid so as to have as little as pos- sible of the latter go with it, on a filter (Fig. 10), and catch the fil- trate in a clean evap- orating dish. Heat the dish as directed in (d) until no more liquid is left. Is there more than a trace of a solid residue ? What do you conclude about the solu- bility of marble in water ? Pour 6 enough dilute hydro- chloric acid on the marble left in the test tube to fill it about one-fourth full. Warm gently so as to keep up a brisk evolu- tion of gas. When the effer- vescence ceases filter through a fresh filter paper and catch the filtrate in a clean evapo- rating dish. Now heat the liquid and evaporate it to dry- ness. Is there any decrepi- tation ? Cautiously taste a bit of the residue not larger than a pin head. Does it taste salty ? Point out the physical Fig. 9 EVAPORATING TO DRYNESS WITH FREE OR BARE FLAME Fig. 10 FILTERING Elementary Chemistry 2 3 Fig. II SUCCESSIVE STEPS IN FOLDING A FILTER PAPER and chemical changes. Let the dish containing the residue stand for at least twenty-four hours and then examine it. It will probably have attracted moisture from the air and will be moist or even liquid if the amount of water attracted is sufficient to dissolve it. The substance is on this account said to be deliquescent; its name is calcium chlorid. Fig. 12 POURING LIQUID FROM A BOTTLE INTO A TEST TUBE NOTE 5. Filtering. Filter paper is fitted into a. funnel as follows : The paper is folded to form a semi-circle and then a quarter of a circle (Fig. 1 1). Three of the quarters are separated from the fourth so as to form a cone which is fitted into the funnel, wetted and smoothed around so as to fit the funnel. When pouring a liquid on a filter, direct the stream of liquid so that it strikes against the side of the paper cone and not into the apex, otherwise there is danger of splashing. (Fig. 10.) The stern of the funnel should touch the inside of the receiver of the filtrate so as to prevent the formation of drops which by their fall might occasion splashing. NOTE 6. Pouring a Liquid from a Bottle. In pouring hold the bottle in the right hand with the thumb close to the label and the little finger under the bottom (Fig."i2). Re- move the stopper with the second and third fingers of the left hand, the thumb and first finger of which Fig. 13 POURING FROM ONE BOTTLE INTO ANOTHER Experiments hold the test tube or other receptacle. Remove the drop of liquid that may adhere to the lip of the bottle by touching it with the stopper, replace the stopper and return the bottle to its proper place. The stoppers and bottles may also be held as shown in Fig. 13. Stoppers should never be placed upon the table top except in extreme cases, and then only upon a piece of clean paper or glass. EXPERIMENT 4. Dry and Wet Reactions, (a] Rub together in a dry mortar a pinch of mercuric chlorid with a pinch of potassium iodid. What is the color and solubility of the product ? (b) Dissolve a pinch of mer- curic chlorid in enough water to fill a test tube about half full ; also a pinch of potassium iodid in about the same volume of water in a second test tube. Mix the solutions. How does the color and solubility of the prod- uct compare with that obtained in (a) ? In which case does the reaction take place the more rapidly ? (c) Mix together on a piece of dry paper about equal bulks (3 cm - circle) of powdered sodium bicarbonate (baking soda) or sodium carbonate (washing soda) with powdered tartaric or oxalic acid. Is there any appa- rent change ? Put the mixture in a beaker a fourth full of water. What happens ? EXPERIMENT 5. Reactions in Gases. Select two wide-mouthed bottles or jars of the same size. Put in one a couple of drops of strong hydrochloric acid and Fig. 14 CYLINDRICAL JARS PLACED MOUTH TO MOUTH io Elementary Chemistry cover the mouth of the bottle with a card. Likewise put a couple of drops of strong ammonia water in the other. Move the covered bottles around so that as much of their inside surfaces as possible may be wetted. Both the liquids give off vapors which are thus made to fill the bottles. Place one bottle on the other in an inverted position (Fig. 14) and slip out the cards. What evidence is there that a reaction has taken place ? What is the nature of the product ? EXPERIMENT 6. Reaction Due to Light. Procure a piece of blue-print paper which has not been exposed to a strong light and tear it in two. Place one of the halves between the leaves of a book so as to keep it from the light and expose the other for ten minutes to direct sunlight, or if that be not available, leave it on the desk until the next laboratory period. Place both pieces of paper in a dish and run water over them to wash out any soluble coloring matter and compare the color of the two pieces. What evidence is there that a chemical reaction has taken place ? EXPERIMENT 7. Mixtures and Compounds. I. (a) Put a pinch of powdered iron or clean and fine iron filings on a piece of smooth paper and move one end of a bar magnet over the underside of the paper just beneath the iron. Can the iron be drawn from one part of the paper to another ? (b) Perform a similar experiment with powdered sulfur instead of iron. (c) Put a pinch of powdered iron in a small test tube and pour over it enough carbon bisulfid to fill the tube about an eighth full. Shake thoroughly. Does the iron seem to dissolve? (d) Decant the liquid into a watch glass and allow it to evaporate in the hood or out of doors. Is more than a trace left ? Experiments I I (c) Repeat (c) and (d) with powdered sulfur instead of iron. What is the residue ? How do you know ? (f) Compare the solubility of iron and sulfur in carbon bisulfid. (g) Put a pinch of powdered iron in a small test tube and cover it with dilute hydrochloric acid. What occurs ? Note particularly any odor. Wet a small piece of filter paper with a few drops of lead acetate solution and cover the mouth of the test tube with it. Does it change color ? (//) Repeat (g) with sulfur instead of iron. Com- pare the solubility of iron and sulfur in hydrochloric acid. Are the above tests sufficient to distinguish iron from sulfur? (i) Weigh out 5.6 ff- of powdered iron and 3.2 & of powdered sulfur and mix them thoroughly in a mortar. What is the color of the mixture ? (j) Place a pinch of the mixture on a piece of paper and see if you can separate the iron from the sulfur by moving a magnet under it as in (a). (k) Put a little of the mixture in a small dry test tube, add carbon bisulfid and shake thoroughly. Decant upon a dry filter and catch the filtrate in a watch glass. What is left after the carbon bisulfid evaporates ? Com- pare with (d) and (c). (/) Place a pinch of the mixture in a test tube and add dilute hydrochloric acid. Compare with (g) and (//). (;//) Now put all of the mixture that remains in a rather small dry test tube and, using a test tube holder, hold just the rounded end of the tube steadily in the tip of a Bunsen flame until the lower part of the mixture begins to glow. Then immediately remove the tube from the flame. (n) When the test tube is cool lay it on a piece of paper and break it by tapping it with a pestle. Separate 12 Elementary Chemistry the substance from the particles of glass and pulverize it in a mortar. Compare its appearance with that of the sulfur and iron and their mixture before heating. (o) Place a pinch of the product on paper and test it with a magnet as in (a) and (/). Compare with (a). (p) Treat a little with carbon bisulfid as in (c), (d), and (k). Result? (</) Add hydrochloric acid to another portion as in (), (/?), and (/). Note the smell of the gas and its action on lead acetate paper. Compare with (g) and (//). Point out all the chemical and physical changes in this experiment. Are the properties of the product from (;//) different enough from those of iron and sulfur to characterize it as a new substance ? Why were defi- nite amounts of the two elements taken ? II. (a) Examine some gunpowder for its physical properties ; apply the tests used in Experiment i. Place a pinch of gunpowder in a spoon and heat it as you did in Experiment 2 ; be careful not to lean over the spoon, as the powder may flash up into the face. Put about 3 ff- (3 cm - circle) of gunpowder in a test tube and add enough carbon bisulfid to fill the test tube about a quarter full. Filter through a small, dry filter paper and catch the filtrate in a clean watch crystal. Set in the hood to evaporate and determine by appropriate tests what the residue is. CAUTION. Carbon bisulfid forms with air an explosive mixture. Do not neglect to extinguish all flames within a yard of you before using it. (b] Spread out the filter paper and shake out upon it the residue in the test tube, so that the carbon bisul- fid may evaporate. (r) Put this residue in a test tube and fill about one- third full of water. Shake the solid and the liquid Experiments together thoroughly, and heat for a moment to boiling. Filter into an evaporating dish, and evaporate to dry- ness over a bare flame. (d) Examine the residue obtained as in Experiments i and 2. Give all your reasons for thinking it to be the substance you take it to be. Shake the black substance remaining in the test tube out on the filter paper and spread it out so that the water may evaporate. (c) Examine the residue when dry to find out what it is, and give your proofs for what you take it to be. Into how many con- stituents have you decomposed or analyzed gun- powder ? Which Fig. J S CHASLYN BALANCE AND ERLENMEYER FLASK Used in illustrating Law of Conservation of Matter of them are ele- ments ? (/) Put some (i cm - circle) saltpeter in a mortar, add about half its btilk of sulfur and grind the substances to a fine powder. Add an equal bulk of charcoal and grind all well together, but do not use too great a pres- sure. Put a pinch of the mixture in a spoon and apply a flame. What happens ? What new substance have you prepared from saltpeter, sulfur, and charcoal ? Is it a mixture or a compound ? EXPERIMENT 8. Law of Conservation of Matter (Persistence of Mass). Fit an Erlenmeyer flask with a tight stopper and fill the flask about a third full of 14 Elementary Chemistry strong lead acetate solution. Fill a test tube which is small enough to slip inside the flask with a strong solu- tion of ferric chlorid and carefully put it in the flask so as not to mix the two liquids. Insert the cork tightly and counterpoise the whole on a balance. (Fig. 15.) Then tip the flask upside down so as to mix the two solutions and, placing the flask again upon the balance pan, see if the equilibrium has been destroyed. What evidence is there that a chemical action has taken place ? Wherein does this experiment illustrate the law in question ? OXYGEN EXPERIMENT 9. Oxygen from Silver Oxid. Put some (2 cm - circle) silver oxid in a test tube and, holding the tube with tongs (Fig. 5), heat it in a Bunsen flame. Bring a splinter of wood with a spark on its end into the mouth of the test tube from time to time and note what happens. Heat until the brown powder is turned into a white mass. How can you prove this to be silver ? How do you know that a gas is given off ? EXPERIMENT 10. Oxygen from Mercuric Oxid. Put enough mercuric oxid in an ignition tube 7 to fill it to the depth of about a centimeter. Grasping the tube with a test tube holder, heat it in a Bunsen flame, very gradually raising its temperature as high as pos- sible. Note any change in the color of the powder as it is being heated. When the tube is red hot, insert (with- out removing it from the flame) a splinter of wood with a spark on its end. What happens? How do you account for it ? After the tube is cool, what is the color of the mercuric oxid which is left ? Is this change of color of a physical or a chemical nature ? Examine the deposit (sublimate} in the upper part of the tube, and find out by its physical properties what it is. Experiments 1 5 NOTE 7. Ignition Tubes. Ignition tubes are made of a spe- cial kind of glass, often called "hard glass," which can with- stand a very high temperature without melting. They should be heated very gradually, as, being made of thicker glass than ordinary test tubes, they are liable to break the more readily when heated. To make an ignition tube, choose a piece of hard glass (thick- walled ordinary glass will do) about 8 mm. i n diameter, $mm. in bore, and 12 to \^cm J long. Heat the tubing in the middle in a Bunsen flame (better, a blast lamp flame) just above the yellow spot, holding the ends in either hand and rotating the tube so as to heat it uniformly. As soon as the glass begins to soften and yield a little, pull it apart a little, keeping it in the flame and rotating it all the while. Draw it apart very slowly so that the glass of the closed end may be thick enough. When the tube separates hold one part up with its closed end in the flame so that it may be rounded off a little and, removing the tube from the flame, blow gently into it so as to make the end slightly bulb- shaped. Let the tubes cool very slowly, /. e. t anneal them by closing the airholes of the burner, and holding them in the smoky flame until they are covered with a deposit of soot. EXPERIMENT IT. Oxygen from Potassium Chlo- rate, and from a Mixture of Potassium Chlorate and Manganese Dioxid. Fill a test tube to a depth of about 2 cm - with potassium chlorate, and holding it with a test tube holder, heat the rounded end in a Bunsen flame. When the solid melts and effervesces freely, insert a glowing splinter of wood into the mouth of the test tube. Drop little bits of wood (not more than 2 mm.} down into the effervescing melt. What happens ? Remove the test tube from the flame and as soon as the effervescence ceases, slide a pinch (be sure not to use too much) of powdered manganese dioxid from a creased paper into the melted potassium chlorate. In what way does the result show that a mixture of potas- sium chlorate and manganese dioxid gives off oxygen at a lower temperature than the former substance alone? WhenUhe tube is cool, fill it with water and let it soak for several hours ; the melt may then be easily removed. i6 Elementary Chemistry EXPERIMENT 12. Preparation of Oxygen from a Mixture of Potassium Chlorate and Manganese Dioxid. Mix about 30^- (^cm, circle) of powdered potassium chlorate with about a third of its bulk of manganese dioxid and transfer to a dry flask (200 to 300 c - c -}. Bore a hole through a cork 8 , fitting the neck of the flask so that an L-tube 9> ! may be pushed through it. Slip over one branch of the L-tube one end of a piece of rubber tubing about 30 cm - long, whose other end is slipped over a delivery tube ! ! . Set the flask on a wire gauze ] 2 on a ring of a stand and secure the neck of the flask with a second ring (Fig. 16). Alternate Apparatus. (Fig. 17.) A retort is pro- vided with a delivery tube and is supported on a ring stand over a wire gauze or sand bath 1 2 . Place the mixture in the flask or retort, and heat with a small flame, removing the flame if the evolution of the gas becomes too brisk. Collect five receivers full by water displace- ment 13 , and pass to Experiment 14. NOTE 8. To Per- forate Corks. To perforate a cork, a round ("rat-tail") file about i$cm. long is required. A cork is chosen of such a size that its narrower end fits a little loosely in the neck of the flask, retort, etc. The cork is softened in a cork squeezer or by rolling it on (i) the table top under a board ; or (2) on the floor under the sole of the shoe. The tip of the tang of the file is heated to redness and the red-hot point used to burn a small and regular hole through the axis of the cork. This hole is then enlarged with the file until the glass tube can just be passed through it by employing a twisting motion. Fig. l6 HEATING A SUBSTANCE IN A FLASK AND COLLECTING THE GAS EVOLVED Experiments Fig. 17 HEATING A SUBSTANCE IN A RETORT AND COLLECTING THE GAS EVOLVED BY WATER DISPLACEMENT Cork borers may also be used. These are tubes of brass or steel, with a cutting edge, and are of various sizes, so as to cut a hole of very nearly the desired diameter at once. NOTE 9. To Cut Glass Tubing. To cut glass tubing, a three- cornered file about 25 cm. long is needed. The tube is laid flat upon the table, and a deep scratch made with the file at the point where the tube is to be cut. The tube is then grasped with the two hands, one on each side of the scratch, while the thumbs are brought together just at the scratch, but on the side opposite. While the fingers are pulling on the tube in the direction of its length, a slight push with the thumbs across the axis of the tube usually suffices to break it squarely off. When a piece of glass tubing is cut the ends have sharp edges which may cut rubber tubing slipped over them. The edges should be smoothed down or " fire polished" by gradually heating them in a flame, all the while twirling the tubing so that the edges are heated uniformly, until the glass softens and the sharp edges become rounded off, but care should be taken that the bore of the tube is not at all lessened. NOTE 10. To Bend Tubing. To bend glass tubing, hold it in a flat luminous flame, such as that offered by an ordinary gas jet (a so-called "bat-wing," "fish-tail," or "wing-top" may be put on the Bunsen burner). Rotate the tube and move it to and fro so as to heat a portion of the tube at least ^cm. in length. When the tube begins to soften let it almost by its own weight bend around to the desired shape. Do not try to bend it suddenly or apply any considerable force. The bend should be very gradual and the bore of the tube remain unchanged in the bend. Always i8 Elementary Chemistry " fire-polish " the ends of the tube. Such a tube is often called an "L-tube," from its resemblance to the letter L. NOTE ii. Putting Apparatus Together. In putting together the parts of an apparatus, it is very necessary that they make tight joints. The corks should be well softened and the tubes inserted firmly. It is a good plan to lubricate glass tubing with glycerin, vaseline, or even water. The best way to test an apparatus for gas-tightness is either to compress the air in it by blowing or draw some out by suction. As usually some part of the apparatus is under water, the water will thereby be made to rise or fall in a tube, and if there is any leak, this water will change its level when the opening where the lips were applied is closed. To attempt to use leaky apparatus is to lose time and labor, and to insure the failure of the experiment. NOTE 12. Heat- ing Glass Vessels. In heating glass ves- sels, wire gauze (best of copper) is usually employed. Sand baths may also be used, and consist of a shallow iron dish containing a little sand. Serviceable ones may be made out of tin-pail or tin-can covers. Squares of asbestos paper are also used in many laboratories. The object of thus interposing a screen is to distribute the heat and render the glass less liable to crack. NOTE 13. Collecting Gases by Water Displacement. This method consists in filling wide-mouthed vessels brimming full of water, covering them tightly with a piece of paper, cardboard or glass, inverting them with the cover pressed against the mouth, placing them mouth downward in a dish filled with water (techni- cally named a pneumatic trough), and removing the cover. The pressure of the atmosphere keeps the water in the vessels, or receivers, as they are commonly called. Most pneumatic troughs are provided with a shelf less than an inch below the surface of the water (Fig. 17), on which the receivers are set. The gas which is evolved is made to pass up into the receiver by means of a delivery tube, and to displace the water. Only gases which are but slightly soluble in water can be col- lected by water displacement. Fig. 1 8 STOPCOCK FUNNEL GAS GENERATOR AND CYLINDER FOR COLLECTING THE GAS Experiments Fig. 19 HOME-MADE STOPCOCK FUNNEL, NO. I EXPERIMENT 13. Oxygen from Sodium Peroxid by Action of Water. Fit a dry flask (200 to 300^-) with a delivery tube and stopcock fun- nel 14 . Place about 20^- ( 7 cm - circle) of sodium peroxid in the flask and allow water to drop slowly upon it from the funnel. Collect five receivers full by water displacement 13 and pass to Ex- periment 14. NOTE 14. Gas Generators. Gas gener- ators are employed when a gas may be formed by the interaction of a solid and a liquid. Of these there are many styles, of which those provided with a stopcock funnel are the best, but stopcock funnels are expensive. A serviceable stopcock funnel may be made by the student as follows : Choose a piece of rubber tubing that will just slip into the stem of a funnel and cut off a piece about -2cm. long (Fig. 19). Cut a hole about i mm - in diameter near one end and, warming the rubber a little, rub cement (made by melting in a dish two parts of beeswax with one of rosin) around trie lower half so as to form a thin coating. Very cautiously (remember that funnels are made of thick glass and are very liable to break if heated rapidly or unevenly) warm the stem of the funnel where it commences to flare out and push the rubber tube into it. When the glass is cold the cement will hold the rubber in position very firmly. Put a little vaseline on a glass rod 15 that slips easily but snugly into the rubber tubs. To close the stopcock, push the rod down so that it may cover the lateral hole. To open it, raise the rod more or less so as to uncover more or less the hole. Such a stopcock cannot of course be used with liquids which have any action on rubber. Pick out a good cork fitting the neck of the flask (or use a rubber stopper), soften it, and perforate it with two holes, through one of which the stem of the funnel passes, and through the other one of the L-tubes, forming a delivery tube (Fig. 18). Another form of home-made stopcock funnel is the following : A funnel tube is cut off short and connected with a long piece of glass tubing by means of a bit of rubber tubing which can be closed with a pinchcock (Fig. 20). Still another form consists of an ordinary thistle or funnel tube, into the stem of which fits a bit of rubber tubing slipped over a glass rod. By pushing the rubber tube into the stem of the funnel and holding it there by the glass rod, the stopcock is closed. Fig. 20 HOME- MADE STOPCOCK FUNNEL, NO. 2 20 Elementary Chemistry EXPERIMENT 14. Properties of Oxygen. The first receiver of gas caught in the three preceding experi- ments contains the air that was in the generator and is to be rejected. Attach a piece of charcoal to a wire, heat it in a flame until it begins to glow, and then removing the glass plate from one of the receivers, insert it into the gas (Fig. 21), replacing the glass plate as far as possible. The wire may be thrust through a card so that the charcoal can be supported in the center of the receiver. Place a little sulfur in a combustion spoon 16 , set it on fire by directing a flame down upon it, and lower it into the second receiver. Put a little red phosphorus in a combustion spoon, light it thoroughly and thrust it into the last receiver. Keep the receiver covered so that the fumes cannot escape into the room. Attach a piece of picture cord wire to a stiff wire, fray out its end a little, heat it and dip it into sulfur so that some may cling to the wire. Set this on fire and at once introduce into a jar full of oxygen. To prevent the intensely hot oxid of iron which is formed from breaking the receiver, it should be a quarter full of water, or a layer of wet sand may first be put into the vessel. The object of tipping the frayed end of the cord with sulfur is to raise the temperature of the iron to the kindling point so that it too will burn. What do these experiments teach about combustion in air and in oxygen ? Fig. 21 BURNING A SUB- STANCE IN OXYGEN Experiments 21 a b c d Fig. 22 COMBUSTION SPOONS NOTE 15. Stirring Rods. To make a glass stirring rod, cut off a piece of solid glass rod of the desired length and round its ends by holding it in the flame of a Bunsen burner. Stirring rods may also be made out of tubing by heating its ends until the glass runs together and closes them up. NOTE 16. Combustion Spoons. Combustion or deflagrating spoons are little cups to hold combustible materials to be burned in a receiver of gas. Besides those procurable at the dealer in chemical apparatus (Fig. 22 a), ser- viceable ones may be improvised by (i) fastening an iron or aluminum thimble about half full of plaster of Paris (which has been mixed with water and allowed to set) to a wire handle (Fig. 22 6) ; (2) hollowing out a piece of chalk and fastening it to a wire handle (Fig. 22 c) ; and (3) twisting a wire around a bit of asbestos paper (Fig. 22 d\ OZONE EXPERIMENT 15. Preparation of Ozone. Put a few drops of ether in a small flask and cork it tightly. The ether will vaporize and a mixture of air and ether vapor will presently fill up the flask. Heat a stout glass rod to redness, and plunge it into the mixture of air and ether vapor. Smell of the product cautiously. Hold a piece of iodo-starch paper over the mouth of the flask and note any change of color. Does ether vapor alone produce any change of color ? CAUTION. Ether is very inflammable. Do not have any flames near when pouring it from a bottle. EXPERIMENT 16. (Quantitative^ To Find the Weight of One Liter of Oxygen. Put about 5^- (i cm - circle) of powdered manganese dioxid in a clean, dry evaporating dish and heat it as hot as possible for at least fifteen minutes so as to dry it thoroughly. In the meantime assemble an apparatus like that shown in 22 Elementary Chemistry Fig. 23. AB is a nine-inch test tube fitted with a two- hole rubber stopper. Through one hole passes a short bit of glass tubing over which a rubber hose provided with a Hofmann cock or pinchcock is slipped ; through the other passes an L-tube, the shorter branch of which fits into the two-hole stopper of an aspirating bottle 17 . The aspirating bottle, D, is filled full of water, and , an " acid bottle, " about half full of Fig. 23 APPARATUS FOR FINDING THE WEIGHT OF A LITER OF OXYGEN temperature of the room. Take about 20^- (5 cm - circle) of dry potassium chlorate and mix it on a piece of smooth paper with the manganese dioxid, which should still be warm. Transfer the mixture to the test tube, which has been previously thoroughly dried, wipe out any dust that may cling to the upper part of the tube, and insert just below the stopper a loose plug of glass wool or a coiled strip of previously ignited asbestos paper, its object being to prevent the oxygen from car- rying off any solid particles in passing from the tube. Experimen ts 23 Weigh the test tube and contents to a centigram as soon as possible after rilling. Holding the tube horizontally, tap it gently so as to make the mixture spread out and lie along the tube, and connect with the aspirating bottle, the tube being supported on a ring of a retort stand. Opening the clips at F and at H (use clip at //), force water into E by blowing at F, so as to drive all air from the long rubber tube. Then by suction draw water back into D until its level reaches nearly to the stopper, raise E so that the water in D and in E is at the same level, and close F tightly. Close H and very cautiously remove the rubber tube from E in such a manner that no water escapes from the tube. Empty the water out of E and drain it for a few seconds. Then place the end of the rubber tube in E and open the clip at H. A little water will flow out because the level in D is higher than that in , but there should not be a continual flow, as that would indicate that the apparatus was leaky. With a small flame gently heat the test tube, begin- ning near its mouth. If the mixture begins to froth at the point heated, heat another portion of it. The flame must not be held steadily at one place, but played to and fro through a distance of about 3 cm -. The glass should not be heated red-hot, as there is then danger of a hole being blown through it. When the "acid bottle" is about three-quarters full, discontinue the heating and let the apparatus stand until it cools to the temperature of the room. In the meanwhile read the barometer. Then lift E up or down (it can be lowered by bringing it down over the side of the table), hold it so that the level of the water remains the same for a minute or so in both bottles, always keeping the end of the rubber tube under water, and close the cock at H. Elementary Chemistry Disconnect the test tube and weigh it again. The difference between this weight and the one previously found is the weight of the oxygen evolved. Remove R without disturbing the water in the rubber tube, and measure the volume of water it con- tains by pouring it out into graduated vessels (Appen- dix BY or by weighing it on a platform balance and subsequently weighing the empty and drained bottle. Take the temperature of the water and reduce the volume of the oxygen to standard conditions. If this reduced volume be denoted by v and if the weight of the oxygen be denoted by zv, the weight of a liter may be computed by means of the pro- portion : v : iv :: 1,000 : x The accepted value for the weight of a liter of oxygen is 1.43^-. What possible sources of error can you point out in the determination of your value ? NOTE 17. Aspirators. A large bottle, Z>, is fitted with a two-hole stopper carry- ing two L-tubes (Fig. 24). A rubber tube a little longer than the bottle is slipped over the outlet tube and may be closed with a pinchcock, //. To aspirate a gas, fill the bottle with water, insert the stopper with its tubes, connect the inlet tube with the apparatus furnishing the gas, B ', remove the pinchcock, start the water flowing so that as it goes out the gas may be drawn into the bottle. Aspirating bottles may also be used to store gases ; when the bottle is full of a gas, slip a bit of rubber tubing over the inlet tube and close it with a pinchcock, and then close the outlet tube. The gas may be forced out by connecting the aspirator with a second one filled with water and placed at a higher level. The water may be made to siphon over from the second bottle into the first, thus expelling the gas. The gas may also be driven out at B by connecting the outlet tube with the water supply of the laboratory. FlR. 24 ARRANGEMENT OF TUBES IN AN ASPIRATING BOTTLE Experiments EXPERIMENT 17. (Quantitative^) To Find the Per- centage of Oxygen in Potassium Chlorate. Clean and dry a porcelain crucible and cover, place upon a pipestem triangle (Fig. 25), and heat gently at first so as not to break the cru- cible, and then as hot as possible for two or three minutes. When the crucible is cool, weigh it to a centi- gram (Appendix B}. Put about 1.5^. (2. circle) of dry pow- dered potassium chlo- rate in the crucible and weigh again. Place the covered crucible on the tri- angle and heat with a Fi 8- 25 HEATING IN A PORCELAIN CRUCIBLE flame about 5 cm - high, which just reaches to the bottom of the crucible. Lift the cover up from time to time with the forceps and regulate the flame so that the melted potassium chlorate is seen to give off its oxygen but slowly. If any should spatter up on the cover, remove the flame, place the cover bottom side upper- most on a clean piece of smooth paper, and with a pin loosen the layer of chlorate and return it to the cruci- ble, being very careful that none is lost. When the bubbling is seen to slacken, increase the size of the flame, and finally heat for ten minutes with a flame large enough to reach to the top of the crucible when its yellow spot is just below the bottom of the crucible. Let cool and weigh, 26 Elementary Chemistry Again heat very hot for about five minutes, and cool and weigh as before. If the weight does not change, pass to the calculations. If the weight is less, heat again, and continue in this way until two successive weights are the same. This operation is called heating to constant weight. The loss of weight is equal to that of the oxygen. The percentage of oxygen in the chlorate is calculated thus: Weight of potass, chlorate : weight of oxygen : : 100 : x The accepted value for the percentage of oxygen in potassium chlorate is 39.2. What is the percentage of error in your result ? Point out any sources of error. Fig. 26 GAS GENERATOR, PNEUMATIC TROUGH, AND RECEIVERS HYDROGEN EXPERIMENT 18. Hydrogen from Acids by Action of Zinc. Arrange a gas generator as shown in Fig. 26. A wide-mouthed bottle is fitted with a two-hole stopper (best of rubber), through which pass a funnel tube 18 and an L-tube. A piece of rubber tubing connects the L-tube with a second one, thus forming a delivery tube. Experiments 27 Cover the bottom of the bottle with granulated zinc, fit in the stopper, push the funnel tube down so that it nearly touches the bottom of the bottle, and run in through the funnel tube enough water to just cover, and thus seal its end. Pour dilute sulfuric or concentrated hydrochloric acid 19 through the funnel so as to cause a brisk evolution of gas, and after testing its purity 20 , collect four receivers full by water displacement and pass to Experiment 19. As an alternate apparatus a stopcock funnel gener- ator (Fig. 1 8) may be used. Zinc is placed in the bot- tle, covered with water, and strong hydrochloric acid dropped in just fast enough to make the gas come off briskly. NOTE 18. Funnel Tubes. Funnel tubes are tubes of glass with one end flared out to form a funnel, or they may be described as small funnels with long stems. The style shown in Fig. 26 is sometimes called a " thistle tube," from its fancied resemblance to the head of a thistle A funnel tube should always have its lower end dip below the liquid in a generator so as to seal it. NOTE 19. To Moderate Action of an Acid. If hydrochloric acid is used and so much is introduced into the generator that hydrogen is given off too rapidly, a little water poured through the funnel will dilute the acid and thus moderate its action. CAUTION. Hydrogen mixed with air is very explosive. NOTE 20. Testing Hydrogen. Never perform experiments with hydrogen until you have convinced yourself that the hydrogen is free from air in the following way : Fill a small test tube with the gas by water displacement. Place the thumb over the mouth of the test tube while it is still under water and, bringing it close to a flame, open it so that the gas may pass into the flame (Fig 27). If the gas ignites with an almost inaudible report, it is pure ; if with a loud report, or sharp whistle, it is mixed with air. Continue to gener- ate the gas until it is pure before collecting it. Fig. 27 DISCHARGING GAS FROM A TEST TUBE INTO A FLAME 28 Elementary CJieviistry EXPERIMENT 19. Properties of Hydrogen. Hold- ing a receiver full of hydrogen in an inverted position (Fig. 28), thrust a lighted splinter up into the gas and then very slowly remove it. Does hydrogen burn ? If so, what is the appearance of its flame ? Set a receiver full of hydrogen, with its mouth upward, on the table, and after waiting at least three minutes, insert a blaz- ing splinter. How do you account for the result ? What property of hydrogen is hereby shown? See if you can pour hydro- gen upward. How can you make sure that hydrogen is in the upper receiver? Pressing a glass plate or a piece of cardboard tightly against the mouth of a receiver full of hy- drogen, place it in- verted upon a receiver of the same size filled with air, and slip out the plate or card (Fig. 14). After at least five minutes remove the UDDCT rCCeiVCT and . keeping it inverted, insert a lighted splinter (Fig 28). Account for the result. What general property of gases is hereby illustrated ? EXPERIMENT 20. Transpiration of Hydrogen. Hold down over the delivery tube (a straight tube is substituted for the L-tube) of a gas generator, from which hydrogen is issuing rapidly, a dry glass tube, Fig. 28 - INTRODUCING A LIGHTED SPLINTER OF WOOD INTO A GAS LIGHTER THAN AIR Experiments 29 closed at one end with a plug of plaster of Paris, with the thumb pressed over the plug-. In a few minutes slowly lift the tube up, keeping it closed with the thumb all the while, until it is clear of the delivery tube ; then dip the open end under water in a beaker or tumbler and remove the thumb (Fig. 29). Let the tube stand for at least fifteen minutes, examining it from time to time. Explain what occurs. EXPERIMENT 21. Combustion of Hydrogen. Wrap several folds of a towel over and around your gas generator so that in case of an explosion the broken glass can be prevented from flying about. Test the purity of the hydrogen 20 , which should be escaping quite rapidly, and then attach a straight glass tube drawn out to a jet 21 to the rubber tube. Ignite the hydrogen and thrust the jet up into an inverted beaker. What col- lects in the beaker ? Pinch the rubber tubing so as to extinguish the flame, dry the inside of the beaker, and as before thrust the jet with unlighted hydrogen escaping from it into the inverted beaker. What occurs ? NOTE 21. Jet Tubes. To make a jet tube, select a piece of glass tubing about i2- long and ^mm. bore with a rather thick wall. Heat the middle in a Bunsen flame, twirling it so as to heat it uni- formly. When it begins to soften, slowly draw it out as shown in Fig. 30. Cut it off at the narrowest point, and fire-polish the wider ends of the two jet tubes thus made. Fig. 2Q APPARATUS FOR SHOWING TRANSPIRATION OF A GAS Fig. 30 STAGES IN MAKING A JET TUBE 3O Elementary Chemistry EXPERIMENT 22. Oxidation and Reduction. Scrape a few bits of copper foil or wire bright and clean and put them into the middle of a glass tube about 30 cm - long. Heat the tube gently just below the copper, sup- porting it on a ring stand with interposed wire gauze, and in a slanting position so that a draft of air may pass through it. Do not heat the glass to redness. The blackening of the copper is due to the formation of copper oxid ; the copper is oxidized. Fig- 31 PASSING A GAS OVER A SUBSTANCE HEATED IN A TUBE Let the tube cool and then slipping over one end of it a delivery tube, and connecting the other end with a hydrogen generator, pass hydrogen through it (Fig. 31). After the hydrogen has been found by test to be pure, heat the copper. What does the change of color go to show ? EXPERIMENT 23. Hydrogen from Water by Action of Sodium. With dry fingers and knife cut off a piece of sodium not more than 5 mm - in diameter 22 and scrape it bright and clean. Wrap the bit of sodium up snugly in a scrap of filter paper which has been moistened in kerosene 22 , and using tongs bring it under a large test tube filled with water and inverted in a pneumatic Experiments trough. Let go of the sodium so that it may rise into the tube. If not enough gas is generated to fill the test tube, use a second piece of sodium. Lift up the tube, keeping its mouth down, and bring it to a flame. How do you know it contains hy- drogen ? NOTE 22. Sodium Must be Kept Dry. Be sure that everything that is used in handling so- dium is dry. The object of dipping the paper in kerosene is to prevent a too rapid access of the water to the metal. Too much paper should not be used, else the water will be prevented from com- ing in contact with the sodium. EXPERIMENT 24. Hydrogen from Steam by Action of Magnesium. Draw out one end of an L-tube so as to form a jet 21 and thrust the other end through a Cork fitting a Small Fig. 32 HYDROGEN FROM STEAM BY THE flask (Fig. 32). Put a little (only a pinch, for if too much is used the heat of the reaction may be so great as to break the tube) powdered magnesium in the tube and shake it down so that it lies along the branch next to the jet. Put a little water in the flask, insert the cork, and heat the water to boiling so that a moderate current of steam passes Elementary Chemistry Fig. 33 HYDROGEN FROM STEAM BY THE ACTION OP IRON through the jet. Apply a flame to the issuing- steam and see if it can be ignited. The little flashes of light are due to the burning of tiny particles of magnesium, which are caught up and carried along by the steam. With a second Bunsen flame heat all the horizontal branch of the L-tube hot enough to prevent the conden- sation of moisture in it. Then heat steadily the portion of the magnesium farthest from the jet until a reaction begins, and at once remove the flame. Can the gas now issuing from the flame be set on fire ? Compare with Experiment 21. EXPERIMENT 25. Hydrogen from Steam by Action of Iron. Place enough small brads in a piece of gas- pipe (or, better, bicycle tubing) 40 cm - to 50^- long and about 2 cm. bore, to fill the middle of the pipe for a distance of about 20 cm - f and then fasten the pipe with wire across a wide ring of a stand (Fig. 33). Attach a Experiments 33 delivery tube to one end of the pipe and to the other an L-tube, with a long pieee of rubber tubing, making connections with a second L-tube inserted in a flask supported on a second ring above the pipe. Bend a thick piece of asbestos board into a gable-roof shape and place it over the pipe. Put a little water in the flask and arrange the ring supporting it so that it nearly touches the asbestos. Heat the middle of the gaspipe as hot as possible, using two burners. Place bits of wet filter paper over the ends of the pipe and keep them dripping wet all the time so as to prevent the charring of the corks. If the water in the flask boils too vigorously, raise the ring supporting it a little. Collect some of the gas given off and test it. EXPERIMENT 26. Hydrogen from Solutions of Caustic Alkalis by Action of Aluminum. Place a few bits of aluminum in a test tube and fill it about a fourth full with caustic soda or potash solution. If effer- vescence is not very brisk, heat a little. Close the tube with the thumb, and after a minute or so open it so as to discharge the gas into a flame (Fig. 27). Account for what occurs. EXPERIMENT 27. Hydrogen from Sodium Hydroxid by Heating with Iron Powder. Make an intimate mixture in a mor- tar of i g- (6 mm -) of sodium hydroxid and 20^- (4^- circle) of iron powder, and introduce it into a hard glass test tube provided with a cork and delivery tube (Fig. 34). Fig. 34 HEATING A SUBSTANCE IN A TEST TUBE AND COLLECTING THE GAS EVOLVED 34 Elementary Chemistry Fig. 35 A COMMON FORM OF WATER BATH Supporting" the tube on wire gauze and under a ring, heat the upper part of the mixture first so as not to cause too brisk an evolution of the gas, and collect it by water displacement. EXPERIMENT 28. Hydrogen from Calcium Hydroxid (Lime) by Ac- tion of Iron Powder or Zinc Dust. Make an intimate mixture of equal volumes (2 cm - circle) of dry calcium hydroxid and iron powder, put it into a hard glass test tube provided with a cork and delivery tube, and heat, using a test tube holder, collecting the hydrogen evolved over water. Zinc dust may be used instead of iron powder in Experi- ments 27 and 28. WATER EXPERIMENT 29. Dis- solved Matter in Differ- ent Waters. Slip a small rubber band over a test tube about a third of the way from its closed end, fill it up to the band with distilled water, pour the water thus measured into a clean evaporating dish (watch glass or saucer), and evaporate to dryness on a water bath 2 3 or sand bath (asbestos board) 12 . Note the nature and Fig. 36 AN IMPROVISED WATER BATH amount of any residue. Repeat these operations with hydrant water and other natural waters which may be available. Compare natures and amounts of residues. Experiments 35 NOTE 23. Water Baths. To avoid raising the temperature of a substance above that of boiling water, water baths are used. A common form (Fig. 35) consists of a copper vessel with a cover made of a series of rings. By removing one or more of these, a dish may be set down nearly to its rim on the bath. Water is kept gently boiling in the bath so that the dish may be surrounded by steam. Care must be taken to replace from time to time the water which boils away, else the temperature will be raised too high. A serviceable water bath may be improvised with a beaker (best with a lip) and stand (Fig. 36). EXPERIMENT 30. Distillation. Fit one end of a long straight tube to a retort or to an L-tube inserted through the neck of a flask. The other end passes into a test tube set in a dish of water. Fill the flask (Fig. 37) or the retort (Fig. 38) about a third full of water and add a piece of copper sulfate (3 >>.). Boil the water in the flask gently and collect a test tube full of the distillate. It is well to cover the part of the test tube which is not under water with a piece of filter paper which is kept wet so as to aid in the condensa- tion. What is the color of the distillate ? Can copper sulfate be totally separated from water by distillation ? Fig- 37 SIMPLE DISTILLING APPARA TUS, FLASK FORM Fill an evaporating dish about a fourth full of alco- hol and set fire to it. While the alcohol is burning, add Fig 38 _ water in small portions at a time with constant stirring until the flame goes out. Clean out the retort or flask, and empty the mixture of alcohol and water into it. Distill the mixture, collecting SIMPLE DISTILLING APPARA- TUS, RETORT FORM 36 Elementary Chemistry enough of the distillate to fill the test tube about a fourth full. Pour the distillate into the evaporating dish and try to set it afire. What does your result prove about the possibility of separating alcohol and water by distillation ? Which is the more volatile, water or alco- hol ? Which has the higher boiling point ? EXPERIMENT 31. Coagulation Filters. Put a pinch of clay in a test tube and fill with water. Shake the water and clay well together and filter (Fig. 10) a por- tion of the muddy water (a suspension of clay in water). Is the filtrate clear? Filter the filtrate a second time and see if it becomes clear. Can clay and water be separated by filtration ? Now add to the muddy water a few drops of alum solution, shake up thoroughly, and filter through a fresh filter. Is the filtrate clear? If not, add a little more alum and filter again. EXPERIMENT 32. Conditions Affecting Solution. (a) fineness of Division. Choose two crystals of po- tassium dichromate, alum or copper sulfate, both just small enough to slip into a test tube, and powder one finely in a mortar. Put the crystal and the powder in separate test tubes and fill both the tubes about half full of water. Close the tubes with the thumbs and shake vigorously. In which case does solution take place the more rapidly ? In which case is the surface of contact between the solid and the liquid the larger ? To save time in dissolving a solid, what preliminary operation ought it to be subjected to ? (b) Temperature. Put about 6 - (3 cm - circle) of powdered potassium dichromate in a test tube, and fill it about a third full of water. Shake the solid and liquid well together for some time. Does the solid all dissolve? Is there a limit to the solubility of a sub- stance at a given temperature ? Heat to boiling for a minute or so. Does the solid all dissolve now ? Cool Experiments 37 the tube and contents by letting cold water run over it. What happens ? What effect has temperature upon the solubility of a substance ? EXPERIMENT 33. (Quantitative^) To Determine the Solubility of Potassium Dichromate in Water. Fill a flask (200 to 300 c - c -) a fourth full of powdered potassium dichromate, and add sufficient water to fill the flask about three-fourths full. Cork the flask tightly and place it in a pneumatic trough filled with water at the temperature of the room. Put a thermometer in the trough and read its temperature at intervals of about two minutes, and each time shake well the solid and liquid in the flask. The temperature should not vary by more than a degree for at least fifteen minutes. Filter a portion of the solution thus saturated into a weighed evaporating dish so as to fill it about half full. Weigh the evaporating dish and solution and then evaporate to dryness on a water bath 23 . Be very careful not to lose any of the solid by spurting. Let the dish and con- tents cool and again weigh. Calculate the percentage composition of the solution. EXPERIMENT 34. (Quantitative.} To Determine the Solubility of Air in Water. Shake a large bottle filled about half full of water vigorously for several minutes so as to saturate it thoroughly with air. The water should be at the temperature of the room, and care should be taken not to warm it up in shaking by the heat of the hands. Fit a small flask (200 to 300 c - c -} with a stopper (best of rubber) and a delivery tube of narrow bore (not more than 2 mm -) of the form shown in Fig. 39. Set the flask on a ring of a stand with interposed wire gauze so that its delivery tube may come under a test tube placed in a beaker set on a second ring of the same stand. Fill both the beaker and the test tube with water, invert the filled test tube in the beaker, and pour out as much Elementary Chemistry water as possible from the beaker without the water in the test tube escaping. Take the temperature of the water in the bottle and fill the flask brimful. Then insert the stopper so that the delivery tube will be filled with water also. There must not be any bub- bles of air either in the flask or the delivery tube. Weigh the flask, delivery tube, and con- tents to decigrams, set the flask upon the wire gauze so that its deliv- ery tube engages un- der the test tube, and heat with a small flame, making the water boil vigorously until a cracking sound is heard, indicating that all the air has been expelled from the water. Remove the delivery tube from the water in the beaker and stop heating. Fill the beaker with water at the temperature of the room, lift the test tube up so that the level of the water inside and outside is the same, and mark it with a small level rubber band slipped over the test tube. Remove the test tube and determine the volume of the air driven out of the water either with a burette (Appendix B) or by weighing the water which fills the tube up to the rubber band. Dry flask and delivery tube and weigh. Record results thus: Fig. 39 APPARATUS FOR DETERMINING THE SOLUBILITY OF AIR IN WATER Experiments 39 Weight of water filling flask and delivery tube = A <?" Volume of air expelled at and mm. of mercury B c.c. Volume of air reduced to o and 760 mm. of mercury = C c.c. No. of c.c. of air at o and 760 mm - dissolved by A c.c. of water. No. of c.c. of air dissolved by 1,000 c.c. of \vaterat = DC.C. Accepted value for solubility of air in water (Appendix C). EXPERIMENT 35. Heat Effects of Solution. Have ready at hand 5.0^- of the solids named in the table below in the form of a fine, dry powder. Measure. (Appendix B) io.o c - c - of water at the temperature of the room into a test tube, insert a thermometer, stir, and read the temperature. Add all at once the first of the powders, stir well with the thermometer, holding the test tube with a holder so as not to warm the solu- tion with the hand, and record the highest temperature attained. Repeat these operations with the other sol- ids, cleaning out the test tube after each trial. Add 5.0^- of alcohol to ic-.o^- of water and find the temperature of the well-stirred mixture. Also add 5.0^- of strong sulfuric acid to io.o c - c - of water and take the maximum temperature. Record results as follows : HEAT EFFECTS OF SOLUTION SUBSTANCES Solvent Temperature Change of Tem- perature Name Amt. Name Amt. Initial Highest or Lowest Maxi- mum Kind Ammonium chlorid.. Calcium chlorid Ammonium nitrate . Potassium nitrate Copper sulfate (dehy- drated) _ . Sugar Potassium carbonate. Sodium carbonate Alcohol Sulfuric acid 40 Elementary Chemistry EXPERIMENT 36. Supersaturation. Fill a test tube about a fourth full of sodium acetate (or sodium sul- fate) crystals and add barely enough water to cover them. Heat cautiously to boiling until a clear solution results and boil vigorously for a minute or so. Set the tube aside in a slanting position so that any dust may fall on the sides of the tube and not reach the solution. After the solution is cool drop into it a very small frag- ment of a sodium acetate (sodium sulfate) crystal and shake the tube. What happens ? EXPERIMENT 37. Water of Crystallization. Place in separate clean and dry small test tubes a few small crystals of potassium nitrate, copper sulfate, and cobalt chlorid. Place the test tubes on the wire gauze and place under them a frame made of iron wire fashioned so that while their closed ends converge to a common center, their mouths just project beyond the gauze and are lower than their closed ends. Adjust the flame of a Bunsen burner so that it keeps red hot a small circle just below the closed ends of the test tubes, being care- ful not to let the flame strike through the gauze. Note carefully the appearance of moisture in the mouths of the tubes. In which case is it the most abundant ? What changes do the substances undergo ? Which of them contain water of crystallization and which me- chanically enclosed water ? When the water of crystal- lization is expelled from a substance, the substance is said to be dehydrated. Using a dilute solution of cobalt chlorid instead of ink, write on paper with a clean, new pen. Is the writ- ing almost invisible ? Waft the paper over a flame so as to \varm it. Do the characters now show and in what color? Breathe upon the writing. What happens? How do you explain the action of this kind of sympa- thetic ink ? Experiments 41 EXPERIMENT 38. (Quantitative.} To Find the Percentage of Water of Crystallization in Gypsum. Clean and weigh to centigrams a porcelain crucible and cover. Place in it enough gypsum in powder or coarse fragments to fill it about a fourth full. Weigh, place it upon a pipestem triangle (Fig. 25), and heat with a small flame for about ten minutes. Let the crucible cool and weigh it. Heat the crucible once more for about five minutes, let cool and weigh. If it has lost in weight, heat it still again, and so on to constant weight. Calculate the percentage of water of crystalli- zation contained in gypsum. Instead of a crucible, test tubes or clay pipes may be used. A test tube is weighed, filled about a sixth full of gypsum, again weighed and heated (held in a test tube holder in a slanting position) to constant weight. EXPERIMENT 39. Deliquescence. Put a little solid potassium hydroxid ($ mm -) in an evaporating dish or watch glass, set it aside in a safe place, and examine it after a few hours. Review Experiment 7. How do you account for the change ? EXPERIMENT 40. Efflorescence. Choose a clear crystal of sodium sulfate, place it upon a watch glass or evaporating dish, set it aside in a safe place, and examine it from time to time. (It is advisable to weigh the dish and crystal so as to keep track of any change in weight.) What change does the crystal undergo ? EXPERIMENT 41. Test for Water. Expel the water of crystallization from a little copper sulfate by heating it in an evaporating dish or a tin-box cover. Place a little of the dehydrated substance on a watch glass and add a drop of strong alcohol. Does the substance turn blue ? Try carbon bisulfid, ether, kerosene, or any other liquids not containing water which are available. Finally try water. How is the result a test for water? 42 Elementary Chemistry EXPERIMENT 42. (Quantitative.) To Ascertain the Volumetric Composition of Water. Choose two long and narrow test tubes as nearly of the same size as possible, and slip over them narrow rubber bands or tie around them bits of cotton string to serve as markers. Place one marker about one- third of the length of one of the tubes from its open end, and the other marker on the second test tube about one-fourth of the length of the tube from the open end. Fill both tubes with water and, holding them in a pneumatic trough, let in air until the level of the water inside and outside is at the markers. Have a hydrogen generator conveniently at hand from which hydrogen is issuing at the rate of about two bubbles a second. Thrust one of the test tubes over the delivery tube, and the instant it is filled with hydrogen remove it and set it aside in the pneumatic trough with its end under water. Do likewise with the other tube. These tubes contain definite, measurable volumes of air and hydrogen. Now a mixture of air and hydrogen which contains the two gases in just the right proportions totally to combine and form water, explodes, when ignited, with a sharp, whistling sound ; otherwise, if the proportions are not just right, the sound of the explosion is fuller and louder. Close the two tubes with the thumbs under water and, bringing them on either side of a flame (Fig. 27), let their contents pass into the flame in rapid succession and note the character of the sounds. There will probably be an easily detectable difference. Now push the marker of the test tube which con- tained the greater volume of hydrogen down a little (a couple of millimeters), and the other marker up about the same distance, thus making the volumes more nearly equal. Fill them with air and with hydro- gen as before, and ignite their contents. Continue in Experiments 43 this way until you can detect but a slight difference, if any, in the sound of the explosions, which should be more like a whistle than a report. Empty out the tubes and drain them. Ascertain the volume up to the marker, either by running- in water from a burette or by weighing. (Appendix B.) Fill the tubes brimming full with measured amounts of water, thus finding the volumes of the mixtures of air and hydrogen, whence by subtraction the volume of the hydrogen may be ascertained. As air contains very nearly one-fifth of oxygen by volume, one-fifth of the volume up to the marker will be the oxygen which has combined with the hydrogen. Enter results thus : First Second test tube. test tube. Volume of air = A' c.c. ~ A c.c. Volume of oxygen ( of A) = B' c.c. B c.c. Volume of hydrogen = C' c.c. C c.c. (B-j-B')^- of oxygen combine with (C -f- C') c - c - of hydrogen, whence i c - c - of oxygen combines with (C + C')/( B + B')^- of hydrogen. The accepted ratio is i : 2. What are the sources of error? HYDROGEN DIOXID EXPERIMENT 43. Hydrogen Dioxid by Action of Sodium Peroxid on Water. Add a dozen or so drops of strong sulfuric acid to about 50^- of cold water in a beaker and stir well. Cool the solution as much as pos- sible (if ice is available, put a few pieces in the solution) and add in small portions with constant stirring about 2#- ( i cm. circle) of sodium peroxid. Pass to Experiment 45. EXPERIMENT 44. Hydrogen Dioxid by Action of Sulfuric Acid on Barium Dioxid. Put about io#- (4 cm. circle) of barium dioxid in a beaker, and moisten it with a few drops of water. Add about 30 c - c - of cold, 44 Elementary Chemistry dilute (about 10 per cent) sulfuric acid, stir well for sev- eral minutes, let the solid settle, and decant the solution of hydrogen dioxid from the insoluble barium sulfate. If the filtrate is not clear, pour it upon the same filter paper and continue in this way until it is perfectly clear. Pass to Experiment 45. EXPERIMENT 45. Properties of Hydrogen Dioxid. Action of Potassium Permanganate Solution. Fill a test tube about a fourth full of the hydrogen dioxid solution prepared in Experiments 43 or 44, add a drop or so of potassium permanganate solution and shake well. The gas evolved is oxygen. Continue adding the perman- ganate until the color is not discharged. Action on lodo-Starcli Paper. Moisten iodo-starch paper with a solution of hydrogen dioxid. What effect? Where else has this paper been used ? W'hat two sub- stances is it a test for ? How may they be distinguished from each other ? Action on Potassium DicJiromate Solution. Fill a large test tube nearly full of water and add just enough potassium dichromate solution to tinge it a very light yellow. Now add a couple of drops of sulfuric acid, and then a dozen or so drops of hydrogen peroxid solu- tion. Shake well and note what happens. Pour some out into a dish and let it stand for a few minutes. Fill a small test tube about a sixth full of hydrogen dioxid solution and add enough ether to form a layer about half a centimeter thick. CAUTION. Do not have any flames near when using ether. On shaking, do the two liquids mix ? Add one drop of potassium dichromate solution and shake gently. Result ? If you are in doubt about the result add another drop, but do not use too much potassium dichromate solution. Experimen ts 45 EXPERIMENT 46. (Quantitative.} To Verify the Law of Definite Proportions by Weight. Weigh out exactly 2.00 of sodium carbonate (washing soda) in a porcelain evaporating dish. Add concentrated hydrochloric acid, a few drops at a time, being careful to avoid any loss from the effervescence. When the sodium carbonate is wholly dissolved, evaporate to dry- ness (Fig. 9) and constant weight. The residue is com- mon salt. Repeat, using exactly 4.00 *" of sodium carbonate. Calculate the ratio of the sodium carbonate to the salt in both cases. How do they compare ? How is this a proof of the law in question ? EXPERIMENT 47. ( Quantitative} To Verify the Law of Definite Proportions by Volume, (a) Put about 25 c.c. of concentrated hydrochloric acid in a beaker and mix with it about an equal volume of water. Fill a burette (Appendix B) with this mixture. Also fill a second burette with concentrated ammonium hydroxid. (b) Run 5.0 c - c - of the acid into a weighed evap- orating dish and add a couple of drops of litmus solution. After reading the burette containing the ammonium hydroxid, run the ammonium hydroxid into the acid slowly with constant stirring until the red color just changes to blue. The acid and ammonium hydroxid combine to form a solid ammonium chlorid. Evaporate to constant weight on a water bath. (c) Put the same volume of acid into a second weighed evaporating dish and add twice as much ammo- nium hydroxid as before. Evaporate to constant weight on a water bath. (d) Run i o.o c - c - of the acid into a third weighed dish and cautiously add just enough ammonium hydroxid to change the color. Evaporate to constant weight. 46 Elementary Chemistry (e) Put a few drops of hydrochloric acid in a dish and evaporate to dryness. Is there any residue ? Does ammonium hydroxid leave a residue when evaporated ? Try it with a few drops. (f) Compare the weights of ammo- nium chlorid obtained in (/;), (c), (d). How do your results verify the law under discus- sion ? EXPERIMENT 48. (Quantitative.) To Verify the Law of Multiple Propor- tions. Arrange an apparatus as shown in Fig. 40. The cylinder should be of at least 500 c - c - capac- ity. Weigh out exactly 2.00^- and also 4.00 & of baking soda (Appendix B). Put the larger amount in an evap- orating dish and heat as hot as possible for at least ten minutes. While the heating is going on, put the smaller portion into the generator and pour IQC-C. O f hydrochloric acid into the stopcock funnel. Fill the cylinder with water and invert it in the pneumatic trough. Run the acid into the generator and collect the carbonic acid gas given off. Be careful not to let any of the gas escape through the stopcock. When no more gas is evolved, remove and clean the generator thoroughly. Mark the level of the water inside the cylinder with a rubber band. Now put the portion which has been heated into the generator ; fill the cylinder afresh with water, and collect the gas given off when 10 c - c - of hydrochloric acid are run in upon the soda. Fig. 40 STOPCOCK FUNNEL GAS GENERATOR AND CYLINDER USED IN ILLUSTRATING THE LAW OF MULTIPLE PROPORTIONS Experiments 47 Are the volumes of gas in the two cases approxi- mately the same? Has the effect of the heating been to expel half of the carbonic acid gas contained in the baking soda? By heating, the baking soda has been converted into washing soda. How much greater a volume of carbonic acid does baking soda contain than does washing soda? How do your results verify the law in question ? NITROGEN AND ITS HYDROGEN COMPOUNDS EXPERIMENT 49. Separation of Nitrogen from the Air. Bend the wire of a combustion spoon as show r n in Fig. 41, and fill the cup with red phosphorus. Ignite the phos- phorus by direct- ing a Bunsen flame down upon it, and, resting the bend of the wire on the bottom of the pneumatic trough, press a large, wide- mouthed bottle over it. Note carefully how the phos- phorus burns. What makes it finally go out? What becomes of the white smoke at first formed ? What makes the water rise in the receiver? Let the apparatus stand until the fumes have completely dis- appeared. Then estimate the ratio of the volume of Fig. 41 APPARATUS FOR REMOVING THE OXYGEN FROM A CONFINED PORTION OF AIR 48 Elementary Chemistry the air taken to the volume of the gas left. Close the receiver with a glass plate and set it upright upon the table. Move the plate just far enough to one side to permit the entrance of a blazing splinter of wood. Does it continue to burn ? Is nitrogen combustible ? Is it a supporter of combustion ? EXPERIMENT 50. Nitrogen by the Decomposition of Ammonium Nitrite. 24 Mix in a mortar about 10^- (6 cm - circle) of ammonium chlorid with about i$ff- of sodium nitrite and place the mixture in a flask provided with a perforated stopper and delivery tube (Fig. 16). Just cover the mixture with water and heat gently with interposed wire gauze until the reaction begins ; then remove the flame. Collect two receivers full by water displacement. If the liquid effervesces too much, cool it by pouring water over the flask. Reject the first bottle full, as it contains the air which was in the apparatus. Remove the second receiver after closing it with a glass slip and, holding it upside down (Why ?), thrust a lighted splinter up into the gas. Is nitrogen a supporter of combustion ? Does it burn ? NOTE 24. Ammonium Nitrite Does Not Keep Well. Hence it is made in this experiment by the reaction between ammonium chlorid and sodium nitrite. The heat caused by the reaction is usually sufficient to decompose the ammonium nitrite into water and nitrogen as soon as it is formed. EXPERIMENT 51. Nitrogen from Potassium Ni- trate by Action of Iron Powder. Mix well io^- ($cm. circle) of iron powder with 0.5 & (2 cm - circle) of pow- dered potassium nitrate, put the mixture in a hard glass test tube, fitted with a cork and delivery tube (Fig. 34), and apply heat. Be careful to heat very gradually, as the reaction may become rather violent. Collect sam- ples of the gas by water displacement, and test them with a blazing splinter. Experiments 49 EXPERIMENT 52. Ammonia from Ammonium Salts by Action of Caustic Alkalis or Lime. Cover a pinch of ammonium chlorid or nitrate in a test tube with po- tassium or sodium hydroxid (caustic potash or soda) solution. Heat gently to boiling and cautiously observe odor by wafting the air above the mouth of the test tube against the nostrils. Put a strip of moistened pink litmus paper 25 across the mouth of the test tube and note any change of color. Put a little slaked lime 2 6 in the palm of one hand and a little ammonium chlorid or nitrate in the other. Smell of each substance. Then rub the substances together between the palms and smell again. Also touch the mixture with a strip of moist pink litmus paper 25 . NOTE 25. Pink Litmus Paper. To make litmus paper of a pink color, put a few drops of dilute hydrochloric acid in a watch glass or on a piece of glass, and draw the strip of paper through it. Wash out the excess of the acid by holding the paper in a stream of water from the hydrant. The blue color may be restored by using ammonium hydroxid instead of hydrochloric acid. As litmus paper is usually sold with its color intermediate between Eink and blue, it is a good practice to treat it as above so as to ave it of a decided blue or pink color before making a test. NOTE 26. Use Freshly Slaked Lime. The lime must be freshly slaked. "Air-slaked " lime generally will not do. EXPERIMENT 53. Ammonia from the Destructive Distillation of Some Animal Substances. Heat some such substance as gelatin, glue, hair, or feathers in a test tube with a moistened strip of pink litmus paper held across its mouth. What products, solid, liquid, and gaseous, are formed ? EXPERIMENT 54. Preparation and Properties of Ammonia. Arrange an apparatus as shown in Fig. 42. Put about 25 # (ycm. circle) ammonium chlorid and about three times its bulk of slaked lime 26 in the flask, and add just enough water to make a pasty mass ; or, fill the flask about a third full of strong ammonia elementary Chemistry Fig. 42 APPARATUS FOR PREPARING AMMONIA water (ammonium hydroxid). The rim of the funnel should dip just below the surface of the water in the dish. Heat very gently, and as soon as the gas evolved is nearly all absorbed by the water, substitute for the funnel a straight glass tube. Insert this delivery tube into a narrow-mouthed bottle and collect the bottle full of the gas by upward displacement 27 . Keeping the receiver always upside down (Why?), cork it tightly (or cover it with a greased glass plate) and set it aside in an inverted position. Collect in like man- ner a second bottle full of the gas. Dip a glass rod into strong hydrochloric acid and bring the adherent drop just above the jet of gas. What occurs ? Replace the fun- nel and continue to absorb the gas as long as it can be made to come off. The solution is ammonium hydroxid. Hold the neck of the first receiver under water and remove the cork. Does it seem to stick in the neck ? If so, why ? What makes the water rush up into the bottle ? Test the water in the bottle with pink litmus Experiments 5 1 paper 25 . Hold the second receiver upside down, re- move the cork and insert a lighted splinter of wood. Does ammonia support combustion ? Does it burn ? To a little of the ammonium hydroxid add a few drops of Nessler's reagent. Also test a little with solu- tions of iron chlorid, ferrous sulfate, aluminum chlorid or sulfate, and copper sulfate (at first very little, and then an excess). Put a little ammonium hydroxid in a small test tube and boil for a few seconds so as to fill the tube with ammonia. Then rapidly invert it in a beaker filled with very dilute copper sulfate solution. What happens, especially in change of color ? NOTE 27. Collecting a Gas by Upward Displacement. When a gas is soluble in water it cannot of course be collected by water displacement. If the gas is lighter than air, it can be collected by delivering it into an inverted receiver ; the delivery tube should be thrust as high up as possible, so that the lighter gas may push the air down and out of the receiver. EXPERIMENT 55. Ammonia by the Interaction of Potassium Nitrate, Potassium Hydroxid, and Iron Powder. Mix together 0.5^- (2 cm - circle) of potassium nitrate, 0.3^- (6 mm - circle) of potassium hydroxid, and 25^- (5 cm. circle) of iron powder, put the mixture in a hard glass test tube and heat gently. How can you prove that ammonia is given off ? What is the gaseous product of heating a mixture of potassium nitrate and iron pow- der (Experiment 51)? What of heating a mixture of potassium hydroxid and aluminum powder (Experiment 26) ? Zinc or aluminum powder would also answer. CARBON EXPERIMENT 56. Formation of Charcoal. Place in a small Hessian crucible or tin- box cover a thin layer of sand and place upon it a small piece of soft wood and of hard wood, a fragment of bone, and a lump of starch. Cover them with a thick layer of sand and Elementary Chemistry heat very hot for at least twenty minutes. Pour off the sand and compare the products. What conclusions can you draw as to the distribution of carbon ? What was the purpose of imbedding the objects in sand ? EXPERIMENT 57. Graphite from Pig Iron. Put about 3^- (2 cm - circle) of borings of foundry pig iron in a beaker and add ioo c - c - of dilute nitric acid (made by mixing io c - c - of the concentrated acid with go c - c - of water). Boil gently (Fig. 43), replacing from time to time the water which has boiled away, until the residue does not seem gritty when rubbed with a glass rod. Fil- ter and wash the resi- due and let it dry. Compare its proper- ties with those of sam- ples of graphite that you can obtain from different sources. EXPERIMENT 58. Preparation of Lampblack. Put a lump (2 mm,} of rosin in a spoon or tin-box cover and set fire to it. Hold the rounded end of a test tube filled with cold water in the flame. Examine the deposit on the tube. Why was the tube filled with cold water? EXPERIMENT 59. Density and Porosity of Char- coal. Put a piece of charcoal in a test tube half full of water. Does the charcoal seem lighter or heavier than water ? Boil the water for several minutes. What Fig. 43 BOILING A LIQUID IN A BEAKER Experiments 5 3 is observed on the surface of the charcoal ? Let the water cool with the charcoal in it, and look at it from time to time. What is your final conclusion as to the density of charcoal ? Do not draw this conclusion until the charcoal has been in the water for some time. Account for its behavior before and after boiling. With the aid of tongs hold a piece of charcoal in a Bunsen flame until it is red hot, and then drop it into water. Wait until it sinks. Explain its sinking. EXPERIMENT 60. Adsorption of Gases by Char- coal. Fill a large test tube half full of w r ater and add to it, drop by drop, ammonium hydroxid, so as to give it a faintly perceptible smell. You should just be able to smell the ammonia when, after shaking up the liquid, the mouth of the test tube is put under the nostrils. Heat some finely powdered charcoal in an evaporating dish nearly to redness, let it cool, and pour it into the weak ammonia water. Shake well for a minute or so, and then apply the tube to the nostrils. Has the smell of ammonia been diminished ? What was the purpose of heating the charcoal beforehand ? EXPERIMENT 61. Reduction by Charcoal. Put a pinch of finely powdered charcoal in a small test tube, a pinch of powdered copper oxid in a second test tube, and a few bits of copper wire or granulated copper in a third tube. Fill each tube about a fifth full of dilute nitric acid and shake well. Note any action that may take place, such as effervescence, colored fumes or liquid. Place the test tubes side by side in a beaker about half full of water, and heat the water until it is so hot that you can hardly bear your hand in it. Note now any changes or reactions in the test tubes. Are the differences in the behavior of the three solids when placed in nitric acid sufficient to characterize them ? In other words, is this "nitric acid test" decisive? 54 Elementary Chemistry Mix well in a mortar 4^- ($ cm ' circle) of copper oxid with 2ff- (4 cm - circle) of powdered charcoal. Place the mixture in a test tube and heat as hot as possible with- out melting the glass for at least five minutes. Does the color of the mixture change ? If so, what substance may it indicate the presence of ? Put a pinch of the product in a small test tube and add nitric acid as above. Is there any evidence that copper has been formed and is present? What role does the charcoal play? EXPERIMENT 62. Decolorizing Action of Bone- black. Into a test tube nearly full of water put enough molasses or litmus solution to tinge the water slightly. Fit a funnel with a filter paper and nearly fill it with boneblack. Pour the mixture prepared upon the bone- black and catch the filtrate in a second test tube. If the filtrate is not perfectly colorless, pour it upon the boneblack again, and continue this until all the color is removed from the mixture. EXPERIMENT 63. Combustibility of Different Forms of Carbon. Place a wire gauze on a ring of a stand at such a height above a Bunsen flame that a circle about 3 cm - in diameter is made red hot. Place in this circle pieces "($ mm -) of graphite (from a "lead pen- cil "), of charcoal, of gas carbon, of soft and of hard coal, and heat until the charcoal changes into ash ; be care- ful to have all the substances equally heated. Describe fully the changes which each substance undergoes. THE COMPOUNDS OF CARBON WITH OXYGEN EXPERIMENT 64. Carbon Dioxid a Product of Com- bustion. Drop a piece of burning paper into a dry, wide- mouthed bottle and cover it with a glass slip. When the paper ceases to burn, pour in some lime water and shake the contents of the bottle vigorously. What happens to the lime water ? Experiments 55 EXPERIMENT 65. Carbon Dioxid Given off in Res- piration. Fill a large test tube a third full of lime water, and by means of a glass tube make the breath bubble through the solution a dozen or so times. What occurs ? EXPERIMENT 66. Carbon Dioxid Produced by Fermentation. Dissolve a handful of brown sugar or an equal bulk of molasses in about a liter of water con- tained in a bottle or flask provided with a delivery tube. Add a little yeast and set the apparatus in a warm place (30 to 40). Collect the gas which soon begins to form in test tubes and test it with lime water. Fig. 44 GENERATING A GAS AND COLLECTING IT BY DOWNWARD DISPLACEMENT EXPERIMENT 67. Carbon Dioxid from a Carbonate by Action of an Acid. Place several lumps of marble (calcium carbonate) in a gas generator and cover them with water. Connect with a wash bottle a fourth full of water (Fig. 44). Pour some strong hydrochloric acid down the funnel so as to cause a brisk evolution of gas. Collect the gas by placing the delivery tube at the 56 Elementary C lie mist ry bottom of a receiver. Carbon dioxid is heavier than air and collects at the bottom of the receiver. This method of collecting a gas is known as that of "down- ward displacement." Collect five receivers full for use in Experiment 68, and close them with glass slips. EXPERIMENT 68. Properties of Carbon Dioxid. Lower a lighted splinter of wood into a receiver of car- bon dioxid. What happens ? Pour a little lime water into another receiver of the gas and shake it up. What happens ? Pour a receiver full of carbon dioxid as you would a receiver of water into a second receiver con- taining only air. Lower a lighted splinter into the second receiver. What evidence is there that the gas has been poured from the one receiver into the other ? Empty just as if the carbon dioxid were water a receiver full of carbon dioxid upon a candle flame. What hap- pens ? Holding one end of a bit of magnesium ribbon by means of tongs, ignite the other end thoroughly, and plunge it into a large receiver full of the gas. What are the black and the white particles formed ? EXPERIMENT 69. Action of Carbon Dioxid on Litmus. Add a few drops of litmus solution to water in a test tube and pass carbon dioxid into it for a few minutes. What change of color ? EXPERIMENT 70. Carbon Dioxid Absorbed by Sodium or Potassium Hydroxid Solutions. Pass carbon dioxid into a solution of caustic potash or soda (potassium or sodium hydroxid solution). When the gas ceases to be absorbed, pour a little of the solution into a test tube and add dilute hydrochloric acid. What does the effervescence that ensues go to show ? Pour the rest of the solution into a shallow dish and let it stand until crystals appear. Place some of these crys- tals in a test tube and add hydrochloric acid. What evi- dence is there that the crystalline mass is a carbonate? Experiments 57 EXPERIMENT 71. Carbon Dioxid in Solution Dis- solves Calcium Carbonate. Mix lime water with an equal volume of water in a test tube and pass carbon dioxid, purified by passing it through water in a wash bottle (Fig. 44), through it for some time. Does the white precipitate of calcium carbonate finally dissolve.? Boil some of this clear solution so as to expel the car- bon dioxid from solution. What happens ? EXPERIMENT 72. Carbon Monoxid by Action of Sulfuric Acid on Sodium Formate. Fit a test tube with a perforated cork through which passes a short, straight piece of glass tubing ending in a jet (Fig. 45). Put enough sodium formate in the tube to fill it to the depth of about a centimeter, and cover it to a depth of about 4 cm - with strong sulfuric acid. Hold- ing the tube with a test tube holder, warm it cautiously so that the contents may not froth over, and light the gas given off. What is the appear- ance of the flame just as soon as the gas is lighted and be- fore the glass tip has been Fig. 45- PREPARING CARBON MON- heated red hot? Be very careful not to let the poisonous gas escape into the room, repeatedly applying a light to the jet tube so as to burn the gas as soon as formed. P^XPERIMENT 73. Carbon Monoxid by the Action of Sulfuric Acid on Potassium Ferrocyanid. Put about io-- (5 cm. circle) of potassium ferrocyanid in a flask (200 to 300 c-c-) provided with a delivery tube ending in a jet, Elementary Chemistry and add about 50^- of strong sulfuric acid. Heat gently (Fig. 46) and ignite the escaping gas ; note the appearance of the flame and any other phenomena that you may observe. EXPERIMENT 74. Oxids of Carbon from Oxalic Acid. Into a flask (200 to 300 c - c -) fitted with a delivery tube put about 5^- (4- circle) of solid oxalic acid and add about 40^- of strong sulfuric acid. Heat cautiously and after the air has all been Driven out of the apparatus, collect by water displacement a long, narrow test tube full of the gas. Close the tube with the thumb un- der water and transfer it to a beaker nearly full of a very dilute solution of caustic soda or potash. Let it stand until the liquid ceases to rise in the tube. What is the decrease in volume due to ? What is the ratio of the volume of the two oxids of carbon obtained from oxalic acid ? EXPERIMENT 75. (Quantitative.) To Find the Weight of a Liter of Carbon Dioxid. Fit a flask (300 to 400 c - c -) with a one-hole rubber stopper through which passes a glass tube a little longer than the flask, over one end of which is slipped a bit of rubber tubing (Fig. 47). Fill the flask brimming full of cold water, and insert the stopper and tube; be careful to exclude all air bubbles and to have the water reach to the end of the rubber tip. Close the rubber tube as near to the glass as possible with a pinchcock, and mark with a pencil a line around the stopper even with the rim of Fig. 46 PREPARING CARBON MON- OXID FROM POTASSIUM FERROCY- ANID Experiments 59 the flask's neck. Weigh to decigrams the flask thus filled with water ; this weight in grams is equal to the volume in cubic centimeters. Empty out the water and dry the apparatus thor- oughly. Multiply the volume by 0.001293 (the weight of i c - c - of air at standard conditions) to get the weight of air filling the flask at standard conditions. Open the pinchcock and connect the rubber tubing with a cur- rent of dry carbon dioxid. Loosen the stopper so that the carbon dioxid delivered at the bottom of the flask can drive out the air. After about five minutes insert the stopper to the same extent as before, i. c., to the pencil line, close the pinchcock, and disconnect from the carbon dioxid generator. Open the pinchcock for an instant so as to let the ex- cess of carbon dioxid escape, and weigh the apparatus to centigrams. Read the ther- mometer and the barometer. Repeat the operation of filling the flask with carbon dioxid so as to make sure that all the air has been expelled ; this will be shown by no in- crease in weight in the second weighing. As soon as a con- stant weight has been attained, again read the thermometer and barometer, using the last readings for the calculations. The difference of the weights of the flask full of air and filled with carbon dioxid, plus the calculated weight of the air, gives the weight of the carbon dioxid. Reduce this volume to o and j6o mm -, and then compute the weight of a liter of carbon dioxid. Fig. 47 APPARATUS FOR FINDING THE WEIGHT OF A LITER OF CARBON DIOXID 6o Elementary Chemistry SOME NITROGEN AND HYDROGEN COMPOUNDS OF CARBON EXPERIMENT 76. Methane from Sodium Acetate by Action of Soda-lime. Pulverize about 10^- of fused and dry sodium acetate and mix it thoroughly in a mortar with an equal weight of fused and dry soda-lime. Heat the mixture in a flask ( 100 to 2oo c - c -) provided with a one-hole cork, de- livery tube and a safety bottle 28 (Fig. 48), and col- lect a couple of receivers full by water displace- ment. Ascertain whether the gas is combustible or a supporter of com- bustion. Pour a little lime water into one of the receivers just after the methane has been ignited. The result proves what element to be present in methane ? How could you prove the presence of hydrogen in it ? EXPERIMENT 77. Ethylene from Alcohol by Ac- tion of Sulfuric Acid. Pour 10^- of water into a flask (200 to 3oo c -< ; -), add slowly with constant stirring 30 c - c - of strong sulfuric acid, and cool the flask by hold- ing it under cold water. Then add io c - c - of alcohol. Fit a cork and delivery tube to the flask, interpose a safety bottle 28 (Fig. 48), heat gently, and collect a couple of receivers full of the gas by water displacement. Note its odor. How does it burn ? Compare its flame with those of the other combustible gases thus far studied. Fig. 48 APPARATUS FOR GENERATING A GAS TO COLLECTED BY WATER DISPLACEMENT Experiments 61 NOTE 28. Safety Bottle. The object of the safety bottle is to prevent any water which may be drawn back through the delivery tube from entering the hot flask and probably breaking it. The entrance and exit tubes of a safety bottle should not project much below the lower surface of the cork. EXPERIMENT 78. Acetylene by Action of Water on Calcium Carbid. Place a few small lumps of cal- cium carbid in a gas generator, and cover them with strong alcohol. Slowly add water through the funnel tube so as to cause a brisk evolution of the gas. Catch a couple of receivers full and ascertain its physical properties. With what kind of a flame does it burn ? EXPERIMENT 79. Destructive Distillation. Fill a test tube to a depth of about 3 cm - with excelsior or soft coal, packing it in tight, and support the tube horizon- tally between two rings of a retort stand (Fig. 34). Fit in a cork and delivery tube, and heat the lower end of the tube, gently at first, but finally as hot as possible without melting the glass. Let the delivery tube dip below the surface of the water in a pneumatic trough, and from time to time catch a test tube full of the gas given off, and test its inflammability. When no more gas is evolved, remove the delivery tube from the water. Test the liquid which has collected in the tube near its mouth with blue litmus paper. What effect ? What are the physical properties of the residue ? EXPERIMENT 80. A Simple Gas Factory. Roll a piece of paper (foolscap size) so as to form a cone with one end about 0.5 cm - in diameter and the other 2 to 3 cm - in diameter. Hold it vertically with the narrow end up and set fire to the other end. Apply a flame to the upper end a little above the paper. Does the escaping gas catch fire ? When the paper has burned about a third of its length, quench the flame by dipping it under water. Unroll the paper and examine any deposit on that part of it which formed the lining of the cone. 62 Elementary Chemistry EXPERIMENT 81. A Candle as a Gas Factory. Heat a small bit of a candle in an old test tube until vapors are formed that, on escaping from the tube, may be ignited. Blow out a candle flame and imme- diately bring a burning match or flame down towards the wick. What evidence is there to show that a gas is being given off ? THE ATMOSPHERE EXPERIMENT 2. (Quantitative^) To Determine the Percentage of Oxygen in the Air. Fill a hydrometer jar nearly full of water at the temperature of the room. Pour a little water in a graduated tube, place its open end in the water in the hydrometer jar, and let in air, if necessary, by raising it up until it nearly fills the gradu- ated portion. Lift the tube up until the level of the water within and without is the same and read off the volume of the air. Note the temperature of the water and the reading of the barometer, and reduce the volume read to stand- ard conditions. Bend a copper wire about twice as long as the graduated tube (Fig. 49) in a V-shape, sharpen one end with a file, and stick on this pointed end a piece of phosphorus which has just been scraped clean under water. Immerse the phosphorus on the end of the wire under the water in the jar, and bring the tube down over it so that the phosphorus pro- jects up into the air. What happens? Fig. 49 DETERMINING THE PERCENTAGE OF OXYGEN IN THE AIR Experiments 63 Let the apparatus stand for at least twenty-four hours, then lift the tube up until the level of the water inside and out is the same and the phosphorus is under water, and read off the volume. Reduce this volume to standard conditions after reading the temperature and pressure. Remove the phosphorus and again scrape it clean under water and replace it in the tube as before, leaving it there until the next day. Again find the vol- ume of the gas, reduce it to standard conditions, and see if it is the same as before. Compute the percentage of oxygen in the sample of air taken. O 1 234567 Fig. 50 TEST TUBE AND SCALE FOR DETERMINING THE VOLUME OF OXYGEN IN A GIVEN VOLUME OF AIR EXPERIMENT 83. The Volume of Oxygen in Air. Select a long, narrow test tube and cut a piece of paper whose length has the same ratio to that of the test tube as the scale has to the test tube in the figure (Fig. 50). Bend the ends of the strip of paper together and crease it in the middle, and do this a second and a third time. Then straighten the paper out so as to form a scale of eight equal divisions to serve as a measure of the vol- ume of the test tube. Instead of the above, any rule or scale may be used. Fill the test tube about one-eighth full of dry pyro- gallic acid, and, holding the test tube so that the thumb may be three-eighths of the distance from the bottom, pour in potassium hydroxid solution up to the level of the thumb. Immediately close the tube with the thumb and shake the air and solution well together for 64 Elementary Chemistry several minutes. Open the test tube with the thumb under water in a pneumatic trough (a beaker will do) and let stand for a few minutes so that the air may come to the temperature of the room. By means of the scale measure the volume of the gas left in the test tube, lifting it up so that the level of the water inside and out may be the same. How many volumes of air did you take ? How many volumes of gas have you now? How many volumes of oxygen were ab- sorbed ? What is the volumetric composition of air ? EXPERIMENT 84. Action of Dust on the Precipita- tion of Water Vapor. Fit a bottle (500 to 2,000 c - c -} with a two-hole rubber stopper, through each of the holes of which passes an L-tube which is connected with a chlorid of calcium tube. To one of the calcium chlorid tubes is attached a small bicycle pump or a rubber bulb with a valve. Put enough water in the bottle to fill it to a depth of about 2 cm -. Insert the stop- pers tightly and, closing with the thumb one end of the calcium chlorid tube not connected with the pump, pump air in through the other. When the pressure has become rather great, suddenly remove the thumb and note what takes place in the bottle. Repeat several times so as to make sure of the appearance of the phe- nomenon. Fill the calcium chlorid tubes loosely with cotton wool and pump in air as before. Do this a num- ber of times so as to replace the air in the bottle with air which has been freed from its dust particles by filtration through cotton. Is there any change in the phenomenon ? Let the bottle stand for several hours and then pump filtered air into it. What happens ? Let it stand for several hours longer and then do as before. Now thrust a lighted match for an instant into the neck of the bottle (after loosening the stopper) so as to introduce some smoke, i. e., dust, into the bottle, Experiments 65 and pump in filtered air. What happens ? What con- clusion can be drawn as to the action of dust particles in the formation of water drops from vapor ? EXPERIMENT 85. (Quantitative^] To Find the Weight of a Liter of Air. Melt off the top of one tomato can and the bottom of another. Pierce a hole about 3 mm - in diameter in the center of the bottom melted off and solder over it a bicycle valve. 1 Solder this bottom on the can, the top of which was removed. Connect with a bicycle pump, and pump in air until the pump works very hard. Disconnect the pump and weigh the can to centigrams. Slip over the valve a piece of rubber tubing in which has been placed a match with its head removed. Con- nect the other end of the tubing with an aspirating bottle, being sure to have the pressure in the bottle equal to that of the atmosphere. Pinch the rubber tubing around the match which should be resting in the valve, and, pressing the match against the valve, open it a little so as to let some of the air escape. Con- tinue doing this until no more air escapes from the can. As the air on expanding cools, wait a few minutes and then open the valve again, having the vessel employed to catch the water driven out of the aspirator at such a height that the water levels are the same. Remove the can and weigh it. The loss in weight represents the weight of the volume of air which has escaped from the can. Measure the volume of this water expelled from the aspirator either by weighing to decigrams or by means of graduates. Reduce the volume to o and 760 mm -. Calculate the weight of one liter of air. J This valve must close perfectly air-tight even when the screw- cap is not placed on it. 66 Elementary Chemistry FIRE AND FLAME EXPERIMENT 86. Kindling Temperature. I. Put a few drops of carbon bisulfid into a beaker and cover it with a card or glass slip. The vapor of the liquid then mixes with the air in the beaker. Heat the end of a glass rod to redness and thrust it into the beaker. Be careful to have your face as far as possible from the beaker. Repeat, using alcohol instead of carbon bisul- fid. What are your conclusions in regard to the tem- peratures at which different C9mbustibles take fire ? II. Try to ignite illuminating gas with a spark (not a flame) at the end of a match stick. Is the tempera- ture of the spark high enough ? Press a piece of wire gauze, held horizontally, down upon a Bunsen flame. Give reasons for what you observe. Pinch the rubber tubing together to extinguish the flame, and then, hold- ing the gauze just above the orifice, light the gas above the gauze. Raise the gauze up and note the behavior of the flame. If the gauze were made of a material which is a poor conductor of heat, how do you think it would modify the phenomena observed ? EXPERIMENT 87. Structure of Flame. I. A candle flame. Examine a candle flame in a place free from drafts, observing all its parts with their colors, and make drawings of each part. Holding it before a blackboard or other dark surface, note the outer portion. Also hold it in direct sunlight and examine the shadow it casts on white paper. Holding a piece of sized paper (asbestos paper is better) horizontally with both hands, press it down for a moment or so on the flame nearly to the wick, and examine the charred or sooty portions of the paper. II. A Bunsen flame. Repeat the above experiments with a Bunsen flame instead of a candle flame. Hold a match stick across the orifice of the burner and note how Experiments 67 the wood is charred. Hold it just above the inner cone and note what happens. Draw out one end of a piece of glass tubing to a bore of a little less than a millimeter, thrust the wider end into the inner cone and ignite the gas escaping from the drawn-out end. Slowly raise the tube until its wider end comes above the inner cone and note what happens. Thrust a pin through a match near its head and put the stick into a burner. Turn on the gas and light it above the match. Hold a piece of new asbestos paper or board vertically so as to divide the flame in halves and note how it is charred. EXPERIMENT 88. Luminosity of Flame. Sprinkle a little charcoal dust into a non-luminous flame ; also rub two pieces of charcoal together near the airholes of a Bunsen burner so that the dust may be carried up into the flame by the inflow of the air. What is the effect upon the flame ? Stir up the dust in the vicinity of a non-luminous flame. Close up the airholes of a Bunsen burner, and essay an explanation for the lumi- nosity of the flame thus produced. Examine a Wels- bach burner and mantle. Wherein does the Welsbach burner resemble the Bunsen burner ? What is the function of the mantle? EXPERIMENT 89. Speed of Propagation of Flame. Slowly turn off the gas of a Bunsen flame so as to diminish its speed of outflow very gradually. What happens ? This is because the speed of flow of the gas becomes less than that of the flame. Now turn the gas full on. At what two orifices is the flame now burning ? What was the cause of the slight explosion ? EXPERIMENT 90. Oxidizing and Reducing Flames. Cut out a little cavity in a piece of charcoal, pack it nearly full of litharge (lead oxid), and direct the reduc- ing flame of a blowpipe steadily upon it for some time. Examine the lead obtained. Now place a bit of lead 6 68 Elementary Chemistry in a cavity in a piece of charcoal and direct the oxidiz- ing flame upon it. Note the fumes and the color of the coating on the charcoal. SALTS, ACIDS, AND BASES EXPERIMENT 91. General Properties of Acids. Fill a beaker with distilled water, and after rinsing off a glass rod, dip it into the distilled water and place the drop that adheres to it on the tongue, noting its taste. Rinse the rod again it must be washed after each test and by means of it place a drop of the distilled water on a piece of blue and of pink litmus paper, being sure that the paper is on a clean surface. What change of color ? Pour about io c - c - of the distilled water into a clean test tube, add not more than three drops of strong sul- furic acid, and stir well together. In the same manner as before taste this acid solution and ascertain its action on pink and on blue litmus paper. Perform similar tests with very dilute solutions of any other acids which are available, as nitric, acetic, hydrochloric, tartaric. Review Experiment 18 and state what is the general action of dilute acids on metals. Test the action of acids on any other indicators which may be available, such as Congo red, phenolphthalein, methyl orange. EXPERIMENT 92. General Properties of Bases. Dissolve a piece (3 mm -) of sodium hydroxid in about IQC.C. of water in a test tube. Pour a drop or so on your finger and rub it with another finger. What is the feel? Dilute a little of this solution with about twenty times its volume of water, and, using a stirring rod, cautiously taste a drop. If the taste is not decided enough, add a little more of the sodium hydroxid solu- tion. Find what effect the solution has on pink and on Experiments 69 blue litmus paper as well as upon any other indicators available. Repeat these tests with potassium hydroxid instead of sodium hydrcxid ; also ammonium hydroxid (review Experiment 54), and with lime water (calcium hydroxid, Ca(OH) 2 , solution). EXPERIMENT 93. Neutralization. Place about 5^- of a very weak solution of sodium hydroxid in an evap- orating dish, and add a little litmus solution or any other indicator. Then with constant stirring add (a drop or so at a time) dilute hydrochloric acid until the blue color changes into a lavender. If too much acid is added, the color will be pink. In that case add some more sodium hydroxid solution, a drop at a time, so as to get the color just blue, and then a very small drop of the acid. When the intermediate color has been obtained, evaporate to dryness. Examine the product as to its physical properties and try its action on litmus paper, as well as upon other indicators that you may hap- pen to have at hand. What is the substance ? Repeat these operations, using dilute nitric acid instead of hydrochloric. OXIDS OF NITROGEN; NITRIC ACID EXPERIMENT 94. Preparation and Properties of Nitrous Oxid. Put about 15^- (6 cm - circle) of ammo- nium nitrate, NH 4 NO 3 , into a flask (or retort) provided with a delivery tube and an interposed safety bottle 28 (Fig. 51). Heat the flask gently and collect a couple of receivers full of the gas by water displacement. Plunge a lighted splinter of wood into a receiver full of the gas. Is the gas combustible or a supporter of combustion ? Set a little red phosphorus or sulfur on fire in a combustion spoon and introduce it into the gas. What other gas behaves in a fashion similar to nitrous oxid ? How would you distinguish the two gases ? Elementary Chemistry Fig. 51 APPARATUS FOR PREPARING NITROUS OXID EXPERIMENT 95. Nitric Oxid ; Its Preparation and Properties. Put about io& of copper 29 (in the form of filings, turnings, bits of wire, or granulated) in a gas generator; just cover it with water 30 and add enough strong nitric acid to cause a brisk evolution of the gas. Add water if the reaction becomes too tumul- tuous. Collect by water displacement six receivers full of the pure gas, saving two receivers full for Experi- ment 98. Let a little of the gas escape from one of the receivers. What causes it to turn brown as soon as it comes in contact with the air ? Insert a lighted splin- ter into one of the receivers. Is the gas combustible or a supporter of combustion ? Introduce a combustion spoon containing burning red phosphorus into a receiver full. Compare the result with that obtained with nitrous oxid. NOTE 29. Ferrous Sulfate. Ferrous sulfate (also known as green vitriol and copperas) may be advantageously substituted for Experiments ji the copper. It should be in the form of small lumps or crystals, and strong nitric acid added. The reaction is more easily con- trolled and a purer gas is obtained. NOTE 30. Use Hot Water. As nitrous oxid is rather soluble in cold water, it is advisable to have the pneumatic trough filled with as hot water as convenient. EXPERIMENT 96. Volumetric Composition of Nitric Oxid. Obtain a glass tube about 20 cm - long and of about i cm - bore, sealed at one end. Fit over the open end a piece of tightly-fitting rubber tubing about gem. long and have ready two Hofmann clamps (Fig. 52). Fill the glass and rubber tube with water and then displace the water with pure nitric oxid, prepared by the reduction of nitric acid by ferrous sulfate. Pinch the tube tightly near the glass tube with one of the clamps, A, and, removing the tube from the water, fill the rubber tube nearly full with an intimate mixture of equal bulks of powdered iron and sulfur. Then close the tube near its end with the second clamp, B. Now open the first clamp so that the mixture of iron and sulfur may fall into the tube. Shake the tube at inter- vals of fifteen to twenty minutes. Then turn the tube upside down and shake as much as possible of the solid Fig. 52 APPARATUS FOR DETERMINING THE VOLUMETRIC COMPOSITION OF NITRIC OXID mixture clown into the rubber tubing. Close the clamp A, as before, open clamp />, and after shaking out the solid mixture, fill the rubber tubing brimful of water, close it with the thumb and place the tubing under water. Now open clamp A What happens? With a rubber band or piece of cotton cord mark the volume of the gas remaining. What gas is it ? Ascer- tain the volume of this and that of the nitric oxid taken 72 Elementary Chemistry at first by running 1 in water from a burette or by weigh- ing-. What conclusion do you draw as to the volume of oxygen and nitrogen composing nitric oxid ? * EXPERIMENT 97. Nitrogen Dioxid. Heat in a test tube a few crystals of manganous nitrate, Mn(NO 3 ) 2 , or lead nitrate, Pb(NO 3 ) 2 . The main gaseous product is nitrogen peroxid. Is it soluble in water ? EXPERIMENT 98. Illustration of the Law of Vol- umetric Proportions* Prepare two gasometric tubes as follows : Obtain two test tubes about 2$ cm - long and i cm - wide. Fill the small tube even full of water and empty it into one of the large tubes, and mark the position of the water level with a rubber band. Add a second tube full and mark the position of the water level, and continue in this way until the tube is full. Proceed in like manner with the second large tube. Introduce into one of the gasometric tubes two vol- umes of nitric oxid (best prepared from nitric acid and ferrous sulfate), and into the other, five volumes of air. Pass the contents of one tube into the other. 31 What is observed ? In two or three minutes read the volume of the residual gas. What gas is formed when nitric oxid comes in contact with oxygen ? Is it soluble in water ? Explain the contraction. Repeat this procedure at least twice, so as to be sure of the results, each time transferring the residual gas into a receiver so that it may be examined and tested as follows : Measure out from the receiver three volumes and add a measured volume of air. Is there any con- traction ? If so, add some more air, and see if there is any contraction. In the same fashion, add volumes of nitric oxid to a measured volume of the residual gas and continue the additions until there is no contraction. Point out in detail how this experiment illustrates the law in question. Experiments 73 NOTE 31. Transferring Gases. To transfer gases from ne vessel into another, the pneumatic trough must be deep enough to allow of the complete submerging of the vessels. They are then placed so that the gas from one may rise and displace the water in the other. EXPERIMENT 99. Preparation and Properties of Nitric Acid. Put into a retort about 15 ff. (5 cm - circle) of powdered soditim or potassium nitrate and add about 30 c.c. of strong sul- furic acid. Arrange the apparatus (Fig. 53) so that the retort's neck passes nearly to the bottom of a test tube or flask set in a dish filled with cold water. Heat gently with interposed wire gauze, noting the be- havior of the mixture in the retort. When the test tube is about a quarter full of the distillate remove the flame ; be sure that the end of the retort's neck is not dipping below the surface of the acid in the test tube. CAUTION. Be very careful not to spill nitric acid on the hands; it produces very bad burns. Note the color of the nitric acid thus prepared, and compare it with that of a freshly-opened bottle of the commercial "c. p." article. How do you account for the difference ? Cautiously note its odor. Pour a few drops on a glass plate or watch crystal and place beside it a glass plate or watch crystal containing a little strong ammonia water. How do you account for the result ? Put a bit of litmus paper in a dish and add a few drops of acid from the test tube ; repeat after Fig. S3 PREPARING NITRIC ACID 74 Elementary Chemistry diluting the acid with about four times its volume of water. Take up a drop on a stirring" rod and touch it to your finger-nail or a quill ; wash it off promptly and put on a drop of ammonium hydroxid. Test its action both when cold and when hot on a little of the follow- ing metals placed in separate test tubes : iron, copper, zinc, lead, and mercury. Pour a drop or so into a little indigo solution. Put a drop on a piece of newspaper and on a piece of the best linen writing paper. Is the difference in the action sufficient to distinguish news- paper (which is made from wood pulp) from writing paper (which is made from Jinen rags)? What is the paper of your notebook made of, wood pulp or linen? EXPERIMENT 100. Decomposition of Nitric Acid by Heat. Support a long-stemmed tobacco pipe on a stand so that its mouthpiece just dips below the water in a dish, Heat the stem red-hot with a Bunsen flame and then pour a few drops of concentrated nitric acid into the bowl so that it may flow down through the heated portion. What makes the bubbles have a reddish-brown color while the gas which collects in the receiver is colorless ? Into what three substances is the nitric acid decomposed ? EXPERIMENT 101. Reduction of Nitric Acid to Ammonia. Put a little granulated zinc into a test tube and add about 5 c - c - of dilute sulfuric acid. After the hydrogen is escaping freely, add a drop at a time (a "medicine dropper" will be found convenient, or a little pipette easily made by drawing out to a jet a piece of glass tubing), very dilute nitric acid, noting carefully what happens when each drop is added. Add only about a dozen drops of the nitric acid. After a few minutes pour part of the solution into another test tube and add an excess of caustic soda solution. Warm a little and cautiously smell of the contents of the tube. Experimcn ts 75 What evidence is there that ammonia is being given off ? Verify your conclusion by the use of litmus paper and by Nessler's solution. How do you explain the formation of the ammonia ? EXPERIMENT 102. Reduction of a Nitrate to a Nitrite. Heat 15^- of sodium or potassium nitrate with 30^- of lead in an iron dish (sand bath pan), stirring the melted mixture with a stiff iron wire or long nail until most of the lead has disappeared. Transfer the cooled mass to a mortar, grind it to a powder, add hot water, stir well and filter. To a portion of the filtrate add a few drops of concentrated sulf uric acid, or potassium or barium nitrate. The yellowish-brown powder formed during the heating is lead oxid. What is the source of the oxygen combining with the lead ? How must the nitrate have been changed ? PREPARATION AND PROPERTIES OF ACIDS, BASES, AND SALTS EXPERIMENT 103. Preparation of a Salt (Mercury lodid) by Direct Union of the Elements. Weigh on a watch glass 2.5^- of mercury 32 , and then also on a watch glass ^.2^- of iodin 33 . Place the mercury in a clean mortar and just cover it with alcohol 34 . Add about a quarter of the iodin and rub it gently into the mercury until the iodin as such seems to have dis- appeared. Then mix in a second quarter-portion and continue until all the iodin is added and the mixture is dry and of a bright red color. Transfer the product to a test tube and add about 5 c - c - of alcohol. Heat the alcohol to boiling for a minute or so by immersing the end of the tube in boiling water contained in a beaker. Pour the solution into an evaporating dish and set aside to cool. Examine carefully the crystals of mer- cury iodid which separate out. Place a few of them 76 Elementary Chemistry in a dry test tube and cause them to sublime by heat- ing the rounded end of the tube. How do you account for the different colors of the sublimate ? Rub it with a glass rod and note any change of color 35 . NOTE 32. Pipette for Handling Mercury. A convenient way to handle small quantities of mercury is by means of a little pipette made by drawing out a piece of narrow glass tubing to a long, tapering point. Mercury is drawn up into the pipette by suction. If the tube then be held in an almost horizontal position, the mercury will not run out, and may be nicely discharged where wan ted" by inclining the pipette a little. NOTE 33. Danger of Corrosion. As both mercury and iodin corrode brass, great care must be exercised not to let them or their fumes come in contact with the brass parts of a balance. Be sure to collect any of either element whteh may become scattered about the balance through careless handling. NOTE 34. Addition of Alcohol. The reason for adding alcohol is to keep down the temperature (the heat of the reaction will be expended largely in evaporating the alcohol) and to bring the iodin and mercury in more intimate contact. The alcohol does not participate in the reaction at all. NOTE 35. Iodin Stains. Iodin stains may be removed by means of sodium sulfite or ammonium sulfid solution. EXPERIMENT 104. Preparation of a Salt (Zinc Sul- fate) by the Solution of a Metal (Zinc) in an Acid (Sulfuric). Place about 5^- of zinc in a beaker or flask and add about 40 c - c - of dilute sulfuric acid. When the evolution of hydrogen has nearly ceased, filter the solu- tion into an evaporating dish and gently heat 3 6 over a wire gauze nearly to boiling, until a thin film appears on the surface of the solution. Then set it aside so that it may cool slowly. At frequent intervals for several days examine the crystals which separate out and carefully note their form. Remove them from the solution and dry them by pressing between folds of filter paper. Do the crystals contain water of crystal- lization ? NOTE 36. Slow Evaporation. Instead of evaporating off the water rapidly by heating, the dish may be set aside so that the water may slowly evaporate during several days. If this be done, better and larger crystals will be obtained. Experiments 77 EXPERIMENT 105. Preparation of a Salt (Ammo- nium C/tlorid) by the Neutralization of Ammonium Hydroxid by Hydrochloric Acid. Dilute 25 c-c. of con- centrated hydrochloric acid with an equal vol- ume of water, mix well, and fill a burette with the mixture 3 7 . Fill a second burette with concentrated ammonium hydroxid (Fig. 54). Run 5.0^- of the acid into an evaporat- ing dish which has pre- viously been weighed to centigrams, and add just enough litmus solution to impart a distinctly pink color. Note the reading on the burette containing the ammonium hydroxid, and run the solution, a few drops at a time, into the acid, with constant stirring, until the red color turns to blue. Then run in the acid, drop by drop, stirring after each addition, until the color is half-way between blue and red. Evaporate the solu- tion to dryness on a water bath 2 2 (the ammonium chlorid volatilizes at a higher tem- perature), let cool and weigh. Again heat for a quarter of an hour and weigh, continuing in this way until the salt is perfectly dry, as shown by no further loss in weight. Fig. 54 BURETTES ARRANGED FOR NEU- TRALIZING A BASE BY AN ACID TO PRO- DUCE A SALT 78 Elementary Chemistry The equation for this neutralization reaction may be written thus : NH 4 OH + HC1 -> NH 4 C1 + H 2 O How many grams of NH 4 C1 have you prepared ? Calcu- late how much NH 4 OH and HC1 were needed. How much NH 4 OH and HC1 were contained in the volume of the solutions used? Calculate how many grams of NH 4 OH and of HC1 there would be in a liter of a solu- tion of the same concentration. NOTE 37. Drying the Burette. If the burette is not perfectly dry, it should be rinsed out, delivery tube and all, with a few cubic centimeters of the acid before filling. The ammonium hydroxid burette should also be rinsed out with that liquid. EXPERIMENT 106. The Solubility Product. Pre- pare a saturated solution of sodium chloric!, NaCl, by shaking the solid in a test tube with water until no more is dissolved. The solution will not be accelerated by heating, as sodium chlorid is nearly as soluble in cold water as in hot. Fill a test tube a quarter full with this saturated solution. Put a few cubic centi- meters of concentrated hydrochloric acid in a test tube provided with a cork and delivery tube, heat gently, and pass the hydrogen chlorid expelled from solution into the solution of salt. Prove experimentally that the white substance precipitated is sodium chlorid, and explain its formation. THE HALOGENS AND THEIR HYDROGEN COMPOUNDS EXPERIMENT 107. Chlorin by Oxidization of Hy- drochloric Acid. Into separate test tubes put a pinch of potassium chlorate, of red lead, and of potassium dichromate, and add a little strong hydrochloric acid to each. If a reaction does not take place promptly, warm a little. Note the physical properties of the gaseous Experiments 79 product, and then stop the action by filling the tube up with water. What are the color and other properties of this solution ? EXPERIMENT 108. Preparation of Chlorin. I. (Hood.) Into a flask (200 to 300 c - c -} fitted with a delivery tube and an interposed safety bottle (Fig. 55), put about 20 ff- (5^- circle) of manganese dioxid and add to it 50^- strong hydro- chloric acid. The delivery tube should reach to the bottom of the receiver, which should be snugly covered with a piece of cardboard pierced with a hole for the pas- sage of the delivery tube. Heat the flask gently and collect by downward displacement four receivers full of the gas. You can tell by the greenish color when the receivers are full, and the full receivers should be covered with glass slips smeared with a little vaseline so as to make gas-tight joints. Pass to Experiment no. EXPERIMENT 109. Preparation of Chlorin. II. (Hood.) Into a gas generator fitted with a stopcock funnel (Fig. 18) put about enough of bleaching powder to cover the bottom of the generator to a depth of a centimeter. The delivery tube should reach to the bot- tom of the receiver, which should be covered with a piece of cardboard with a hole through it for the passage of the delivery tube. Let strong hydrochloric acid drop from the funnel upon the bleaching powder just fast Fig. 55 PREPARING CHLORIN 8o Elementary Chemistry enough to keep up a brisk evolution of the gas, and col- lect four receivers full by downward displacement, cov- ering a receiver when full (as shown by the green color) with a glass slip smeared with vaseline. Pass to Ex- periment no. EXPERIMENT no. Properties of Chlorin. (Hood.) Thrust a piece of flaming paper into a receiver filled with chlorin, moving the glass slip only a little aside and at once covering the receiver again so as to prevent the fumes from escaping. Is the gas combustible? Does it support combustion ? Moving the glass slip aside again, sprinkle a pinch of powdered antimony into the gas. Also introduce a loose bundle of very fine brass or copper wires which have been heated to redness. Is the gas a supporter of combustion ? Com- pare it in this respect with oxygen. Into a second receiver put some paper with writing (both by ink and by pencil) on it and some pieces of dry calico, and into a third some paper with writing on it and some pieces of moistened calico. What differ- ences are to be observed in the bleaching action in the two receivers ? Repeat with the fourth receiver any of the above experiments, the results of which you are in doubt about and wish to verify. EXPERIMENT m. Chlorin Water. Drop into a test tube a few small crystals of potassium chlorate, cover them with concentrated hydrochloric acid diluted with an equal volume of water, warm a little, and as soon as the chlorin begins to escape from the tube, fill it nearly full of water. Pour a little indigo solution into a test tube and add an equal volume of the chlorin water. Is the color discharged ? Try the action of the chiorin water on solutions of litmus, of cochineal, and of copper sulfate. Explain any differences in the bleaching action. Experiments 81 EXPERIMENT 112. Preparation and Properties of Bromin. Put about 10^- (^ cm - circle) of potassium bromid in a mortar and add an equal bulk of man- ganese dioxid. Mix them well together and introduce the mixture into a dry retort, and then add about io c - c - of concentrated sulfur ic acid. Support the re- tort on the stand so that its neck may enter a test tube or flask set in a dish filled with cold water (Fig. 56). Put a little water in the test tube and ad- just so that the neck of the retort just dips into the water. Heat the retort very gently and collect the bromin given off until no more red vapor is seen in the retort. Note the phys- ical properties of the bromin. Pour a drop or so of bromin into a dry receiver, cover with a piece of paper or a glass slip, and shake and invert the receiver so that the bromin may rapidly vaporize and its vapors fill the vessel. Try its bleach- ing action as was done with chlorin and compare results. Pour what bromin is left into the bottle labeled "Bromin" which is standing on the side table. EXPERIMENT 113. Preparation and Properties of lodin. Grind well together in a mortar a half dozen crystals of potassium iodid with an equal bulk of man- ganese dioxid, put the mixture in an Erlenmeyer flask, and add about 15^- of a mixture of equal volumes of concentrated sulfuric acid and water. (Pour the acid 82 Elementary Chemistry into the water, not the water into the acid.) Set the flask on a wire gauze on a ring stand, and insert in its neck loosely a perforated cork holding a small test tube filled with cold water (Fig. 57). Another appara- tus is a tall, slender beaker with a watch glass cover- ing it and filled with cold water (Fig. 58). Heat the flask with a very small flame, just enough to cause the iodin liberated from the potassium iodid to vaporize and collect on the sides of the test tube kept at a low temperature by the cold water. When the test tube is covered with crystals of iodin, dis- continue the heating, re- move the test tube, and scrape the iodin into an evaporating dish. Note its physical properties. Fig. 57 PREPARING IODIN ' ln J 1 . Heat a small crystal in a dry test tube and when the tube is filled with the vapor, invert it and draw conclusions as to the relative weights of air and iodin vapor. Touch your finger to a crystal. What is the color of the stain ? Will water remove it ? Will alcohol ? Will a solution of potassium iodid? In which of these three liquids is iodin readily soluble? Place the rest of the iodin in the bottle labeled " Iodin " which is standing on the side table. EXPERIMENT 114. Tests for Free Bromin and Iodin. Prepare a test tube full of chlorin water (Ex- periment in). Dissolve a bit of potassium iodid and of potassium bromid not larger than a pinhead in a small Experiments test tube a quarter full of water, a different test tube for each substance. Make some thin starch paste by rubbing up a small lump (5 mm -) of starch with a little water in a mortar to the consistence of cream, and then boiling it in an evaporating dish with about 50^- of water until it is clear. Pour three or four drops of this starch paste into 10^- of water in a test tube and shake it up well ; then add a drop of an aqueous solution of iodin. What is the change in color? Heat the solution gently until the color disappears, and then cool it by immersing in cold water. This is a very delicate test for iodin when not in Combination. Repeat Fig. 58 ANOTHER APPARATUS FOR PREPAR- this test, using bro- min water instead of an iodin solution. Is the test as decisive as for iodin ? Pour three or four drops of starch paste into 10^- of water in a test tube, shake it up well, and add a drop or so of the solution of potassium iodid you have pre- pared. Is there any change of color ? Now add a dozen or so drops of the chlorin water. Explain what occurs. Repeat with the solution of potassium bromid instead of the iodid. Compare the results. Put a couple of drops of an aqueous solution of iodin in about io c - c - of water in a test tube, add about 84 Elementary Chemistry 2 c-c. of carbon bisulfid, and shake the two liquids well together. Does the color of the carbon bisulfid change ? Repeat, using a solution of bromin instead of iodin. Compare the two results. Repeat, using a solution of chlorin water. Does this give a decisive test ? Add about 2 c - c - of carbon bisulfid to the solution of potassium iodid prepared and shake them well together. Does the color change? Add a few drops of chlorin water and shake. What result? Repeat, using the solution of potassium bromid. Compare results. Could you prove by these tests that bromin was present in a solution of unknown composition if iodin was also pres- ent? Try it on a mixture of potassium bromid and potassium iodid solutions. EXPERIMENT 115. Action of Concentrated Sulfuric Acid on Halid Salts. Place in separate test tubes a couple of small crystals of sodium chlorid, of potassium bromid, and of potassium iodid, and add to each about 2 c - c - of concentrated sulfuric acid. Cautiously compare the smells of the gases evolved. Heat gently and note the appearance of any colored gases, if they have not been noticeable without heating. What elements are set free ? Put a pinch of calcium fluorid (fluorspar) in a small test tube and add about 2 c - c - of concentrated sulfuric acid. Heat until a gas is given off vigorously. Note the physical properties of this gas and after five min- utes or so pour out the reacting mixture into a plentiful supply of water. Wash out the test tube and see if the glass has lost its transparency in spots, and if so, account for it. To clean the test tubes pour their contents out into a large amount of water. Do not run water into tJie tubes upon the hot sulfuric acid, as there is danger of an explosion. Experiments EXPERIMENT 116. Preparation and Properties of Hydrochloric Acid. Put io c - c - of cold water in a beaker and add to it slowly and with constant stirring, SQC.C. of concentrated sulfuric acid. Set the mixture aside to cool. Put about 30^- (6 cm - circle) of common salt in a flask provided with a safety bottle and delivery tube, to the end of which may be attached a small funnel (Fig. 59) or a straight piece of large glass tub- ing. Add the cold acid and heat gently with the funnel attached to the end of the delivery tube, un- til the gas given off is nearly all absorbed by the water in which the rim of the funnel just dips. Then collect by down- ward displacement four dry receivers of the gas, cov- ering them with glass plates when full. Let the gas pass into some distilled water contained in a dish, using the funnel attachment, and save the solution for Expe- riment 1 1 8. Invert a receiver full of the gas and, holding its mouth under water in a pneumatic trough, open it. How do you account for what happens ? What other gas studied has exhibited a similar property ? Thrust a blazing splinter of wood into a second receiver. Does the gas burn or support combustion ? Hold a piece of wet filter paper over the mouth of another receiver. Fig. 59 PREPARING HYDROCHLORIC ACID 86 Elementary Chemistry What is the cause of the phenomenon? Drop in the last receiver a piece of filter paper moistened with strong" ammonia water. What happens ? What is the substance formed ? EXPERIMENT 117. Analysis of Hydrogen Chlorid. (a) Place a bit (3 ) of sodium in a bulb tube (Fig. 60), support it horizontally, and connect it on one side with a generator from which a brisk current of hydrogen chlorid (generated by dropping con- Fig. 60 sutB TUBE centrated sulfuric acid into concentrated hydrochloric acid contained in a stopcock generator) is issuing, and on 'the other with a delivery tube. As soon as all the air has been swept from the tube (How can that be told?), heat the sodium cau- tiously until it takes fire. Now collect in a test tube a sample of the gas given off and discharge it into a flame. What is the gas ? When the sodium no longer burns, disconnect the generator (letting the gas pass into water by means of a funnel, as described in Experiment 116), and, after the bulb tube has cooled, break it open and prove by appropriate tests that common salt, NaCl, has been formed. In the burning of the sodium, what substances were the combustible and the supporter of combustion, respectively ? (b) Put some manganese dioxid into an evaporating dish and heat as hot as possible for about ten minutes so as to remove all moisture from the dioxid. Arrange an apparatus . as shown in Fig. 31. Place in the tube some of the manganese dioxid and connect with the gas generator. As the hydrogen chlorid passes through the tube, heat the manganese dioxid gently by just brushing a flame along the tube. Collect the gas given off over water and establish its identity by suitable tests. Experiments 87 How do you account for the moisture that collects just beyond the dioxid ? EXPERIMENT 118. Tests for Chlorids, Bromids, and lodids. Prepare dilute solutions (about 3 per cent) of sodium chlorid, of potassium bromid, and of potas- sium iodid. To a few drops each of these solutions add an equal volume of silver nitrate solution. Compare the colors and properties of the precipitates. Boil the solutions and note the behavior of the precipitates. Add ammonium hydroxid until pieces of litmus paper placed in the tubes are blue, shake well, and note which pre- cipitates dissolve. What is the effect of adding enough nitric acid to make the litmus red ? Add silver nitrate solution to a little of the solution of hydrogen chlorid prepared in Experiment 116, and to as many chlorids, bromids, and iodids as are available. How do all the results compare ? How can a test for a fluorid be devised from Experiment 115 ? EXPERIMENT 119. {Quantitative.} To Find the Atomic Weight of Chlorin. Clean, dry, and weigh to centigrams an evaporating dish. Fill it about one- fourth full of finely powdered sodium chlorid and heat until decrepitation ceases. Let cool and weigh. Cover the salt with strong nitric acid, evaporate to dryness on a water bath, and heat with free flame until the sodium nitrate which has been formed just begins to melt. Let cool and weigh. To make sure that all the chlorin has been expelled, moisten the salt with concentrated nitric acid, heat and weigh again, repeating until a constant weight is obtained. The reaction is : NaCl + HN0 3 > NaNO 3 + HC1 A known weight (a) of sodium chlorid is converted into a known weight (6) of sodium nitrate. If the atomic weight of chlorin be denoted by .r, and those of sodium, nitrogen, and 88 Elementary Chemistry oxygen arc 23, 14, and 16, respectively, then the molecular weight of NaCl is: + ^ and that of NaNO 3 is : 23 + 14 + (3 X 16)1=85 a 23 + x Then -= b 8 85 a 23 b and x = b EXPERIMENT 120. (Quantitative^ To Ascertain the Strength of a Given Sample of Hydrochloric Acid. Fill a burette with the acid to be tested. Put about IQC-C- of a 5 per cent solution of sodium hydroxid in an evaporating dish, and add a few drops of some indicator. Run the acid into the alkali with constant stirring until neutralization is obtained. Evaporate to dryness without spattering. Heat the dish to constant weight. Calculate the weight of hydrogen chlorid in one liter of the solution. The equation for the neutralization of sodium hydroxid by hydrochloric acid is : NaOH + HC1 > NaCl + H 2 O 40 + 36.5 58-5 + 18 from which it is seen that 58. $& of NaCl are formed when 36. 5 of HC1 are used. The weight of the HC1 in the volume of the solution taken stands then in the same ratio to the weight of the NaCl found as does 36.5 to 58.5. The weight of HC1 contained in a liter of the acid solution is calculated by means of the pro- portion : Volume of acid taken inc-c. Weight of acid found 1,000 c - c - x EXPERIMENT 121. (Quantitative^] To Find the Strength of a Given Sample of Nitric Acid. The directions of Experiment 1 20 apply to rinding the strength of a given sample of nitric acid ; sodium nitrate is formed. Experiments 89 THE ALKALI METALS EXPERIMENT 122. Properties of Sodium and Potassium, (a) Examine a small piece of sodium ; note its most obvious properties, such as color, luster, and hardness. Cut a slice off it and immediately note the metallic luster. Review Experiment 23 (action of sodium on water). Cautiously dissolve a small piece in a little water in an evaporating dish. What is the action of the solution on litmus ? Evaporate to dryness and examine residue carefully. What is it ? (b) Repeat (), using" potassium. EXPERIMENT 123. Preparation and Properties of Potassium Carbonate, (a] Fill a test tube half full of hardwood ashes, cover with water, shake well together, warm gently and filter. Test the filtrate (i) with both blue and pink litmus paper, (2) for potassium (Experi- ment 127), and (3) for a carbonate (add HC1 ; a result- ing effervescence indicates CO 2 ). (b} Put about 5^- (4^- circle) of cream of tartar (acid potassium tartrate) in an iron dish and heat strongly in the hood until the residue is white. Grind the residue in a mortar with water, filter, and apply the same tests as in (a). (c) Mix thoroughly about 5^- (^ cm. circle) of pow- dered potassium nitrate with an equal bulk of powdered charcoal, and place the mixture in an evaporating dish. Heat an iron dish or plate red-hot and, standing at arm's length and grasping the evaporating dish with tongs, pour the mixture upon the iron. If it does not deflagrate at once, heat still hotter, being careful not to have your face or hands above the mixture. When deflagration has occurred and the product is cool, grind it in a mortar with a little water, filter, and test the ni- trate as in (a}. 90 Elementary Chemistry EXPERIMENT 124. Preparation and Properties of Sodium and Potassium Hydroxids. Make a solution of about 50 & (10 cm - circle) of sodium carbonate in about 300 c-c. of water and place it in an iron dish. To about 20 ff- of lime add enough water to slake it and make a milky mixture, "milk of lime." Heat the sodium car- bonate solution to gentle boiling, add the milk of lime and boil for five minutes, stirring constantly with a large nail or a file. Let the precipitate settle, draw off a little of the clear liquid with a tube drawn out so as to form a small pipette, 3 2 transfer it to a test tube and add an equal volume of dilute hydrochloric acid. If there is effervescence, all of the 'sodium carbonate has not been changed into the hydroxid ; so add a little more milk of lime and boil. If there is no effervescence, decant the clear liquid into a beaker. As sodium hydroxid attacks glass and porcelain, it is not advisable to evaporate the solution to dryness. The solution may be preserved in a rubber-stoppered bottle, labeled "Sodium Hydroxid," for use in subsequent work. Examine a piece of commercial sodium hydroxid and note its most prominent physical properties. Potassium hydroxid is to be prepared according to the same directions as given for sodium hydroxid, using potassium carbonate instead of sodium carbonate. EXPERIMENT 125. Preparation and Properties of Ammonium Amalgam. Put about 2 c - c - of mercury into a dry test tube, add a small piece (2 "**) of sodium, cork the test tube very loosely, and heat gently. As soon as a flash of light has indicated that the sodium has formed an amalgam with the mercury, introduce another piece of sodium, heat, if necessary, as before, and continue in this way until the amalgam has become solid. (An evaporating dish may be used instead of the test tube.) Experiments 91 Put about io c - c - of a strong solution of ammonium chlorid in an evaporating dish, and introduce into it about a quarter of the sodium amalgam. (The test tube will probably have to be broken to get the amal- gam out.) How does the amalgam change ? Take up some of the substance in the fingers and describe its "feel." What class of substances give this " feel " ? Put the rest of the sodium amalgam into a test tube, fill nearly full with strong ammonium chlorid solution, and when the ammonium amalgam begins to run out of the tube, fill it completely full with water, close with the thumb and invert over water. Try to keep as much of the ammonium amalgam as possible under the mouth of the test tube so that the gas which forms may be collected therein. When the test tube is full, test the gas. What is it? EXPERIMENT 126. Solvay Process of Sodium Car- bonate Manufacture. Prepare saturated solutions (about 100 <:) of ammonium carbonate and of sodium chlorid by shaking the finely powdered salts for some time with water. Decant the saturated solutions and pass washed carbon dioxid into the ammonium car- bonate until no more is absorbed. Now mix the two solutions, stir well, and run in carbon dioxid. If a pre- cipitate does not appear in a few minutes, shake well for some time, and run in carbon dioxid again. When a considerable amount of the precipitate has formed, prove it to contain carbon dioxid and sodium by appro- priate tests. EXPERIMENT 127. Flame Tests. Wash apiece of platinum wire as clean as possible and then hold it ir> a Bunsen flame until the latter is no longer tinged by vt. Dip its end in some sodium compound and bring into the flame ; note the color. Clean the wire again, dip into some potassium compound, and hold in the 92 Elementary Chemistry flame. Unless the potassium compound is entirely free from an admixture of sodium compounds, its character- istic color will be masked by that of sodium. When the flame is observed through cobalt blue glass, however, as the sodium flame color is absorbed, that of potassium alone is seen. If a lithium salt is available, familiarize yourself with its flame test also. EXPERIMENT 128. Preparation and Properties of the Nitrates of the Alkali Metals, (a) Put a little sodium hydroxid (or carbonate) into a dish, add a little water, and with constant stirring dilute nitric acid until a slightly acid reaction, (litmus paper) is obtained. Set the dish aside and examine it from day to day. (b) Go through similar operations with potassium hydroxid or carbonate instead of sodium. (c) When crystals have formed from both solutions, remove several specimens of each and compare their shape carefully. Write a careful description of each. Do you now see any reason for calling sodium nitrate cubical niter, as is sometimes done ? (d) Heat a few crystals of potassium nitrate in a test tube until they melt and effervesce. Now drop into the tube a piece (2 ) of charcoal. Describe what happens. Repeat with sulfur instead of charcoal. EXPERIMENT 129. Test for a Nitrate. Fill a small test tube about a fifth full of clear crystals of ferrous sulfate (green vitriol), and then about half full of water. Shake until a clear solution results. To this add a crystal of potassium nitrate about the size of a pin- head. Fill another test tube about a sixth full of concen- trated sulfuric acid and, holding both test tubes as nearly horizontal as possible, run the solution upon the sulfuric acid so that the two liquids mix as little as Experiments 93 possible. The brown ring shown where the solution floats upon the acid indicates the presence of a nitrate. Make a fresh solution of ferrous sulfate, and repeat the test without adding 1 potassium nitrate. Does the brown ring appear? EQUIVALENT WEIGHTS EXPERIMENT 130. (Quantitative^) Equivalent of Sodium. Weigh out to centigrams a piece of clean lead foil about 10 cm - square. Cut off a piece of sodium (about 4 mm - long and 2 mm - cross section), scrape off the coating of oxid and, after wiping it dry on filter paper, roll it into a cylindrical form. The weight of this cylinder should be about 0.9^-. Carefully roll the sodium up in the foil, leaving one end open, but pinch- ing the other end tightly together. By this arrange- ment the exposed surface of the sodium alone can be acted upon by water, and the evolution of hydrogen is quite steady. Weigh to centigrams the sodium and foil. The weight of the sodium is found by subtracting the weight of the foil from that of the foil and sodium. Fill a 500 c - c - graduated cylinder with water, close it with a piece of paper, and invert it in a pneumatic trough containing only a shallow depth of water. Drop the sodium wrapped in the foil in the water and at once place over it the inverted cylinder to catch all of the escaping hydrogen. When no more gas is given off, bring the water inside and outside the cylinder to the same level by raising the cylinder or by pouring water into the trough, and read off the volume. Also read the barometer and the thermometer. Reduce the vol- ume to standard conditions, correcting for aqueous ten- sion, and multiply the reduced volume by 0.09 (the weight of a liter of hydrogen) to find the weight of hydrogen evolved. The quotient obtained by dividing 94 Elementary Chemistry the weight of the sodium by that of the hydrogen is the equivalent of sodium. EXPB:RIMENT 131. (Quantitative^) Equivalent of Zinc. I. Weigh out to centigrams about 5 & of zinc (chemically pure, if possible), and put it into a gas gen- erator provided with a stopcock funnel. Connect the generator with an aspirating bottle (Fig. 24) of at least 2 l - capacity. Cover the zinc with a little \vater and close the stopcock. The delivery tube is placed in a vessel of water with the levels of the liquid in the ves- sel and in the aspirator the same when the delivery tube is open. Close the delivery tube and place it in a tared bottle or beaker holding at least 2 / -. Measure out with a pipette or a graduate 50^- of strong hydrochloric acid, put a portion of it in the stop- cock funnel, open the cock cautiously and let the acid run into the generator; be very careful to prevent any air being drawn into the generator. Add the acid from time to time so as to keep up a rapid evolution of the gas. When no more hydrogen is given off, add all of the acid, if it has not already all been added, arrange the aspirating and receiving bottle so that their water levels are the same and, opening the stopcock, let the acid drain into the generator. Let the apparatus stand for several minutes to come to the temperature of the room, and then close the delivery tube and lift it out of the receiving vessel. Weigh or measure the volume of the water expelled from the aspirator by the hydrogen, read the barometer and thermometer, and reduce the volume to standard conditions, allowing for aqueous tension. Multiply this reduced volume by 0.09 (the weight of a liter of hydrogen) to get the weight of the hydrogen evolved. Divide the weight of the zinc by the weight of the hydrogen ; the quotient is the equiv- alent of zinc desired. Experiments 95 EXPERIMENT 132. (Quantitative^ Equivalent of Magnesium. The apparatus and operations are like those in Experiment 131 : about 2?- of the metal should be taken. EXPERIMENT 133. (Quantitative.} Equivalent of Zinc. II. (Hood.) Clean, dry, and weigh to centi- grams an evaporating dish, together with a funnel, which, when inverted, fits securely into the dish. Put 3 to 4-?- of zinc (preferably chemically pure, although ordinary or mossy zinc will do) in the dish, replace the funnel and weigh to centigrams. Support the dish on a ring of a stand, and pour in beside the funnel a little strong nitric acid so that it can flow under the funnel and attack the zinc. As soon as the action subsides a little, add more acid, and continue in this way until all the acid is dissolved. Now evaporate to dryness, using a large flame. When the contents of the dish appear dry, gradually increase the heat, finally heating as hot as possible for at least five minutes. Let the dish cool and weigh it. Again heat to redness for several min- utes and weigh, continuing in this way until the dish and contents do not lose more than 3 c s- on heating. The substance remaining is zinc oxid ; the zinc nitrate at first formed is decomposed by the heating. How many grams of zinc oxid have you obtained? How much oxygen has combined with the zinc taken ? What is the ratio of the weights of the zinc and oxy- gen ? Taking the equivalent of oxygen as 8, what is the equivalent of zinc as deduced from this experi- ment? EXPERIMENT 134. (Quantitative^ To Determine the Vapor Density of Alcohol by Dumas' Method. Fit a clean, dry flask (100 to 250 c - c -) with a one-hole rubber stopper through which is thrust a bit of glass tubing with its upper end drawn out to a diameter of Elementary Chemistry about a millimeter (Fig. 61), and after rubbing the stopper with a little vaseline so as to make it fit gas-tight, weigh the apparatus to centigrams (or better, milligrams). Take the temperature and pressure of the air. Put about 20 c - c - of alcohol into the flask and immerse it up to its neck in boiling water contained in a beaker or can, hold- ing it submerged by means of a clamp. Take the temperature of the boiling water. When the alcohol has almost all boiled away bring a Bunsen flame to the tip of the glass tube, and as soon as the alcohol flame goes out (an in- dication that the flask contains only alcohol vapor) seal off. Weigh the flask again with the same degree of accuracy as before. Hold the neck of the flask under water and with tongs or pinchers break off the tip of the sealed tube. The flask should promptly fill almost completely with water; if it does not, the experiment must be repeated. Weigh the flask thus filled with water, to decigrams only, on a platform balance. The difference Fig. 6l DETERMINING THE VAPOR DENSITY OF ALCOHOL A short piece of rubber tubing, closed by a pinch- cock, is substituted for the glass tip Experiments 97 between the weights of the flask filled with water and with air gives the weight of the water, which, as one cubic centimeter of water weighs one gram, also gives the volume of the air and of the alcohol vapor. The calculation of the results are given on page 215 of the text. SULFUR AND ITS COMPOUNDS EXPERIMENT 135. Properties of Sulfur, (a) Re- view the observations you made on sulfur in Experi- ments i and 2. (b) Fill a test tube nearly half full of sulfur and, grasping it with a holder, heat it carefully. What is the color of the sulfur just after it melts ? Pour a drop or so into cold water and compare the product with the original sulfur taken. Heat the tube so as to raise the temperature of the melted sulfur gradually, and from time to time tilt the tube. What changes occur in its color and viscosity ? Do you find that at a certain tem- perature the sulfur becomes so viscid that you can invert the tube without the sulfur running out ? Heat to boiling. Pour the boiling sulfur slowly and in a thin stream into cold water contained in a dish or beaker, moving the tube around so that the sulfur may solidify in a long spiral rod. Examine the product, especially as to color, hardness, and elasticity. Put it away in the desk and examine it from time to time for a week or so. What changes take place ? (c) Fill a combustion cup with sulfur, set it on fire, and then put the cup in the bottom of a wide-mouthed bottle, covering it with a piece of cardboard. When the sulfur ceases to burn, introduce a piece of dry blue litmus paper. What change of color ? Then put in a piece of wet blue litmus paper and note result. (d) Review Experiment 7, I. 98 Elementary Chemistry NOTE. Experiment ij6 must be performed in the hood. EXPERIMENT 136. Preparation and Properties of Hydrogen Sulfid. Place a little ferrous sulfid in a test tube and add some dilute sulfuric acid. If a gas is not given off, heat gently. Attach a delivery tube and collect a small test tube full of the gas by down- ward displacement (Fig. 44). Ignite the gas and see if you can detect the odor of burning sulfur. Pass the gas for several minutes into about 2 C - C - of strong nitric acid in a test tube. When the inside of the end of the delivery tube becomes coated with a yellow substance, substitute a new delivery tube and put it into a second test tube filled with water. This will yield a solution of hydrogen sulfid. Rinse out the first delivery tube, pick out some of the deposit and by means of appropri- ate tests establish its identity. Add some of the hydrogen sulfid solution to a little dilute copper sulfate, CuSO 4 , solution. Result ? Repeat with lead acetate, Pb(C 2 H 3 O 2 ) 2 , solution; with cad- mium sulfate, CdSO 4 , solution ; with potassium perman- ganate (KMnO 4 ) solution, bromin water, and chlorin water. What is the result in each case ? If copper, lead, cadmium, and sulfur are all bivalent elements, what are the formulas of the products ? Write the equations for the reactions. Repeat these tests, delivering the hydrogen sulfid gas directly into the solutions of the salts. EXPERIMENT 137. Preparation of Sulfur Dioxid. (a) By the burning of sulfur. Review Experi- ment 2. (b) By the decomposition of sulfuric acid by copper. Put about 10^- of copper in a flask provided with a cork and delivery tube with interposed "safety bottle" (Fig. 55), and add about 40 c - c - of strong sulfuric acid. Heat the flask cautiously, removing the flame when the Experiments 99 effervescence may become too brisk, and collect two receivers full by downward displacement. Cover the bottles well and reserve for use in Experiment 138. Let the gas pass into a beaker half full of water for a few minutes, so as to prepare a solution of sulfur dioxid (sulfurous acid). (c) By t/ie action of dilute sulfuric acid on sodium sulfite. Put a layer of sodium sulfite nearly a centi- meter thick in the bottom of a gas generator, barely cover it with water, and add through the funnel tube from time to time dilute sulfuric acid so as to keep up a rapid evolution of gas. Collect t\vo receivers full by dow r nward displacement, cover them well and reserve for Experiment 138. Prepare a solution of sulfur dioxid by passing the gas into some water in a beaker or a bottle, and save for Experiment 139. EXPERIMENT 138. Properties of Sulfur Dioxid. Bleaching Action, Place in a receiver full of sulfur dioxid a piece of moistened calico, some petals of a red flower (carnation), cover and allow to stand for half an hour or so. What happens ? Remove the object intro- duced and place it in a dish containing very dilute sul- furic acid. What change in color ensues ? Oxidation by Nitric Acid. Pour a few drops of strong nitric acid into a receiver filled with sulfur dioxid, cover and move the receiver around so that its inside walls may become moistened with the acid. What visible evidence is there that the nitric acid is being reduced ? To prove that the sulfur dioxid has been changed into the trioxid (which dissolves in the water to form sulfuric acid), rinse out the receiver with a little water, pour into a test tube and add barium chlorid solution. The appearance of the white precipi- tate of barium sulfate indicates the presence of sulfuric acid. ioo Elementary Chemistry EXPERIMENT 139. Properties of Sulfurous Acid. Test the action of the solution of sulfur dioxicl prepared in Experiment 137 on litmus paper. Cautiously taste a drop of it on a stirring rod. Pour some of it into an evaporating dish, add a few drops of litmus solution or other indicator, neutralize with sodium hydroxid solu- tion and evaporate the solution to dryness. How can you prove that the white residue is the salt, sodium sulfite, Na 2 SO 3 ? Add a drop or so of potassium permanganate solu- tion to a little sulfurous acid in a test tube. Repeat, using potassium dichromate instead of permanganate. Compare results. EXPERIMENT 140. Properties of Sulfuric Acid. Decomposition by /teat : Place not more than one drop of strong sulfuric acid in a porcelain dish and heat. Heat generated on mixing with water : Pour a few drops of strong sulfuric acid into a test tube half filled with water. Action of organic substances: Try the action successively of a few drops of strong sulfuric acid on (a) a splinter of wood, (/;) a piece of paper, (c) a piece of colored cloth, (d) a little sugar, (c) a little starch. It may be necessary to heat gently in the last two cases. PHOSPHORUS CAUTION. All experiments with phosphorus should be carried out with the utmost caution, as the ready inflammability of the yellow modification of the element makes such experiments dangerous. The waxy modification should never be touched with the fingers and should be handled and cut UNDER WATER. At the conclusion of an experiment all bits of phosphorus left over should be carefully collected and burned. Experiments 101 EXPERIMENT 141. Physical Properties of Phos- phorus. Examine both red and yellow phosphorus, carefully noting their chief characteristics. Put a piece (3 mm.) of yellow phosphorus in a small dry test tube and add about 3 c - c - of carbon bisulfid. CAUTION. Be sure that no flames are near. Shake carefully for a minute or so. Pour the solu- tion, every bit of if, upon two or three pieces of filter paper laid on a ring of a retort stand and set the stand back out of the way. While waiting for the carbon bisulfid to evaporate, put a pinch of red phosphorus in a small dry test tube, add about 3 c - c - of carbon bisulfid, shake for a minute or so, filter through a dry filter paper, catch the filtrate in a watch glass, and allow to evaporate (in the hood). Is red phosphorus soluble in carbon bisulfid ? What hap- pens to the solution of yellow phosphorus poured on the filter paper? How do you account for the result? EXPERIMENT 142. Conversion of Red Phosphorus into Yellow Phosphorus. Put a pinch of red phos- phorus in the bottom of a small ignition tube 7 , hold the tube horizontally with the tongs, and gently heat the bottom of the tube. When nearly all the red phos- phorus has disappeared, let the tube cool, then make a scratch just below the deposit that has collected in the cooler part of the tube and break the tube. Rub the deposit with a glass rod or match stick. How do you know that yellow phosphorus has been formed ? Do not neglect to heat both parts of the tube to redness so as to burn up all the phosphorus. EXPERIMENT 143. Preparation and Properties of Phosphin. Fill a test tube fitted with a two-hole cork, through which pass tubes as shown in Fig. 62, about one-fourth full with sodium hydroxid solution, and put into it a piece (4 *) of phosphorus. Connect the tube 102 Elementary Chemistry which dips into the soda solution with the gas supply and pass through the apparatus ordinary illuminating gas until the air is expelled. How can you prove this to be the case? Shut off the gas and gently heat the contents of the test tube, keeping the end of the delivery tube below water in a dish. How do you account for the rings of smoke that appear ? EXPERIMENT 144. Preparation of Me- taphosphoric Acid. Put a little heap of red phosphorus on a piece of asbestos paper (or in a porce- lain crucible) set in a crockery plate, ignite the phosphorus and invert over it a perfectly dry wide-rnouthed bottle. When the phosphorus ceases to burn set the bottle upright. Pour a few drops of cold water on the phos- phorus pentoxid formed, noting any hissing noise, and test the solution with blue litmus. Put the solution into a test tube and add silver nitrate solution. What is the precipitate formed ? EXPERIMENT 145. Preparation of Orthophos- phoric Acid. Put a little (i cm - circle) red phosphorus in an evaporating dish, cover it with nitric acid, and heat gently. When the action has ceased, filter, if the solution is not clear, and evaporate the filtrate on the water bath. Redissolve the sirup which remains in a little water. What is its action on blue litmus paper? FlG. 62 CONVENIENT APPARATUS FOR PRE- PARING PHOSPHIN Experimen ts 103 Add silver nitrate solution and note nature of the pre- cipitate of silver orthophosphate, Ag 3 PO 4 . If the pre- cipitate is of a dark color, it is evident that some phos- phorus acid was formed also. In that case it is well to add silver nitrate solution to a solution of commercial orthophosphoric acid. EXPERIMENT 146. Reactions of Phosphates. To a solution of sodium hydrogen phosphate, Na 2 HPO 4 , add some calcium chlorid, CaCl 2 , solution. The pre- cipitate is secondary calcium phosphate, CaHPO 4 . Prepare some "magnesia mixture" by mixing a little ammonia hydroxid and ammonium chlorid with magne- sium sulfate, and add it to a solution of acid sodium phosphate. The precipitate is magnesium ammonium phosphate, (NH 4 )MgPO 4 . ARSENIC AND ANTIMONY EXPERIMENT 147. Properties of Arsenic. Note the physical properties of arsenic. In what respects does it resemble metals? Heat a small particle of the element on a porcelain crucible cover, noting particu- larly any odor. EXPERIMENT 148. Arsin. {Marsh's Test for Arsenic.) Generate hydrogen in a generator provided with a long ( 2 5 cm ') glass delivery tube drawn out to a jet. Use none but chemically pure materials. When the air is displaced, light the hydrogen at the tip. Heat the glass tube nearest the generator with a Bunsen flame. If a deposit appears in the cold part of the tube, the zinc or sulfuric acid is impure and the experiment should be discontinued and other materials used. If no subli- mate appears and the hydrogen burns with colorless or slightly yellow flame, and leaves no spot on the bottom of a porcelain dish pressed down upon it an instant, pour a few drops of an arsenical solution down the IO4 Elementary Chemistry funnel tube. Heat the tube and note the appearance of sublimate and the color of hydrogen flame. Press the porcelain dish in the flame a moment and add a couple of drops of sodium hypochlorite solution to the spot. Soak pieces of green paper in water and test the water for arsenic as above. EXPERIMENT 149. Arsenic Trioxid, Trichlorid, and Trisulfid. (a) Mix a pinch of arsenic trioxid with an equal bulk of powdered charcoal, put the mixture in an ignition tube, and slip down over it a loosely fitting plug of charcoal. With the tongs hold the tube in a flame so as to keep the charcoal plug red- hot while heating the mixture of charcoal and oxid. What is the nature of the deposit that forms in the cooler part of the tube ? How can you prove this deposit to be arsenic ? (b) Heat carefully a pinch of arsenic trioxid with sodium hydroxid solution. Sodium arsenite, Na 2 AsO 3 , is formed. (c) Boil a little of the trioxid with concentrated hydrochloric acid. Result ? Dilute with an equal vol- ume of water. Arsenic trichlorid is formed. (d) Pass hydrogen sulfid into the solution from (c). What is the color and appearance of the precipitate ? Let the precipitate settle, pour off the supernatant liquid, add some ammonium sulfid to the residue, warm gently, and shake well for some time. Soluble ammonium sulfo-arsenite, ( ) 2 AsS 3 , is formed. To a little of this solution add a slight excess of hydrochloric acid. What happens ? EXPERIMENT 150. Arsenic Acid. Boil a little arsenic with nitric acid for some time, then add just enough ammonium hydroxid to effect neutralization. To part of this solution add silver nitrate solution, and Experiments 105 to another, "magnesia mixture." Compare results with those obtained in Experiment 146. EXPERIMENT 151. Properties of Antimony. Note the physical properties of various samples of antimony that may be available. EXPERIMENT 152. Stibin. Follow the directions in Experiment 148, substituting antimony trichlorid (Experiment 153) for the arsenical solution. EXPERIMENT 153. Antimony Trioxid, Trichlorid, and Trisulfid. (a) Repeat Experiment 149 (a), substi- tuting antimony trioxid for arsenic trioxid, and com- pare results. (b) Boil a little powdered antimony with sodium hydroxid solution and compare results with those obtained in Experiment 149 (#). (c) Place some powdered antimony in a test tube and add about 3 c - c - of concentrated hydrochloric acid and one cubic centimeter of concentrated nitric acid. If a reaction does not start promptly, warm a little, and let it continue for at least ten minutes. Then dilute with five times its bulk of water and, if the solution is not clear, filter it. Pass hydrogen sulfid into the solu- tion of antimony trichlorid thus prepared. If a precip- itate does not soon form, add more water. Treat the precipitate of antimony trisulfid, Sb 2 S 3 , as directed in Experiment 149 (c) and (d). (d) Heat some powdered antimony with concen- trated nitric acid and compare results with those obtained in Experiment 150. BISMUTH EXPERIMENT 154. Properties of Bismuth. Note the physical properties of bismuth. Try to dissolve a bit of it in (i) concentrated hydrochloric and (2) con- centrated nitric acid. io6 Elementary Chemistry EXPERIMENT 155. Reactions of Salts of Bismuth. Place a few small crystals of bismuth nitrate in a test tube, fill the tube a quarter full with water, and add small amounts of concentrated hydrochloric acid until a clear solution is obtained. Pour a few drops of the solution into water, nearly filling- a test tube. The white precipitate is bismuth subnitrate, BiONO 3 . Pass hydrogen sulfid through the rest of the solution. Filter out the bismuth sulfid, Bi 2 S 3 , and treat with warm yel- low ammonium sulfid. Filter and acidify the filtrate with hydrochloric acid. Compare the result with Ex- periments 149 (d) and 153 (c). How can sulfid of bis- muth be separated from those of arsenic and antimony ? MAGNESIUM EXPERIMENT 156. Properties of Magnesium. Scrape a piece of magnesium wire or ribbon bright and note its most obvious physical properties. Grasp one end of a short piece with tongs and hold it in a Bunsen flame. What is the product and what are its properties ? Treat a little magnesium in a test tube with dilute hydrochloric or sulfuric acid. What gas is evolved? EXPERIMENT 157. Reactions of Magnesium Salts. To a little magnesium sulfate solution add sodium or ammonium carbonate solution. Also add sodium or ammonium carbonate solution to magnesium chlorid solution. Compare results. What are the products? To about 5 c - c - of magnesium sulfate solution add about one cubic centimeter each of ammonium hydroxid and ammonium chlorid solution. Then add disodium hydrogen phosphate solution. The precipitate is mag- nesium ammonium phosphate (NH 4 )MgPO 4 . EXPERIMENT 158. Preparation of Magnesium Sulfate. Place about 20 #- of magnesite in a beaker or flask and add 30 to 40 c - c - of dilute sulfuric acid. If Experiments 107 effervescence is not vigorous, heat a little. When solu- tion is complete, filter and evaporate the filtrate to crystallization on a water bath. Pour off the mother liquor from the crystals and dry them by pressing between folds of filter paper. EXPERIMENT 159. Preparation and Properties of Calcium Oxid (Lime) and Hydroxid (Slaked Lime). Test a piece of marble (12 mm -) with wet red litmus paper. What reaction does it show ? Support the lump on a frame of iron wire laid across a ring of a stand, and heat as hot as possible, using two Bunsen flames, or, better, a blast lamp. After heating for about fifteen minutes remove the flames, and as soon as the lump is cold, test it again with wet red litmus paper. What change has supervened ? Place the lump of quicklime in a dish or saucer and pour water upon it drop by drop as long as it is taken up readily. Do not .add too much water. Keep the lump under observation for some time, and note any changes (heat, volume, appearance). Put some of this slaked lime in a bottle and fill the bottle with distilled water. Shake up well, let settle, and decant the clear liquid into another bottle, and label it "Lime Water." EXPERIMENT 160. Some Properties of Several Calcium Compounds. Review Experiment 67. Place a piece of old mortar in a test tube, add dilute hydro- chloric acid, and identify the gas. Stir up some (5 cm - circle) plaster of Paris with enough water to make a thick paste. Spread the paste on a piece of paper and lay on it a coin covered with a thin coating of vaseline, embedding it slightly in the paste. (Do not delay to wash out the dish, as the plaster of Paris is hard to remove after it has set.) Carefully remove the coin after the plaster has set for io8 Elementary Chemistry an hour or more. To about 2 c - c - of a solution of calcium salt (chloric! or nitrate) add ammonium or sodium car- bonate solution. Repeat, using ammonium oxalate solution instead of a carbonate solution. Try the flame test (Experiment 127) with (i) cal- cium chlorid and (2) calcium sulfate. Review Experiment 38 for water of crystallization of gypsum. EXPERIMENT 161. Reactions of Strontium and Barium Salts, (a) To a little strontium chlorid solu- tion in a test tube add a few drops of ammonium car- bonate solution. Also ascertain the reaction between a solution of strontium chlorid and dilute sulfuric acid. (I?) Test solutions of barium chlorid with ammonium carbonate and dilute sulfuric acid. Try the flame tests, using (i) strontium chlorid, (2) strontium nitrate, (3) barium chlorid, and (4) barium nitrate. Look at the flames through a spectroscope or through a diffraction grating, if these instruments are at hand. BORON AND SILICON EXPERIMENT 162. Preparation of Boric Acid. Put about 2$#- (7 cm - circle) of borax in a beaker and add about ioo c - c - of water. Heat and stir until the borax is all dissolved ; filter if the solution is not clear. To the hot solution add enough strong hydrochloric acid to make it decidedly acid to litmus paper. Allow the solution to cool and stand for some time. Then filter off the boric acid crystals which have formed, and purify them by recrystallization from the smallest pos- sible amount of boiling water. EXPERIMENT 163. Characteristic Reaction of Boron Compounds. Dissolve a pinch of boric acid in about 2 c - c - of strong alcohol contained in an evapo- rating dish. Dip a tuft of asbestos into the solution Experiments 109 and, holding it with tongs, set the alcohol on fire. What is the color of the name ? Ignite the rest of the solu- tion in the dish. EXPERIMENT 164. Borax Bead. Make a small (less than a millimeter in diameter) loop at the end of a piece of platinum wire by winding it around the point of a lead pencil. Heat it and touch it to a small lump (2 **) of borax. Then heat the borax until a clear, glass-like bead is obtained in the loop. Bring the hot bead in con- tact with a minute particle of some cobalt or iron com- pound and heat in the flame. What color is imparted to the bead ? EXPERIMENT 165. Preparation of Magnesium Sil- icid and of Silicon Hydrid. Mix well on a piece of paper equal parts (2 cm - circle) of powdered magnesium and very fine sand, place the mixture in a small test tube and, grasping it with a test tube holder or paper and tongs, with its mouth pointing so that any of the substance which may be projected from the tube can do no harm, hold it steadily in the tip of a Bunsen flame. After the completion of the reaction break the test tube and throw small portions of the product (mag- nesium silicid) into dilute hydrochloric acid contained in an evaporating dish or beaker. What takes place ? What compound of silicon is spontaneously inflammable ? EXPERIMENT 166. Preparation of Silicic Acids. To about 5 c - c - of a concentrated solution of " water glass " (a crude mixture of sodium and potassium sili- cates) add in small proportions hydrochloric acid until the mixture is strongly acid to litmus paper. Put a little of the thick, gelatinous mass (a mixture of ortho- silicic and metasilicic acids) on a piece of platinum foil, evaporate to dryness, and heat strongly. Add a drop of water to the white residue, and test it with litmus paper. What is the powder ? no Elementary Chemistry ZINC EXPERIMENT 167. Properties of Zinc. Ascertain the most obvious characteristics of as many different forms (mossy, granulated, powdered, stick) of zinc as possible. Review Experiments 18 and 104. In Experi- ment 1 8 hydrogen and zinc chlorid were formed ; in Experiment 104 hydrogen and sodium zincate. EXPERIMENT 168. Reactions of Zinc Salts, (a) Fill a test tube about a fourth full of zinc sulfate or chlorid solution and add a drop or two of sodium hydroxid solution. What is the precipitate formed ? Now add little by little enough sodium hydroxid solu- tion to redissolve the precipitate formed at first. The alkalin solution contains sodium zincate. (b) Fill a test tube about a third full of zinc sulfate solution and add a drop of dilute hydrochloric acid. What is the reaction of the mixture (litmus) ? Pass in hydrogen sulfid for a few minutes. Result ? No\v transfer the mixture to a beaker and add half its vol- ume of ammonium sulfid. The precipitate is zinc sul- fid. Test with litmus. What must the reaction of a zinc salt solution be in order that the sulfid may be precipitated ? EXPERIMENT 169. Blowpipe Reactions. Heat a small piece of zinc on charcoal in the oxidizing flame of a blowpipe. Moisten the incrustation with a drop of cobalt nitrate solution and heat again in the oxid- izing flame. Result? CADMIUM EXPERIMENT 170. Properties and Reactions. Examine a piece of the cadmium, and note its most obvious properties. Into a dilute solution of cadmium chlorid or sulfate pass hydrogen sulfid gas. The precipitate which forms Experiments 1 1 1 is cadmium sulfid, CdS. Make the solution acid by adding a few drops of hydrochloric acid. Is cadmium sulfid soluble in dilute hydrochloric acid ? Wash the precipitate by decantation and add ammo- nium sulfid solution. Is the precipitate redissolved? How can cadmium sulfid be distinguished from other yellow sulfids? Add sodium hydroxid solution in excess to a solution of a cadmium salt. Is the hydroxid precipitated solu- ble in caustic alkali solution? MERCURY EXPERIMENT 171. Preparation of Mercury. Put a little cinnabar near one end of a glass tube (15"*- long) open at both ends, and heat the glass under the cinnabar strongly, holding the tube in a slanting posi- tion and rotating it constantly. What gaseous products are formed? What is deposited in the cooler part of the tube ? Mix a pinch of mercury chlorid with two or three times its bulk of dry powdered sodium carbonate, and heat the mixture in an ignition tube. Note the nature of the sublimate. EXPERIMENT 172. Mercurous Nitrate. Fill the rounded end of a test tube nearly full of mercury, add about 5 c - c - of water, and then about $ c - c - of concentrated nitric acid. Let the action go on for an hour or so. In the meantime perform Experiment 173. Pour the contents of the tube off from any mercury that is left into a small beaker, dissolve in the least possible amount of water any crystals which may have formed, rinse out the tube with about 2O C - C - of water, put the rinse water into the beaker, and add one or two drops of concen- trated nitric acid, so as to have a clear solution. Save the solution for Experiment 174. H2 Elementary Chemistry EXPERIMENT 173. Mercuric Nitrate. Dissolve about half as much mercury as was used in Experiment 172 in about io c - c - of concentrated nitric acid. Dilute the solution of mercuric nitrate thus formed with an equal volume of water. EXPERIMENT 174. Reactions of Mercurous Salts. To 2 c - c - of mercurous nitrate solution add hydrogen sulfid. The precipitate is a mixture of mercuric sulfid and mercury. Add to separate portions of the solu- tion, hydrochloric acid and potassium iodid solution, respectively. Add ammonium hydroxid to the precipi- tate from hydrochloric acid. What are the precipitates ? Put a strip of zinc and of copper (or copper wire) into portions of the mercurous nitrate solution. In a few minutes remove them and rub them dry. What has happened ? Rub a cent or a dime with a piece of paper' wet with mercurous nitrate solution. EXPERIMENT 175. Reactions of Mercuric Salts. Pass hydrogen sulfid into the mercuric nitrate solution. The precipitate is mercuric sulfid, HgS. Add to sepa- rate portions of mercuric nitrate solution, hydrochloric acid and potassium io^id solution (this drop by drop). What are the precipitates ? ALUMINUM EXPERIMENT 1 76. Properties of Aluminum. Exam- ine as many different forms of aluminum as are avail- able, also of its alloys ; note their most prominent physical features. EXPERIMENT 177. Action of Acids and Alkalis on Aluminum. Fill the rounded end of a test tube with aluminum, add about twice its volume of concentrated hydrochloric acid, and warm and test the gas evolved. Repeat, using sodium hydroxid solution (cf. Experi- ment 27). The solution contains sodium aluminate. Experiments 113 EXPERIMENT 178. Action of Mordants. Soak a piece of white cotton cloth in a strong solution of cochi- neal or indigo for a minute or so ; then wring it out and dry it. Try to wash out the color, using soap. Dip a similar piece of cloth in a solution of aluminum acetate and dry it. Then soak it in the cochineal or indigo solution and dry it. Try to wash out its color. EXPERIMENT 179. Alums. Weigh out to a decigram quantities of aluminum sulfate, A1 2 (SO 4 ) 3 -(- i8H 2 O, and potassium sulfate, K 2 SO 4 , in the ratio of their molecular weights, i. e. 770 : 137. Fifteen grams of the first salt to 3 grams of the last are good working quan- tities. Dissolve each in the smallest possible quantity of boiling water in a test tube. Mix the two solutions hot in an evaporating dish and set aside to cool and crys- tallize. Note taste and form of crystals, Mix equal volumes of solutions of aluminum sul- fate and ammonium sulfate saturated at the boiling temperature. Set aside to crystallize. The product is ammonium alum. NOTE. Large crystals may be obtained by hanging a thread or string in the solution. EXPERIMENT 180. Reactions of Aluminum Com- pounds. Add a dilute solution of sodium carbonate to a dilute solution of alum. Filter the precipitate and wash it thoroughly. Transfer to a test tube, cover it with water, and add -hydrochloric acid. If the precipi- tate is a carbonate, there will be effervescence. Add ammonium sulfid solution to a solution of alum. Filter and wash the precipitate and, placing it in a test tube, add hydrochloric acid. If the precipitate is a sulfid, hydrogen sulfid gas will be evolved. To some aluminum sulfate solution in a test tube add about one-fifth as much sodium hydroxid. Transfer 114 Elementary Chemistry about half of the precipitate of aluminum hydroxid, A1(OH) 3 , thus formed to another test tube, and add an excess of sodium hydroxid. Sodium aluminate is formed. Is it soluble ? To the other half of the pre- cipitate add dilute hydrochloric acid. Compare results with those obtained for zinc in Experiment 168. TIN EXPERIMENT 181. Physical Properties. Examine a stick of tin and a piece of tin foil, and note the physical properties of the metal. Bend a stick of tin when held close to the ear. What information does your sense of hearing give you in regard to tin ? EXPERIMENT 182. Crystallization of Tin. Hold- ing a piece of tinplate by means of tongs, heat it in a flame until the tin coating commences to melt. Then immediately plunge it into cold water. Rub it over with a piece of filter paper wet with dilute aqua regia, then with paper wet with a solution of a caustic alkali. Note the crystalline figures brought out by the action of the solvents. EXPERIMENT 183. Action of Acids on Tin. Fill the rounded end of a test tube with granulated tin, and add enough concentrated hydrochloric acid to fill the test tube about a sixth full. Heat gently (in the hood) until effervescence commences and regulate the heat- ing so as to cause the hydrogen to be given off rapidly. When the action is about at an end, fill the test tube full of water, and save the solution of stannous chlorid thus formed for Experiments 184, 185, and 186. Put a small piece of tin in a test tube and add a little concen- trated nitric acid. As soon as the reaction begins set the tube in a bottle in the hood. The white product is metastannic acid. Heat a little tin with strong sulfuric acid in a test tube. Result ? Experiments 1 1 5 EXPERIMENT 184. Preparation of a Solution of Stannic Chlorid. Fill a small test tube about a sixth full of the stannous chlorid solution prepared in Experi- ment 183, and add a little aqua regia, or add bromin in small portions until its color ceases to be discharged, and boil to expel the excess of acid or bromin. What is the action of the aqua regia or the bromin ? Preserve the solution for use in Experiment 185. EXPERIMENT 185. Distinction Between Stannous and Stannic Salts, (a] To a little of the stannous chlorid solution prepared in Experiment 183 add a few drops of mercuric chlorid solution. Note the white precipitate of mercurous chlorid, HgCl. Add more of the mercuric solution and heat gently. The gray tinge imparted to the precipitate is due to mercury resulting from the reduction of the mercurous chlorid. (b) Add a few drops of mercuric chlorid solution to some of the stannic chlorid solution prepared in Experiment 184. What is the result? (c) Saturate with hydrogen sulfid (i) a little of the stannous chlorid solution, and (2) of the stannic chlorid solution, and compare results. (it) Neutralize the contents of each of the test tubes with ammonium hydroxid and add yellow ammo- nium sulfid. Shake up the mixtures in each case and compare results. Take fresh portions of the solutions of stannous and stannic chlorid, and add to each sodium hydroxid solution, a drop or two at a time. EXPERIMENT 186. Replacement of Tin by Zinc. Fill a test tube about one-fourth full of the stannous chlorid solution prepared in Experiment 183, and fill up with water. Put a narrow strip of sheet zinc in this diluted solution and examine after a little while. What is the appearance of the zinc ? 9 1 1 6 Elementary Chemistry EXPERIMENT 187. (Quantitative.'] (Hood.) To Determine the Equivalent of Tin. Weigh about 5.00^- of tin foil in an evaporating dish. Put most of it on a piece of paper and moisten what is left in the dish with strong nitric acid. When the action slackens, put a little more foil into the dish and then a little more acid. Use as little acid as possible, but be sure that all the tin is attacked and that there is no loss of metal from spattering. Cautiously evaporate to dryness with free flame, and finally heat as hot as possible for at least ten minutes. Weigh when it is cool, and after moistening with the acid heat again ; continue in this way until the weight remains practically unchanged. The product is a compound of oxygen. Taking the equivalent of oxygen as 7.94, calculate that of tin. If tin is quadrivalent in this compound, what is its atomic weight ? The specific heat of tin is 0.056 ; what is its atomic weight as deduced by Dulong and Petit's Rule ? LEAD EXPERIMENT 188. Physical Properties of Lead. Examine as many different samples of lead as possible. Cut a piece of lead with a knife and note appearance of freshly cut surface. EXPERIMENT 189. Deposition of Lead by Zinc. Fill a test tube nearly full of a solution of lead acetate (about 10 per cent) and put in it a narrow strip of sheet zinc. Examine after an hour or so. Pour off a little of the solution and test it for zinc. To remove the lead that may still be present add dilute sulfuric acid to the solution. As lead sulfate is not wholly insoluble in water, add an equal bulk of alcohol, in which the sulfate is quite insoluble. Filter off the lead sulfate, neutralize the filtrate with ammo- nium hydroxid, and add ammonium sulfid ; a white pre- cipitate of zinc sulfid results. In case all the lead has Experiments 117 not been removed from solution by sulfuric acid, the precipitate caused by ammonium sulfid will not be white, but more or less of a blackish color, depending tipon the amount of lead sulfid also precipitated. Hy- drogen sulfid is a better precipitant of lead than sulfuric acid, and it is possible to remove all the lead by its use. Acidify the solution with hydrochloric acid, pass hydro- gen sulfid through it, filter, and add ammonium hydroxid and then ammonium sulfid. EXPERIMENT 190. Action of Acids on Lead. Scrape three small pieces of lead bright and clean, place them in test tubes and cover with (i) nitric, (2) hydrochloric, and (3) sulfuric acid. If no action takes place promptly, heat to boiling. Note the nature of any gaseous products and change in the appearance of the lead. If the lead dissolves in any of the acids, let the action continue to completion, pour out the solution into an evaporating dish, and set aside to crystallize. EXPERIMENT 191. Preparation and Properties of Lead Monoxid. Heat on charcoal in the oxidizing flame of a blowpipe a very small bit of lead, and note any vapors and incrustation formed on the charcoal. Examine some litharge as to its physical properties and test its solubility in nitric, acetic, sulfuric, and hydro- chloric acids, both cold and hot. EXPERIMENT 192. Preparation and Properties of Red Lead. Mix about 2&- (2 cm - circle) of lead mon- oxid with about 0.5^- (2 cm - circle) of powdered potas- sium chlorate or nitrate, and heat the mixture in an iron spoon or dish. Note the physical properties of the product and compare it with other samples of red lead. Ascertain in what common acids red lead is soluble. EXPERIMENT 193. Preparation and Properties of Lead Dioxid. Place about 2 s- (2 cm - circle) of red lead in a test tube, add some dilute nitric acid, and heat to iiS Elementary Chemistry boiling for several minutes. Filter and wash the brown residue. Put a little of it in a test tube, add concen- trated hydrochloric acid, and heat gently. What gas is evolved ? What other peroxid behaves with hydro- chloric acid in a similar manner? EXPERIMENT 194. Reactions of Lead Salts. Put a little dilute solution of lead nitrate or acetate in six separate test tubes and add to one of each the follow- ing reagents, noting the nature of the precipitates : (1) Hydrogen sulfid. (2) Hydrochloric acid. Add several times as much water and heat to boiling. What change ? Cool by holding test tube in running^ water. What is the nature of the product ? (3) Sulfuric acid. (4) Potassium iodid solution. (5) Potassium dichromate solution. (6) Sodium hydroxid solution gradually and in small portions until in excess. EXPERIMENT 195. Action of Water on Lead. Fill a flask half full of water and bubble the breath through it for some time so as to charge the water with carbon dioxid. Scrape a piece of lead bright and clean, put it in the flask, cork, and let stand for a day or so. Then test portions of the water for lead by Experiment 189. If no lead is found to be present, let the lead act on the water for a day or so longer, or evaporate off most of the water and test again. Bear in mind that the lead which has dissolved may be so slight that the precipitate of lead sulfid may be so minute as merely to tinge the liquid brown. COPPER EXPERIMENT 196. Properties of Copper. Examine as many different forms of copper as are procurable ; note their most prominent characteristics. File a piece Experiments 119 of copper wire bright and heat it red hot. What is the black coating? Compare with Experiments 22 and no. EXPERIMENT 197. Precipitate of Copper. Hang a strip of zinc (scraped clean) in a neutral solution of copper sulfate ; also in another test tube containing copper sulfate solution suspend an iron nail filed bright. What soon occurs ? EXPERIMENT 198. Preparation and Properties of Cuprous Oxid. Dissolve 2 & of copper sulfate in 30 c - c - of water and add 10^- of Rochelle salt (sodium potas- sium tartrate) previously dissolved in 20 c - c - of water. Warm and filter. To the filtrate add IQC.C. o f a dilute solution of grape sugar, and then enough sodium hydroxid solution to dissolve any precipitate, and as much again, so as to make the solution strongly alka- lin. Boil gently until a decided change occurs. Filter off the cuprous oxid, Cu 2 O, formed, dry it, and compare with cupric oxid, CuO. EXPERIMENT 199. Reactions of Copper Salts. To a little copper sulfate add ammonium hydroxid in excess. Then repeat with sodium hydroxid instead of ammo- nium hydroxid. Heat a solution of copper sulfate to boiling and add sodium hydroxid. This precipitate is cupric oxid, CuO. Review Experiment 136 for the action of hydrogen sulfid on solutions of copper salts. Review Experiment 37 for water of crystallization in copper sulfate crystals. Dip a copper or platinum wire into copper sulfate solution, then take it out and heat it in a Bunsen flame; note the color imparted. EXPERIMENT 200. (Quantitative.) To Find the Equivalent of Copper. Clean some copper foil or wire with emery paper so that it is bright, and weigh to centigrams 3^- of it. Place the weighed copper in a I2O Elementary Chemistry small flask, barely cover it with water, and add concen- trated nitric acid in small portions, allowing plenty of time for the action to cease before adding a fresh por- tion. When solution is complete, transfer the liquid to a weighed evaporating dish, being careful not to lose any, and rinse out the flask two or three times with ^c.c. O f W ater, adding the rinsings to the dish. Cautiously evaporate to dryncss. The blue com- pound is copper nitrate, Cu(NO 3 ) 2 , which, when heated to a high temperature, decomposes into nitric oxid, oxy- gen, and copper oxid, CuO. Heat for at least ten min- utes as hot as possible even after the decomposition has seemed complete and then weigh the copper oxid. Heat again and so on to constant weight. The equivalent of oxygen is 7.94; find that of copper. Copper is bivalent in this compound. What then is its atomic weight ? SILVER EXPERIMENT 201. Preparation and Properties of Silver. I. Fill an evaporating dish a third full of sil- ver nitrate solution, and introduce a few globules of mercury. Set the dish aside in a safe place for a couple of days. The silver will then be found forming little crystals, usually attached to the mercury. Remove them with steel forceps and, after washing them well, put them in a bottle labeled " Silver." II. Pour concentrated nitric acid over a ten-cent piece in an evaporating dish or beaker, and when the action slackens, add more acid. Toward the last, heat may be applied. Add three or four times its volume of water and then hydrochloric acid until all the silver is removed as silver chlorid, AgCl. Let this precipitate settle and wash by clecantation several times. Then filter and wash free from an acid reaction. Divide it into two equal parts with a knife or spatula. Experiments \ 2 1 Place one part in a dish, cover with dilute sulfuric acid, and add a piece of zinc. The silver which collects as a gray powder is to be separated from the zinc, washed and dried. It is then to be placed in a hollow excavation in a piece of charcoal and heated with a blowpipe until it fuses into a globule. Place the second part in a cavity in a piece of char- coal, cover it with sodium carbonate, and reduce it with a blowpipe flame. Scrape the minute globules together and fuse them together into a single bead. EXPERIMENT 202. Reactions of Silver Salts, (a) Add a soluble chlorid solution, such as HC1 or NaCl, to a solution of silver nitrate. Boil, filter, and expose the silver chlorid to sunlight. Result ? (b) Add a potassium bromid solution to a solution of silver nitrate. Heat to boiling, filter, and separate the precipitate into two parts. To one add sodium thiosulfate solution, Na 2 S 2 O 3 . Result? Expose the other half to light. Result ? (c) Add potassium iodid solution to silver nitrate solution. Compare the properties of the precipitate with those of silver chlorid and bromid obtained in (a) and (b). IRON EXPERIMENT 203. Properties of Iron. Examine as many different forms as possible of the varieties of iron, note their most obvious physical properties, and try the action of a magnet on each. Which becomes permanently magnetized ? Introduce a pinch of iron powder into a Bunsen flame. What happens ? Review Experiments 7, I. (;/*); 25, 27, 28, and 51. To get "clean" ferrous reactions the ferrous solution must not be given a chance to oxidize. If the hydro- chloric acid solution be poured directly from the test tube while hydrogen is still being evolved, there is no 122 Elementary Chemistry danger of any ferric chlorid being present. Solutions of ferrous sulfate prepared from the crystals nearly always oxidize a little so that the true ferrous reaction is obscured by the ferric reaction. EXPERIMENT 204. Reactions of Ferrous Salts. Fill a test tube about a fifth full of iron (filings or small brads), add enough dilute hydrochloric acid to fill the test tube nearly half full, and warm, if necessary, to start the reaction. By appropriate tests identify the gas given off. Ferrous chlorid is formed in solution. (a) As soon as the action has almost ceased, pour a little of the solution into some sodium or ammonium hydroxid solution. Note the changes of color in the precipitate of ferrous hydroxid produced. To what are they due ? (l>) Add a little of the ferrous chlorid solution to a solution of potassium ferricyanid, and note nature of the precipitate of ferrous ferricyanid (Turnbull's blue). (<r) Add a third portion of the chlorid to potassium ferrocyanid solution. Result ? (d) Add a fourth portion to potassium sulfocya- nate solution, KCNS. Result ? Save what ferrous chlorid is left for Experiment 205. EXPERIMENT 205. Reactions of Ferric Salts. Add more hydrochloric acid to the iron used in Experiment 204 and, after the reaction has almost ceased, filter the solution into a beaker and add 2 c - c - of concentrated nitric acid. Boil for a few minutes and note any change of color. The solution now contains ferric chlorid as well as ferric nitrate. To ascertain whether the conversion of the ferrous into the ferric state is complete or not, put a few drops in a test tube and add a little potassium ferrocyanid. If a blue precipitate is formed, add one cubic centimeter more nitric acid and boil again. Put a little of this ferric Experiments 123 solution into each of four test tubes and add the four reagents used in Experiment 204. Tabulate the results of Experiments 204 and 205 as follows : Ferrous Salt Ferric Salt REAGENT Precipitate or Solution Color Precipitate or Solution Color NaOH .. . K 3 Fe(CN) 6 __ K 4 Fe(CN) R KCNS.... How may a ferrous salt be distinguished from a ferric ? EXPERIMENT 206. Oxidation of Ferrous Salts. Place a clear crystal or so of ferrous sulfate in a test tube and fill the tube half full of water. Shake the tube until the crystal has dissolved. (a] Put half of the solution into another test tube, add a little hydrochloric acid, warm somewhat, and add a few crystals of potassium chlorate. Heat to boiling and test for a ferric and a ferrous salt. (b) To the rest of the ferrous sulfate solution add a little sulfuric acid, heat to boiling, then run in drop by drop an equal volume of concentrated nitric acid and boil for a few minutes. Test portions of the result- ing solution for the presence of ferric and ferrous salts. EXPERIMENT 207. Reduction of Ferric Salts. To a solution of ferric chlorid add a little hydrochloric acid and drop in some iron so as to give a good evolu- tion of hydrogen. Add more acid, if necessary, to keep up the action for at least a quarter of an hour, then test a little of the solution for the presence of a ferrous compound. If the test is not decisive, continue the reduction until it is ; be sure that hydrogen is given off copiously. 124 Elementary Chemistry EXPERIMENT 208. Manufacture of Ink. Mix a strong solution of ferrous sulfate with a little of a solu- tion of powdered nutgalls. What is the color of the mixture ? Does it deepen on standing for a few min- utes ? Dip a pen into it and see how it writes. To a small portion of the ink add some oxalic acid solution. What good method does the result suggest in regard to removing ink stains ? EXPERIMENT 209. Borax Bead Test for Iron. Touch a hot borax bead (Experiment 164) to some iron compound so that a small portion is taken up by it, and heat in the oxidizing flame of a blowpipe until the bead is colored a decided^ yellow. Then heat it in the reducing flame until it becomes green. NICKEL EXPERIMENT 210. Reactions of Nickel Salts. Make the following tests on a dilute solution of nickel sulfate : (a) Add sodium hydroxid solution, a few drops at first, then an excess, and warm. (b) Add ammonium sulfid solution and see if the nickel sulfid precipitated is soluble in hydrochloric acid. (c) Perform the borax bead test in both the oxi- dizing and reducing flames. COBALT EXPERIMENT 211. Reactions of Cobalt Salts. Use a dilute solution of cobalt chlorid or nitrate, and add the reagents directed in Experiment 210. EXPERIMENT 212. Analysis of a Nickel Coin. Put a five-cent "nickel" in an evaporating dish, cover with nitric acid, and warm for a few minutes. Pour the solution into a beaker and dilute with an equal vol- ume of water. Add ammonium sulfid solution to this Experiments 1 2 5 solution until no more precipitate is formed. Filter (saving- the nitrate), wash the precipitate several times, pierce a hole in the apex of the filter paper, and wash the precipitate through with a little nitric acid into a test tube. Heat until it dissolves. What is the color of the solution, and the presence of what metal is indicated by this color ? To a little of the solution add ammonium hydroxid to alkalinity. What is the effect on the color of the solution ? What metals do these tests show to have been in the coin ? Evaporate the first filtrate nearly to dryness. What is the color of the concentrated solution ? The salts of what metal have this color ? Test the solution with a borax bead. What do you conclude ? What is the qualitative composition of a nickel coin ? CHROMIUM AND MANGANESE EXPERIMENT 213. Reactions of Chromic Salts. (a] Add a drop or so of sodium hydroxid solution to 2 c - c - of a solution of a chromic salt (chromic chlorid or chrome alum). The precipitate is chromic hydroxid Cr(OH) 3 . Add an excess of the sodium hydroxid solu- tion and shake. Then heat to boiling. Compare results with those obtained with zinc and aluminum. (b) Add a little and then an excess of ammonium sulfid to a chromic solution and compare the result with that in (a). Does chromium form a sulfid? Do aluminum and zinc ? EXPERIMENT 214. Borax Bead Test for Chrom- ium. Touch a borax bead to a bit of chromium alum and heat in both oxidizing and reducing flame of a blowpipe. The green coloration is very characteristic. EXPERIMENT 215. Reduction of Chromates to Chromic Compounds. To 10 c - c - of potassium dichro- inate solution add 2 c.c. each of concentrated hydrochloric 126 Elementary Chemistry acid and of alcohol, and warm gently. The chromate is reduced to chromic chlorid and the alcohol is oxi- dized to aldehyde. Note the green color characteristic of chromic compounds and the peculiar odor of the aldehyde. EXPERIMENT 216. Properties of Chromates. (a) Examine some crystals of potassium chromate and potassium dichromate. What is the color of their solu- tions ? (b) To a solution of potassium chromate add a little concentrated hydrochloric acid. The change of color shows that the chromate has been changed into the dichromate. (V) To a solution of potassium dichromate add potassium hydroxid drop by drop until the color changes to yellow, an indication of the formation of a chromate. (d) Place a little potassium dichromate in a test tube, cover with concentrated hydrochloric acid, and heat gently. What evidence is there that the acid is oxidized ? Repeat with potassium chromate. (e) To a solution of ferrous sulfate add a little hydrochloric acid and then drop by drop a solution of potassium dichromate. Test a portion of the solution for ferric salts by means of potassium sulfocyanid solution. EXPERIMENT 217. Reactions of Manganous Salts. (a) Add ammonium hydroxid to a manganous solution (sulfate or chlorid). The precipitate is manganous hydroxid, Mn(OH) 2 . (b) Add ammonium sulfid to a manganous solution. The precipitate is manganous sulfid, MnS. Divide it into two parts and add hydrochloric acid to one and acetic acid to the other, then add an excess of ammo- nium hydroxid to each. What are your conclusions regarding the solubility of manganese sulfid ? Experiments 127 EXPERIMENT 218. Borax Bead Test for Man- ganese. Put a little of any manganese compound in a borax bead and heat it in the oxidizing and in the reducing flame of a blowpipe ; note the color of the bead in each case. EXPERIMENT 219. Oxidation with Potassium Per- manganate. Mix with a solution of ferrous sulfate a few drops of sulfuric acid, and add, drop by drop, a solution of potassium permanganate. How can you show that the permanganate oxidizes the ferrous to the ferric salt ? Review Experiment 43. SOME ORGANIC COMPOUNDS EXPERIMENT 220. Preparation and Properties of Aldehydes. Formaldehyde. Put about 4 C - C - of methyl alcohol in a test tube and set the tube in a vertical position in a rack or bottle. Make a spiral of copper wire by winding it around a lead pencil, slip the spiral off, and, holding it with the tongs, heat it as hot as possible. Quickly drop the heated spiral into the methyl alcohol. The pungent odor produced is due to the formation of formaldehyde vapor. AcetaldeJiyde. To about 3^- of potassium dichro- mate solution in a test tube add a little concentrated hydrochloric acid and a few drops of ethyl alcohol. Heat gently. What does the change in color of the mixture indicate ? Acetaldehyde is formed by the oxi- dation of the alcohol, and the peculiar odor is due to acetaldehyde vapor which is given off. EXPERIMENT 221. Preparation and Properties of Ethyl Acetate. Mix about 2 C - C - of ethyl alcohol with an equal volume of dilute acetic acid in a test tube, and add a half dozen or so drops of concentrated sulfuric acid. Heat to boiling and note the odor of the ethyl acetate formed. 128 Elementary Chemistry EXPERIMENT 222. Preparation and Properties of Soap. Put loc^- 6 "- of a 10 to 12 per cent solution of sodium hydroxid in an iron or tinned dish. Add either 35^- of lard or 100^- of castor oil, and boil gently for about half an hour. Then add in small portions about 2$<?- of finely powdered salt, NaCl, and boil a few minutes after all the salt has been added. When the mixture is cool remove the soap formed. What reaction does your soap show when tested by litmus paper ? Add dilute sulfuric acid to a solution of part of your soap in distilled water until no more solid separates out. Remove the mixture of stearic and palmitic acids thus obtained and note its physical properties. Put 2 C - C - of your soap solution into two separate test tubes, and add to one a little magnesium sulfate solution and to the other a little calcium sulfate solu- tion. What occurs in each case, and what takes place on boiling the mixtures for a minute or so ? Saturate lime water with carbon dioxid as in Experiment 71 until a clear solution of acid calcium carbonate is obtained. Add a little to a soap solution and note what happens both before and after boiling the mixture. EXPERIMENT 223. Fehling's Test for Sugar. Dis- solve a little cane sugar in water, add a few drops of sulfuric acid, and boil gently for about five minutes so as to change the cane sugar into grape sugar. Mix 2 C - C - each of copper sulfate, Rochelle salt, and sodium hydroxid solutions in a test tube and heat to boiling. Add a few drops of the grape sugar solution and boil for three minutes. If no decided change occurs, add more sodium hydroxid and more grape sugar and boil again. The red substance obtained by the reducing action of the sugar on the copper sulfate precipitate obtained is cuprous oxid. Experiments 1 29 EXPERIMENT 224. Preparation and Properties of Oxalic Acid. Place 5^"- of cane sugar in an evaporat- ing dish, and add, in portions of about $ c - c -, 50^- f concentrated nitric acid previously diluted with a tenth of its volume of water. As the sugar reduces the nitric acid with evolution of the red fumes of nitrogen per- oxid, the operation should be conducted in the hood. Evaporate on a water bath until the volume of the liquid is less than lo^-. When the solution cools, crys- tals of oxalic acid separate out. Wash these crystals with a little water and note their physical properties. Do not taste the acid, however, as it is poisonous. Dissolve a crystal of potassium permanganate in a test tube a third full of water, and add half as much diluted sulfuric acid. Add a few drops of this solution to a solution of oxalic acid. Note the change in color. Add a drop of ink to a solution of oxalic acid. Result ? EXPERIMENT 225. Preparation and Properties of Nitrobenzene. Pour 15 c - c - of concentrated nitric acid into a flask (250 c - c -) and add an equal volume of con- centrated sulfuric acid. Cool the mixture by holding the flask so that tap water may flow around its sides. Add, a few drops at a time, io c - c - of benzene, shaking well and cooling the mixture thoroughly after each addition. Pour the product into a bottle (1,000 to 1,500 c - c -) previously filled with cold water. The oily liquid which sinks to the bottom is nitrobenzene. Wash the nitrobenzene free from acid by running a current of water into the bottle for some time, decant as much of the water as possible, and then pour the oil and the remainder of the water upon a wet filter paper. When the water has drained off, place a test tube under the funnel, punch a hole in the apex of the filter paper, and catch the nitrobenzene. 130 Elementary Chemistry To remove the water which is mixed with the oil put a few pieces of fused calcium chlorid in the test tube and let stand for several hours. Note the physical properties of the nitrobenzene. EXPERIMENT 226. Preparation and Properties of Aniline. Put 10^- of nitrobenzene in a flask (250^-), add 20 c - c - of water and 15^"- of fine iron filings. Shake well together and add 2 c - c - of concentrated hydrochloric acid. Hold the flask in the hand and move it around in a small Bunsen flame so as to keep the contents well agitated. If the effervescence becomes too violent remove the flask from the flame, and, if needs be, cool it by immersion in water. Continue the heating until the odor of nitrobenzene has disappeared or is very faint. If the effervescence ceases, add a little more acid. Now add enough 10 per cent solution of sodium hydroxid to make the mixture strongly alkalin (litmus), shake well, let settle for some time, and then decant into a bottle. Clean the flask out (using concentrated hydrochloric acid, if necessary), and decant from the bottle into the flask. Connect the flask with a con- denser and distil until the distillate no longer has a milky appearance. The aniline distils with the steam and on standing for some time settles out as an almost colorless oil which is heavier than water. Note its physical properties. APPENDIXES APPENDIX A QUALITATIVE ANALYSIS INTRODUCTORY Qualitative chemical analysis has to do with the operations and methods which are employed in finding out what elements and radicals are contained in a substance or mixture of substances. Qualitative analysis consists mainly of the study of the solu- bilities of substances. In the usual scheme of analysis the sub- stance to be analyzed is first brought into solution. A solution of a known compound (a reagent) is then added to this solution, and if a precipitate of certain properties is formed, a definite conclusion may be drawn as to the presence of certain elements or radicals in the original substance taken. Other known solutions are added to the filtrate from this precipitate, and from the formation of additional precipitates and observation of their properties further conclusions can be drawn as to the composition of the original substance The solubilities of certain salts of the commoner metals permit of their classification into five groups, which are usually given the name of the reagent which is added to effect the precipitation. These groups are: Precipitated as sulfids, PbS, HgS, CuS, CdS, Bi 2 S 3 ,SnS or SnS 2 , Sb 2 S 3 , or Sb 2 S 5 , As 2 S 3 or As 2 S 5 , by hydrogen sulfid. The last three are soluble in yellow ammonium sulfid, the others not. f Lead ] Mercury (tc salts) II. Hydrogen Sulfid Group Copper Cadmium Bismuth Tin Antimony A lb Arsenic [i] 11 Elementary Chemistry Aluminum 1 Chromium III. Ammonium Sulfid Grout? Iron Cobalt Nickel Manganese Zinc tated as hydroxids, A1(OH) 3 , Cr(OH) 3 , Fe(OH) 8 , by am- monium hydroxid. The last four are precipitated as sul- fids, CoS, NiS, MnS, ZnS, by j ammonium sulfid. IV. Ammonium Carbonate Group Calcium 1 Precipitated as carbonates, Strontium CaCO 3 , SrCO 3 , BaCO 3 , Barium MgCO 3 (soluble in NH 4 C1), Magnesium J by ammonium carbonate. V. Alkali Metals f Lithium I Sodium I Potassium I Ammonj,um Not precipitated by any com- mon reagents. I. HYDROCHLORIC ACID GROUP METHOD OF ANALYSIS Add HC1 a little at a time to the solution as long as a precipi- tate (ptt.) is formed. Shake up well, filter, and wash twice with a little cold water. Punch a hole in the apex of the filter paper and wash the precipitate into a beaker. Boil the water and filter while hot. Residue: AgCl, HgCl. Wash with hot water and twice pour over it enough Residue: Filtrate : Hg-NH 2 -Cl and Hg. AgCl-2NH 8 Acidify with A black resi- HNO 3 ; a white due proves the ptt. proves the presence of mer- presence of cury. silver. Filtrate: PbCl 2 Divide into two portions. PORTION I. Add K 2 Cr.,O 7 or K 2 CrO 4 ; a yellow ptt. soluble in NaOH indicates the pres- ence of lead. PORTION II. Add KI ; a yel- low ptt. soluble in hot water and recrystallizing in plates on cooling proves the presence of lead. Qualitative Analysis iii REACTIONS OF SOLUTIONS OF SILVER, LEAD, AND MERCUROUS SALTS SILVER HC1 precipitates AgCl, white, curdy, changing on exposure to the light from lavender to black ; soluble in NH 4 OH, forming AgCl 2NH 3 , from which solution HNO 3 reprecipitates AgCl. LEAD HC1 precipitates PbCl 2 , white, flocculent, soluble in hot water, crystallizing in long needles when solution cools. H 2 SO 4 precipitates PbSO 4 , white. K 2 Cr 2 O 7 or K 2 CrO 4 precipitates PbCrO 4 , yellow, soluble in NaOH. Kl precipitates PbI 2 , yellow, soluble in hot water, from which when cold it crystallizes in shining plates. H 2 S precipitates PbS, black, changed by hot and moderately MERCURY HC1 precipitates HgCl, white, changed by NH 4 OH into a black mixture of HgNH,Cl and Hg. II. HYDROGEN SULFID GROUP METHOD OF ANALYSIS Warm the nitrate from the Hydrochloric Acid Group and pass a current of hydrogen sulfid through it. Make sure that precipi- tation is complete by filtering a small portion, diluting the nitrate, and treating it with H 2 S a few minutes. Filter and wash thoroughly with hot water. Put a small portion of the precipitate in an evaporating dish ; add a little ammonium polysulfid. If this precipitate dissolves completely, Division A is absent ; if not, treat the remainder of the precipitate with ammonium polysulfid and warm (not boil} for about three minutes with occasional stirring. Filter while hot and proceed as indicated in table for Division A. IV Elementary Chemistry DIVISION A Boil the precipitate in an evaporating dish with a small amount of a mixture of equal volumes of strong nitric acid and water until brown fumes cease to be given off freely. Dilute with a little water and filter. Filtrate : Lead, Bismuth, Copper, Cadmium Salts. Add a little strong H 2 SO 4 and evaporate with care until dense white fumes appear. Add an equal volume of dilute H 2 SO 4 and filter. Boil with a very little Filtrate : Residue: aqua regia. Bismuth, Copper, Cadmium Salts. PbS0 4 Filter, boil the filtrate Add NH 4 OH until strongly alkalin. Wash, until chlo- A deep blue solution proves^the pres- warm the rin is ex- ence of copper. A white ptt. indicates bismuth. Filter and wash. ptt. with ammonium pelled, then add SnCU acetate and warm. Fil Copper, Ca If copper is absent : trate : dmium Salts. If copper is present : Precipitate Bi (OH) a or basic salt of bismuth. and a few drops of HC 2 H 3 2 and filter. To the fil- A gray or black ptt. proves the presence of mercury. Make slight- ly acid with Acidify with dil. HC1 and Add two or three trate add K 2 Cr0 4 or dil. HCland precipitate drops of K 2 Cr 2 O 7 . treat with with H 2 S. HC1 to the A yellow H 2 S. Filter and ptt. in the ptt. soluble A yellow boil the ptt. funnel and in NaOH ptt. proves the pres- immediately with dilute allow the filtrate to proves the presence of ence of cad- H 2 S0 4 . Fil- drop into a lead. mium. ter, rejecting beaker of the residue. water. Dilute the A white colorless fil- ptt. proves trate with an the pres- equal volume ence of bis- of water and muth. treat with H 2 S. A yellow ptt. proves the presence of cadmium. Residue: Mercuric Salt. Qualitative Analysis v REACTIONS OF SOLUTIONS OF MERCURIC, CUPRIC, CADMIUM, AND BISMUTH SALTS MERCURY II 2 S precipitates HgS, black, insoluble in hot and concentrated HNO 3 , but changed by prolonged action of that reagent into Hg(NO 3 ) 2 - 2 HgS, white and insoluble in concentrated HNO 3 . Both Hg(NO 3 ) 2 * 2 HgS and HgS are changed by aqua regia into sulfur and HgCl 2 , which is soluble. HgS is insoluble in (NH 4 ) 2 S. SnCl 2 reduces HgCl 2 to HgCl, white. An excess of SnCl 2 reduces the HgCl more or less to mercury, which gives the HgCl a darker color. COPPER H 2 S precipitates CuS, black, changed by hot and concentrated HNO 3 into sulfur and Cu(NO 3 ) 2 , which is soluble. CuS is insol- uble in dilute H 2 SO 4 . CuS is slightly soluble in (NH 4 ) 2 S. NH 4 OH precipitates light blue basic salts, readily soluble in excess, producing deep blue solutions of ammonia cupric salts, as CuSO 2 -4NH 3 . CADMIUM H 2 S precipitates CdS, varying in color from light yellow to orange according to the conditions under which precipitation takes place; easily soluble in concentrated HC1 or in hot and dilute H,SO 4 ; changed by hot and concentrated HNO 3 into sulfur and Cd(NO 3 ) 2 , which is soluble. CdS is insoluble in (NH 4 ) 2 S. NH 4 OH precipitates Cd(OH) 2 , white, readily soluble in excess, producing ammonia cadmium salts, as Cd(NO 3 ) 2 ' 4NH 3 . BISMUTH H 2 S precipitates Bi 2 S 3 , dark brown ; changed by hot and con- centrated HNO 3 into sulfur and Bi(NO 3 ) 3 , which is soluble. Bi 2 S 3 is insoluble in (NH 4 ) 2 S. H 4 O added in large proportion to solutions of bismuth salts which do not contain too much acid, precipitates basic salts, as BiOCl, (BiO) 2 SO 4 , BiONO 3 , etc. NH 4 OH precipitates Bi(OH) 3 or a basic salt, white ; insoluble in excess ; soluble in dilute HC1. Elementary Chemistry DIVISION B Slightly acidify the ammonium sulfid solution with HC1. [If the precipitate is white it is probably only sulfur.] Filter, reject- ing the filtrate, as it contains no metals, transfer the precipitate to a beaker, add a little concentrated HC1, heat to boiling for a few minutes, and filter. Filtrate: Tin, Antimony salts. Place a bright iron wire or nail in the filtrate, warm gently, let stand for fifteen minutes, and then filter. Filtrate : SnCl 2 Add HgCl 2 . A white ptt. get- ting gray when more of HgCl 2 is added and heat applied, proves presence of tin. Precipitate: Antimony (in metallic state). Wash thoroughly and transfer to a beaker. Dis- solve in a little cone. HC1 to which a few drops of cone. HNO 3 has been added. Evaporate nearly to dryness ; then add a large proportion of water. The formation of a white ptt. proves the presence of antimony. [Proof may be confirmed by passing H 2 S into solu- tion with formation of orange ptt.] Residue: Arsenic Sulfids. Dissolve in hot, cone. HN0 3 . Add a little of the solu- tion to a test tube nearly half full of a solution of ammo- nium molybdate, and warm gently. A yellow crystal- line ptt. proves the presence of arsenic. Also try the special tests. REACTIONS OF SOLUTIONS OF TIN, ANTIMONY, AND ARSENIC SALTS TIN (Stannous) H 2 S precipitates SnS, dark brown ; soluble in warm concen- trated HC1 ; soluble in (NH 4 ) 2 S, forming sulfo-stannates, as (NH 4 ) 2 SnS 3 , from which a dilute acid precipitates SnS 2 , yellow. HgCl 2 is reduced by SnCl 2 in HC1 solution to HgCl, white; an excess of SnCl 2 reduces some of the HgCl to mercury, which imparts a darker color to the precipitate. TIN (Stannic) H 2 S precipitates SnS 2 , yellow, from solutions not containing too much HC1 ; soluble in warm concentrated HC1 ; soluble in (NH 4 ) 2 S, forming sulfo-stannates, as (NH 4 ) 2 SnS 3 . Qualitative Analysis vii ANTIMONY (pus) H 2 S precipitates Sb 2 S 3 , orange red ; soluble in warm, concen- trated HC1 ; oxidized by hot, concentrated HNO 3 , forming sulfur and H 3 SbO 4 , which is soluble. Sb 2 S 3 is soluble in (NH 4 ) 2 S ; forming sulfo-antimonates, as (NH 4 ) 3 SbS <l , from which dilute acids precipitate Sb 2 S 5 , orange red. When SbCl 3 is added to a large proportion of water, SbOCl, white, is produced, which is changed directly to Sb 2 S 3 when treated with H 2 S. ANTIMONY (fc) H 2 S precipitates Sb 2 S 5 , orange red, and resembling Sb 2 S 3 in its behavior toward most reagents. ARSENIC (ous) H 2 S precipitates As 2 S 3 , lemon yellow; almost insoluble in warm, concentrated HC1 ; oxidized by hot concentrated HNO 3 to H 3 AsO 4 , which is soluble, sulfur being set free. As 2 S 3 is soluble in (NH 4 ) 2 S, forming sulfo-arsenates, as (NH 4 ) 3 AsS 4 , from which HC1 precipitates As 2 S 5 . ARSENIC (tc) H 2 S precipitates As 2 S 5 , lemon yellow, and resembling As 2 S 3 in its behavior toward most reagents. The precipitation takes place slowly and is more complete if the solution is warm, when H 2 S reduces the arsenic solution to the arsenious condition and As 2 S 3 is precipitated. (NH 4 ) 2 MoO 4 , ammonium molybdate, added in excess to a solution of arsenic acid containing HNO 3 precipitates ammonium arseno-molybdate, yellow. Precipitation is best obtained by adding the arsenic solution to a small test tube half full of (NH 4 ) 2 MoO 4 . The mixture should then be warmed, but should not be heated above 70, lest MoO 3 , white, be precipitated. III. AMMONIUM SULFID GROUP METHOD OF ANALYSIS Add NH 4 OH to slight alkalinity, heat to boiling, then add (NH 4 ) 2 S in slight excess ; heat again to boiling and allow the precipitate to settle. Filter and wash thoroughly with hot water. Without delay treat the precipitate in an evaporating dish with a mixture of equal volumes of strong HC1 and water, stirring well. Filter and wash immediately. Vlll Elementary Chemistry Residue: Nickel, Cobalt Sul- Filtrate: Iron, Aluminum, Chromium, Zinc, Manganese Chlorids. rids. Expel any H 2 S which may be present by Test with borax boiling and divide into two unequal portions. bead ; blue, cobalt ; PORTION I. Evaporate the smaller portion brown, nickel. to small bulk, add a little chlorin w r ater, To detect one of and boil until excess of chlorin is' expelled. these metals in the To the cooled solution add KCNS. A red presence of the other, color proves the presence of iron. dissolve the residue PORTION II. To the larger portion add in a little aqua regia. Filter and evaporate a little cone. HNO 3 and boil. Evaporate to small bulk. Nearly neutralize with to small bulk. Heat to boiling and add (NH 4 ),CO 3 , and, transferring the solution to a flask, add five times its volume of sus- an equal bulk of bro- min water and then pended BaCO 3 . Shake the flask vigorously from time to time for half an hour and then of NaOH. Boil vig- filter. orously and add a little bromin water from time to time. Precipitate: Filtrate: Zinc, Wash thoroughly Chromium, Aluminum, Manganese Salts. with boiling water Iron Hydroxids. PORTION I. Add by decantation, filter and boil the ptt. with NH 4 OH and NH 4 C1 PORTION I. Fuse on platinum foil with Na 2 CO 3 andKNO 3 . A HC 2 H 3 O 2 and then H 2 S . A white ptt. soluble and filter. yellow product indicates in HC1 proves the the presence of chro- presence ot %ittc* Residue: Filtrate: mium. Dissolve in PORTION II. Put Cobalt Nickel. water and make acid a very little in an [Co(OH) 3 ] Test with borax bead. Treat withH 2 S A black ptt. indi- with HC 2 H 3 O 2 . A red ptt. with AgNO 3 and a yellow ptt. with Pb(C 2 H 3 O 2 ) 2 proves the presence of chro- evaporating dish, add 1 cubic centi- meter of cone. H 2 SO 4 and heat until dense white cates the mium. fumes appear. presence PORTION II. Add an Transfer the cooled of nickel. equal bulk of solid contents of the v^onnrm Na 2 CO 3 , half as much dish to a test tube with bo- TO V Vlf^Q (\ Ba(OH) 2 , and 5 cubic half full of H 2 S0 4 , I tiX IJt-cUl. centimeters of water. add PbO 2 , heat to Boil two or three min- boiling and allow utes. Filter, and to the to stand until sus- filtrate add NH 4 C1 and pended matter set- boil for some time. A tles. A red or white ptt. , best seen purple colored so- against a dark back- lution proves the ground, proves the presence of man- presence of aluminum. ganese. Qualitative Analysis ix REACTIONS OF SOLUTIONS OF NICKEL, COBALT, IRON, MANGANESE, ZINC, ALUMINUM, AND CHROMIUM SALTS NICKEL NH 4 OH in small proportion precipitates Ni(OH) 2 , green; if in excess, greenish blue basic salts. The precipitates are soluble in NH 4 OH in the presence of ammonium salts. Both solutions and precipitates are changed by (NH 4 ) 2 S into NiS, black. KOH or NaOH precipitates Ni(OH) 2 , green ; insoluble in excess. Ni(OH) 2 is oxidized by boiling with bromin water and NaOH to Ni(OH) 3 , black ; when this is boiled with NH 4 OH and NH 4 C1 it dissolves. (NH 4 ) 2 S precipitates from neutral or alkalin solutions NiS, black; somewhat soluble in excess of (NH 4 ) 2 S, more readily in the presence of NH 4 OH, forming a dark brown .solution from which NiS is reprecipitated if the solvent is removed by boiling. NiS is insoluble in cold and not very dilute HC1 ; it is changed by aqua regia to free sulfur and NiCl 2 , which dissolves. NiS is oxidized by the oxygen of the air to NiSO 4 . A borax bead is colored brown when fused with a compound of nickel. COBALT NH 4 OH precipitates blue basic salts ; easily soluble in NH 4 OH in the presence of ammonium salts. Both precipitate and solution are changed by (NH.^S into CoS. KOH or NaOH precipitates from cold solutions a blue basic salt which, when warmed with the alkali, changes to Co(OH) 2 , pink. Co(OH) 2 is oxidized to Co(OH) 3 , black, by boiling with bromin water and NaOH. The Co(OH) 3 is not affected by boil- ing with NH 4 OH and NH 4 C1. (NH 4 ) 2 S precipitates from neutral or alkalin solutions CoS, black ; insoluble in excess ; practically insoluble in not very dilute HC1 ; attacked by aqua regia, forming sulfur and CoCl 2 , which dissolves. CoS is oxidized by the air to CoSO 4 . A borax bead is colored blue when fused with a compound of cobalt. IRON {Ferrous} NOTE. As ferrous salts oxidize very readily to ferric, it is only by taking special precautions that a solution of ferrous salt can x Elementary Chemistry be kept from oxidizing. The solution of FeSO 4 should be heated with iron filings and H 2 SO 4 , when the hydrogen will reduce any ferric salt to the ferrous condition. NH 4 OH in neutral solutions precipitates incompletely Fe(OH) 2 , which oxidizes promptly to compounds first green, then black, and finally reddish brown Fe(OH* 3 . When these precip- itates are treated with H 2 S they change into FeS, black. KOH or NaOH precipitates Fe(OH) 2 , white, but oxidizing as described above. (NH 4 ) 2 S precipitates FeS, black'; attacked by hot concentrated HNO 3 , forming sulfur and Fe(NO 3 ) 3 , which dissolves. FeS is soluble in dilute HC1, and on exposure to moist air oxidizes to FeSO 4 , and finally to a basic ferric sulfate which is brown. BaCO 3 , shaken with a cold, neutral, or slightly acid solution of FeCl 2 , does not precipitate a compound of iron. It is most con- venient to employ the BaCCXj suspended in water. KCNS, potassium sulfocyanate, produces no red coloration in solutions of ferrous salts. Concentrated HNO 3 , or chlorin water, oxidizes ferrous to ferric salts very promptly at the boiling temperature. IRON (Ferric} NH 4 OH, KOH, or NaOH, precipitates Fe(OH) 3 , reddish brown and gelatinous ; changed by (NH 4 ) 2 S into FeS, black. BaCO 3 , when shaken with a cold, neutral, or but slightly acid solution of a ferric salt, precipitates Fe(OH) 3 or a basic salt. KCNS, potassium sulfocyanate, in excess, forms with solutions of ferric salts a deep red complex soluble salt. H 2 S reduces acid solutions of ferric salts to the ferrous condi- tion with separation of sulfur. MANGANESE (pus) NH 4 OH, KOH, or NaOH, precipitates Mn(OH) 2 , white, oxi- dized quickly to dark brown compounds. The precipitate is changed to MnS by (NH 4 ) 2 S. (NH 4 ) 2 S precipitates MnS, pink, soluble in dilute acids ; when exposed to the air it turns brown. BaCO 3 , shaken with a cold, neutral, or slightly acid solution of MnCl 2 , does not precipitate a compound of manganese. Fusion with Na 2 CO 3 and KNO 3 oxidizes manganese com- pounds to green salts of manganic acid, K 2 MnO 4 and Na 2 MnO 4 . Qualitative Analysis xi PbO 2 , lead dioxid, boiled with H 2 SO 4 and a little of a man- ganese compound, oxidizes the latter to permanganic acid, HMnO 4 , which imparts a pink or purple color to the solution. If a chlorid or HC1 be present in any considerable quantity it must be removed by evaporating with concentrated H 2 SO 4 until dense fumes appear. ZINC NH 4 OH produces in neutral solutions a partial precipitation of Zn(OH) 2 , white and gelatinous ; soluble in ammonium salts producing double salts ; changed by (NH 4 ),S into ZnS. H 2 S precipitates ZnS, white, incompletely from neutral solu- tions of zinc salts of the inorganic acids ; it is soluble in most dilute acids, but is only slightly soluble in acetic acid, and wholly insoluble in a solution containing an alkalin acetate, as NaC 2 H 3 O 2 . (NH 4 ) 2 S precipitates ZnS, white. BaCO 3 , when shaken with a cold, neutral, or but slightly acid solution of ZnCl 2 , does not precipitate any compound of zinc. ALUMINUM NH 4 OH precipitates A1(OH) 3 , white, gelatinous; somewhat soluble in excess, the A1(OH) 3 being reprecipitated by heat. (NH 4 ) 2 S precipitates A1(OH) 3 , as the sulfid is decomposed by water. BaCO 3 , when shaken with a cold, neutral, or slightly acid solu- tion of A1C1 3 , precipitates A1(OH) 3 or basic carbonates. CHROMIUM NH 4 OH precipitates Cr(OH) 3 , green, gelatinous, difficultly soluble in excess and reprecipitated by boiling. (NH 4 ) 2 S precipitates Cr(OH) 3 . BaCO 3 , when shaken with a cold, neutral, or but slightly acid solution of CrCl 3 , precipitates Cr(OH) 3 or basic carbonates. Fusion with KNO 3 and Na 2 CO 3 oxidizes chromium compounds to K 2 CrO 4 and Na 2 CrO 4 , yellow. If the fused mass is dissolved in water and the solution acidified with acetic acid, the addition of lead acetate precipitates PbCrO 4 , yellow. Xll Elementary Chemistry IV. AMMONIUM CARBONATE GROUP (The Alkalin Earth Metals] METHOD OF ANALYSIS To the solution add NH 4 C1, NH 4 OH, and then (NH 4 ) 2 CO 3 . Warm, and if a precipitate appears, filter and wash. Precipitate: BaCO 3 , SrCO 3 , CaCO 3 Filtrate : Pour small portions of warm acetic acid upon the Mg. salt. ptt., avoiding an excess, until it is dissolved. To a AddNH 4 OH small portion of the solution add K 2 Cr 2 O 7 , and if a and ptt. appears add K 2 Cr 2 O 7 to all of the solution, and Na 2 HPO 4 . warm and filter. R u'b the Precipitate : Filtrate : inner surface of the test BaCrO 4 Sr(C 2 H 3 2 ) 2 , Ca(C 2 H 3 2 ) 2 tube with a glass rod. A Dissolve in HC1, warm Make alkalin with NH 4 OH, add (NH 4 ) 2 CO 3 and warm. Filter the crystalline ptt. proves the solution ptt. (if none appears, Sr and Ca are the presence and add a absent), wash thoroughly, and dis- of magne- few drops of solve on the filter with the least sium. H 2 S0 4 . A possible quantity of HC1. Evaporate white ptt. just to dryness, dissolve in a little (which, how- water, filter if not clear, and evapo- ever, may rate to small bulk. Divide into two appear yel- portions. low from the K 2 Cr 2 O 7 in the solution) PORTION I PORTION II proves the SrCl 2 CaCl 2 presence of Add a little Add a little barium. CaSO 4 , heat to K 2 SO 4 and heat to boiling, and if boiling. If a ptt. no ptt. appears forms, filter it off at once let stand and to the filtrate for at least ten add NH 4 OH till minutes. A fine alkalin, then white ptt. proves (NH 4 ) 2 C 2 O 4 and the presence of warm. A white strontium. ptt. proves the presence of cal- cium. Qualitative Analysis xiii REACTIONS OF SOLUTIONS OF BARIUM, STRONTIUM, CALCIUM, AND MAGNESIUM SALTS BARIUM Na 2 CO 3 or (NH 4 ) CO 3 precipitates from neutral or alkalin solutions BaCO 3 , white, flocculent at first, but becoming crystal- line when gently warmed. BaCO 3 is very slightly soluble in NH 4 C1; freely soluble in HC1 and acetic acid, HC 2 H 3 O 2 , with effervescence. H 2 SO 5 precipitates BaSO 4 , white, practically insoluble in water, acids, or alkalis. Na 2 CO 3 or(NH 4 ),CO 3 precipitates SrCO 3 , resembling BaCO 3 . STRONTIUM H 2 SO 4 precipitates SrSO 4 . Calcium sulfate, although but slightly soluble in water, is more soluble than SrSO 4 , so that CaSO 4 will precipitate SrSO 4 from a concentrated solution of a strontium salt. Precipitation is more complete when the mixture is warmed or when a concentrated solution of K 2 SO 4 is used instead of the CaSO 4 . K 2 CrO 4 or K 2 Cr 2 O 7 does not precipitate SrCrO 4 from dilute solutions acidified with HC 2 H 3 O 2 . CALCIUM Na 2 CO 3 or(NH 4 ) 2 CO 3 precipitates CaCO 3 , resembling BaCO 3 . K 2 CrO 4 or K 2 Cr 2 O 7 produces no precipitate in dilute solutions acidified with HC 2 H 3 O 2 , since CaCrO 4 is soluble in both water and HC 2 H 3 O 2 . (NH 4 ) 2 C 2 6 4 precipitates CaC 2 O 4 , white, crystalline. H 2 SO 4 or a soluble sulfate, as K 2 SO 4 , precipitates CaSO 4 only from concentrated solutions, and then but partially. MAGNESIUM NH 4 OH precipitates from neutral solutions containing no ammonium salts one-half of the magnesium as Mg(OH) 2 . The other half unites with the ammonium salt which is formed to produce double salts, such as MgCl 2 2NH 4 C1. These double salts are soluble in water and not precipitated by NH 4 OH or (NH 4 ) 2 CO 3 . The object of adding NH 4 C1 in the analysis is to form the double salt and thus prevent the precipitation of the magnesium. XIV Elementary Chemistry Na 2 HPO 4 or NaNH 4 HPO 4 precipitates from solutions of double salts, such as MgCl./ 2 NH 4 C1, in the presence of NH 4 OH, MgNH 4 PO 4 , white and crystalline. Crystallization may be hastened by stirring the solution with a glass rod. V, THE ALKALI METALS: AMMONIUM, SODIUM, POTASSIUM METHOD OF ANALYSIS Ammonia. Put a little of the original substance in a small beaker and add NaOH. Cover the beaker with a watch glass, on the under side of which is placed a moistened piece of red litmus paper. Heat gently, but not to boiling. If the litmus paper turns blue the presence of ammonia is proved. Sodium and Potassium. Evaporate the filtrate from the ammonium carbonate group to dryness and heat until no more fumes of ammonium salts are given off. Divide the residue into two portions. PORTION I. Sodium, Potas- sium Salts. Moisten a small portion with HC1, slip a clean platinum wire into it and introduce into the Bunsen flame. A yellow flame proves the presence of sodium ; a violet flame proves the pres- ence of potassium. If sodium is present, view the flame through a blue glass, whereby the yellow rays are cut off, but the violet allowed to pass. PORTION II. Potassium, So- dium Salts. Dissolve in least possible amount of water and divide solu- tion into two portions. PORTION I. Add platinum chlorid solution and keep under observation for some time. A yellow ptt. proves pres- ence of potas- sium. PORTION II. Add picric acid solution. A yel- low ptt. indi- cates presence of potassium. REACTIONS OF SOLUTIONS OF AMMONIUM, POTASSIUM, AND vSoDiUM SALTS When AMMONIA KOH or NaOH when warmed with an ammonium salt liberates ammonia, which turns moist red litmus paper blue. any ammonium salts are heated they break up into Qualitative Analysis xv volatile constituents so that through heat ammonia may be sepa- rated from non-volatile substances. SODIUM Flame test. A sodium salt introduced into a Bunsen flame on a platinum wire colors it an intense yellow. POTASSIUM Platinum chlorid, PtCl 4 , produces a yellow precipitate. Picric acid produces a yellow precipitate. Flame test. A potassium salt introduced into a Bunsen flame on a platinum wire colors it violet. As this color is marked by even a very small proportion of sodium, if that element is present, the flame should be observed through blue glass, which absorbs the yellow light. DETECTION OF ACIDS I. BARIUM CHLORID GROUP Sulfuric acid, H.,SO 4 , precipitates BaSO 4 , white, insoluble in HC1. In neutral solution phosphoric acid, H 3 PO 4 , precipitates Ba 3 PO 4 , white, soluble in HC1. Sulfurous acid, H 2 SO 3 , precipitates BaSO 3 , white, soluble in HC1 with evolution of SO., (odor). II. SILVER NITRATE GROUP Hydrochloric acid, HC1, precipitates AgCl ; white curds very soluble in NH 4 OH. Hydrobromic acid, HBr, precipitates AgBr, pale yellow, slowly soluble in NH 4 OH. Hydriodic acid, HI, precipitates Agl, yellow, very slightly soluble in NH 4 OH. III. SPECIAL TESTS FOR SOME COMMON ACIDS Carbonates. Most carbonates give up their carbon dioxid when acted upon by HC1 or HNO 3 . (See Experiment 67.) Sulfids. HC1 evolves H 2 S readily from the sulfids of the alkali and alkalin earth metals, and from sulfids of magnesium, manganese, zinc, and iron; less readily from those of lead, bis- muth, cadmium, antimony, tin, nickel, and cobalt ; from other sulfids with difficulty or not at all. x r /i Elementary Chemistry H 2 S blackens filter paper moistened with lead acetate solution. A sulfid, when fused with a small piece of solid NaOH on a crucible cover, forms Na 2 S, which, when moistened and placed on a silver coin, gives a black stain of Ag 2 S. Ace fates. Concentrated H.,SO 4 when warmed with an acetate liberates acetic acid, HC 2 H 3 O 2 , recognizable odor. (See also ethyl acetate, Experiment 221.) In neutral solution FeCl gives a dark red color to a solution of an acetate. Nitrates. (See Experiment 129.) APPENDIX B THE METRIC SYSTEM OF WEIGHTS AND MEASURES The metric system of weights and measures is employed in the affairs of everyday life in most of the countries of continental Europe, and is almost exclu- sively used in science. The fundamental unit is the meter, which is a unit of length a little over a yard long. The other units of length are derived from the meter by successively multiplying and dividing it by ten. The names of these derived units are indicated by prefixes. Thus, the multiple prefixes are the Greek words for ten, deca-, hundred, hecto-, and thousand, kilo-, and the sub- multiple prefixes are the Latin words for ten, deci-, hundred, centi-, and thousand, milli-. The unit of weight or mass is the gram, which is the weight of a cubic centimeter of water at 4. The same prefixes as are given above are used in expressing the names for the multiples and sub-multiples of the gram. The unit of volume is the liter, which is the volume occupied by 1,000 cubic centimeters (one cubic deci- meter of water); 1,000 grams (one kilogram) of water occupies one liter at 4. In this system fractions must always be expressed decimally, and only one unit should be employed in designating a quantity measured. Thus, the fractions %, y$, ^A, etc., are written 0.5, 0.33, 0.75, and so on. Also the weight of an object is not given as nine grams, four decigrams, and six centigrams, even when abbre- viated into 9^-, 4^-, and 6 ^-, but should be written 9.46^-. [ xvii ] 3h XV111 Elementary Chemistry The relations between the units, multiples, and sub- multiples of the metric system are shown in the TABLE OF THE METRIC SYSTEM Length Weight Volume Notation Kilometer Kilogram Kiloliter IOOO. Hectometer Hectogram Hectoliter IOO. Decameter _. Decagram Decaliter 10. METER GRAM LITER i . Decimeter Decigram Deciliter O. I Centimeter Centigram _ Centiliter . . O.OI Millimeter Milligram.. Milliliter O.OOI It is evident from the table that 10 millimeters equal one centimeter, 10 centimeters equal one decimeter, 10 decimeters equal one meter, 10 meters equal one hecto- meter, and 10 hectometers equal one kilometer. Anal- ogous statements are true for the units of weight and volume. The abbreviations most often used in this book are : cm. f or centimeter ; c - c - for cubic centimeter ; L for liter ; and # for gram. The relations of the weights and measures of the metric system to the weights and measures commonly used in English-speaking countries are shown by the TABLE OF METRIC EQUIVALENTS One meter 39-37 inches One kilometer 0.62 mile One centimeter o 39 inch One liter . i 06 liquid, quart One gram 15-43 grains One kilogram 2 2 pounds (Avoir.) One metric ton 2204 pounds One inch _ 2.54 centimeters One mile 1.61 kilometers One cubic inch 16.39 cubic centimeters One liquid quart 0-95 liter One pound (Avoir.) 0-45 kilogram One ounce 28.35 grams Onfi o-rflin fAnoth "k __ o . 06/18 eram APPENDIX C 100 INSTRUMENTS FOR WEIGHING AND MEASURING The Thermometer. The thermometer is an in- strument for measuring temperatures. Its action de- pends upon the fact that liquids expand when heated, and contract when cooled. The liquids in common use are mercury or alcohol ; water is not suitable, as it freezes at too high a temperature. Chemical thermometers (Fig. a) consist of a glass tube with minute bore, which is blown out into a bulb at the end. The bulb is almost invariably made cylindri- cal in shape so that the thermometer may be thrust through a cork closing a flask, test tube, or bottle, the tempera- ture of the interior of which is to be found. Details as to the making of ther- mometers cannot be gone into here, but brief mention may be made of the method employed in graduating the instrument. The bulb is placed in a dish filled with melting ice, and the position of the liquid in the stem marked on the glass. The instrument is then placed in steam issuing from water which is kept briskly boiling under a pressure of one atmos- phere. The liquid expands much more than does the glass and rises in the stem. This new position is also [xix] Fig. a THERMOMETERS XX Elementary Chemistry marked on the glass. The portion of the stem between the points thus fixed is divided into a certain number of equal parts, the number depending" upon what scale is adopted. The stem above and below these fixed points is likewise divided into parts which are equal to those between the two fixed points. In the Centigrade scale, which is in general use in continental Europe, and in almost exclusive use among scientists, the interval between the temperature of melt- ing ice and boiling water is divided into 100 equal parts ; the lower tem- perature is set at o and the higher at 100. The Centigrade scale alone is employed in this book. In the Fahrenheit sca/e, which is in general use in English-speaking countries, the interval between the fixed points is divided into 180 equal parts, and the temperature of melting ice is set at 32 and that of boiling water at 212. The value of a Centigrade degree is 1.8 times that of a Fahrenheit de- gree, and 32 Fahrenheit marks the same temperature as o Centigrade. To convert degrees C. into de- grees F., multiply by 1.8 and add 32. To convert degrees F. into degrees C., subtract 32 and divide by 1.8. The Barometer. The barometer is used for meas- uring the pressure of the atmosphere. In its simplest form it consists of a straight glass tube, about a meter long and closed at one end. This is completely filled Fig. & A SIMPLE BAROMETER Instruments for Weighing and Measuring xxi with mercury, which is boiled in the tube in order to drive out every trace of air or moisture, and its open end then placed under the surface of mercury in a dish (Fig. b). The mercury falls in the tube to a height of about f j6 cm -. The liquid does not all run out of the tube because the atmosphere pressing down upon the mer- cury in the dish pushes it up until the weight of liquid in the tube exactly balances the pressure of the atmos- phere. If for any cause the pressure of the atmosphere Fig. C A TRIP BALANCE becomes greater, it will push the mercury higher up in the tube ; and in a similar fashion, if the atmospheric pressure becomes less, it cannot support so long a column, and accordingly the liquid in the tube falls somewhat. The Balance. The balance serves to find the weight of an object. When the weight is to be ascer- tained only to tenths of grams, the form of balance known as the "trip " (Fig. c] is excellent. The weights accompanying need have no pieces less than 5 f- t as the beam and sliding weight in the front permit of the weighing to tenths of grams up to 5 s-. XX11 Elementary Chemistry In the quantitative work of this book, a balance weighing to hundredths of grams at least is required. Balances sensi- tive to a milli- gram are even better, but are much more ex- pensive and must be enclosed in a glass case to pre- vent currents of air from making them work too erratically. Either an equal-armed balance (Fig. d] or an unequal-armed one (Fig. e) may be used. Of the former there are numerous excellent makes on the market. They require the use of a box of weights contain- ing tenths and hundredths of grams. The form of balance in Fig. e was devised by the author for the quantitative work of the elementary chemistry labor- atory. Its advan- tages are ease in moving about, rapidity of weigh- ing, and " non-losableness " of the weights, which are rings moving along the beam. Fig. e UNEQUAL-ARMED BALANCE Instruments for Weighing and Measuring xxiii RULES TO BE OBSERVED IN WEIGHING 1. Always leave the balance and weight in a clean and usable condition. 2. Never handle Hie vv eights with the fingers ; use forceps. 3. Do not weigh anything but metals (mercury and sodium ex- cepted) en the bare scale pan. Liquids should be weighed in a dish or a beaker, the weight of which has already been found. Solids should be placed on a piece of paper creased twice at so c - c - right angles so as to sink in a little at the center (Fig. c). Graduated Vessels. For measuring rather large volumes of liquids graduated cylinders (Figs. / and g) of 2$o c - c - or 50^- capacity are used. Volumetric flasks (Fig. h) are also employed. For measuring small vol- umes of liquids pipettes (Fig. i) and burettes (Fig. 54, page 77) are used. Pip- ettes are usually graduated to deliver 5 c - c -, io c - c - t 25^-, or 50 c - c -. In using a pipette, its tip is dipped into the liquid, which is then sucked up nearly to the top by the mouth, and the upper opening quickly closed with the finger. By lifting up the fore finger so as to let air into the upper p . g fc _ VOLU _ part of the pipette the liquid may be METRIC FLASK Fig. f 250^. CYLINDER XXIV Elementary Chemistry made to drop out until its level comes even with the mark on the stem. The definite volume of liquid thus measured may then be delivered into the vessel in which it is to be used. Burettes are usually graduated into tenths of cubic centimeters and may hold either 25 c - c - or 50 c - c - ; but as sometimes the spaces are divided into 0.2 c - c -, that is, fifths of a cubic centimeter, a burette should be carefully examined before it is used in order that it may be read correctly according to its scale of division. They are clamped vertically to a support and rilled by pouring in the liquid. Enough liquid is allowed to run out by opening the clamp to drive out all air in the delivery tube,\and then by noting the reading of the level of the liquid in the burette, the required volume may be run out into the vessel being used. A convenient stopcock consists of a glass bead made from a rod a little larger in diameter than the bore of the bit of rubber tubing attached to the burette. This bead is slipped into the rubber tube between the burette pig. * and the delivery tip. By PIPETTE : B squeezing the rubber a little, a channel is formed between it and the bead, through which the liquid in the burette may flow. The size of this channel can be regulated with such ease that the liquid may be delivered with great nicety. The surface of liquids which ^cvet glass is curved upward near Fig. / READING A BURETTE The correct reading is along. O. Readings such as A and B must not be taken Instruments for Weighing and Measuring xxv the glass so that in small tubes the surface is concave. The name of meniscus has been given to this curved surface. The position of a liquid surface with respect to a scale is always reckoned at the lowest point in the meniscus, and the eye should be placed so that a line passing from it to the tube is perpendicular to the tube (Fig.y). In the case of liquids which, like mercury, do not wet glass, the meniscus is convex, and readings are taken at its highest point. It is a good plan for the student to determine the capacity of his test tubes, beakers, and flasks by pouring water into them from one of the above vessels. Their volume once determined, no time is lost in ascertaining what size of beaker, flask, or test tube is to be used in the experiments ; they may also serye as rough and ready measuring vessels. NAME OF ELEMENT Aluminum _ Antimony.. Argon Arsenic Barium Bismuth Boron Bromin Cadmium .. Calcium Carbon Chlorin Chromium _ Cobalt ...'.. Copper Fluorin Gold Hydrogen . . lodin Iron Lead Lithium Magnesium Manganese. Mercury Nickel Nitrogen Oxygen Phosphorus . Platinum Potassium... Silicon Silver Sodium Strontium... Sulfur Tin .... Zinc .. APPENDIX D TABLE I PHYSICAL CONSTANTS < Name of Discoverer and Date of Discovery Wohler (1827) Basil Valentine (1460) Ramsay and Ray leigh__.( 1894) Albert Magnus (i3th cent.) Davy .(1808) Basil Valentine (i5th cent.) Gay-Lussac and Thenard (1808) Balard ..(1826) Stromeyer (1841) Davy (1808) Known from earliest times Scheele ...(1774) Vauquelin ( 1 797) Brand (i?35) Known from earliest times Moissan (1886) Known from earliest times Cavendish (1776) Courtois (1812) Known from earliest times Known from earliest times. . Liebig and Bussy . , (1830) Gahn and John ( I 8o7) Known from earliest times Cronstedt (1751) Rutherford _. (1772) Priestley ( 1 774) Brand (1674) Waston... _. (1750) Davy (1807) Berzelius (1823) Known from earliest times Davy (1807) Davy (1808) Known from earliest times Known from earliest times 1 5th century [ xxvi ] TABLES >OME OF THE ELEMENTS Atomic Weights Valence Melting Point Boiling Point Specific Gravity l H = i O - ib Approxi mate 26 9 19-3 1Q.6 27.1 120.2 TO. 9 27 120 4O III. Ill, V 700 (?) 440 -) 1300 (?) 2.67 6. 7 2 J ' V 74-4 .9 y v 75-o T- W 75 III, V 446-457 Red heat 5-69 36.4 137-4 137 II Above that of cast iron ) 3-75 06.9 208.5 208 III, V 268 1700 9.9 10.9 II. ii III In electric furnace p 2.6 79-36 79.96 80 I 7-3 63 3.1 (liq.) ii. 6 112.4 112 II 320 770 8.72 39-8 40.1 40 II Red heat p i. 6-1. 8 ( Diamond 3.5 11.91 12.00 12 IV p ? \ Graphite 2.2 \ Charcoal 1.5 35-18 35-45 35-5 I IO2 34 1-33 (liq-) 5i-7 52.1 5 2 II, III p p 6-7 58.56 59-o 59 II 1800 p 8.6 63.1 63.6 63-5 I, II IO5O ? 8.9 18.9 19. ig I ? 95 7 197.2 197 III 1030 p 19-3 l.OOO 1.008 I I 252. 5 i 25.90 126.85 127 I 114 1 20 4-95 55-5 55-9 56 II, III I TOO p 7.88 05-35 206.9 207 II, IV 325 p n-37 6.98 7-03 7 I 1 80 p o-59 24.18 24.36 24 II 750 1 100 i-75 54.6 55-o 55 TI 7-2 98.5 200 200 j I -38:9 357 13-59 58-3 58-7 58.5 ,i 1600 p 8.9 13-93 14.04 H III, V 2O3 194 13-93 15.88 16.00 16 II 1825 15.88 30.77 31.0 3i III, V 44.2 287] Yellow 1.83 Red 2.21 93 3 194-8 195 IV 2000 p 21-5 38.86 39-15 39 I 62.1 667 4.9 28.2 28 4 28 IV Above cast iron p 2-5 07. 12 107 93 108 I IOOO p 10.5 22.88 23-05 23 I 97-6 742 0-97 86.94 87.6 87 II Red heat p 2-5 31.83 32.06 32 IIJV.VI II4-5 448 2.0 18.1 119.0 119 II, IV 227 1600 7-3 64.9 65-4 65 II 420 930 7-i i Referred to water if the element be in a solid or a liquid state ; to tydrogen if in a gaseous state. [ xxvii ] xxviii Elementary Chemistry TABLE II TENSION OF WATER VAPOR 15 12 -itnm. 21 20 gfnm. 16 I7.K mm. 2_1 C 222 7#W. 17 14 4//tt. 25 27 >mm. 18 15 ^mm. 26 2Z omm. 10 1 6 3/w. 27 26 t; /#/. 20 . ij.^mm. 28 28 I w. 21 1 8 ^tnm. 2Q 29 Sim. ig -jmm. 30 v i.e. mm. TABLE III SOLUTIONS TO BE PREPARED The figures in parentheses indicate the number of cubic centi- meters (if the substance is a liquid) and the number of grams (if the substance is a solid) that are to be dissolved in water ; the solution should then be diluted to one liter. Acetic acid, (140) of 80$ acid. Alum (any one), (100). Aluminum chlorid, (TOO). Aluminum sulfate, (25). Ammonium carbonate. Dis- solve 2oo<?"- in a mixture of 100^- of cone. NH 4 OH and 600 c.c. of water, and after solu- tion is complete dilute to one liter. Ammonium chlorid, (100). Ammonium hydroxid, (250) of cone. NH 4 OH. Ammonium molybdate. Dis- solve $og- of molybdic acid in a mixture of 100^- of cone. NH 4 OH and I$QC.C. of water. Dilute 250^- of cone, nitric acid with $QQC.C. of water and pour into first solution slowly and with constant stirring. Let stand in a warm place for 48 hours and decant the clear supernatant solution for use. Ammonium nitrate, (25). Ammonium oxalate, (50). Ammonium polysulfid. Dis- solve some sulfur in ammo- nium sulfid solution. Ammonium sulfid. Pass H 2 S into one liter of cone. NH 4 OH to saturation. Then add 750 c.c. cone. NH 4 OH and one liter of water. Ammonium sulfocyanid (also called thiocyanate), (10). Antimony chlorid. Dissolve 25^- in a mixture of 250^- of cone. HC1 and 750 c.c. of water. Arsenic chlorid. Dissolve 50^- sodium arsenite, Na 3 AsO 3 , in i ,000^- c. of water and add in small portions cone. HC1 until further addition occasions no effervescence. Barium carbonate. In suspen- sion in water. Tables xxix Barium chloric! , (60). Barium hydroxid. Dissolve 50^- in one liter of hot water, let stand over night, and filter or decant. Keep in tightly stoppered bottle. Bismuth nitrate, (25). The solu- tion must contain a little free nitric acid. Boric acid, (40). Saturated solu- tion. Bromin solution. Dissolve 2^- of KBr in 250 c.c. of water, add 6<"- (2 c.c.) of bromin, and shake until bromin is dis- solved, Bromin water. Put 4o<?"-(i3 c.c.) in a liter of water. Keep bot- tle tightly stoppered and in the dark. Cadmium chlorid, (25). Calcium chlorid, (25). Calcium hydroxid, (lime water). Put some freshly slaked lime in a bottle, fill bottle with water, shake, and when solu- tion is clear, decant and reject 'it, as it may contain some impurities from the lime. Fill the bottle with water again and shake well. Calcium sulfate. . Prepare satu- rated solution in same manner as lime water above. Chromium chlorid, (25). To ijoooc-c. of potassium dichro- mate solution add $oc.c. of cone. HC1 and 25 c.c. of alco- hol. Boil for half an hour gently and, if, after standing over night, the solution is not clear green add more alcohol and boil again. Chromium sulfate, (30). Chlorin water. Pass chlorin gas into water until it smells strongly of the gas. Better make small quantities when needed by adding a little cone. HC1 to a few crystals of KC1O 3 in a test tube and as soon as the gas escapes from mouth of tube, adding water to stop reaction. Cobalt chlorid, (50). Cobalt nitrate, (35). Cochineal. Grind a little with water and dilute to desired tint. Copper nitrate, (40). Copper sulfate, (35). Disodium hydrogen phosphate, (120). Ferric chlorid, (100). Ferrous sulfate. Dissolve i5o<?"- of clear crystals in one liter of water, and add 5 c.c. of cone. H 2 SO 4 and a few pieces of iron (tacks or small nails). Hydrochloric acid, (250) of cone, acid. Indigo. Slowly add lotf- of powdered indigo to 25 c.c. of fuming sulfuric acid. Let stand for a day and then add slowly with constant stirring to one liter of water. Lead acetate, (90). Lead nitrate, (40). Litmus. Grind a little with water to a paste and dilute to desired tint. XXX Elementary Chemistry Magnesium chlorid, (25). Magnesium sulfate, (100). Manganous chlorid, (75). Manganous sulfate, (35). Mercuric chlorid, (30). Nessler's Reagent. Dissolve 35^"- of potassium iodid in 100 c.c. of water ; also dissolve 16^"- of mercuric chlorid in 300^-^ of water. Add the latter solution to the former slowly with constant stirring until the precipitate ceases to be redissolved. Then add a solution of 65<?"- of potassium hydroxid in 60 c.c. of water and filter. Put the solution into a number of small bottles and cover the corks with par- affin. Keep in a cool, dark place, and when the solution is needed, do not open more than one bottle at a time. Nickel chlorid, (25). Nickel nitrate, (35). Nitric acid, (250) of cone. acid. Phenolphthalein. Dissolve one gram in IOQC.C. o f alcohol and dilute with water until a pre- cipitate begins to form ; then add enough alcohol to clarify solution. Platinum chlorid. Use com- mercial solution, or, dissolve scrap platinum in aqua regia, evaporate nearly to dryness, and dissolve residue in enough water to make about 10 per cent solution. Potassium bromid, (30). Potassium chromate, (100). Potassium chlorid, (50). Potassium dichromate, (50). Potassium ferricyanid, (30). Potassium ferrocyanid, (50). Potassium hydroxid, (150). Potassium iodid, (25). Potassium nitrate, (100). Potassium sulfate, (100). Potassium sulfocyanate, (50). Silver nitrate, (40). Keep in amber glass bottle. Sodium acetate, (130). Sodium ammonium phosphate, (7o). Sodium chlorid, (100). Sodium hydroxid, (175). Sodium sulfite, (200). Stannous chlorid. Dissolve So.?"- in IOQC.C. of hot cone. HC1 and keep a few pieces of tin in the solution. Make only when needed, as it does not keep well. Starch paste. Grind about lotf- to a paste with a little cold water, then boil with 250 c.c. of water until clear. Strontium chlorid, (30). Strontium nitrate, (30). Sulfuric acid, (250) of cone. acid. Pour acid in small portions, with stirring, into the full amount of water required for dilution. Tartar emetic, (100). Zinc chlorid, (50). Zinc sulfate, (140). APPENDIX E SIGNIFICANT FIGURES AND FORMS OF RECORD IN QUANTITATIVE WORK All the figures of a number are called significant excepting the ciphers at the right of a whole number and the ciphers at the left of a decimal fraction ; thus, the significant figures of 30,600 as well as of 0.000306 are 306. In all measurements one significant figure more than is known to be correct is kept in the number express- ing the result of the measurement ; this figure is said to be the least accurate figure or the doubtful figure of the number. Thus, suppose the volumes of water dis- placed from an aspirating bottle in three determinations of the weight of a liter of oxygen (Experiment 16) were found to be in each case, 1685 c - c -, 1680 c - c -, and 1689 c - c - , the sum of these three numbers is 5054, and their mean is 1684.666 -f c.c. 9 or 1684.66! c-c; or 1684.67^-. No one of these is proper, for each assumes a greater accuracy than we have any warrant for ; moreover, the second is irrational in its combining a common with a decimal fraction. The three determinations differ in units' place ; hence, we are not sure of units' place. We must accordingly drop the entire decimal part of the average number ; but as the decimal is greater than 0.5, it is customary to change the figure 4 in the average to 5, so that the average is 1685. If the decimal had been less than 5, it would have been dropped, and the average would have remained 1684. [ xxxi ] xxxii Elementary Chemistry Again, suppose that in three weighings of a dish the following results were obtained: 24.^^^-^ 24. 35^-, and 24.32^-. The sum of these numbers is 73.00, and their average arithmetically may be 24.3333 + or 2 4-33y, but if the above rules be observed, the average must be 24.33. It i s to be noted that the sum is given as 73.00 and not as 73. By writing the two ciphers in the deci- mal we indicate that we know that the tenths and hun- dredths are zero, while the 73 without the ciphers leaves us in doubt. Let another illustration emphasize this last point. Suppose the weight of a vessel be found on a balance sensitive to a hundredth of a gram, but that neither the tenths nor the hundredths gram-weights are needed to secure equilibrium, ilf only the ten- and two-gram weights are on the pan of the balance, its weight is written i2.oo<?"- and not just 12^-. The ciphers indicate the degree of accuracy attained. They mean that the tenths and hundredths were tried in determining the weight, but were not needed. By expressing a weight as 12.00^- you indicate that a balance sensitive to hun- dredths of grams was used, while 12.0^- would mean that a balance sensitive only to tenths of grams was employed. In the directions for the quantitative experiments the degree of accuracy is denoted by the number of decimal places kept in specifying a quantity to be taken. Thus, in Experiment 46, exactly 2.00^- are specified, which means that on a balance sensitive to hundredths of grams, two grams, and not more or less by a hun- dredth of a gram, are to be taken. In Experiment 16 the directions are to take about 5 & of manganese dioxid. This quantity may be weighed roughly, that is, to about a gram, it making no difference if 4^- or 6^- should hap- pen to be taken. If the amount had been written 5.0 &-, Significant Figures and Forms of Record xxxiii it would have been necessary to use a more sensitive balance and weigh to tenths of grams. Suppose that it were found that 2.68<^- of oxygen occupied a volume of 1,871 c - c -, i. e., 1.871 L . Then the quotient of 2.68 divided by 1.871 gives the weight of one liter. The question arises : How many figures of the quotient are to be retained ? It is apparent that if only weighings to hundredths of grams were made, then only hundredths should be kept. Accordingly the quotient is 1.43. Arithmetical operations on data obtained in quanti- tative experiments may be much abbreviated, with no loss in accuracy, by dropping after an operation of mul- tiplication or division all except the significant figures in a number. To illustrate, let us solve the following problem : Find the reduced volume of 283 c - c - of a gas measured at 662 >> and 22. It is to be noted that no one of the three numbers given has more than three figures ; hence, there are only three significant figures. Substituting in the for- mula ( 27), we have Below are given two calculations of the value of V, the one to the right retaining all figures after each mul- tiplication, the one to the left retaining in each product only three (significant) figures. 283 283 273 273 849 1981 566 77259 77259 3b xxxiv Elementary Chemistry 773 77259 662 662 4638 463554 4638 463554 5^726 5H45458 2 95 295 760 760 17700 17700 2065 2065 224200 224200 224) 512(228.5 224200) 51145458 (228.1 448 " _ 640 6305 448 4484 1920 18214 I79 2 17936 1280 2785 As is seen, the reduced volumes differ only in the first decimal place. But as the units are doubtful, the tenths are not significant. As the tenths in 228.5 i g -5> the number according to custom is increased to 229. It is thus manifest that the abbreviated operations give as good results as the detailed one. FORMS OF RECORD OF DATA It always saves time and energy to enter data as soon as obtained in some approved tabular form. Always use a note book, never a scrap of paper. Preserve all the arithmetical work so that, if necessary, it may be checked up with a second determination. Some forms of tabular entries are given at the end of the directions Forms of Record of Data xxxv for the performance of various experiments. A very common operation in quantitative work is the fol- lowing : A dish or other vessel is weighed, some substance placed in it, and a second weighing made. The differ- ence in the weights gives the weight of the substance. A good form of record for this operation is this : Wt. of dish, crucible, or test tube + substance = 47. 63^"- Wt. " _.. _ = 23.42^"- Wt. of substance = 24. 21^"- Suppose a substance is being heated to constant weight in an evaporating dish. A convenient form of record is the following : Wt. of dish + substance after heating for 20 min = 47.84^- Wt. " + " " 10 " more = 47.67^- Wt. + " 10 " " = 47.63<r- Wt. " + " " " " 10 " " = 47.63^- Wt. " = 23. 42 <r- Wt. of substance = 24. 21^"- Other similar forms may be readily devised by the student. It is a good plan to decide upon what form of record is to be used before commencing a quantita- tive experiment. The very preparation of a form often helps wonderfully in keeping track of the steps in an experiment. APPENDIX F LABORATORY EQUIPMENT The subjoined lists contain the apparatus and the chemicals required for the experiments in this book. Prices and quantities have not been given, but the author will be pleased to give infor- mation to teachers using the book as to the quantities of apparatus and chemicals used by his own classes. Prices may be obtained from any of the dealers in chemical supplies. LIST A i INDIVIDUAL APPARATUS This list comprises the pieces of apparatus constantly used by a single student, who should be provided with each piece. Iron tongs. Platinum wire. Blowpipe. Iron forceps. 'Triangular file, 6". 'Round file, 8". Wire gauze or asbestos board. 'Wing-top burner. Mortar and pestle, 4". Iron spoon. 2 Derlagrating spoon, i 2 Glass rod, 5". i Two-hole rubber stopper to fit large test tubes. 3 ft. rubber tubing, 3/ 16 ". 3 ft. glass tubing, medium wall, Test tubes, Test tubes, 6x^". Test tubes, gx i". Beaker, 100 c. c. Beaker, 250 c. c. Flask, 100 c. c. Flask, 250 c. c. Retort, 250 c. c. Glass plates, 4x4". Thistle tube. Funnel, 2^". 'Porcelain crucible, i oz. 'Pipestem triangle. Evaporating dish, 3". 2 Test-tube holder. 2 Test-tube brush. Test-tube rack. to fit rubber stopper. 1 These pieces of apparatus may be used by several students in common. 2 These pieces of apparatus may readily be made by the student himself. [ xxxvi ] Laboratory Equipment xxxvii LIST B TABLE APPARATUS This list includes the apparatus which should be kept at the laboratory desk used by the student or on a side table. It is a part of the equipment to be used by different classes. 'Mohr pinch-cocks. 'Iron and copper wire. 'Sand. 'Graduated cylinders, looc. c. and 500 c. c. 'Bar magnets. 'Splinters of wood. 'Wax tapers. 'Meter sticks. 'Trip scales and weights. 'Chaslyn balances. i It is not feasible to give quantities for these articles ; as many as possible should be provided, although it is possible to get along with few. i Retort stand with two rings and a clamp. 6 Wide-mouthed bottles or receivers. i Pneumatic trough, i Bunsen burner. 3 ft. rubber hose for attaching Bunsen burner. '"Acid bottles." 'Assorted corks. 'Hofmann screw-cocks. LIST C DEMONSTRATION APPARATUS This list comprises the apparatus which the teacher should have for demonstrating experiments. It should be of the best quality and not mere makeshift. i Eudiometer and trough, i Electrolysis of water appa- ratus. i Safety tube. 1 Kipp's gas generator (it is well to have two or three all charged and ready to deliver at any time such gases as hydrogen, carbon dioxid, etc.). 2 U-tubes, 6" and 8". i Liebig's condenser. Thermometer. Bulb tube. Induction coil. Battery to run coil. Large lamp chimney. 'Rubber stoppers of various sizes. 'Ignition tubes. 'Supply of glass tubing of various sizes. 'Supply of rubber tubing of various sizes. i Refer to note in List B. XXXV111 Elementary Chemistry LIST D CHEMICALS The chemicals should as far as possible be of " c. p." grade. Acid, acetic. citric. hydrochloric. nitric. oxalic. pyrogallic. sulfuric. tartaric. Alcohol, ethyl. methyl. Alum, chrome. potash. Aluminum, metal. sulfate. Ammonium, chlorid. hydroxid. nitrate. oxalate. sulfid. Antimony, metal. Arsenic, metal. Arsenious oxid. Asbestos. Barium, chlorid. nitrate. Bismuth, metal. nitrate. Bleaching powder. Borax. Cadmium chlorid. Calcium, carbid. carbonate (marble). chlorid. fluorid. oxid (lime). sulfate (gypsum). Carbon bisulfid. Charcoal, animal. wood. Coal, hard. soft. Cobalt, chlorid. nitrate. Cochineal. Copper, metal. nitrate. sulfate. Ether. Glycerin. Indigo, lodin. Iron, metal (filings and wire). chlorid. sulfate. sulfid. Lead, metal. nitrate. monoxid (litharge). red. Litmus, paper. Magnesium, metal (powdered and ribbon). sulfate. Manganese, dioxid. sulfate. Mercury. Mercuric chlorid. nitrate. oxid. Mercurous nitrate. Nickel chlorid. Laboratory Equipment xxxix Phenolphthalein. Sodium, metal. Picture cord (iron). bicarbonate. Potassium, metal. carbonate. bromid. chlorid. carbonate. hydroxid. chlorate. nitrate. chromate. phosphate. dichromate. silicate. ferricyanid. sulfate. ferrocyanid. sulfite. hydroxid. Stannous chlorid. iodid. Starch. permanganate. Strontium nitrate. sulfate. Sulfur, flowers and roll. sulfocyanid. Tin, granulated. Rosin. Vaseline. Silver nitrate. Zinc, granulated and sheet. Soda-lime. sulfate. W^TT^ -5, '43 (6061 S) V/D \ / r\ / * ID IDOO4 50