Jhemical Experiment!' General and uivtical Yv'illiams i of Olivias Lry LIBRARY OF THE UNIVERSITY OF CALIFORNIA 01 FT OP" x? ^ Received Accession No.> Sl5~~ . C/<25S A/b CHEMICAL EXPERIMENTS GENERAL AND ANALYTICAL FOR USE WITH ANY TEXT-BOOK OF CHEMISTRY, OR WITHOUT A TEXT-BOOK K. P. WILLIAMS N x Instructor in Chemistry, English High School, Boston, and Author of " Introduction to Chemical Science," " Laboratory Manual," etc. OS t t_ . _ . __ BOSTON, U.S.A., AND LONDON PUBLISHED BY GINN & COMPANY 1895 COPYRIGHT, 1895 BY R. P. WILLIAMS ALL BIGHTS RESERVED PEEFAOE. THE rapid growth of the laboratory method of teaching chem- istry since the author's Manual was issued in 1888 has called for a larger and more comprehensive work of a similar sort for high schools, academies, and colleges. To such a call tfre present book is a response. In preparing the experiments the author has endeavored, first, to select such as are most instructive and best illustrate the subject without being too elaborate ; second, to arrange them in an order calculated to lead up by the most natural and easiest steps to a knowledge of the science ; third, to make the subject fascinating by giving just enough information and suggestion to interest the experimenter, and to make him work for the knowledge to be gained. Finally, the author has aimed to make the book simple enough for the dull and slow pupil, and by the introduction of supplementary and original work elaborate enough for the most acute. Great care has been taken to give minute and accurate directions for performing the experiments. " Terms " at the end of experiments are for pupils to study outside the laboratory, and are often repeated. They may also be discussed in the laboratory. Metal analysis has received a somewhat unique treatment. Each metal of a group is first taken separately, and the analytical reactions are given. This method shows the pupil at once why a given re-agent is added, and what its effect is. The product is given when the substance is in solution as well as when it is precipitated. The group is next treated in the same way. This method clarifies the subject greatly in the pupil's mind, and is believed to be a valuable departure in teaching analysis. iv PREFACE. The new orthography recommended by the Chemical Section of the A. A. A. S. has been adopted, as a step towards uniformity and progress. It is recommended that wherever it is possible each laboratory period cover the space of two hours (even if there can be only one period per week), and that the last 20 or 30 minutes be taken to question the class rapidly on the work of the day, discuss and explain the use of terms, etc. The books should be inspected after each exercise, or perhaps after each experiment has been written out. It is by no means necessary to perform every experiment, or to follow the order here given, if the teacher prefers to do otherwise. A diversity of opinion exists among teachers, and a diversity of time and talent among pupils and classes. In no place better than in the laboratory, under a competent instructor, can a " cast-iron rule " be done away with, and variety of arrangement and method be adopted. The author would be glad to receive criticisms, as well as suggestions as to other methods, or experiments, or different ways of performing experiments. Especially would he be glad to know what it has been difficult, in the matter of directions or principles, for pupils to understand. The author desires to acknowledge valuable suggestions in the preparation of this work from the following persons : Messrs. J. Y. Bergen, Jr., C. W. Gerould, E. F. Holden, A. S. Perkins, K S. French, H. I. Lord, E. S. Chapin ; and Misses D. M. Stickney, M. L. Foster, and others. CAMBRIDGE, December 1, 1895. INDIVIDUAL APPARATUS. Each pupil should be provided with the apparatus given below, but in cases where great economy must be exercised different pupils may, by working at different times, use the same set. The author has selected apparatus specially adapted, as to exact dimensions, quality, and cheapness, for performing in the best way the experiments herein described, and sets or separate pieces of this, together with other apparatus and chemicals, can be had of the L. E. Knott Apparatus Co., 14 Ashburton Place, Boston, to which firm teachers are referred for catalogs. 4 re-agent bottles, 250 cc. glass stop- pers, blown labels: NH 4 OH, HC1, HNO 3 , H 2 S0 4 . 1 pneumatic trough. 1 Hessian crucible. 2 beakers. 2 pieces wire gauze. 1 piece platinum wire. 1 mouth blowpipe. 6 pieces glass tubing. 4 pieces hard glass tubing. 1 test-tube brush. 1 small tube brush. 1 doz. test tubes. 4 cork stoppers, for tubes. 1 fish-tail attachment for Bunsen burner. 1 blowpipe attachment with rest for Bunsen burner. piece sheet copper. glass retort. tumbler. piece cobalt glass. horn spatula. sheet litmus paper. 00 filter papers. bunch splints. sheet turmeric paper. 1 camel's-hair brush. 1 magnet. 4 wide-mouthed bottles. 1 2-holed rubber stopper to fit above. 4 pieces window-glass. glass funnel. porcelain evap. dish. asbestos board. sand bath. pair iron forceps. triangular file. round file. piece copper wire. 1 piece lead wire. 1 piece zinc wire. 1 wooden test-tube holder. 1 wire test-tube rack. 1 thistle tube. 1 Bohemian flask. 1 2-holed rubber stopper to fit flask. Bunsen burner, iron ring stand. 2 ft. rubber tubing. 1 ft. " " 1 metric ruler. 1 graduate. 1 small leaden dish. GENERAL APPARATUS. The requirements of general apparatus for a laboratory are too numerous and varied to be given here. A few of the pieces in more general demand for experiments in this book are as follows : Glass-stoppered bottles. Graduates. Funnels. Fruit jars (for making solutions). Scales, with metric weights. Ignition tubes. Beakers. Filter-stands. Glass and rubber tubing. Steel glass-cutters. Steel wire-cutters. Mortars and pestles. Flasks. Filter papers, etc., etc. CHEMICALS. ESTIMATE FOR A CLASS OF TWENTY IN GENERAL CHEMISTRY AND ANALYTICAL REACTIONS, NOT INCLUDING GENERAL REACTIONS AND SUPPLEMENTARY WORK. Acid, acetic, HC 2 H 3 O 2 4 Ib. " boric, H 3 B0 3 i " " hydrochloric, HC1 25 " " hydrofluoric, HF i " " hydrofluosilicic, H 2 SiF 6 .... i " " nitric, HNO 3 12 " " oxalic, H 2 C 2 4 f " " phosphoric, H 3 PO4 J " " sulfuric, H 2 S0 4 18 " " tartaric, H 2 C 4 H 4 6 i " Alcohol, C 2 H 5 OH 1 qt. Alum, K 2 A1 2 (SO 4 ) 4 1 Ib. Aluminum chlorid, A1C1 3 -J- " Ammonium carbon., (NH 4 ) 2 C0 3 1 " chlorid, NH 4 C1 2 " " hydroxid, NH 4 OH..20 " " nitrate, NH 4 NO 3 1 " " oxalate, (NH 4 ) 2 C 2 4 i " " sulfate, (NH 4 ) 2 S0 4 .. i " Antimony cryst., Sb ^ " ' " chlorid, SbCl 3 i " Arsenious oxid, As 4 O 6 1 oz. Arsenopyrite, FeAsS Jib. Barium chlorid, BaCl 2 i " " hydroxid, Ba(OH) 2 i " Bismuth oxychlorid, BiOCl i " Calcium chlorid, CaCl 2 i ' " fluorid, powdered, CaF 2 k " " hypochlorite, CaCl 2 0.... i " " sulfate, CaS0 4 i " " oxid, CaO 2 " Carbon bisulfid, CS 2 i Charcoal, animal, gran., C 1 " ' " powdered, C.. 1 " " wood, u C.. 1 " * C 20 pieces Cobalt chlorid, CoCl 2 i Ib. " nitrate, Co(N0 3 ) 2 .... Cochineal Copper, turnings, Cu " sheet, Cu i " chlorid, CuCl 2 1 " nitrate, Cu(NO 3 ) 2 i ** oxid, CuO 1 i " i " 3 " VI CHEMICALS. Vii Copper sulfate, CuSO 4 i Ib. Ether, (C 2 H 5 ) 2 i " Gold leaf, Au 1 bk. Indigo i Ib. lodin, 1 2oz. Iron, fine turnings, Fe 1 Ib. " by hydrogen, Fe , -J- " " perchlorid, FeCl 3 1 " " protosulfid, FeS 5 " " pyrite, FeS 2 i " " sulfate, FeSO 4 1 " Lead, sheet, Pb 1 " " wire, i in. diam., Pb 12 ft. " acetate, Pb(C 2 H 3 02)2 i Ib. " chlorid, PbCl 2 i " " nitrate, Pb(N0 3 ) 2 2 " " protoxid, PbO i " " tetroxid (red), Pb 3 4 i " Litmus, cubes 1 oz. Marble chips, CaC0 3 3 Ib. Magnesium ribbon, Mg 10 ft. " chlorid, MgCl 2 i Ib. sulfate, MgSO 4 " Manganese chlorid, MnCl 2 " " dioxid, gran., Mn0 2 .. " " powd.,Mn0 2 li " Mercury, Hg $ " " bichlorid, HgCl 2 " " protochlorid, HgCl " " pernitrate, Hg(N0 3 ) 2 .... i " " protonitrate, HgN0 3 .... i " " oxid, HgO 1 " Nessler's sol i " Phosphorus, P 2 oz. Picture wire 1 roll Platinum chlorid, sol., PtCl 4 loz. Potassium, metallic, K " " bromid, KBr Ib. " carbonate, K 2 C0 3 1-J- " " chlorid, KI " u chlorate, KC1O 3 2 " " chromate, K 2 CrO 4 .... i " " cyanid, KCN " Potassium, dichromate, K 2 Cr 2 O 7 1 Ib. " ferrocy., K 4 Fe(CN) 6 .. 1 " ' ferricy., K 3 Fe(CN) 6 .. f " iodid,KI 1 " " hydroxid, KOH 1 " " nitrate, KN0 3 1 " u nitrite, KN0 2 i " *' permangan., KMnO 4 i " " sulfocyanid, KSCN.... i " " tartrate, K 2 C 4 H 4 6 .... i " Silica, powdered, Si0 2 i " Silver nitrate, AgNO 3 4 oz. Sodium, metallic, Na fa " " acetate, NaC 2 H 3 O 2 i Ib. . " arsenite, HNa 2 As0 3 | " " bicarbonate, HNaC0 3 .... i " " bisulfate, HNaS0 4 i " borate, Na 2 B 4 O 7 -J- " " carbonate, Na 2 C0 3 3 * " chlorid, NaCl 4 " u hydroxid (caust.),NaOH 3 " " nitrate, NaNO 3 2 " " nitrite, NaNO 2 -J- * oxalate, Na 2 C 2 O 4 \ " " phosphate, HNa 2 P0 4 1 " sulfate, Na 2 S0 4 " sulfid, Na 2 S " sulfite, Na 2 S0 3 " thiosulfate, Na 2 S 2 3 Starch, C 6 Hi O 5 Strontium chlorid, SrCl 2 Sugar, Ci 2 H 22 On Sulfur, brimstone, S 2 " ** flowers, S 1 Tin bichlorid, SnCl 2 i " Turmeric paper 1 sheet Turpentine, Ci Hi 6 loz. Zinc, gran., Zn 3 Ib. " wire, i in. diam 12ft. " (arsenic-free) lib. " chlorid, ZnCl 2 i " u nitrate, Zn(N0 3 ) 2 i u Litmus paper i quire 1 I " i " 1 " i " i" 1 " SOLUTIONS, ETC. In making solutions for metal analysis, chlorids of the metals are usually taken (except in Group I, in which nitrates are used, the chlorids being insol- uble). From 25 e to 50 & of solids are usually dissolved hi 500 cc of distilled water, and filtered if necessary. Many are sat., as Ca(O H) 2 . Substances for analysis, as well as acids and other re-agents, should be C. P. Concentrated acids are used unless the dilute are called for. A few exceptional sols, are given below : HNa2P0 4 , 40. (NH 4 ) 2 C0 3 , 100. (NH 4 ) 2 S0 4 , 5. KCy, 50. KNO 2 , 50. NH 4 C1, 60. K 2 Cr 2 7 , 25. KOH, 60. NaOH, 60. Dilute acids are made by mixing one volume of concentrated acid with four volumes of water. NH 4 OH. If NH 4 OH of 26 is obtained, it should be diluted with three times its volume of water before using. HgN0 3 is best prepared by putting into a large e.d. say 25s of Hg, and adding to it a mixture of 25 cc HNO 3 and 25 cc of H 2 O, and letting it stand till action stops, then adding 400 cc or 500 cc of H 2 O. More Hg should be used than will dissolve, and some should be left in the bottle. PbCl 2 is only slightly soluble in water. A saturated sol. should be used. BiClg is prepared by adding water and HC1 to oxychlorid of bismuth, BiOCl. First add the H 2 O, then acidulate it with the acid, say 1 vol. of H Cl to 20 of H 2 O, it being insol. in H 2 O alone. AsCl s . Add H 2 to sodium arsenite HNa 2 AsO 3 , then add HC1 with stirring till effervescence stops. SbCl 3 . Pour a little butter of antimony, SbCl 3 , into H 2 0, then acidulate with HC1. SnC^. This must also be acidulated with HC1, and a little Sn should be left hi the bottom of the bottle. CrCl 3 , This may be made from K 2 Cr 2 7 sol. by adding some HC1 (say ^) and a little alcohol, boiling some time and letting it stand, when it turns from red to green. (NH 4 ) 2 S. Pass H 2 S gas into dilute NH 4 OH till the sol. gives no ppt. with MgSO 4 sol., then filter. It should be nearly colorless. (NH 4 ) 2 S X (ammonium polysulfid). Stir sulfur flowers in the (NH 4 ) 2 S, as above prepared, then filter. It is yellow. Cochineal sol, Grind up a handful of cochineal in a mortar, and add water, stir, and filter. Litmus sol. Pulverize litmus cubes, and add water. Indigo sol. (sulfindigotic acid). Slowly mix and stir 5s indigo with 25 CC H 2 SO 4 (or better H 2 S 2 O 7 , fuming sulfuric acid) in a beaker immersed in cold water. Cover the beaker, and after 48 hours add 500 cc H 2 0, stir and filter. Many substances in sol. easily break up on standing, and hence should be freshly prepared. For acid radicals compounds of Na or K are commonly used, as they are soluble. vin RULES AND SUGGESTIONS FOR PUPILS. Pupils should read .these rules carefully, and should refer to them whenever in doubt on any point. 1. Each pupil should provide himself with a towel, to keep his bench clean, and any apron or other clothing desired for protection in the laboratory. A long linen duster or duck coat reaching to the feet is the best protection. Without something of the sort clothing may be injured at any moment. 2. The bench at which the pupil works must be left clean and dry after every laboratory exercise. Wipe off a ring-stand, lamp, or other apparatus on which a re-agent has fallen, wipe out a p.t. after using it, and keep re-agent bottles, apparatus, books, and lockers clean. 3. Pupils are held responsible for apparatus, and should replace anything that is lost or broken. 4. In experimenting have your apparatus neatly arranged without artificial props, wedges, or uncouth-looking material. Have every d.t. and stopper fit tightly to prevent leakage of gas. If a gas generates well, but does not pass into the rec. , there is some leakage, due probably to loose bearings. 5. In heating a t.t. on the r.s. hold the lamp in the hand, move it slowly, and now and then take it away from the tube for a moment, to prevent melting and breaking the latter. 6. Mixtures of solids should be made on paper. Be careful not to mix chemicals or re-agents except as directed. 7. To shake the contents of a t.t. cover its mouth with the thumb (Exp. 4, Fig. 10), or the hand, or a stopper, hold it away from the bench, and shake it vigorously. 8. Never put down a stopper when using a re-agent bottle, but hold it between the first and second fingers (Exp. 6, Fig. 11), and replace it when you put down the bottle. Do not pour back any excess of a re-agent from a t.t. or other rec. into a re-agent bottle, and do not dip a stirring rod into a re-agent bottle. 9. In pouring a liquid into a t.t. (or graduate) hold the latter on a level with the eye, and towards the light, so as to see any change. The thumb-nail may be placed at the upper limit to which it is desired the liquid should reach. When much heat is liberated, as when sulfuric acid is poured into water, a tube-holder should be used ; paper folded several times serves for this purpose. 10. Pour only liquids, fine powders, or soluble salts into the sinks, always opening the faucet first to let the water run. Other solids should be thrown into the jars. Great care must be taken not to clog the discharge-pipes. 11. Have flasks and tubes perfectly dry on the outside before applying heat. Tubes of thick glass, if they contain no liquid, should be heated gradually at ix TABLE OF COMMON ELEMENTS. ARRANGED ACCORDING TO ELECTRO-CHEMICAL ORDER. NAME. SYMBOL. Oxygen 0" Sulfur S", iv (vi) Nitrogen N'", v - etc. Fluorin F', 00 Chlorin Cl', 00 Bromin Br', CO lodin T, (v) Phosphorus P"', 'V Arsenic As'", v Chromium Cr", '", vi Boron B"' Carbon CD, iv Antimony Sb"', v Silicon Si" Hydrogen H' Gold Au('), "' Platinum Pt("), IV Mercury Hg', " Silver Ag 7 Copper Cu('), " Bismuth Bi'", ( v > Tin Sn", 'v Cadmium Cd" Cobalt Co", ('") Nickel Ni", ('") Lead Pb", OT, Iron Fe", "' Zinc Zn" Manganese Mn", ("') Aluminum Al'" Magnesium Mg" Calcium Ca" Strontium Sr" Barium Ba" Sodium Na' Potassium K' AT. WT. VAPOR DENSITY. STATE, 16 16 G 32 32 S 14 14 G 19 G 35.5 35.5 G 80 80 L 127 127 S 31 62 S 75 150 S 52 S 11 S 12 S 120 S 28 S 1 1 G 197 S 197 S 200 100 L 108 S 63 S 207 S 117 S 112 56 S 59 S 58 S 206 S 56 S 65 32i S 55 S 27 S 24 S 40 S 87 S- 137 S 23 S 39 S A ( ) indicates a rare valence. Atomic weights are only approximate. xii ABBREVIATIONS. Ac. acetate, C 2 H 8 2 . gr. green. alk. alkali or alkaline. insol. insoluble. Am. ammonium, NH 4 . i.t. ignition tube. app. apparatus. M. metal (valence 1). b. black. . o.f. oxidizing flame. B.B. before the blowpipe. Ox. oxalate. B.B.C.C. before the blowpipe on ppd. precipitated. charcoal. ppg. precipitating. bl. blue. ppn. precipitation. cc. cubic centimeters. ppt. precipitate. cm. centimeters. p.t. pneumatic trough. col. color. qcm. square centimeters. cone. concentrated. re-agt. re-agent. cpd. compound. rec. receiver. cryst. crystalline. res. residue. Cy. cyanid, CN. r.f. reducing flame. dil. dilute. r.s. ring stand. dis. dissolve. sat. saturate. dist. distinguish. sep. separate. d.s. deflagrating spoon. si. slight or slightly. d.t. delivery tube. sol. solution or soluble. e.d. evaporating dish. sp. gr. specific gravity. evap. evaporate. s.r. stirring rod. ex. excess. Tr. tartrate. Exp. experiment. t.t. test tube. fil. filtrate. up. disp. upward displacement. g. grams. v. vide, see. gel. gelatinous. vol. volume. gen. generator. yel. yellow. Xlll INDEX TO EXPERIMENTS. 1. Metric Measurements. 35. Oxids of Nitrogen. 69. Manganese. 2. Glass Manipulation. 36. Carbon Dioxid. 70. Zinc. 3. " " 37. Chlorin. 71. Group IV. 4. Physical Changes. 38. Euchlorin. 72. Barium. 5. 39. Bromin. 73. Strontium. 6. Chemical " 40. lodin. 74. Calcium. 7. Elements and Compounds. 41. Sulfur. 75. Magnesium. 8. Oxygen, Preparation. 42. Hydrogen Sulfid. 76. Group V. 9. " Combustion. 43. Phosphorus. 77. Sodium. 10. 44. Arsenic. 78. Potassium. 11. Nitrogen, Separation. 45. Compounds of Boron. 79. Ammonium t 12. " and Air. 46. " " Silicon. 80. Group VI. 13. Hydrogen from Acids. 47. Oxidation and Reduction. 81. Borates. 14. " " Water. 48. Lead. 82. Nitrates. 15. Carbon, Preparation. 49. Silver. 83. Nitrites. 16. " Properties. 50. Mercury. 84. Chlorates. 17. Combustion. 51. Group I. 85. Carbonates. 18. " 52. Mercury. 86. Sulfids. 19. Positive and Negative Elements. 53. Lead. 87. Sulfltes. 20. Acids, Bases, Salts. 54. Bismuth. 88. Thiosulfates. 21. Acid, Alkaline, Neutral Reactions. 55. Cadmium. 89. Fluorids. 22. Soluble Salts by Neutralization. 56. Copper. 90. Chlorids. 23. " " from Metals. 57. Group H, A. 91. Bromids. 24. " " " Carbonates, etc. 58. Arsenic. 92. lodids. 25. Insoluble Salts by Precipitation. 59. Tin. 93. Acetates. 26. Hydrochloric Acid. 60. Antimony. 94. Cyanids. 27. " " 61. Group H,B. 95. Tartrates. 28. Hydrofluoric 62. Iron. 96. Oxalates. 29. Nitric 63. " 97. Silicates. 30. Aqua Regia. 64. Aluminum. 98. Ferrocyanids. 31. Sulfuric Acid. 65. Chromium. 99. Ferricyanids. 32. Ammonium Hydroxid. 66. Group in. 100. Sulfates. 33. Fixed Alkalies. 67. Cobalt. 101. Chromates. 34. Oxids of Nitrogen. 68. Nickel. 102. Phosphates. xiv XT 1. METRIC MEASUREMENTS. I. Length. Note the length of 10 cm on a metric ruler, then estimate by the eye alone this length on the cover of a book, and on various objects, verifying each result till you can carry in mind 10 cm . Estimate the number of inches it covers, and verify. In the same way experiment with l cm . Measure the perpendicular distance between the blue lines on a sheet of foolscap paper. Measure the diameter of the older nickel five-cent piece. Make a drawing of the fol- lowing measurements on the opposite page : one square decimeter, i.e. 10 cm on a side ; l qcm . II. Volume. Measure in a graduate 10 CC of water, then pour it into a t.t. Note, without marking, what proportion of the t.t. is filled. Make a drawing of it on the opposite page. Pour out the water, then pour into the t.t. as near the same volume as possible, estimating by the eye alone. Verify the result by pouring the water into the graduate. Kepeat this till you can estimate quite accurately. Try it with a t.t. of another size. Estimate l cc of the liquid in the same way. Draw a figure of a cube l cm on a side. In future experiments estimate volumes, without measuring, unless special accuracy is required. III. Weight. Balance a piece of paper on each pan of a pair of scales. On one pan put a 10 g weight and balance this with fine salt or sugar. Note with the eye the quantity of the substance, then remove it. Now estimate a like quantity and verify by weighing it. Repeat the experiment several times. Weigh 1 or 2 g and estimate as before. See if l g can be piled on a one-cent coin. Weigh one of the old nickel five-cent pieces. In subsequent experiments estimate quantity of solids, unless accuracy is desired. Supplementary. Commit to memory the metric tables for length, volume and weight (v. Physics). How many cc in a liter ? How many grams should a liter of water weigh ? 10 CC of water ? Hg weighs 13.6 times as much as water. What will 5| cc of Hg weigh ? A rectangular block of marble is 3 X 4 X 2 cm and has sp. gr. 2.5. What does it weigh in grams ? 2. GLASS MANIPULATION. I. Ignition Tubes. Take a piece of ignition tubing 20 or 25 cm long, hold it steadily in a Bunsen flame just above the inner greenish cone (Fig. 1), and rotate it. When it begins to soften draw it out slightly (Fig. 2, a) and raise it a little in the flame. Do not pull or twist the glass but let the heat gradually separate it, so as not to have long threads attached. The ends may be rounded (Fig. 2, b) by holding in the edge of the flame (Fig. 3). Finally anneal the glass by closing the lower open- ings of the lamp and holding the heated end in the flame to cover it with soot, then letting Fi it cool gradually without touching any object. Unless great care is taken in this, the glass will break when next put into the flame. Save the tubes for sub- sequent experiments. II. Stirring Rod. Weld the ends of a piece of glass tubing about lo cm long and or ij- cm in diameter by holding each end successively in a Bunsen flame above the green cone (Fig. 3), and rotating till the openings are sealed. Use care in cooling as before. Fig. 3. Supplementary. Bulb Tubes. Draw out a piece of tubing as in 1, then melt the closed ends by holding and rotating as in Fig. 3. When the glass is sufficiently Fig. 4. softened, blow moderately into the open end, repeating the operation till the tube assumes the desired shape (Fig. 4). 3. GLASS MANIPULATION. III. Connecting Tubes, Use an ordinary gas flame (or a fish-tail attachment to a Bunsen burner) for bending glass, as the Bunsen flame is too hot. Turn down the gas till the flame is about 5 cm across, then bend each of 3 pieces of tubing, 16 cm long, in the middle and at right angles, by letting the glass rest lightly in the fingers of both hands and holding it lengthwise of the flame and just above the dark part (Fig. 5). Ko- tate it slowly and hold very steadily. When it begins to soften take it quickly from the flame and holding it between the eye and a window frame bend it at right angles. If it does not bend easily, heat it again. Bend also one piece of tubing (50 cm long), 5 or 6 cm from one end. Kound the sharp corners of each by holding the tip ends of the tubes in the edge of a Bunsen flame for a minute (Fig. 3). Do not let any part of the heated glass touch any object and avoid wiping off the soot till the glass is cool enough to handle, when it should be cleaned. IV. Delivery Tubes, Examine the angles (all obtuse) and the relative lengths of the parts in Fig. 6 and in a model, noting that the bends a and c are very near the ends, and a and b are close together. Do this work very carefully. Use a piece of glass tubing 50 cm long, holding it as before. Make the bends in the order a, b, c. Hold the glass con- stantly in the flame, turning it 6 occasionally to heat both sides. When it yields remove and bend it out of the flame. To make the bends at b and c, turn the glass quickly and closing one eye sight along the tube so as to have all parts lie in the same plane. Round the sharp edges 1 and 2 in the flame, as before, and cool with care. Show all results to the instructor. V. Perforating Corks. Fit a cork to a t.t., remove it and with a round file bore a hole in it holding the cork in the left hand and pressing the end of the file against its larger surface. Observe constantly during the operation whether the perforation is perpendicular to the surface of the cork. The orifice must be perfectly circular and a little smaller than the tube it is to receive. When completed, adjust to the d.t. and t.t. Detach the stopper from the t.t., not from the d.t. 4. PHYSICAL CHANGES. Fig. 7. Solution. See whether crystals of granulated sugar, C 12 (H 2 0) U , can be crushed. Put into a t.t. 5 g or more of the sugar, just cover it with water, H 2 0, and boil in a Bunsen flame for a minute, using a t.t. holder of wood, metal, or paper (Fig. 7), till the sugar dissolves. Cool it by holding the tube under a jet of water, and when cool taste a drop of the liquid. Have the sugar particles been divided by dissolving? How do you know? Arrange a filter paper (Fig. 8) and filter the sol., using a filter stand and collect- ing the filtrate in another t.t. (Fig. 9). Touch a drop of the filtrate to the tongue with a stirring rod (s.r.). Note whether the sugar has gone through the filter paper. Divide the liquid into two parts. Save one for Exp. 6, and dilute the other with an equal vol. of H 2 ; then cover the t.t. with the thumb or hand, invert it (Fig. 10) and, holding it away from the table, shake the contents vigorously. Taste a drop of the sol. Note whether the Fig 9 sugar particles have been further, divided. Supplementary, Read very carefully Rule 14 and the Model for Taking Notes, (a) Dis. a little CuCl 2 or Cu(NO 3 ) 2 in water, boiling as before, and filter but do not taste the sol. (b) Dis. also a little NaCl, filter and taste the filtrate. Evaporate. Do substances in sol. pass through a filter paper ? Many substances like SiO 2 and BaS 0* are not sol. in water or acids, others, like Zn, Cu, etc., are sol. hi acids only, (c) Heat a platinum wire in a Bunsen flame. Note if it undergoes change. Fig. 8. Fig. 10. Terms: Physical division, physical solution, insoluble, dilution, molecule, evaporation, properties, filtrate, residue. 5. PHYSICAL CHANGES. Solution and Crystallization. 1. Fill an e.d. f full of water, heat it, and add small pieces of alum until the liquid becomes thick. Replace the water lost by evap- oration. Now put in a narrow piece of cotton cloth so that it lies in the liquid but does not touch the bottom of the dish, and set the latter aside to cool. Observe occasionally, meantime doing the following : 2. Cautiously boil about 5 g copper sulfate in 5 CC H 2 in a t.t. until it is dissolved. Then place the t.t. in an oblique position and let the liquid cool. If necessary, leave till the next laboratory hour. Note the formation of crystals in 1 and 2, and observe their form, color, luster, angles, etc. Are these illustrations of physical or of chemical changes, and why ? Trace each step in the process. Which seems more soluble, alum or sulfate of copper ? Are they more soluble in hot or in cold water ? 3. Put a few crystals of copper sulfate into an i.t. or small t.t. and slowly heat. Observe the sides of the tube and any change of color, luster, hardness, and form in the crystals. Explain. When the tube is cool add a drop of water. 4. Experiment in the same way with some of the crystals of alum, tasting the powder obtained by heating. 5. Put a crystal of sodium sulfate and a small piece of calcium chlorid on separate pieces of paper and leave them in the locker exposed to the air till the next exercise. Describe the result with explanation. Supplementary. (a) Put into an e.d. as much powdered S as will stay on the point of a very small knife blade. Cover it with a very little C S 2 (keep the flame at a distance from this substance) so as to dis. the S, let it evaporate in a draft of air, then watch closely as the C S 2 evaporates. Describe and explain the phenomena. Put a drop of this sol. on a microscopic slide and watch it closely under the microscope as the CS 2 evaporates, (b) Dissolve and re-crystallize Na 2 SO 4 . (c) Mix sols, of alum and CuSO 4 and try to crystallize the two substances together. Are the above salts soluble or insoluble ? Terms: Crystal, amorphous substance, mother liquor, saturation, super- saturation, water of crystallization, deliquescent, efflorescent, luster. 6. CHEMICAL, CHANGES. I. Sulfuric Acid and Sugar. To the sol. saved from Exp. 4 slowly add sulf uric acid, H 2 S 4 , in a small stream, holding the tube with a t.t. holder, and the bottle as in Fig. 11 (read Rule 9), till the substance changes color. Add a little more acid, and if the sugar solution is strong enough it will cause the substance to swell and run over the tube. Observe the color, odor, and temperature, but do not taste it. Does it appear Fig. 11. to be a solid or a liquid ? Sugar is a compound of C and H 2 0. H 2 S0 4 has great affinity for water. From these facts explain the phenomena. Clean the tube with water, using a brush if necessary. II. Heat and Sugar. See whether heat will break up sugar, by dipping a short piece of glass tubing moistened with water into a little sugar and holding it in a Bunsen flame. Describe all you see, note the odor, and state your conclusions. What produced the chemical change ? III. Combustion of Wood. Hold a small stick in a flame. State whether the changes observed are chemical, or physical, with reasons. IV. Changes in Solutions. Add a little hydrogen chlorid, HC1, to 5 CC Pb(N0 8 ) a sol. The hydrogen chlorid and the lead nitrate have become lead chlorid and hydrogen nitrate. The former product is insoluble and is therefore thrown down (precipitated). To 5 CC of CuCl 2 sol. add a little N H 4 H ammonium hydroxid and notice any evidence of change. Supplementary. (a) To 5 CC of HgCl 2 sol. add a few drops of KI sol. (b) Add a few drops of KI sol. to 5 CC of Pb(NO 3 )2 sol. (c) On a few bits of Cu in an e.d. pour a few drops of nitric acid, HNOa. Describe all you see. Are these chemical, or physical changes ? Why ? Terms : Combustion, chemical solution, affinity, precipitation, chemical 7. ELEMENTS AND COMPOUNDS. Fig. 12. Synthesis. Fill an i.t. (from Exp. 2) not over -j- full of an intimate mixture of one part by weight of S (finely pow- dered brimstone, or flowers of S) with two parts of fine Cu filings. Observe that the two elements are entirely distinct, and note the color and luster of each. Now heat the tube very slowly for a minute (moving it alternately out of the flame and into it, so as not to break the glass) then heat very strongly, 'the upper part first (Fig. 12). Watch the contents of the tube for evidence of a chemical change. What is the evidence ? When this change has taken place throughout the whole mass let the tube cool for a minute, then heat an instant, break the -tube with a jet of water, and examine the substance. Note whether it resembles Cu or S in color or luster. Describe fully what you saw, state what is supposed to have taken place, and give an equation to express it. Supplementary. (a) Mix Fe filings and S (in about the same proportion as Cu and S), try to separate the Fe with a magnet and the S with C S 2 from a part, then heat the other part in an i.t. Test the product with magnet and CS 2 ; also by adding a little H 2 O and then HC1 in an e.d. An offensive gas is liberated which either element alone would not give if similarly treated. Describe fully with equations, (b) Light a match, and as it burns watch the colors of the flame and see if there is any evidence of a product being formed. The match contains the elements P, S, and C, which combine with the element O in the air to form compounds called oxids of P, S, and C (v. Exp. 9). (c) Burn a piece of charcoal and observe. The products are for the most part invisible gases, (d) Heat in an i.t. a little granular pyrite, FeS 2 , and finally test the residue with a magnet. Terms: Synthesis, sulfid, oxid, binary compound, element, gas, luster, residue. Fig. 13. 8. PREPARATION OF OXYGEN. Fill 4 or 5 wide-mouthed bottles recs. with water, invert them on the shelf of a p.t. in which the water is 3 or 4 cm above the shelf. Mix on a paper 5 or 10 g KC10 a (not pulverized) and 3 or 4 of powdered Mn0 2 . Put the mixture into a large dry t.t. which should not be over J- full. Adjust a stopper and d.t. and hang the app. on a r.s. (Fig. 13). Direct a Bunsen flame against the t.t., holding the lamp and slowly moving it. Avoid heating too long in one place (take it away from the tube occasionally for a few seconds), or the tube will melt. Watch the bubbles in the d.t., collect the escaping gas in the recs., and notice the bubbles as they burst, and whether the gas has color. Explain, and after a time observe again. Is there evidence of a gas, or a solid, or both ? As soon as the flame is taken away remove the d.t. from the trough to prevent the water drawing back and break- ing the tube. Why is there this back action ? Let the recs. remain on the shelf till wanted, or, if taken out, keep them covered with glass plates (Fig. 14). After doing Exp. 9 clean the t.t. by covering the residue with water, closing the mouth of the tube with the thumb or hand, and shaking the contents vigorously, holding it away from the table. Supplementary. Does the O occupy more, or less, volume than the factors from which it was obtained ? Why ? Would it weigh more, or less ? Why ? The MnO 2 takes no part in the reaction, but is used to distribute and equalize the heat and lower the temperature of dissociation. Name all the substances in the t.t. at the end of the exp. Fig. 14. Terms : Factors, products, dissociation. 9. COMBUSTION IN OXYGEN. 1. Put a burning splinter into a rec. of for an instant, note the color and vigor of the flame, then remove, blow out the flame and put in the glowing stick. Repeat till there is no effect. State accurately everything you saw and heard. Wood consists largely of C. Explain the combustion and write an equation for it. Test the product by adding 4 or 5 CC of lime water, Ca(OH) 2 sol.; shake it well and notice the effect. 2. Make a d.s. by hollowing out the end of a crayon, or electric light carbon, and attaching a Cu wire. Put into it a bit of S, hold the whole in a flame till the S burns, then lower it into a rec. of (Fig. 15). Notice the color and vigor of the flame, and the color and state of the product, explain what you see and write the equa- tion. Name the product and test it by cautiously noting the odor, and also by putting a drop of K 2 Cr 2 7 sol. on paper and holding it in the gas, noting any Fig - 15 - change of color. 3. Put into an e.d. with a pair of forceps (don't handle it) a piece of P, half as large as a pea. Dry it by rolling it lightly on paper, then put it into a d.s. Heat for an instant the end of a wire or file, touch the P with it and lower the spoon at once into a rec. of 0. Observe the color of the flame and of the product. Describe, also write the equations. When combustion stops burn every bit of the P by holding the d.s. in a flame. Add a few cc of H 2 to the rec., shake it well and drop in a piece of blue litmus paper. Supplementary. What became of the in the above cases ? Would the product in each case weigh more or less than the C, S, P ? How do you know ? (a) Cover the bottom of a rec. of O with sand or H 2 1 or 2 cm deep. With forceps hold for an instant in a flame one end of a picture-cord wire 5 or 10 cm long, then dip it into a bit of powdered S. Hold it again in the flame till the S burns, then thrust it into the rec. of O. If the Fe does not burn try it again, or repeat with another rec. (have but little S on the wire). Describe the combustion and the product, and give the equation, (b) With forceps hold in the flame a piece of Mg ribbon till it begins to burn, then instantly thrust it into a rec. of O. (c) Try Zn tipped with S. Terms : Supporter of combustion, combustible, kindling point. 1O. OXYGEN. Fig. 16. I. Oxygen from Oxids. Heat strongly 1 or 2 g of HgO in a t.t. or i.t. and thrust a glowing splinter into the tube while still holding it in the flame (Fig. 16). Note the color of the HgO while it is being heated, observe the sides of the tube, and finally pour out and carefully examine the contents. Explain, and give the reaction. Save the residue. II. Oxygen from Nitrates. Put into a t.t. about 1 of Pb (N0 8 ) 2 , heat it and test the gas as before. Note any snapping, the color of the fumes, which are N 2 and (the O being colorless), and the color of the residue, PbO. Also write the equation. III. Oxygen from Chlorates. Try to obtain oxygen in the same way by heating a few crystals of K C10 3 . Test as before, and write full notes. Supplementary. What 3 classes of substances have you found which yield O ? From which is the oxygen obtained most easily ? N 2 O will also support combustion of C, S, P, but not as readily as pure O. Heat and test : (a) (b) NaNO 3 . Terms: Oxid, chlorate, chlorid, nitrate, residue. 11. SEPARATION OF NITROGEN. Fill a p.t. with water 3 or 4 CC above the shelf. Prepare a d.s. with a wire bent sharply 5 or 6 cm from the crayon. Pass the wire through the orifice in the shelf so that it will reach half way up an inverted rec., fasten it there (so as to be easily removable) with the mouth of the rec. under water (Fig. 17). When adjusted remove the rec., leaving the wire. Using forceps and e.d. put a piece of P (the size of half a pea) into Fi s- 17 - the spoon. Touch it with a warm (but not too hot) wire or file handle, and instantly invert the rec. over it as be- fore, pressing the latter down and holding it steadily with the hand till combustion ceases. Was there any escape of gas ? Before re- moving the d.s. be sure the combustion has stopped, and let no air enter. Compare the combustion and the product with the same in the oxygen exp. Describe fully with equation. Finally remove the crayon without admitting air or disturbing the rec. Burn any remaining P in a flame and leave the rec. till the gas becomes toler- ably clear, then remove with a glass plate, turning the rec. right side up and keeping the water in the bottom. Set this aside for Exp. 12. Supplementary. (a) Try to separate the N in air with S in a d.s., setting the S on fire by holding a flame over the adjusted spoon, (b) Try paper or charcoal. What elements do these exps. show to exist in the. air ? N may also be separated by forcing air over red hot Cu, which forms CuO. It may be obtained from compounds, such as nitrates and ammonia. 12. NITROGEN AND AIR. I. Properties of N. (1) Put a burning stick into the rec. of N (Exp. 11), sliding along the glass cover enough to admit it. Note the effect on the stick and on the gas. Try it with a glowing stick. Is the spark rekindled, or extinguished ? (2) See whether the P, S, and C on the end of a match will burn in the gas. Is there any equation ? Why ? Is N a combustible ? A supporter of combustion ? (3) Test the liquid with blue litmus paper. Describe and explain. II, Composition of Air. Measure accurately the water in the rec. of N by pouring it into a graduate and recording the volume in cc. Then measure the total capacity of the rec. in the same way, and compute the percentage of and of N (by volume) in the air, giving the computation and remembering that the first vol. of water represents the vol. of burned. If any air was forced out in Exp. 11, will the per cent of found be too large or too small ? Explain. Supplementary. Compare the properties of N with those of 0. Air con- tains also C 2 (tested for by Exp. 36) and H 2 O (shown by setting a pitcher of cold water in a warm room). Make tests for each and explain. From the per- centage of N there must be subtracted about 1% of the recently discovered ele- ment argon, A, a gas more inert than N. Terms: Inert substance, percentage by volume and by weight, acid, litmus paper. 13. HYDROGEN FROM ACIDS. Fig. 19. I. Preparation. Fill 4 or 5 recs. with water and invert in a p.t., then put into the gen. (Fig. 18) (or use the same app. as for making 0) 8 or 10 g granu- lated Zn, cover with H 2 and add 5 CC of HC1 through the thistle tube. Have the bearings perfectly tight, and, without applying heat, collect the gas like 0. Observe and describe the action and note any heat. If action stops add more H Cl. Leave the recs. of gas in the ^s- is. p.t. till wanted in II (or if removed keep them inverted, Fig. 19). Has the gas any color ? Why ? Clean the app. and save the Zn. II. Tests. (1) Lift a small rec. of H, hold it inverted, and thrust a burning stick into the gas. Note any explo- sion and whether the gas or splinter burns. (2) Try it with another rec. and then cautiously look into the open mouth of the latter, noting the colors of flame. Explain fully the explosion, combustion, etc., with equation. Note the (3) color and (4) odor of (the impure) H. (5) Collect by up. disp. a t.t. of H, and test by putting it mouth to mouth with a t.t. of air and then bringing the two open tubes successively to a flame. Supplementary. (a) Put 2 or 3 small pieces of Zn into a t.t. (use a t.t. holder), cover it with water and add a little H 2 S0 4 . Notice the action, test the combustibility of the gas, and write the equations, (b) Put into a t.t. a few Fe filings, add H 2 O and HC1. Test the gas as before, (c) Try Fe and H 2 SO 4 . Make a complete record of all work. From what class of substances has H been obtained, and how ? Is H a combustible ? A supporter ? (d) Try the action of Zn and H 2 S O 4 , without H 2 O, cautiously noting the odor, (e) Pass H into euchlorin (Exp. 38). (f) Fill a rec. half full of water, invert it in a p.t., letting air fill the upper half. Now fill the rest with H from a gen., then bring the mouth of the rec. to a flame, (g) Make a philosopher's lamp (Fig. 20), but before lighting the hydrogen, test the gas by collecting a t.t. full by upward displacement and bring- ing it to a flame. If a sharp sound ensues there is danger, as the gen. contains air. If only a low muffled sound, the gas may be lighted. Lower a larger open glass tube over the flame. Other flames give the same result. Terms : Upward and downward displacement, philosopher's lamp, singing flame. Fig. 20. 14. HYDROGEN FROM WATER. I, Action of Na on H 2 0. (1) Put into a clean rec. 15 or 20 CC of H 2 O. Have a cover of paper or cardboard, not glass. Observe the color and luster of freshly cut Na; take a small piece from the naphtha in which it is kept (using forceps and dry e.d.), drop it into the rec., and cover the latter at once (Fig. 21). Describe the action, note any fumes or gas (try to ignite it), and write equations. When action stops take off the cover and bring the fumes near a Bunsen flame, or hold the lower openings of the burner close to the mouth of the rec. and notice the color im- parted to the flame. This is the flame test for Na and its cpds. Are the fumes solid or gaseous, and what becomes of them ? (2) Hold a piece of moist red litmus paper in the fumes, also put one into the liquid. Test the liquid by adding a little to these sols.: (3) FeCl 3 ; (4)FeS0 4 ; (5) A1C1 8 . (6) Try the action of Na on hot H 2 by boiling a little H 2 O in a t.t. and pouring it into a rec., then dropping a piece of Na on it and covering it at once. Note all the phenomena and write equations for : (a) the action of Na on H 2 ; (b) the combustion of H, and (c) Na ; (d) the sol. of Na 2 0. II, Action of K on H 2 0. Perform the exp. as above, using K and cold H 2 0, and making similar observations, notes, and tests, including flame tests. Supplementary. Which has greater affinity for H 2 0, Na or K ? (a) Col- lect H by putting a small piece of Na in a wire cage and quickly thrust it under an inverted t.t. full of H 2 O in a p.t. Test the gas. What proportion of H in water is replaced by K or Na ? Are the metals heavier or lighter than H 2 O ? (a) Moisten a piece of paper, put it into a rec. and drop on the moist paper a bit of Na and cover it. When action stops try to light the fumes by bringing a Bunsen flame to the mouth of the rec. (b) Try the same with K. 15. AMORPHOUS CARBON. I. Carbon from Wood. Put 2 or 3 small, thin pieces of wood into a small Hessian cruci- ble and cover them with sand (Fig. 22). Apply a Bunsen flame for half an hour, or until gases cease to come off (meanwhile do II, III, and Exp. 16). Notice any gases rising and try to kindle them. Observe the color and odor. Finally remove the carbon with forceps and save the sand. Examine the carbon as to color, weight, volume, porosity, and brittleness (compare with the original 22 wood). See whether it burns with flame or only glows, on igniting it in a flame. II. Carbon from Candle, Oil, Gas. Hold a short piece of white crayon, or of glass tubing, in the flame of a Bunsen burner, with the lower openings closed, then open the orifices and try to burn off the deposit. Try to collect C from a candle flame and from that of a kerosene lamp in the same way. The candle, oil, and gas consist mainly of cpds. of C and H. Which seems to burn at the lower temperature, C or H ? III. Carbon from Sugar, Starch. Heat in a narrow tube a very little sugar, also starch. State what you see and conclude. Supplementary. Gases burn with flame. Solids glow. What has the destructive distillation of wood in I. done ? Cpds. of C and H (called hydro- carbons) are solid, liquid, or gaseous, (a) Try to obtain carbon in any other way, (b) Hold a piece of charcoal in water for a minute, (c) Weigh a piece of wood, then distil it, and finally weigh the product, (d) Put some small pieces of wood into an i.t., attach a d.t. and heat. Collect the gas (Fig. 13). (e) Test the gas. Terms : Amorphous, crystalline, dimorphous, trimorphous, porosity, specific gravity. 16. PROPERTIES OF CHARCOAL,, I. Carbon a Reducing Agent, Fill an i.t. not over full of an intimate mixture of CuO and C (powdered charcoal), about 7 parts CuO to 1 part C by weight. Heat it very cautiously at first, then strongly till you see evidence of a chemical change. What is the evidence ? What caused the mixture to rise? After the action stops is there any change in color ? When sure that no more action will ensue, cool it for a minute and pour the contents into a dry e.d. Examine it carefully as to color and luster. Explain, giving an equation to express the chemical change. Finally test the residue by adding 2 or 3 CC HN0 3 , noting the color of the fumes and of the residue. See whether HN0 8 has a similar effect on the original mixture of CuO and C. What does the test show ? II. Carbon a Decolorizer. Shake up 5 or 10 g of bone black animal charcoal in a t.t, or rec. with 10 or 20 CC cochineal sol., then filter and notice the color of the liquid. If not perfectly colorless pour it again on the same filter, using more carbon if needed. Try in the same way sols, of indigo and litmus ; also of K 2 Cr 2 7 and K Mn0 4 . Can you draw any general inference of the decolorizing action on animal, vege- table, and mineral pigments, the first three being animal or vege- table, the last two mineral ? K 2 Cr 2 7 may be turned slightly yellow by alkali in the bone black. III. Carbon a Deodorizer or Disinfectant. Prepare a sol. of H 2 S (Exp. 42). Notice the odor of the gas and its solubility. Put into a rec. 5 or 10 g of powdered charcoal and pour upon it 10 or 20 CC H 2 S sol. and shake the mixture well. Then pour the whole on a filter, collect the filtrate in a clean t.t. and see if any odor remains ; if so, mix and filter again, using more char- coal if necessary. The H 2 S has been absorbed physically into the pores of the coal and partially oxidized there. This illustrates the absorbent action of charcoal on gases, animal effluvia, and micro- organisms in the sick room. 17. EXPERIMENTS IN COMBUSTION. I. Structure of Flame. (1) Make a careful examination of the parts and colors of a candle flame, and make a drawing to show them. Move the candle slightly in the air to show the outer flame. This is best seen in a dark room. Describe fully. (2) Examine the structure of a Bunsen burner (unscrew the top if necessary), make a drawing to show the orifices, and state what use they subserve. Keplace the tube and light the gas. Hold the flame in front of a dark object (as a blackboard), examine the parts, make a drawing, give a brief description, and state the color of each part. If possible, put the flame in direct sunlight, and study the parts from its shadow, to confirm your results. II. Combustion of Flame, (1) Put a moist stick across the base of the Bunsen flame for an instant, and notice what parts are burned. Hold a stick just above the inner cone of the flame. Make sketches of results. (2) Press quickly down on the flame with a paper, or pasteboard, remove before it burns, and notice the shape of the charred part, or press down on the flame with a fine wire gauze, and observe by the glowing of the wire where the heat is most intense. Sketch. (3) Put one end of a small d.t. into the inner blue cone, not into the lamp, and try to light the gas at the other end. (4) Thrust a match quickly into the inner cone near the bottom. If done quickly the phosphorus will not take fire. The match contains a supporter and a combustible. Why does it not burn ? In what parts of the flame does combustion occur ? Supplementary. Examine : (a) an ordinary gas flame ; (b) the flame of a kerosene lamp ; (c) the flame of a burning splinter, or match, holding it vertical and breaking off the charred part as fast as it forms. Have all flames practi- cally the same structure ? 18. EXPERIMENTS IN COMBUSTION. III. Light of Flame. (1) Sprinkle a very little charcoal dust into a Bunsen flame, and note any change of light or color, or, better, dip a fine splinter into powdered charcoal and thrust it into the openings at the base. Notice flame. (2) File a nail or other metallic substance over the flame, or sprinkle in CuO, or " iron by hydrogen." (3) Also stir up the dust near the flame, or tap the lamp with the fingers. What produces flame ? What is the cause of light in a flame, and what flames give light ? (4) Close the orifices at the base of the burner, and explain the change of light. (5) Set fire to a small piece of charcoal, by holding it in a flame, and see whether it burns with flame or only glows. What does this show ? IV. Kindling Point. (1) Light the gas and hold a fine wire gauze 3 or 4 cm above the burner. Why does it not burn above the wire ? (2) Extinguish, then relight the gas above the gauze. Result and explanation. Gradually lift the wire till the gas will not burn. (3) Again light the gas above the gauze, and hold another gauze above the flame, so as to confine it above and below. State three conditions of combus- tion, define each, and show how this exp. illustrates them. Supplementary. Why does a lamp smoke ? Why does phosphorus take fire spontaneously ? Why does gunpowder explode ? Why will it burn with- out air ? Why do we exclude the air to put out a fire ? Why does blowing a flame sometimes cause it to burn, and sometimes extinguish it ? Why does cannel coal burn with flame ? When will a mixture of H and air not explode ? Why will some substances burn in water ? See which has the lower kindling point, P or S, by putting each on one end of a piece of iron at equal distances from a flame which heats the other end. Terms : Kindling temperature, spontaneous combustion, combustible, sup- porter. 19. POSITIVE AND NEGATIVE ELEMENTS. I. Dis, Ag in HN0 3 and ppt. Ag with Cu. Put a ten-cent silver coin into an e.d. and add 10 or 20 drops of HN0 3 . Warm it, if necessary, over asbestos, and watch the result as to action, color of liquid, color of fumes, etc., and give the reason for each, with equa- tion. When action stops, or the coin is dissolved, add 10 CC H 2 0, then pour it into a t.t. and put in a copper wire (Fig. 23). Leave for 10 to 30 minutes. At this point begin II., but observe any deposit on the wire, noting its color, luster, texture, crystalline form, and any change in the color of the liquid. Ex- plain, giving equation. Save the Ag. Which has greater affinity for N 3 , H, or Ag ? Why is H not set free ? II. Dis. Cu in HN0 3 and ppt. Cn with Pb. Put into a t.t. or e.d. a thin piece of sheet Cu, say l and (6) restore the color with KOH sol. Supplementary. (a) Add a few drops of H 2 O to a sol. of red litmus, and also to one of blue, (b) Add to both red and blue litmus sols, a sol. of NaCl. (c) Try N H 4 C1 sol. (d) K N 8 sol. (e) H NaC O 3 sol. (f ) H K S O 4 . (g) CuS O 4 . Terms : Acid, alkaline, and neutral reactions. 22. SOLUBLE SALTS BY NEUTRALIZATION. I. Sodium Chlorid. Pour into an e.d. not over 5 CC NaOH sol., and into a clean t.t. or beaker 4 or 5 CC HC1. Now add some of this latter, a little at a time (Fig. 25), to the NaOH sol., stirring it meantime till the product is neutral to litmus paper ; when nearly neutral add a drop at a time with a s.r. and test with both colors, using only the end of the paper and keeping it on the side of the e.d. If blue litmus paper is reddened by the sol., add NaOH sol., a few drops at a time. If red litmus is turned blue add a drop of H Cl. When the sol. does not affect either red or blue litmus left in it for a minute, show it with both papers in it to the instructor, then filter and evaporate the liquid to dryness by boiling it over a plate and abestos paper (Fig. 26). When it is cool, examine the residue and taste it. What is the object of evaporation ? Explain what took place when the acid and base were mixed, and give the equation to express it. Sift a little of the salt into the flame. The color shows a cpd. of Na. Test for Cl by Exp. 27. II. Potassium Sulfate. Into an e.d. put 5 CC KOH sol. and neutralize it with dilute H 2 S0 4 , using both test papers. When sure it is neutral, evaporate most of the water and taste the product. Explain the action, giving the equation. Sift a little into a flame. The color shows a K cpd. (best seen through blue glass). Test S0 4 by Exp. 31. III. Ammonium Nitrate. Neutralize NH 4 OH with HN0 3 (preferably dilute) in the same way as before. Stop evaporation when dense fumes begin to ap- pear. These fumes indicate a decomposition of the salt by heat (v. Exp. 34). Supplementary. How would you make by neutralization NaN Os, K N O 3 , K Cl, N H 4 C1, (N H 4 ) 2 S O 4 ? Write also equation for each. Weak acids will not neutralize strong bases, and vice versa. Hence, salts like NaaC O 8 are not neutral. How do these exps. illustrate the law of definite proportion ? Terms : Neutralization, double decomposition, definite proportion, evapora- tion, fumes. 23. SOLUBLE SALTS FROM METALS. I. Zinc Chlorid. To a piece of Zn in a t.t. add water and a little HC1. Describe and explain the action, and when it ceases, pour the liquid into an e.d. and evaporate to dryness. Observe and taste the salt. Name it and write the equation. To test the salt, add a little H 2 O to dis- solve it and divide the sol. into 4 parts. Test for Cl by Exp. 27, and for Zn by Exp. 70. II. Iron Sulfate. Dissolve as above a few Fe filings in dil. H 2 S 4 . When action stops add H 2 O, filter, and evaporate the filtrate. Then dissolve the salt in water after having examined it. Name it and write the equation. Test it for Fe by Exp. 63, and for S 4 by Exp. 31. III. Copper Nitrate. Dissolve a little Cu in dil. H N 3 , pour off the liquid, evaporate, and then add H 2 0. Test for Cu by Exp. 56. and for N0 3 by 82. Make full notes. Supplementary. The salts in Exps. 22, 23 are sol. in water. Insoluble salts are not made in this way. PbCl 2 is only partially insoluble, hence HC1 will not dissolve much Pb. Table A shows that there are but two soluble salts of Pb ; hence most acids do not act upon that metal. By reference to this table you can judge what acids will probably act on a given metal. Will H 2 S O 4 dis. Ba? Pb? Cu? Will H Cl probably dis. Sn ? Ag? Hg? Mg? Will H 3 P0 4 dis. Pb? Ca? Ag? (a) Try any of the above. (b) Try .to dis. Pb in HC 2 H 8 O 2 . Compare chemical sol., as shown in 23, with physical sol., Exp. 4. What two processes in chemical sol.? Terms : Insoluble, soluble, saturation, supersaturation. 24. SOLUBLE SALTS FROM CARBONATES, HYDROXIDS, OXLDS. I, Carbonates. (1) To a piece of CaC0 3 (marble or limestone) in a t.t. add H 2 0, and a little H Cl. When the action stops, pour a little of the liquid into an e.d., evaporate and notice the residue. See if it will dis. in H 2 0. State your observations and the reaction. Test for the presence of Ca by Exp. 74. (2) Try Na 2 C0 3 (or HNaC0 3 ) with HC1. (3) CaC0 3 may be tried with H 2 S0 4 or HN0 3 . II. Hydroxids. (1) To some Fe(OH) 3 (made by adding NH 4 OH to FeCl 3 sol., and pouring off the supernatant liquid after the ppt. settles) add drop by drop just enough HC1 to dissolve it. (2) Try also HNO 3 and H 2 S0 4 on separate ppts. of Fe(OH) 3 . Evaporate and dis. in H 2 as before. Test for Fe by Exp. 63. (3) Try A1(OH) 3 (made from A1C1 3 sol. and NH 4 OH) with HC1. Evaporate, dis. in H 2 O, and test for Al by Exp. 64. HE. Oxids. To 28 PbO (litharge) in an e.d. add some dil. HN0 3 and heat it. Decant on a filter, partly evap. the filtrate, add H 2 0, and test for Pb by Exp. 48. Supplementary. Notice from Table A what carbonates and hydroxids are soluble, (a) Add H 2 to a little Na 2 CO 3 (or K 2 C0 3 ) in a t.t. and boil a minute, (b) In another tube cautiously add HC1 to Na^COs.. Explain the difference between (a) and (b). (c) Into (a) pour cautiously a little H Cl. De- scribe the action and explain it with reaction. Sol. salts may be made from many other classes of cpds. besides the above. Terms : Physical and chemical solution, decantation. 25. INSOLUBLE SALTS BY PRECIPITATION. Insol. Salts of Pb. (1) Pour into a t.t. 5 CC Pb(N0 3 ) 2 sol. and add a few drops HC1. (2) Try it again, substituting Nad sol. for HC1. (3) Use also a sol. of N H 4 C1. Record results and write equations. (4) Now in place of Pb(NO 3 ) 2 use a sol. of Pb(C 2 H 3 2 ) 2 , try the action of the same three reagents as previously used, and make a similar record. What is the ppt. in each case ? Could you obtain the same ppt. by putting together any other sols., and if so, what ones ? To 5 CC of each of the following sols, in a t.t. add a little sol. of Pb(N 3 ) 2 or Pb(C 2 H 3 2 ) 2 and write the equation, underlining the ppt. and writing the color above. (5) K 2 O0 4 . (6) K I. (7) K Br. (8) NaOH. (9) Na 2 C0 3 . (10) Na 2 S0 4 . (11) K 4 FeCy 6 . Supplementary. What are the only two soluble salts of Pb ? Law of Ppn. : Whenever a mixture is made of two sols., one of which contains the positive part and the other the negative part of an insoluble cpd., a ppt. of the insol. cpd. will always form. From Table A what salts of Ba are insol. ? (a) Try to make some of them by the application of the above law. (b) Also try Fe(0 H) 3 . (c) Make HgS. (d) Try to make MnS. (e) Make CaC O 8 . Terms: Insoluble, precipitation, positive, negative. 26. HYDROCHLORIC ACII>, HC1. Preparation. (1) Fill 2 recs. % full of water. Connect the apparatus as in Fig. 27, observing how the tubes extend. (A safety-tube may also be used if desired.) Then put into a flask 10 g NaCl (preferably fused) and 20 CC H 2 S0 4 which has previ- ously been mixed with 5 CC of H 2 0. Be sure you have enough acid, or the flask is liable to crack. Heat slowly for 10 or 15 minutes over asbestos, but do not let the froth extend to the neck of the flask. Look for any current in the liquid of the rec. and explain. (2) Detach the apparatus (at a, Fig. 27) and pass some of the escap- ing gas over a few drops of NH 4 OH in an e.d. (If much gas is accidentally breathed, inhale NH 3 .) Describe the fumes (note whether they have any odor different from H Cl or N H 3 ), name them, state the color, and write the equation for their production. This is the ammonia test for H Cl. Ascertain whether the product is gaseous, or solid, by dipping a rod into strong H Cl and holding it over a bottle of NH 4 OH. (3) Pass some of the gas from the gen. into a sol. of blue litmus. What does this show as to the solubility of HC1 ? What else does it show ? Supplementary. How would you test for the presence of N H 8 ? Generate HC1 if possible from : (a) KC1 ; (b) NH 4 C1, using an open t.t. and applying the usual tests, (c) Try PbCl2. Law of Formation of Gases : When two substances, which can react so as to liberate a gas, are put together, that reaction will always take place and the gas be formed. Fig. 27. Terms : Wolff bottle, flask, safety -tube, muriatic acid. 27. HYDROCHLORIC ACID, HC1. Properties and Tests, (1) Test the liquid in each bottle (Exp. 26) with blue litmus paper. (2) Taste a drop, using a s.r. (3) Cautiously note the odor. (4) Put a piece of Zn into a t.t. and pour over it 5 or 10 CC of the contents of the first Wolff bottle. (5) If a gas escapes, test its combustibility. Explain fully with observations and equations. (6) Put into a t.t. 5 CC Pb(N 8 ) 2 sol. and add a little of the liquid from the first bottle. If a ppt. falls, pour a small part of it into another t.t., add a little H 2 0, and boil a minute. Does it dissolve ? What does that show ? Now add a little K 2 Cr 2 7 (or K 2 Cr0 4 ) sol. Explain. (7) To 5 CC AgN 3 sol. add a little of the acid. If a ppt. falls let it settle, then pour off most of the supernatant liquid, leaving the residue ; then add N H 4 H and shake it. Finally acidify cautiously with HN0 3 . Explain all results. (8) Test HgN 3 sol. in the same way, adding N H 4 H at the end, but not HN0 3 . By any of the above exps. can you determine which bottle contains the stronger acid ? Supplementary. (a) Add HC1 to Cu(NO 3 ) 2 sol. and explain the result, (b) Separate Ag from Cu in a mixture of solutions of their nitrates. Try the action of HC1 on sols, of : (c) Co(NO 3 ) 2 ; (d) NaNO 3 ; (e) KN0 3 ; (f) MgSO 4 . What 3 chlorids are insol. in H 2 O, and how are they made ? Terms : Analysis, reagent, pungent, acidify, alkalize. 28. ETCHING WITH HYDROFLUORIC ACID, HF. Cover thinly with beeswax or paraffin one side of a small piece of glass. Spread the wax evenly over the surface, by warming the other side of the glass and pour- ing off the excess of melted wax. With a sharp metallic point, as the handle of a file, mark Fig. 28. some design through the wax when cold (Fig. 28). Put into a lead dish (it will spoil a porce- lain e.d.) a very little HF sol. (be exceedingly careful not to get any on the flesh) and with a camel's-hair brush spread some of it over the design on the glass. Do this several times. Finally, after a few minutes wash away the acid from the glass, melt and pour off the wax, wiping off what remains with a cloth wet in naphtha, or alcohol. Examine closely the result and describe it. By reason of its affinity for Si0 2 , HF acts on the glass and forms SiF 4 . The equation should be written. Supplementary. Etch a t.t. so as to make a graduate of it. Why cannot H F sol. be kept in glass bottles ? H F is made by treating powdered CaF 2 (fluorite) with H 2 S 4 in a lead dish. Write the equation (v. Exp. 89 for other tests). The fumes must not be inhaled. Terms : Etching, fluor spar, fluorid, fluorite, silica. 29. NITRIC ACID, HNO 8 . Fig. 29. I. Preparation. Introduce into a glass retort through the tubulure, holding the foi*mer so as not to have the chemicals touch the neck of the retort (Fig. 29), 10 or 15* fine NaN0 8 (or KN0 3 ) and 20 or 25 CC 3 H 2 S0 4 . Adjust the apparatus as in Fig. 30, having the neck of the retort pass to the bottom of a wide t.t., which is surrounded by water in a wide tumbler, or bottle. The water is to cool and condense the acid from the vaporous state in which it passes over. Apply the Bunsen flame, using a plate and as- bestos, for 15 or 20 minutes. Notice the liquid running down the neck of the retort, also any colored fumes name and account for the latter, and see whether they increase with the heat the color of the liquid in the t.t., and the cause of it. Do the ordi- nary reactions (which should be writ- ten) account for the fumes ? Observe also the color of the product in the retort. Heat may have reduced some of the white Na 2 S0 4 to dark-colored Na 2 S. Use great care not to get any of the acid on the hands. The anti- dote, after thorough washing, is HNaC0 3 (v. Eule 19). II. Tests. (1) Test the vapor from the end of the retort with a few drops of N H 4 H. (2) Put a drop or more of the acid on a very few Cu filings in an e.d. Observe and explain with equation. (3) Try with a s.r. the action of a drop on the finger-nail, then wash it off and add a drop of NH 4 OH. This shows its action on animal mat- ter. (4) Try it also on a feather or on silk. (5) Try its decolor- izing action on 3 or 4 CC of indigo sol. in a t.t. Try its action on insoluble salts, e.g.: (6) CuS ; (7) CaC0 8 ; (8) BiOCl. State what this shows of the solubility of the respective nitrates (v. alsoExp. 82). Supplementary. (a) Compare the action of H N O 3 and H 2 S O 4 on wood. Could HNO 3 be made from Pb(NO 3 ) 2 ? How are nitrates made? (b) Make Zn(NO 8 ) 2 . (c) Try to dis. a little Sn in HN 3 in an e.d. (d) Try Sb. (e) Put a drop of commercial HNO 3 on writing paper, another on newspaper. The latter contains wood pulp, (f) Try to decolorize anilin solutions. Terms: Fuming nitric acid, metastannic acid, xanthoproteic acid, salt of nitric acid, nitrate, tubulure. Fig. 30. 30. AQUA REGIA. I. Preparation. Pour 2 or 3 CC of HISTOg into a t.t. containing 6 or 8 CC of HC1. If there is no evidence of chemical action, warm the mixture a minute and observe. To what is the color due ? Give reaction. II. Tests. (1) Into a part of the aqua regia introduce a little gold leaf by winding it around a moist s.r., not letting it touch the sides of the t.t. (2) Into another part drop a bit of Pt foil, qcm . If no action ensues, heat it. Pt does not dis. as readily as Au. Try the solvent action of aqua regia on : (3) Zn ; (4) Fe ; (5) Cu ; (6) Pb. Give the usual explanations, reactions, etc., for each of the above exps. Why should not the 'acid act as well on Pb as on the others ? Supplementary. See if Au will dis. in : (a) HC1, or (b) HNO 3 . Also try (c) Pt. Try Hg in (d) H Cl, then in (e) aqua regia. (f ) Try Fe in each and notice the color of each liquid after filtering. Explain, (g) Test the 2 chlorids of Fe by Exp. 63. Terms : Nitro-hydrochloric acid, gold chlorid, ferrous and ferric chlorids. 31. SULFURIC ACID, I, Preparation. Burn a small piece of S in a rec. in which there is H 2 enough to cover the bottom, using a d.s. and confining the fumes as much as possible by covering the mouth of the rec. Pour into an e.d. 1 or 2 CC HN0 3 , and dip into this a piece of strong paper, or cloth, or a wood shaving, and lower it into the rec. of S 2 , holding it there for some time without dropping any acid from it into the rec. See whether the fumes change color. Repeat the operation several times. Explain the phenomena and give all reactions. Cover the rec. with the hand and shake the liquid and the gases well together. II. Tests. (1) Apply the litmus test. (2) Put a drop of the liquid on writing paper, and evaporate it so as not to burn the paper. See whether the paper is charred, blackened, or made rotten by the liquid. Explain. This is a test for free H 2 S0 4 . (3) Add a little of the liquid to 5 or 10 CC BaCl 2 sol. (or Ba(N0 3 ) 2 ) in a t.t., state the effect and give an equation. If you obtain a ppt., add a little H Cl and shake it well. Does it dissolve ? (4) Pour into a t.t. containing 5 CC H 2 O the same amount of H 2 S 4 from the shelf bottles. Observe any thermal effects on this mixture and explain. Save the dilute acid in a separate rec. (5) Apply tests (2) and (3) above to this mixture. (6) Pour a few drops of concentrated acid upon 1 or 2 g sugar in an e.d. (7) Dip a small stick into a t.t. which contains 1 or 2 CC H 2 S O 4 . (8) Pulverize a bit of starch, add a few drops of the acid. If no change occurs, cautiously heat it for a minute. Sugar is C 12 (H 2 0)n ; starch is C 6 (H 2 0) 5 ; cellulose is C 18 (H 2 0) 15 ; explain the action of the acid. Supplementary. Why is commercial H 2 S O 4 liable to be of a brown color ? (a) Measure accurately 10 CC of concentrated acid in a graduate, leave it in an open t.t. or rec. for a week, then measure it carefully again. Explain the result, (b) Test commercial acid for PbS0 4 by pouring a little into an equal vol. of H 2 O in a t.t. BaSO 4 is the only salt of Ba that is not dis. by HC1. (c) Test Na 2 SO 4 sol. with BaCl 2 . Explain, (d) Test a sol. of Na 2 SO 3 for Terms : Salt of sulfuric acid, fuming sulfuric acid, sulfate, starch, cellulose. 32. AMMONIUM HYDBOXID, NH 4 OH; AMMONIA, NH 3 . I. Preparation, Powder and put into a flask about 10* NH 4 C1 and 7 Ca(OH) 2 (freshly slaked is best). Add 20 CC H 2 and connect with Wolff bottles containing H 2 (Fig. 31), as in the HC1 exp. Heat 10 or 15 minutes, using a plate and asbestos paper. Observe the phenomena, especially the pressure in the different bottles and the absorption of gas, and write the reaction. While the mixture is heating, do III. Fig. 31. II, Tests. (1) Disconnect the flask while the gas is escaping (a, Fig. 31) r put 2 or 3 drops HC1 into an e.d., and pass the gas over it from the gen. Observe the fumes, giving equation. (2) Let the flask cool as it stands, and test the liquid in each bottle (odor and litmus). Put sols. (5 CC each) of the following substances into separate tubes, and add a little of the prepared liquid to each : (3) FeS 4 ; (4) FeCl 3 ; (5) A1C1 8 . Observe colors, especially -of ferrous and ferric cpds. (6) Test likewise CuCl 2 sol., first with very little NH 4 OH, then with excess. State and explain all phenomena. III. Ammonia. Mix 2 or 3* of fine NH 4 N0 3 with an equal quantity of Ca(OH) 2 , put them into a t.t., and warm it over a flame. See whether a gas escapes by : (1) cautiously taking the odor ; (2) testing with red litmus paper ; (3) with H Cl. Supplementary. (a) Put into a t.t. a gram or two of either (NH 4 ) 2 SO 4r N H 4 NO 3 , NH 4 C1, or (NH 4 ) 2 C 2 O 4 , and add a little NaOH (or KO H) sol., warm it, and apply tests. What two classes of cpds. are used to obtain ammonia ? Are the above examples of double decomposition, and why ? Relation between ammonia and ammonium hydroxid ? (b) Fill a t.t. with NH 8 by upward dis- placement, and invert it over a rec. of water. Observe and explain. Terms : Volatile alkali, fixed alkali. 33. FIXED ALKALIES. I, Sodium Hydroxid, NaOH. To 5 CC of a saturated sol. of Na 2 C0 3 add about an equal quantity of Ca(0 H) 2 sol. Shake the mixture well and observe. If a ppt. falls, name it and write the equation. What goes into solution ? Let the ppt. settle, then add some of the supernatant liquid to sols. of : (a) Fe(S0 4 ) ; (b) FeCl 3 ; (c) A1C1 3 . Effects, colors, and equa- tions should be given in each case. If any effect different from what is expected occurs, it should be noted and explained. II. Potassium Hydroxid, KOH. Treat a sat. sol. of K 2 C 8 in precisely the same way as Na 2 C 3 above, making close observations and taking full notes as before, including all the tests given. Supplementary. Compare the action of fixed alkalies with that of N H 4 O H on sols, of Fe and Al salts, (a) Obtain some NaO H or KO H in the solid state. In what other ways were NaO H and KOH made in the laboratory ? (b) Would Ca(OH) 2 actonNaCltoformNaOH? (c) Ca(0 H) 2 on Na^S O 4 ? (d) Is FeCl 3 sol. acid, alkaline, or neutral ? (e) Is A1(O H) 3 soluble hi excess of NaO H or KOH sol.? Terms : Hydroxid, hydrate, alkali metals, metals of alkaline earths. Fig. 32. 34. OXIDS OF NITKOGEN. I. Nitrogen Monoxid, N 2 (Nitrous Oxid). (1) Put into a flask (of 200 CC capacity) 10* of NH 4 N 8 , not too coarsely crystalline (so as not to break the flask in melting). Connect the flask with a large t.t. (resting in a rec. of H 2 0, Fig. 32), or with a rec. which contains no water (Fig. 33), and from this t.t. or rec. have a d.t. leading to a p.t, so as to collect the gas over water. Ha.ve the joints tight and the tubes pass through the stoppers. Apply heat not too rapidly, notice the order of changes and give the main reaction. Are there any fumes in the flask ? Is the gas colored, and why ? Obtain 2 recs. of gas, then remove the lamp and take the d.t. from the water, letting the flask cool on the r.s. (2) Taste a drop of the liquid in the large t.t. or rec., and also test with litmus, red and blue. Some NH 4 N0 3 will probably have been driven over, also some NO, N0 2 , HN0 3 , etc., formed by breaking up of NH 4 N0 3 . (3) Test the gas with a burn- ing stick, also with a glowing one. (4) Test the combustibility of S (well burning when introduced), and (5) of P. Compare the bril- liancy of flame and the products obtained with those in 0, and write all equations. Supplementary. Compare the action of heat on NH 4 N0 3 with that on Pb(N0 3 ) 2 in Exp. 10. Compare with the action of NaNO 3 + H 2 SO 4 (Exp. 29). Learn the symbols and names of all the oxids of N. Try the action of heat (using a t.t.) on: (a) KN0 3 ; (b) Hg(N0 3 ) 2 ; (c) Zn(NO 3 ) 2 ; (d) Pb(NO 3 ) 2 . Fig. 33. Terms : Laughing gas, nitrous oxid, nitrates, nitrites. 35. OXIDS OF NITROGEN. II. Nitrogen Dioxid NO or N 2 2 (nitric oxid). (1) Arrange the app., with inverted recs., as for the hydrogen exp. Then put into the gen. (or t.t.) 5 g Cu turnings, cover them with water and add through the thistle tube 5 CC of HN0 3 . Collect 2 or 3 recs. of the gas. If action stops add a little HN0 3 (or Cu, if necessary). Save any Cu that is left. Explain the different colors of the gases and the color of the liquid. (2) Test the gas with a burning stick. Explain the fumes. Test also with (3) S and (4) P (well burning). In (4) see whether the solid gradually separates from the gas. Take full notes. III. Nitrogen Trioxid N 2 3 and Tetroxid N0 2 or N 2 4 (peroxid). (1) Lift a rec. of the gas N 0, just prepared, from the shelf of the p.t. What is the effect, what is the new gas, and how is it formed ? (2) Heat 1 or 2 crystals of Pb(N0 3 ) 2 in a t.t., and while the gas escapes insert a glowing stick into the tube. (3) Put a fragment of starch into a t.t. and add a few drops of HN0 3 . Heat cautiously. Supplementary. State how the oxids of N are derived from H N O 3 and nitrates. What action have heat and reducing agents on nitrates ? (a) Notice the action of direct sunlight on strong H N O 3 in stoppered bottles, (b) Try the action of heat on other nitrates, e.g., Cu(NO 3 ) 2 , KNO 3 . (c) Heat a bit of powdered charcoal on a plate or asbestos, and when it is hot add a drop of HN0 3 with a s.r. N 2 3 and N0 2 are both red and not distinguishable. Find how N 2 Og is prepared, and its relation to HNO 3 . Terms : Nitrous and nitric anhydrids, nitrogen peroxid, nitric oxid. 36. CARBON DIOXED, CO 2 . I. Preparation. Put 10 or 15 g CaC 3 (marble, in lumps) into a t.t. or gen. (Fig. 34), cover with H 2 O and after having the app. all prepared add 5 CC HC1. Add more of the reagents as needed. Enough must be used to produce vigorous action. Attach a delivery tube and collect a rec. of gas by downward displace- ment, having the tube reach to the bottom of the rec. Fig. 34. It will take only a minute. II, Tests. (1) Test the gas with a burning stick. (2) Let the gas bubble from a d.t. into 5 CC Ca(OH) 2 sol. in another t.t. and look for a ppt. Let the action continue until the liquid clears. (3) When the sol. is clear, boil it for a minute and notice the reappear- ance of the ppt. Explain all the phenomena very fully, giving equations at the proper places. (4) Pass the gas into a sol. of blue litmus. (5) Observe the Ca flame (bring the open mouth of the C0 2 gen. close to a Bunsen flame). Small particles of CaCl 2 are carried up by the gas. (6) Also dip a stick into the sol., hold it in the flame and notice the color. (7) Take 2 or 3 CC Ca(0 H) 2 sol. in a clean t.t. and breathe into it through a glass tube. What does the result show ? (8) Put a little lime water into an e.d. and look for a scum after a few minutes ; or draw the air through a rec. of lime water (Fig. 35), by suction, applying The air enters at a, and any C 2 is drawn through Fig. 35. the lips at b. the lime water. Explain. Supplementary. (a) See whether you can obtain C 2 from Na 2 C 3 . Use an open t.t. and test the gas with a drop of Ca(0 H) 2 sol. on a s.r. (b) Use also HNaC0 3 . (c) K 2 CO 3 . (d) Test some oyster, clam, or other shells with a drop of HC1, and see whether there is effervescence ; or put them into a gen. and test the gas. (e) Obtain CaCl 2 from the C O 2 gen. (f ) Test that salt for Cl (Exp. 90). (g) For Ca (Exp. 74). (h) Obtain CaSO 4 from CaC 8 . (i) Ca(NO 3 ) 2 . Terms: Carbonate of lime, quicklime, slaked lime, lime water, milk of lime, sulfate of lime. 37. CHLOKIN. I. Preparation from Hydrochloric Acid. Put into a flask (or t.t.) 5 g Mn0 2 (preferably granulated) and 10 CC H Cl. Shake them well together, apply gentle heat, and avoid inhaling the gas, but collect it by downward displacement in a rec. loosely covered with paper. Add more HC1 if it is needed. Ob- serve and describe, with equations. Note when the rec. is filled, to avoid passing the gas into the room. If accidentally any is inhaled, the antidote is vapor of alcohol (inhale from a handkerchief) ; or NH 3 will do. State the color of the gas, its sp. gr. compared with air, its effect on the nasal organs. II. Tests and Properties, (1) Drop into the rec. a piece of dry Turkey-red cloth (or of calico), also bits of printed and written paper. If there is little or no effect add a very little water, shake the gas, water, cloth and paper well together, and note the effect. Which bleach better, wet or dry fabrics ? (2) Into another rec. of Cl (dried if possible) file a little Sb (or stibnite, Sb 2 S 3 ). Describe the result and give an equation. Is this a case of ordinary combustion ? Pass some Cl from the gen. into sols, of : (3) AgN0 3 ; (4) Pb(N0 3 ) 2 ; (5) H 2 S. Supplementary. (a) Put into a small beaker 5s bleaching powder, CaCl 2 0, set this into a larger rec. or beaker, putting into this last the substance to be bleached. Cover the large rec. with pasteboard, through which passes a thistle- tube into the smaller. Pour through the thistle- tube 5 CC dilute H 2 SO 4 (half H 2 O and half acid). Add more, if needed, (b) Mix a gram of fine NaCl with a gram of Mn0 2 , add in a t.t. 2 CC H 2 O and 3 c c H 2 SO 4 , and heat. Observe any gas. Test it with N H 3 , or otherwise, (c) Dip some unglazed paper into oil of turpentine, CioHie, in an e.d.; warm it by holding the paper near a flame for an instant (or heat the turpentine in an e.d. over a waterbath), but do not set it on fire. Then at once thrust the paper into a rec. of Cl. Explain the combustion and describe all you saw, giving the equation. Clean the rec. with naphtha or petroleum. Terms : Bleaching, bleaching powder, calcium hypochlorite, chlorid of lime. 38. EUCHLORIN, C1O 2 , CL I. Preparation. Drop into a t.t. 3 or 4 crystals of K C10 3 . Add a few drops H 01, heat for an instant and then add 5 or 10 CC H 2 0. II. Tests. (1) Observe carefully the action, noting the color and odor (cautiously), and give equation. (2) To 2 CC indigo sol. in a t.t. add a little euchlorin. Is the color discharged ? Test in the same way sols, of (3) litmus and of (4) cochineal. (5) Try K 2 O 2 7 sol. (a mineral pigment ; the other three are vegetable or animal coloring matters). What do you conclude from this ? (6) Very cautiously add 2 or 3 drops of H 2 S 4 to 2 or 3 small crystals'of K C10 3 in a t.t. at arm's length from the operator, then fill the t.t. with H 2 0. Describe the result with equation. (7) Try to bleach a piece of Turkey-red cloth or calico by putting it into some euchlorin and leaving it a few minutes. Supplementary. (a) Try to bleach K Mn0 4 sol. Will euchlorin dis. : (b) Au ? (c) Zn ? (d) Cu ? Try its action on sols, of : (e) AgN0 3 ; (f)Pb(N0 3 ) 2 ; (g)HgN0 3 . Terms : Euchlorin, oxids of chlorin, detonation. y /v 39. BKOMIN AND BROMIDS. I. Preparation of Br. (1) Make some starch paste by pulverizing a piece of starch not larger than a pea, adding 10 CC H 2 and boiling several minutes in a t.t.; cool it and dil. with 10 CC H 2 0, shaking it well. Boil again if necessary. [Save part of this for subsequent exps.] (2) Mix 1 or 2 crystals of KBr with an equal quantity of Mn0 2 , put them into a t.t. and add a few drops H 2 S0 4 . Heat the mixture and observe carefully. Write the equation, and explain the action. H, Tests. (1) Dip a strip of paper into the starch paste, wind it around the end of a s.r. and carefully put it into the t.t., so as not to touch the sides. Then heat the mixture in the t.t. Observe the effect of the Br on the starch. The product is supposed to be starch bromid. Avoid getting much Br into the air in the room, or inhaling it. Alcohol vapor, or ammonia, is the antidote, as for Cl. Do you notice any effect of Br vapor on the eyes ? (2) To a sol. of KBr add a few drops of euchlorin. Describe and explain, stating which is the more stable or stronger cpd., KBr or KC1, and how this exp. shows it. (3) Add to a few drops of starch paste 10 CC H 2 0, shake it well, add a few drops of KBr sol. and one drop of euchlorin. Describe and explain. Supplementary. Liquid Br should be examined, (a) Try the action of Br on a mixture of starch paste and KI sol. Try the action of H 2 S0 4 on (b) a few drops of K Br sol. , also on (c) a crystal of K Br. (d) Pour a little Br vapor from a gen. into 5 CC of KI sol. (e) Put a drop of CS 2 into a t.t. with a few drops of KBr sol., then add a few drops of euchlorin and shake it. Notice the color of the C S 2 at the bottom of the tube. The Br was set free and dis. by the CS 2 . 40. IODIN AND IODIDS. I, Preparation of I. Prepare I like Br in the previous exp., using KI instead of KBr. Notice the difference in its action, color, state, etc., and give a full description with equation. II. Properties and Tests. (1) Make the same tests with starch as in Exp. 39, noting the different results. (2) Warm 1 or 2 crystals of I in a dry t.t. Notice the color of vapor, and its relative weight (pour a little into a dry e.d.). (3) While warming the tube hold a s.r. half way down the t.t. Look for a sublimate on the rod and on the sides of the tube, examining carefully its form, luster, and color. (4) Put into a small t.t. 1 or 2 crystals of I, add 3 or 4 CC of alcohol, C 2 H 5 OH, and warm a minute. Explain, then (5) add a drop of this with a s.r. to a drop of starch sol. shaken up with 10 or 15 CC of H 2 0. Ob- serve the color of the product (starch iodid), and boil it a moment to see whether the color disappears. If not, too much I was used. When it is cool (hold the tube under a jet of water) observe again. Supplementary. (a) See whether a crystal of I will dis. in H 2 O. To de- termine this apply the starch test, (b) To 5 or 10 CC H 2 O add a drop or two of CS 2 and of KI sol. (examine), then one drop of euchlorin. Shake well, let stand, and note the color of the C S 2 globule, (c) Test the solubility of I in ether (C 2 H 5 ) 2 O, keeping the latter away from the flame, (d) Obtain crystals by letting the ether sol. evaporate, (e) To 10 CC H 2 O add a few drops KI sol. and a few drops of starch paste. Shake well together and note the color. Now add one drop of euchlorin (Exp. 38). If too much euchlorin is added the sol. becomes green or black (ppt. of I). Describe the coloration and explain fully, (f) Repeat (e) of Exp. 39 with KI sol. Terms : Sublimation, sublime, crystal, tincture. 41. EXPERIMENTS WITH SULFUR. I. Crystallization, Into a small beaker or large t.t. put 10 or 15 g S, and slowly melt it over a lamp (using sand bath or asbestos), not allowing it to become darker than amber-color. When it is melted remove the lamp, leave the beaker in position (or hold the t.t. in the hand), and when crystals begin to shoot across the surface, pour the liquid S remaining into water in an e.d. Explain. Loosen the S by pouring round the edges a little H N 3 . Warm if necessary, when the mass may be removed with a thin knife-blade. II. Allotropy. Put 10 g S into a t.t. and slowly melt it. Notice the yellow color, and see that the liquid (now above 100) is very thin. Slowly continue to heat it till it becomes black. Note that it is now very thick and can scarcely be poured (about 200). Apply more heat till it grows thin again (above 300). Now heat to boiling (over 400), note the color of the vapor, and any sublimate on the t.t. If it takes fire (S burns at 230), cover the mouth of the tube with paper or cardboard for a minute. Pour the S into an e.d. of water. Pull it and note its elasticity. Is it now crystalline, or amorphous ? See whether it afterward changes. Clean the t.t. as before. III. Solubility. Place in an e.d. -J g pulverized brimstone and cover it with CS 2 (avoid a flame, as CS 2 is explosively inflammable). See whether any dissolves. Let it stand till the C S 2 has evaporated, watching it meantime. Describe fully the phenomena. Supplementary. (a) Try to dis, a little S in ether, (C 2 H 5 ) 2 O, and let 'it evaporate. Is S soluble in H 2 ? (b) Grind together on a brick with, a pestle or other implement, not over a half gram of S and K C10 3 . (c) Make gunpowder by mixing intimately very fine KNO 3 , C, and S (a small quantity of each). Pile the mixture on a brick and cautiously set it on fire. If this reaction is correct, in what proportion should the constituents be mixed :2KNO 3 + 3C + S = K 2 S +3 CO 2 + 2 N ? (d) Obtain flowers of S by sublimation and see whether they are crystalline or globular (use compound microscope), (e) Add HC1 to a sol. of Na-jS^s and look for a S ppt. (f ) Obtain S O 2 from S, also from H 2 S 4 . (g) Try to bleach with it a green leaf or a blue petal. Terms : allotropy, allotropic, fusion, crystalline, globular, amorphous. 42. HYDROGEN SULFLD. Preparation and Tests. (1) Put into a gen. (rec. or t.t.) 5*FeS, 10 CC H 2 0, and 5 ec HC1 (or H 2 S0 4 ). Adjust a d.t., having the joints perfectly tight, and pass the gas for a minute or two into 5 CC H 2 in an- other t.t. or beaker (Fig. 36). Note the odor. Can you determine whether e gas is soluble in H 2 ? (2) See whether the sol. is acid, alkaline, or Fi g-36. neutral. With a s.r. put a drop of H 2 S sol. on bright coins of (3) Ag and (4) Cu. State the effect, products, reactions. (5) Put a drop of Pb(C 2 H 3 2 )2 sol. on paper and pass the gas over it from the tube of the generator. Describe the effect (this is the characteristic test for H 2 S) and write the equation. Is there any other way in which you would recognize this gas ? (6) Try the combustibility of H 2 S, using a philosopher's lamp. (7) If it burns, hold a glass tube or a crayon in the flame. Explain. II. As a Reagent. Add a little H 2 S sol. to 5 CC of each of the following sols., describe the results, write equations where necessary, and explain why there is no effect in certain cases : (1) HgCl 2 , (2) CuCl 2 , (3) BaCl 2 , (4) CaCl 2 . (5) Next mix 3 or 4 CC CuCl 2 sol. and the same quantity of BaCl 2 sol., add H 2 S sol., shake it well and filter. What is the residue and what does the filtrate contain? (6) Now to the filtrate add a sol. of Na 2 C0 3 . State the effect, give the reaction, and explain how the Cu and the Ba have been separated. III. Test for Sulfids. To a little Na 2 S or CaS add H 2 S0 4 . If any gas arises (heat if necessary) try the Pb(C 2 H 3 2 ) 2 test. Supplementary. See whether you can separate (a) Cu from Ca ; (b) Ca from Hg ; (c) Hg from Ba ; (d) Fe from Cu. How are some insol. sulfids made ? (e) Test FeS for a sulfid ? What sulfids are insoluble ? Terms : sulfuretted hydrogen, sugar of lead, sulfid. 43. PHOSPHORUS. Caution: Phosphorus must be handled with forceps, as the burns from it heal very slowly, and all experiments with it must be done cautiously. None should be dropped upon the floor, nor left upon the apparatus, and all must finally be burned. C S 2 must be kept away from the flame. I. Spontaneous Combustion, (1) Into an e.d. put 10 or 20 CC of C S 2 (for a class) and drop into it 3 or 4 small pieces of P. Notice the odor of CS 2 and whether the P dissolves in it. Also observe the color and luster of newly cut P. (2) Dip a piece of unglazed paper into the sol., then place it on the ring of a r.s. till it is dry, looking out for any action. If such occurs state fully ivhat has caused it and whether it is a case of ordinary combustion. II, Combustion under Water. Put into a large t.t. 4 or 5 crystals of KC10 3 , cover it with H 2 and add a small piece of P. Rest the t.t. in a rec., and then slowly add 2 or 3 CC H 2 S O 4 through a thistle tube which reaches to the P and K C10 3 . Account for the phenomena. What color is the liquid, and what is the cause of it? HKS0 4 , HC10 4 , C10 2 and H 2 are formed. Write the equation for forming them, and for the combustion. What compound of P is finally formed ? Supplementary. (a) Put a small piece of P into a dry e.d. in a dark room, observe, and explain the result, (b) Put a piece of P on a dry- plate or e.d., set it on fire and at once cover with a dry inverted rec. When the fumes settle add a very little water. Test the product with litmus, (c) Cover a small piece of P with bone black in a plate, and leave for some time. If no action ensues burn the P before leaving the Exp. Terms : spontaneous combustion, phosphorescence. % w > : r <3 V^ * 44. ARSENIC. I. Marsh's Test. Caution : AsH 3 is a deadly poison, and must not be inhaled. If the H is ignited before introducing the As compound there is little danger. Prepare a hydrogen gen., with or without a CaCl 2 drying attach- ment, and with lamp tube (Fig. 37, or model). Put in a few pieces of arsenic-free Zn, some distilled water, and C.P. HC1. After a few minutes test the H gas (Exp. 13) before lighting, and when no sharp explosion occurs light the gas, and observe the color of the flame. Test 37 - for As by holding an e.d. over the flame. Now pour through the thistle tube 1 or 2 CC of a sol. that may be supposed to contain some cpd. of As. This sol. may be obtained either by dissolving HNa 2 As0 3 in H 2 with a little HC1, or by immersing in HC1 a small piece of green paper tag from which any As that may be present will dis. as AsCl 3 . Note any change in the color of the flame; hold an e.d. or other cold body in the flame and look for a deposit ; put a Bunsen flame under the drawn out tube (Fig. 37) and look for a sublimate just beyond. Absence of a sublimate in either 'case indicates absence of As. Explain fully, writing all equations. II. Reinsch's Test. Into a sol. of an As salt (obtained by HC1 as above) in a beaker or e.d. put a small strip of bright Cu foil and heat for a few minutes. Notice that the foil changes color. After a few minutes remove it, dry it by carefully pressing between folds of blotting paper, cut it into strips, and put them into a t.t. ; heat the latter. Notice the vapor and sublimate, As 4 6 , on the tube. This sublimate may be examined under the microscope after first breaking the tube. Explain all results, using equations. Supplementary. (a) Reduce As 4 O 6 as follows : Mix intimately a bit of it not larger than a wheat grain with as much powdered charcoal, put the mixture into a small t.t. or i.t. and heat strongly. Note the vapor, color, sublimate, (b) Make Scheele's green by mixing sols, of CuCl 2 and HNa^AsOs (or other sol. cpds.) and having them nearly neutral, (c) Try the effect on these mixtures of (d) excess of HC1, (e) excess of NH 4 OH. (f) See whether As 4 6 is very soluble in H 2 by putting a very little into a t.t. and heating with H 2 0. (g) Heat a little powdered arsenopyrite, FeAsS, in a t.t. and note the odor, (h) Test some wall paper, or colored silk, for As. 45. COMPOUNDS OF BORON. I. Boric Acid. Put 5* of Na 2 B 4 7 into a t.t., add 10 CC of dil. H 2 S0 4 and boil till it is clear, adding more water if necessary. Then cool it by holding the tube under a jet of water, keeping watch for crystals. When it is cool pour off the supernatant liquid and rinse the crystals once or twice with water to remove the H 2 S 4 , then put them into an e.d. Add a very little water, and when the crystals have dissolved dip into the sol. a piece of turmeric paper, which should then be dried and the color noted. Describe fully the results. II. Borax Beads. Make a loop in the end of a Pt wire (which is welded into a short glass tube, Fig. 38) . Moisten c=s=s=^ o the loop end and dip it into some powdered borax, Na 2 B 4 7 . Now heat it, using the mouth blowpipe, dipping it again into the borax if more is wanted, and heating till a clear transparent bead is obtained. Describe and explain the phenomena. Beads may be colored as follows : If blue is wanted dip the clear bead into a very dil. sol. of some Co salt, as CoCl 2 , and fuse again. -(If too much Co is used it will look dark.) For other colors v. Table G. Detach the beads by suddenly jerking the Pt wire while the bead is fused. Save the beads, and label them, stating the coloring material. Supplementary. (a) See whether H 3 B 3 is more, or less, soluble in hot water than in cold, (b) Make a bead of H 3 B 3 if possible, (c) Stir a little H 3 B O 3 in an e.d. with a few drops of CgHsOH. Then take some of the mixture on a short glass tube and hold it in a Bunsen flame, noting the color imparted to the latter, (d) Try the same with Na^O?, (e) then with Na2B 4 O 7 to which has been added a few drops of H 2 S0 4 . Terms: borax bead, flux. 46. COMPOUNDS OF SILICON. I. Silicic Acid and Silica. Pour a few cubic centimeters of water glass, H 4 Si0 4 , into an e.d. and add a little H Cl. Note the phenomena, describe the result and write the equation. Pour off the extra HC1 and rinse the residue, H 4 Si0 4 , 2 or 3 times with H 2 0. Now heat it over a Bunsen flame, with stirring. This leaves Si0 2 . Write the equation, and note how the product feels when rolled between the fingers. Is silicic acid made differently from other acids ? Pulverize (in a mortar if necessary) some of the Si0 2 obtained, to use in the following. II. Silicates by Solution. Make a strong sol. of NaO H (or K H) and add to it some of the Si0 2 obtained above, very finely powdered. Heat and stir the mixture for some time. See whether the Si0 2 dissolves, and write an equation. III. Silicates by Fusion, Glass. Make a small mixture of equal parts of powdered Na 2 C0 3 and K 2 C0 3 and fuse the mixture into a bead as in the case of borax. Note that the bead is opaque when cold. Is it so when hot ? Dip this bead when hot into a little Si0 2 powdered very finely, then heat again more strongly in the hottest part of the flame. If it is not transparent when cold, dip it again into the Si0 2 and heat more strongly than before. See whether it now resembles glass. Describe all phenomena and write the equations. Colors may be obtained as in borax beads, Table G. Supplementary. (a) Try to dis. finely powdered Si0 2 in a strong sol. of Na 2 CO 3 , boiling the mixture, (b) Try to fuse Si0 2 in a borax bead. Terms: fusible, infusible, fusion, transparent, opaque, silica, silicate, glass, water glass. 47. OXIDATION AND REDUCTION. I. Oxidation. (1) Into each of two tubes put 5 CC FeS0 4 sol. (freshly dissolved). To one of these add a few drops HN0 3 and boil a minute, then cool. To each of the tubes add 5 CC NaO H sol. (or NH 4 OH). Observe the color effects, explain their causes, and give equations for the ppts. Explain the action of H]ST0 3 . (2) Put a small fragment of Pb on a piece of charcoal, slightly hollowed out with the handle of the forceps. Fit a metallic tube to a Bunsen burner, and with a mouth blow-pipe blow the oxidizing flame (outer) strongly and steadily against the Pb for 4 or 5 minutes (Fig. 39). What first takes place? As you stop blowing, notice the yellow vapor that escapes from the globule of Pb : also the yellow a, red^Snfflame. coating of Pb on the charcoal. Explain fully, b, oxidizing flame. using equations. II. Reduction. (1) Pour a little FeCl 3 sol. into two tubes. Pass S 2 gas, or H, from a gen. into one of these for a few minutes. Next add NH 4 OH to each. Compare the products and explain, with equations. What action has the S0 2 ortheH? Try the action of Zn and H, or of Zn alone. (2) Put g PbO on a piece of charcoal hollowed out as before. With the blow-pipe blow the reducing flame (inner) steadily against it for some time, or until a metallic globule is obtained. What is it? Explain fully, with equation. See whether the globule is sectile (can be cut) or malleable (can be flattened by pressure). Extinguish the fire, if the coal still glows, with a drop of water. Supplementary. Notice that the action of the flames here is like that of oxidizing and reducing agents generally, (a) Experiment with other metals and oxids. (b) See whether Fe(OH) 2 or Fe(OH) 3 tends to change to the other on standing. Which is the more stable cpd. ? (c) Try sols, of FeS 4 and FeCl 3 in the same way. (d) Try to oxidize FeSO 4 sol. with a little euchlorine. (e) Oxidize HgN0 3 with HNO 3 . (f) Try to reduce K 2 Cr 2 O 7 sol. to CrCl 3 with a little HC1, C 2 H 5 OH and heat. Note the change in color, also test by Exp. 48. Are these oxidizing, or reducing agents: (g) KC10 3 , (h) KNO 3 , (i) C, (j) Cu ? (k) Pulverize about a gram of K N O 3 and mix it with a like quantity of fine charcoal. Put into a dry i.t. and heat. (1) Try KNO 3 and S in the same way. Terms: Oxidation, reduction, oxidizing agent, reducing agent, oxidizing flame, reducing flame. 48. LEAD, Pb". ANALYTICAL REACTIONS. DIRECTIONS. PPT. COLOR. SOL. 1. Ppt. PbCl 2 (v, Ag, Hg'). To Pb(N0 3 ) 2 sol. add HC1, filter (test fil.), wash, reject washing (and fil. if no more PbCl2 falls). (1) PbCl 2 white 2. Dis. PbCl 2 in hot H 2 0. (v. Ag, Hg')- Pour on res. (1) boiling H 2 from t.t. Save fil. Repeat this several times. (a) PbCl 2 3. Final test for Pb. To first filtrate (a) add K 2 Cr 2 7 sol. (or K 2 Cr0 4 ). (2) PbCr0 4 yellow Supplementary. 1. PbCl 2 is somewhat sol. in H 2 0, hence traces of it are tested for in Grp. II. 3. If there is much free acid in a sol. the K 2 Cr 2 7 test is not to be relied on. H 2 S 4 should then be used. What other Pb salt might be used for sol. (Table A) ? (a) Allow some of the hot water sol. of PbCl 2 to cool in a t.t. and look for crystals. Explain, (b) See which is the stronger cpd. PbCl 2 or PbCr0 4 . (c) Make several other final tests for Pb. GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENT. REMARKS. 1 2 AmOH NaOH Pb 2 0(OH) 2 Pb(OH) 2 white u ( NaOH (ex.), With PbAc 2 no ppt., Pb 2 OAc 2 being sol. 8 Am 2 C0 3 Pb 3 (C0 3 ) 2 (OH) 2 u STaOH (ex.), 4 NfeCOa Pb 3 (C0 8 ) 2 (OH) 2 u INO 5 HC1 PbCl 2 (i ]_ I 2 (boiling) FTfll (sL) Re-ppts., cryst., on cooling. G H 2 S PbS black dil. HNO.t HN0 3 (str.) forms PbS0 4 . H 2 S + HX0 8 ppts. S. 7 Am 2 S PbS u dil. HNOs HN0 8 (str.) forms PbS0 4 . Am 2 S + HX0 8 ppts. S. 8 KI PbI 2 yellow H 2 boiling Re-ppts., cryst., on cooling. 9 H 2 S0 4 PbS0 4 white TaOH'(ex ) Dis.by Na 2 S 2 O 3 (v. BaS0 4 ). 10 K 2 Cr 2 7 PbCr0 4 yellow gaUS HC1 changes ppt. to PbCl 2 . 11 Am 2 0x PbOx white WE*^ 12 HNa 2 P0 4 Pb 3 (P0 4 ), (4 'JaOH (ex.), 13 KCy PbCy 2 U KCy (ex), Boiling re-ppts. 14 KiFeCy,, Pb^eCy* *' 15 Zn Pb metallic dil. HNOs Also Al, Cd, Co, Mg. 16 Mb. } Pb " dil. HN0 3 Yel. PbO on C.C. 49. SILVER, AgT- ANALYTICAL REACTIONS. BISECTIONS. PPT. COLOB. SOL. 1. Ppt.AgCl(v. Pb, HgO To AgN0 3 sol. add HC1, filter (test fil.), wash res., reject fil. and washings. (l)AgCl white 2. Dis. AgCl in NH 4 OH (v. Hg', Pb). To (1) add NH 4 OH on filter, and catch fil. in t.t. (a) (NH 3 ) 3 (AgCl) 2 3. Be-ppt. AgCl. Cautiously acidify (a) with HN0 3 (2) AgCl white Supplementary. 1. Strong HC1 dis. AgCl (and HgCl somewhat) ; hence avoid excess. 2. In testing for trace of Ag, evap. NH 3 before adding HN0 3 . 3. Never add the latter in large excess. AgCl is not re-ppd. by H Cl except in cone. sols, (a) Sep. Ag from Pb. Are most salts of Ag soluble (Table A) ? Can these exist together in sol: (b) AgN0 3 and HgCl 2 ? (c) AgNO 3 and CuCl 2 ? GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENT. EEMABKS. 1 AmOH brown (AmOHx.,, AgOH is not known. ( HAc',H 2 S04 3> 2 NaOH ' ' n 3 Am 2 C0 3 Ag 2 C0 3 white Am.oCOs (ex.), AmOH,HN0 3 4 TflTflrfifO ** u 5 6 HCl H 2 S AgCl Ag 2 S black |AmOH,KCy, (Na^Os boilingHNO, HN0 3 re-ppts. Light re- duces to Ag 2 Cl, violet, black. 7 Am,S " u 8 KBr AgBr white AmOH (si.) 9 El Agl (yellow- jwhite KI (ex.) Insol. in AmOH. 10 K 2 Cr s O T Ag,Cr04 (dark (AmOH, \HN0 8 HCl changes it to AgCl. 11 Am 2 0x Ag 2 0x white AmOH 12 HNa 2 P0 4 Ag 3 P0 4 yellow ( AmOH, (HNOs 13 KCy AgCy white KCy (ex.) 14 Ag 4 FeCVrt {yellow- Boiling gives metallic Ag. j white 15 Zn Ag gray dil. HNO< Also Bi, Cu, Fe, Hg, Pb. 16 Na 2 C0 3 , ) B.B.C.C. ) Ag it HNOs Metallic globule. 50. MERCURY (ous), Hg'. ANALYTICAL REACTIONS. DIRECTIONS. PPT. COLOR. SOL. 1. Ppt. HgCl (v. Ag, Pb). ToHgN0 3 sol. add HC1, filter (test fil.), wash, reject fil. and wash- ings. (l)HgCl white 2. AmOE on HgCl (v. Ag, Pb). On (1) pour a little AmOH, wash and reject washings. (2)NH 2 Hg 2 Cl black 3. Dis. NH 2 Hg 2 Cl in aqua regia. On (2) pour a few drops aqua regia, save fil. (a) HgCl 2 4. Ee-ppt.Hgd. Dilute (a), add SnCl 2 sol. (3) HgCl Hg white gray Supplementary. 1. Hg', not Hg", must be used as HgCl 2 is sol. 3. The smallest quantity of aqua regia that will dis. the ppt. must be used. 4. SnCl 2 sol. must be newly prepared, and with plenty of HC1, or it will oxidize to SnCU and Sn 2 O C1 2 . (a) Sep. Hg' from Ag. (b) Hg / from Pb. Explain action of SnCl 2 on HgCl 2 . (c) Can HgN O 3 and CuCl 2 exist in sol. together ? (d) HgN 3 andCdC! 2 ? GENERAL REACTIONS. RK-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 AmOH NHjHg 2 N0 3 black HN0 3 ,aq.reg. 2 NaOH Hg 2 ( brown- ] black Hg 2 O (instable) = Hg + HgO. HgOH not known. 3 Am,C0 3 NH,Hg 2 N0 3 black Acids, 4 NazCOs HgzCOs gray Forms black Hg 2 on boil- ing. 5 HC1 HgCl white HNO, With AmOH = NH 2 Hg 2 Cl (black). 6 H 2 S Hg 8 S black aq.reg. Hg 2 S (instable) - HgS+ Hg 7 Am 2 S 1 1 8 El Hgl (yellow- ] green KI (ex). Ex. forms HgI 2 (sol.) + Hg. Acids decompose it. 9 H 2 S0 4 Hg 2 S0 4 white HNOs In strong sol. only. 10 K 2 Cr 2 7 Hg 2 CrO* yellow HN0 3 11 AmoOx Hg 2 0x white 12 HNa 2 F0 4 HgsPO* 13 ZCy HgCy 2 + Hg gray H 2 Hg ppd. 14 K.FeCyB Hg4FeCy fi white HNOs 15 Zn. Hg gray HNOs, aq.reg. Also Al, Bi, Cd, Cu, Mg. Sn amalgamates with M. 1 A Na,C0 8 , ) He- a Heat in tube with Na 2 C0 3 lo B.B.C.C. ) **& + C, and Hg sublimes. 51. GROUP I. - Pb", Ag , Hg . ANALYTICAL REACTIONS. PPT. DIRECTIONS. SOL. 1. Fpt. PbCl 2 , AgCl, HgCl. Sat. sol. with HC1, filter, wash, reject washings. 2. Sep. Pb from Ag.Hg. On (1) pour boiling H 2 0. Repeat till last fil. gives no ppt. with K 2 Cr 2 O 7 sol. 3. Final test for Pb. To (a) add K 2 Cr 2 O 7 sol. (or K 2 Cr 2 O 4 ). 4. Sep. Ag. from Hg. On (2) pour warm AmOH two or three times. 5. Final test for Ag. Acidify (b) with HN0 3 . 6. Dis. NH 2 Hg 2 Cl. To (4) add very little aqua regia. 7. Final test for Hg. To (c) add SnCl 2 sol. (l)PbCl 2 ,AgCl,HgCl (2) AgCl, HgCl (3) PbCr0 4 (4) NHoHg 2 Cl (5) AgCl (6) HgCl, Hg (a) PbCl 2 (b)(NH 3 ) 3 (AgCl) (c) HgCl, Supplementary. 1. Avoid large excess of HC1, as it may interfere with the ppts. of H 2 S, Grp. II- AgCl is less sol. than HgCl, HgCl than PbCl 2 . H Cl may give a ppt. outside of Group I as follows : of S, if a sulfid or thiosulfate is present ; of BaCl 2 (sat. sol.) which is sol. in H 2 O but insol. in strong HC1 ; of BiOCl, SbOCl, Sn 2 OCl 2 , from sols, acidified with other acids than HC1 (these are sol. in excess of HC1); of As 2 S 3 , Sb 2 S 3 , SnS 2 , AgCy, XiCy 2 , H 4 Si0 4 , H 3 B0 3 , Zn(OH) 2 , A1(OH) 3 , from an alk. sol. In any of the above cases if an appreciable ppt. falls, insol. in H 2 or HC1, dis. and analyze separately. 2. PbCl 2 should all be removed by successive additions of hot H 2 (test the last fil. with a drop of AgNO 3 sol.), as NH 4 OH changes it to white insol. Pb 2 OCl 2 , some of which appears in the fil. H N O 3 however dis. it. It may be better to boil the liquid which holds the first ppt. before filtering, then filter and test the fil. for Pb. 3. What other reagent might be used here ? 4. Why is not AgN0 3 formed ? I have a white powder which is PbCl 2 , HgCl, or AgCl. What reagent will determine which it is ? 52. MERCURY (ic), Hgr'. ANALYTICAL REACTIONS. DIRECTIONS. PPT. COLOR. SOL. 1. Ppt. HgS(v.Pb,Bi,Cd,Cu,As,Sn,Sb). Sat. sol. with H 2 S gas, filter (test fil.), wash. (1) HgS black 2. HgS insol. in Am 2 S, (v. As, Sn, Sb). To (1) in e.d. add Am 2 S x , stir, boil, 1 decant, wash. (2) HgS u 3. HgS insol. in dil. HN0 3 (v.Pb,Bi,Cd, Cu). Cover (2) with dil. HNO 3 , boil a minute, decant. (3) HgS u 4. Dis. HgS in aqua regia (v. Hg'). To (3) add little aqua regia, stir, boil if necessary. (S) (a) HgCl 2 5. Ppt. HgCl and Hg with SnCl 2 (v. Hg', Sn"). Boil (a) to expel all Cl, add SnCl 2 sol. (4) HgCl white Hg gray Supplementary. 1. Hg" salts often give with H 2 S a ppt. first white, then yellow, red, brown, black. Double salts., e.g. HgCl 2 (HgS) 2 are first formed. 3. Strong HN0 3 may convert HgS into Hg(N0 8 ) 2 (HgS) 2 , white, insoluble ; hence test a white res. for Hg. 4. In dis. HgS use the smallest quantity of aqua regia (usually only a few drops). The sol. may afterwards be diluted. 5. SnClj sol. is pearly, and must not be confounded with a Hg ppt. How detect HgN 3 in a mixture with Hg(N0 3 ) 2 ? Hg(N0 3 ) 2 in presence of HgNO 3 ? Explain the action of SnCl 2 on HgCl 2 . Is HgS sol. in strong H N0 3 ? Why is Hg" not put into Group I ? GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. I AmOH NH 2 HgCl white AmOH, HC1 Hg(N0 3 ) 2 gives NHg 2 N0 8 . 2 NaOH HgO y el. -red HN0 3 Hg(OH) 2 not known. 3 Am 2 C0 3 NH 2 HgCl white AmOH, HC1 4 NfeCOs (HgO) 3 HgC0 3 (var.) C red j white Forms HgO on boiling. 5 SnCl; HgCl, Hg gray HN0 3 ,aq.reg. 6 H 2 S HgS black aqua regia May be first white, then 7 Am 2 S (i a red, brown, black. 8 KBr HgBr 2 white hot H 2 El HgI 2 red 1 HgCl 2 \ KI (ex.), HC1 10 K 2 Cr 2 7 HgCr0 4 orange HNOs 11 Am : 0x HgOx white dil. HN0 3 With HgCl 2 no ppt. forms. 12 HNazPO* Hg3(P0 4 )j (i acids, Am. salts 13 KCy HgCy 2 it KCy (ex.) 14 K4FeCy 6 Hg 2 FeCy 6 K On stand, becomes Pruss. blue. 15 Zn Hg gray Forms amalgam with the metal 1 /> Na 2 C0 3 \ TT-_ u (v. Exp. 50). 16 B.B.C.C.J Hg 53. L.EAD, Pb". ANALYTICAL REACTIONS. DIRECTIONS. PPT. COLOR. SOL. 1. Ppt. PbS (v. Hg", Bi, Cd, Cu, As, Sn, Sb). Sat. sol. with H 2 S, filter (testfil.), wash. 2. PbS insol. in Am 2 S x (v. As, Sn, Sb). (1) PbS ( brown- ( black To (1) in e.d. add Am 2 S x , warm, decant, wash. (2) PbS u 3. Dis. PbS in HN0 3 (v. Kg"). Boil (2) with dil. HN0 3 , evap., add H 2 0. (a) Pb(N0 3 ) 2 4. Ppt. PbS0 4 (v. Bi, Cd, Cu). To (a) add dil. H 2 S04+C 2 H 6 OH, and shake it. (3) PbS0 4 white Supplementary. 1. Pb sometimes gives colored ppts. at first, like Hg", if much HC1 is present. If there is much mineral acid, it must be diluted or partly neutralized before H 2 S will give a ppt. 3. Strong HNO 3 oxidizes PbS to PbSO 4 , and dil. acid does so somewhat. Some PbSO 4 dis. in HN0 3 , and some may be left with HgS. Test the latter with boiling AmAc sol., filter and add HAc + K 2 Cr 2 7 sol. Before adding H 2 SO 4 all HN0 3 should be expelled by evaporation, (a) Sep. Hg" from Pb. Test the relative solubility in water of (b) PbCl 2 , (c) PbS, (d) PbSO 4 . Can these salts exist together in a sol.: (e) Pb(NO 3 ) 2 + MgS0 4 ? (f) Pb(NO 3 ) 2 + Na 2 CrO 4 ? (g) Pb(NO 3 ) 2 + NaCl ? Explain. Exp. 48 gives General Reactions for Pb. 54. BISMUTH, Ei'". ANALYTICAL REACTIONS. DIRECTIONS. PPT. COLOR. SOL. 1. Ppt. Bi 2 S 3 (v. Hg, Pb, Cd, Cu, As, Sb, Sn). Sat. sol. with H 2 S, filter, wash. 2. Bi 2 S 3 insol. in Am 2 S x (v. As, Sn, Sb). To (1) add Am 2 S x . (1) Bi 2 S 3 (2) Bi 2 S 3 ( brown- j black u 3. Dis. Bi 2 S 3 in HN0 3 (v. Hg.). To (2) add dil. HNO 3 , boil a min- ute, filter. (S) (a) Bi(N0 3 ) 3 4. Bi not ppt. by H 2 S0 4 (v. Pb). To (a) add few drops H 2 S0 4 . (b) Bi(N0 3 ) 3 5. Final test for Bi (v. Cd, Cu). To (b) add excess AmOH, shake, let stand. (3) Bi(OH) 3 white Supplementary. 1. Diluting an acid sol. of Bi may ppt. BiOCl, BiON0 3 , etc., but H 2 S changes these to Bi 2 S 8 . 5. NH 4 OH must be added in excess, otherwise Bi will not ppt. here, but with Cd (v. Group II, A), (a) Pour a few drops of the BiCl 3 sol. into a t.t. of H 2 O. BiCl 3 reacts with H 2 O, and forms insoluble BiOCl (v. Sb). (b) Test Bi(NO 3 ) 3 sol. in the same way. BiNO 3 (OH) 2 (variable) is ppd. Name the ppts. Try to dis. them with acids: (c) HC1, (d) HNO 3 , (e) HAc. Most salts of Bi react with H 2 O. This confirmatory test may be tried in analysis. Ppt. (f) a Bi salt and (g) a Pb salt (in 2 tubes) with K 2 Cr 2 O 7 sol., and test solubility of each in NaOH sol. What would this reaction distinguish ? Now add (i) Bi from Pb ; (j) Bi from Ag. SnCl 2 sol. to each, (h) Sep. Bi from Hg"; GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 AmOH Bi OH*; white Acids Boil, gives Bi 2 O 3 (yel.-wh.). 2 NaOH <( " No. ppt. with H 2 Tr or H 3 Ci. 3 AmgCOs Bi 2 2 C0 3 " 4 Na 2 CO s ti u d 5 SnClo BiO black With excess NaOH (T. Cl). 6 Ht8 BiA u HN0 3 (dil.) Insol. in Am 2 S x . 7 Am 2 S t( d u u u KI \ (BiOD (dark HC1 / Bil . (brown 9 H 2 BiOCl white HC1 Others give basic salt. 10 11 K 2 Cr 2 7 j or Z 2 Cr0 4 ) Bi 2 0(Cr0 4 ) 2 yellow HNO Insol. in NaOH (v. Pb). 12 Am 2 0x Bi 2 0xs white HN0 3 13 HN^POi BiP0 4 " HC1 Insol. in HNO 3 or HAc. 14 KCy Bi(OH) 3 " Acids Insol. in excess KCy., 15 K 4 FeCy BuFeCyis ( yellow- 1 white HNO Reppts. on boiling. 16 Zn Bi spongy " Also Cu, Fe, Pb, Sn. 17 B.B.C.C. i Bi dark " Incrustation yellow. i 55. CAI>MIUM, Cd". ANALYTICAL REACTIONS. DIRECTIONS. PPT. COLOR. SOL. 1. Ppt. CdS (v. Hg, Pb, Bi, Cu, As, Sb, Sn). Sat. sol. with H 2 S; filter, wash. (1) CdS yellow 2. CdS insol. in Am 2 S x (v. As, Sb, Sn). To (1) add Am 2 S x in e.d.; stir. (2) CdS yellow 3. Dis. CdS in HN0 3 (v. Hg). Boil (2) a minute with dil. HNO 3 . Filter if necessary. (S) (a) Cd(N0 3 ) 2 4. Cd not ppd. by H 2 S0 4 (v. Pb). To (a) add a drop or two dil. H 2 S0 4 . (b) Cd(N0 3 ) 2 5. Cd(OH) 2 dis. by excess AmOH (v. Bi). To (b) add excess. AmOH. (c) (NH 3 ) 2 CdO(AmN0 3 )2 6. Cd not ppd. by KCy (v. Cu). To (c) add little KCy sol. (d) (KCy) 2 CdCy 2 7. Ke-ppt. CdS (v. Cu). Sat. (d) with H 2 S. (3) CdS yellow Supplementary. 1. If a large excess of acid is present the sol. must be diluted before H 2 S will act. (a) Sep. Cd from Bi. (b) Sep. Cd from Hg". (c) Sep. Cd from Pb. What sol. salts, if any, of Cd have the corresponding salts of Cu insol. , or vice versa (v. Table A) ? (e) Devise any method of separating Cd from Cu, dependent upon this, and try it. GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 AmOH Cd(OH) 2 white AmOH(ex) 2 NaOH it Acids Insol. in excess. 3 Am 2 C0 3 CdC0 3 4 NfeCOs u Free Am prevents, ppt. 5 H 2 S CdS yellow i Hot, dil. iHNOs 6 Am 2 S u n 7 K 2 Cr 2 OT CdCrO* It HNO. In concentrated sols. only. 8 Am 2 0x CdOx white Acids (si.) 9 HNa^ Cd3(P0 4 ) 2 u Acids 10 KCy CdCy 2 u KCy (ex.) Re-ppd. by H 2 S. 11 K^FeCyB Cd 2 FeCy B u (HC1 1 AmOH 12 KaFeCyr, Cd 3 Fe a Cy 12 yellow i AmOH IHC1 13 Zn Cd gray Also Al, Mg. 14 Na.COs ) B.B.C.C. \ CdO ( brown- ! yellow Incrustation, no globule. 56. COPPER, Cu". ANALYTICAL REACTIONS. DIRECTIONS. PPT. COLOR. SOL. 1. Ppt. CuS (v. Hg, Pb, Bi, Cd, As, Sb, Sn). Sat. sol. with H 2 S, filter, wash. 2. CuS insol. in Am 2 S x (v. As, Sb, Sn). To (1) add Arn 2 S x ; stir. 3. Dis. CuS in HN0 3 (v. Hg). To (2) add dil. HNO 3 , boil a min- ute, filter if necessary. (1) CuS (2) CuS (S) ( brown- I black ( brown- l black (a) Cu(N0 3 ) 2 4. Cu not ppd, by H 2 S0 4 (v. Pb). To (a) add a drop or two H 2 SO 4 . (b) Cu(N0 3 ) 2 5. Cu salts sol. in excess AmOH (v. Bi). To (b) add excess AmOH. (c) (NH 3 ) 2 CuO(AmN0 3 ) 2 6. Action of KCy on Cu salts (v. Cd.). To (c) add KCy sol. until blue color disappears. (d) (KCy) 2 CuCy.> 7. Inaction of H 2 S on (KCy) 2 CuCyo (v. Cd). Pass H 2 S into (d). (e) (KCy) 2 CuCy. 2 8. Final test for Cu. To (e) add HC1. (3) CuS { brown- ( black Supplementary. 5. If the sol. does not become blue on adding NH 4 OH, Cu is absent. 2. CuS dis. slightly in (NH 4 ) 2 S X . Neutralizing such a sol. with HC1 gives a liver-colored ppt. (a) Sep. Cu and Pb; (b) Cu and Hg"; (c) Cu and Bi. (d) Can CuCl 2 exist in sol. with Na^COa ? (e) Cu(NO 3 ) 2 and Na 2 S ? (f) CuCl 2 and MgSO 4 ? GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 AmOH Cu(OH) 2 blue AmOH (ex.) Unsat., pale-blue basic. 2 NaOH u Boiling gives black CuO. 3 Am 2 C0 3 Cu 2 (OH) 2 C0 3 u Am 2 C0 3 (ex.) it U U U 4 H 2 S CuS black HNOs, KCy 5 Am 2 S u " d 6 KI CuI,I yel.-wh. KI(ex.) 7 K 2 Cr0 4 Cu 2 Cr0 4 (OH) 2 red-br. 8 Am 2 0x CuOx ( blue- i white j M. acids i Am 2 0x(ex.) 9 HNa 2 P0 4 HCuP0 4 U ' Acids Cu (ex.) gives Cu 3 (PO 4 ) 2 . 10 KCy CuCy 2 gr.-yel. KCy (ex.) H 2 S has no effect on KCy. 11 Cu 2 FeCy 6 red-br. AmOH Dil. sol. gives red color. 12 KBr+H 6 2 S0 4 None. red A drop or two of each. 13 Zn Cu " HNOs Also Al, Bi, Fe, Ni, Pb, Sn. 14 B.B.C.C. i " u " No incrustation. 57. GROUP II, A.-Ug 9 Pb, Bi, Cd, Cu. ANALYTICAL PEACTIONS. DIRECTIONS. PPT. SOL. 1. Ppt. HgS, PbS, Bi. 2 S;j, CdS, CuS {v?As,~Sn, Sb). Sat. sol. with H 2 S gas, filter, test filtrate, wash residue until washings give no ppt. with a drop AgNO 3 . 2. Separate Hg from Pb, Bi, Cd, Cu. To (1) add little dil. HN0 3 , boil a minute, decant, leave residue. 3. Dis. HgS in aqua regia. To (2) add a few drops aqua regia, stir, warm if neces- sary. 4. Final test for Hg (v. Hg", Sn). Boil to expel all free Cl, add SnCl 2 sol. 5. Sep. Pb from Bi, Cd, Cu. Expel all HNO 3 from (a), add little dil. H 2 S0 4 +C 2 H 5 OH, shake, let stand, filter, test fil. 6. Sep. Bi from Cd, Cu. To (c) add AmOH, shake, let stand, filter. 7. Sep. Cd from Cu. To (d) add KCy sol. until any blue color disappears, then sat. (e) with H 2 S. 8. Final test for Cu. Acidify (f) with HC1. (1) HgS, PbS, Bi 2 S 3 , CdS, CuS (2) HgS (S) (S) (3) HgCl, Hg (4) PbS0 4 (5) Bi(OH) 3 (6) CdS (7) CuS (a) Pb(N0 3 ) 2 , Bi(N0 3 ) 3 Cd(N0 3 ) 2l Cu(N0 3 ) 2 (b) HgCl 2 (c) Bi(N0 3 ) 3 Cd(N0 3 ) 2 Cu(N0 3 ) 2 (d) (NH 3 ) 2 CdO(AmN0 3 ) 2 (NH 3 ) 2 CuO(AmN0 3 ) 2 (e) (KCy) 2 CdCy 2 (KCy) 2 CuCy 2 (f) (KCy) 2 CuCy 2 Supplementary. 1. Acidulate the original sol. with HC1 (not HNO 3 , which, like other oxidizing agents, decomposes H 2 S). Unless the sol. is acid, Co, Ni, Zn are liable to ppt. if present. If too acid, Cd, Pb, etc., will not ppt. If no ppt. falls, dil. the sol. 1. Be sure the sol. is sat. with H 2 S ; to ascertain this test the fil. 2. A black res. may not be HgS, but S with enclosed particles of PbS, Bi 2 S 3 , CuS. Hence confirm by SnCl 2 . 5. Test a small part of the sol. for Pb at first. 6. Excess of AinO H must be used to ppt. all the Bi (which otherwise may appear in the final Cd test) and to dis. Cu(OH) 2 and Cd(OH) 2 at first formed. Bi may be confirmed by dis. ppt. in a few drops of HC1, evapo- rating free acid and adding to H 2 0. 6. If the color is not blue on adding AmO H no appreciable Cu is present. Unless previously removed Pb will ppt. with AmOH. 7. The final Cd ppt. must be yellow. If not, some of the other metals have failed to ppt. at the right place, and will appear here. As, Sn, Sb Group II, B are omitted here for brevity. They are ppd. by H 2 S, and may be separated from the whole of Group II by dissolving in Am 2 S x (v. Exp. 61). If Group I metals were not removed by HC1, would they ppt. with Group II (test each with H 2 S) ? 58. ARSENIC, As'". ANALYTICAL REACTIONS. DIRECTIONS. PPT. COLOR. SOL. 1. Ppt. As 2 S 3 (v. Group II, A; Sn, Sb). Sat. sol. with H 2 S, filter (test fil.), wash. (1) As 2 S 3 yellow 2. As 2 S 3 insol. in HC1 (v. Sn, Sb). Cover (1) with HC1, boil a min- ute, filter, wash. (2) As 2 S 3 yellow 3. Dis. As 2 S 3 in Am 2 S x . To (2) add Am 2 S x , boil, filter if necessary. (S) (a) Am 3 AsS 3 4. Re-ppt. As 2 S 3 . Cautiously acidify (a) with HC1. (3) As 2 S 3 ,(S) yellow Supplementary. The original sol. should be acidified with H Cl. (a) Try a neutral sol. with H 2 S, also (b) an alkaline. H 2 S acts very slowly on As v , but more rapidly when hot than when cold, ppg. As 2 S 3 + S. Test (c) an acid, (d) a neutral, (e) an alkaline sol. of As salts with a sol. of a Cu salt. What 2 yellow ppte. formed by H 2 S ? (f) Test the solubility of each in Am 2 S x . GENERAL REACTIONS. RB-AGT. PPT. COLOR. SOLVENTS. REMARKS. fAmfVH 1 AgNO, AgsAsOs yellow 1 AJliUXl < dil. HCl LAmCl As v (neutral) + AgNO 3 = Ag 3 AsO 4 (red-brown). 2 H,S ASaS., ( lemon- / yellow fAm 2 CO s 4 Am 2 S x LNaOH Re-ppd. by HCl. 3 AmcS d 4 CnS0 4 HCuAsOs green (AmOH I ail. acids Scheele's green (Paris green). 5 KMnO* Decolorized. f!n A /* ( CuCXAsoOv* u (AmOH Schweinfurt green. U vQAUl iCuACj land acids Paris green. 7 Cu As gray aq. reg, Heated with HCl (Reinsch's test). 8 H (nascent) AsH 3 (ga) Burns with pale-white flame. Deposits As on porcelain. AsH 3 very poisonous (Marsh's test). 9 Na,C0 8 +KCy As gray HCl Sublimed if heated dry. 10 *C (heated) u Garlic odor. 11 lAmCPAmOH 1 +MgS0 4 AmMgAs0 4 white For Asv only. 12 Am 3 MoO, AmAs'MoO;, yellow Composition uncertain (v. M 8 P0 4 ). 59. TIN, Sn' . ANALYTICAL REACTIONS. DIRECTIONS. PPT. COLOR. SOL. 1. Ppt. SnS (v. Group II, A ; As, Sb). Sat. sol. with H 2 S, filter, wash. (1) SnS chocolate 2. Dis. SnS in HC1 (v. As). To (1) add HC1, boil, filter if necessary. (S) (a) SnCl 2 3. Hg test for Sn. To (a) add HgCl 2 sol. (2) HgCl, Hg white gray Supplementary. SnCl2 sol. should be freshly prepared, and both Sn and H Cl left in the sol. Otherwise SnCl 4 and Sn 2 O C1 2 are formed. Sn iv with H 2 S gives yellow SnS 2 , sol. in Am 2 S x , or Am 2 CO 3 . (a) Try to dis. Sn in HN0 3 (strong and dil.). Try to dis. part of the res. in (b) HC1, part in (c) aqua regia. What metals have no nitrates? Which of the following can exist in sol. together ? (d) SnCl 2 and HgCl ; (e) SnCl 4 and HgCl ; (f) SnCl 4 and HgCl 2 . (g) Change SnCl 2 to SnCl 4 ; (h) SnCl 4 to SnCl 2 . Give proof of the change in both cases, (i) Sep. Sn from As. (j) Can SnCl 2 and AgN0 3 exist in sol. together ? (k) SnCl 2 and PbCl 2 ? GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 AmOH Sn(OH) 2 white NaOH Ppt. from Sn iv is SnO(OH) 2 , white. 2 NaOH " " ii Boiling gives SnO. Boiling NaOH+HoTr gives Sn (black). 3 Am.CO " it " Insol. in excess (v. Sb"'). 4 Na ; CO " " ' " 5 HgCl 2 HgCl+Hg }white, If dil. HgCl, if strong Hg. {WoATT {Normal Am 2 S does not 6 H 2 S SnS brown il d wil HC1 dis. SnS. If Sniv i s present, ppt. is XX vl SnS 2 (yellow). 7 El SnI 2 yellow HC1, NaOH In neutral, concentr. sol. 8 Am 2 0x SnOx white HC1 9 HN^PO, SH3(P0 4 ) 2 " Acids 10 ECy Sn(OH) 2 " HC1, NaOH HCy (very poisonous) is evolved. 11 E4FeCy6 Sn 2 FeCy B ' 12 HN0 3 , Cl Oxidizes Sn" to Sn iv . 13 or H,0 Sn 2 OCl- white HC1 SnCl 4 also formed and dis- solved. Sn and HC1 add- ed retard action. 14 Zn Sn igray, I spongy * Also Al, Cd, Mg. Na 2 COs ) Use excess Na 2 C0 3 and 15 B.B.C.C. ) little KCy. 6O. ANTIMONY, Sb'". ANALYTICAL REACTIONS. DIRECTIONS. PPT. COLOR. SOL. 1. Ppt. Sb 2 S 3 (v. Group II, A-, As, Sn). Sat. sol. with H 2 S, filter, wash. 2. Dis. Sb 2 S 3 in HC1 (v. As). To (1) add HC1, boil, filter if necessary. 3. Inaction of HgCl 2 on SbCl s (v. Sn). Divide (a), to half add HgCl 2 sol. 4. Ke-ppt. Sb 2 S 3 . Dilute other half (a), add H 2 S. (1) Sb 2 S 3 Sb 2 S 3 orange (a) SbCl:; (b) SbCl 3 Supplementary. Sb 2 S 8 will not ppt. from too acid or too alkaline sols., and only imperfectly from neutral. SbCl 3 is insol. in H 2 O, reacting with it to form insol. SbOCl (which H 2 S changes to Sb 2 S 3 ). It should be acidulated with HC1. Try to dis. Sb in HNO 3 . If not sol., test the res. (a) with HC1, (b) with aqua regia. (c) Add HgCl 2 sol. to SbCl 3 sol. Explain, (d) Apply the "spot test," i.e. Marsh's test (Exp. 44), to Sb. (e) Sep. Sb from Sn ; (f) Sb from As. Would you be likely to find SbCl 3 in sol. with the first group metals ? With a purely aqueous sol. of Group II, A ? GENERAL REACTIONS. KE-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 AmOH BM, white (Hot NaOH (ex.), I HC1 Sol. should be slight- ly acid. 2 NaOH (( tt " " " 3 Am 2 CO: f( u (1 U U 4" (HC1, u u u AftilAJa 1 hot Am 2 C0 3 5 H 2 SbOCl (var.) u Acids Part only ppts. fAm 2 Sx, 6 Hs8 Sb 2 S 3 orange j NaOH, IhotHCl 7 Am 2 S u u i< If too acid or too al- kaline, no ppt. 8 El no ppt. yellow Sb v ppts. I. 9 Am 2 0x Sb(NH s ) 3 Ox 3 white Ppts. slowly. 10 ECy uncertain " 11 EtFeCye u u Insol. in acids. 12 Zn Sb black aqua regia Also Bi, Cu, Mg, Fe, Sn. rMetallic, brittle, 13 Na,CO, 1 B.B.C.C. i " " aqua regia 1 white incrust., 1 green flame, white I fumes (Sb 2 O 3 ). 61. GROUP II, B. As, Sn, Sb. ANALYTICAL REACTIONS. DIRECTIONS. PPT. SOL. 1. Ppt. As 2 S 3 , SnS, Sb.>S 3 (v. Group II, ^)- Sat. sol. with H 2 S, filter, wash. 2. Sep. Sn and Sb from As. Warm (1) in e.d. some time with HC1, decant on filter. 3. Dis. As 2 S 3 . To (2) add Am 2 S x , boil, filter if necessary. 4. Final test for As. Cautiously acidify (b) with HC1. 5. Final test for Sn. Divide (a), to half add HgCl 2 sol. 6. Final test for Sb. Dilute other half (a), add H 2 S. (1) As 2 S 3 , SnS, Sb 2 S 3 (2) As 2 S 3 (S) (S) (3) As 2 S 3 (S) (4) HgCl, Hg. (5) Sb. 2 S ; > (a) SnCl 2 , SbCl 3 (b) Am 3 AsS, Supplementary. 1. If there is very much HC1 in the sol., Sb and Sn may not ppt. To determine this, dilute a little of the sol., and test with H 2 S. 2. The sol. should be warmed with H Cl in excess some time, not boiled, or As will go into solution. As 2 S3 may be dis. by a sat. sol. of Am 2 CO 3 (made without AmOH), warmed, and sep. from Sb and Sn ; then ppt. As 2 S 3 with HC1 (cautiously). 3. If no appreciable res. is left in 2 except S, omit 3. 6. If Sb is present, an orange ppt. will appear first, followed later (if Sn is also there) by chocolate SnS. Metals of Group II, J3, are sep. from those of Group II, J., by dis. the sulfids of the former in Am 2 S x (not Am 2 S). A white ppt. , on adding HC1 is liable to be S. (a) Sep. SbCl 3 from CuCl 2 ; (b) SnCl 2 from BiCl 3 . 62. IRON (ic), Fe'". ANALYTICAL REACTIONS. DIRECTIONS. PPT. COLOR. SOL. 1. Ppt. Fe(OH) 3 (v. Cr, Al). To sol. add AmCl sol. , AmOH, warm, filter, wash res. (1) Fe(OH) 3 red I brown 2. Dis. Fe(OH) 3 in HC1 (v. Cr, Al). To (1) in e.d. add dil. HC1, stir. (a) FeCl 3 3. Be-ppt. Fe(OH) 3 with NaOH (v. Cr, Al). To (a) add excess NaOH sol. (2) Fe(OH) 3 (red 1 brown Supplementary. To reduce Fe'" to Fe" v. Exp. 47. To oxidize Fe" to Fe'" v. Exp. 47. Test FeCl 3 sol. (Fe'") in t.t. with a few drops of (a) K 4 FeCy 6 , (b) K 3 FeCy 6 , (c) KSCy, (d) NaOH. (e) Test also FeS0 4 sol. (Fe") with the same reagents, and tabulate results. Then state what will distinguish Fe" from Fe'". (f) Dis. a little Fe in dil. H 2 SO 4 , nearly evap., add H 2 O, and then determine whether FeS0 4 or Fe 2 (SO 4 ) 3 is found, (g) Dis. a little Fe in aqua regia, evap., dil., test as before, (h) Test also the product after dis. in HC1. (i) Sep. Fe'" from Cu"; (j) Fe" from Bi'". (It is better to oxidize Fe" to Fe'" before separation.) (k) Can a sol. contain both FeCl 3 and HgNO 3 ? (1) FeS0 4 and Cu(NO 3 ) 2 ? (m) Make FeP0 4 . Will H 2 S ppt. FeS ? Fe 2 S 3 is not formed in aqueous analysis. GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 AmOH Fe(OH) 3 (red ( brown Acids Variable to Fe 2 2 (OH) 2 . 2 NaOH a it U .<( li 8 Am 2 C0 3 it it it a u it Traces Fe 2 (C0 3 ) 3 . 4 NaaCOs K n Variable to Fe 2 2 (OH) 2 . 5 HNaPO* FeP0 4 white M. acids Fe" x (except FeAc 3 ) ppt. by this and NaAc (v. M 3 P0 4 ). 6 AmaOx Fe 2 0x 3 u Acids 7 KCy Fe(OH) 3 |red I brown d HCy formed (very poi- sonous). 8 Z4FeCy 6 Fe4Fe s Cy 18 blue H 2 SO* Prussian blue. NaOH + ppt. = Fe(OH) 3 . 9 KsFeCye No action; distinguishes Fe'" from Fe". 10 KSCy FeCy 3 S 3 ( blood- ied Color only, no ppt. Disting. Fe'" from Fe". 11 H 2 S S white Reduces Fe"' to Fe". 12 Am,S FeS+S black Acids First reduces Fe'" to Fe". 13 j Tannic acid ( and galls. Fe'" tannate it Basis of writing ink. 14 NaAc Fe 2 Ac 3 (OH) 3 red 15 ( SO,, H 8 S 1 Zn, SnCl 2 Reduce Fe'" to Fe". 63. IRON, Fe". GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 AuiOH Fe(OH) 2 (green i black ( AmCl (si.), ( Acids White, if pure. Oxidizes to Fe(OH) 3 , red-brown. 2 NaOH (C a u u u u 3 Am 2 C0 3 FeC0 3 white u Oxidizes to Fe(OH) 3 . 4 NaoCO; u " 11 U U 5 H,S FeS black u With FeAc 2 only a slight ppt. 6 Am_>S u u it Oxidizes to FeO(S0 4 ) 2 . 7 Am,0x FeOx yellow- white M, acids Kino 8 HNa2P0 4 HFeP0 4 Diue- white Acids Fe 3 (PO 4 ) 2 also formed. 9 KCy FeCy 2 yellow- red KCy (ex.) 10 K4FeCy 6 K 2 Fe 2 Cy 6 blue- white Oxidizes in air to Prus- sian blue. 11 K-FeCy, Fe 3 Fe 2 Cyi2 blue Distinguishes Fe" from Fe"'. 12 KSCy no effect a u u 13 HN0 3 , KC10 3 14 Cl, &c. Fe'" (no ppt.) red Oxidizes Fe" to Fe'". 15 f Tannic acid i + tincture I gaUs Fe" tannate ( white to I black Oxidizes to Fe'" tannate (black ink). Supplementary. In the separation of Fe" it is first oxidized to Fe'", and then tested as in Group III. To ascertain whether you have a ferrous (Fe") or a ferric (Fe'") salt, test the original sol. by the table below, (a) Prepare some Prussian blue ; (b) Everitt's salt ; (c) Turnbull's blue ; (d) black ink. TESTS FOR FERROUS AND FERRIC IRON. RE-AGT. FE". FE"'. K4FeCy 6 Z 2 FeFeCy 6 (bluish white). Potassium ferrous-ferro-cya- nid or Everitt's salt. Fe4Fe 3 Cyi8 (deep-blue). Ferric-ferro-cyanid or Prus- sian blue. ZsFeCye Fe 3 Fe 2 Cyi 2 (dark-blue). Ferrous-ferri-cyanid or Turn- bull's blue. FeFeCy 6 (green or brown color only). Ferric-f erri-cy anid . KSCy No effect. Fe(SCy) 3 (blood-red color only). Ferric-sulpho-cyanid. KOH Fe(OH) 2 (white to dirty green). Ferrous hydroxid. Fe(OH) 8 (red-brown). Ferric hydroxid. 64. ALUMINUM, Al"'. ANALYTICAL REACTIONS. DIRECTIONS. PPT. COLOR. SOL. 1. Ppt. A1(OH) 3 (v. Fe, Cr). To sol. add AmCl sol. , AmOH, boil, filter. (1) A1(OH) 3 white 2. Dis. A1(OH) 3 in HC1 (v. Fe, Cr). To (1) add dil. HC1, stir. (a) A1C1 3 3. Dis. A1(OH) 3 in NaOH (v. Fe, Cr, Zn). To (a) add excess, strong NaOH sol., shake. (b) Na2Al 2 4 4. A1(OH) 3 insol. in AmOH. Acidify (b) with HC1, add AmOH. (2) A1(OH) 3 u Supplementary. 3. NaO H sol. must be in excess, and strong enough to dis. the A1(OH) 3 first formed, (a) Sep. Fe from Al. (b) Test action of limited NaO H sol. on Al. (c) Is A1 2 S 3 formed in aqueous analysis [try H 2 S and Am 2 S ; a ppt. is A1(OH) 3 ] ? (d) Test Al'" and AmCl sol. with NaOH sol. (e) Now ppt. A1(OH) 3 with AmCl and NaOH, and try to dis. it in excess, (f) Sep. Cu and Al ; (g) Bi and Al. (h) Obtain A1C1 3 from several cpds. of Al, in two or three different ways, (i) Obtain alum crystals by mixing sols, of sulfates of Al and K (Exp. 5). Try to dis. Al in (j) HC1, (k) HNO 3 . GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. rNaOH(ex.) forms 1 AmOH A1(OH) 3 (gray ( white NaOH, acids I Na2Al 2 O 4 ,notre- I ppd. by boiling I (v. Zn). f NaOH (ex.) forms 2 NaOH ti u u ^ Na2Al 2 4 ; AmCl [ re-ppts. it. 3 Am 2 C0 3 u Na 2 C0 3 Liberates CO 2 . 4 Na-COs " NazCOs (ex.) u u 5 Am,S (( white Acids H 2 S evolved. KJeCye uncertain it 7 HNa,POi A1P0 4 NaOH, HC1 8 NasStOs A1(OH) 3 +S Acids S0 2 liberated. TFirst heat : infus. 9 | B.B.C.C 7 . I + Co(N0 3 ) 2 blue Add a drop of Co(N0 3 ) 2 sol., I heat: blue. ii iff r- |U 65. CHROMIUM (ic), Cr"'. ANALYTICAL REACTIONS. DIRECTIONS. PPT. COLOR. SOL. 1. Ppt. Cr(OH) 3 (v. Fe, Al). To sol. add AmCl sol., AmOH; warm. (1) Cr(OH) 3 green 2. Dis. Cr(OH) 3 in HC1 (v, Fe, Al). To (1) add dil. HC1, stir, filter if necessary. (a) CrCl 3 3. Oxidize Cr'" to Cr vi . Evap. (a) almost to dryness, then add 1 or 2 crystals KC10 3 , and evap. to dryness ; add H 2 O, filter if necessary. (b) K 2 Cr 2 7 4. Action of NaOH on KoCr_,0 7 . To (b) add NaOH sol. (c) K 2 Cr0 4 5. Ppt. PbCr0 4 . Acidify (c) with HAc, add Pb(N0 3 ) 2 sol. (2) PbCr0 4 yellow Supplementary. 1. Cr(OH) 3 may dis. in cold water, but re-ppts. on boiling. 3. Cr"' must be oxidized to Cr, or it will ppt. with NaOH sol. (a) Sep. Cr"' from AY", (b) To K 2 Cr 2 7 sol. add successive small portions of AmOH, shaking each time, till the color becomes yellow. Alkalies reduce red dichromates to yellow chromates; acids have the reverse effect, (c) Slowly acidify the chromate with HC1. (d) Will Cr(OH) 3 ppt. from K 2 Cr 2 O 7 sol.? (e) Reduce Cr vi to Cr'". (f ) Sep. Cr'" and Fe'" ; (g) Cr"' and Cd. (h) Make Cr 2 (S0 4 ) 3 from K 2 Cr 2 7 . (i) Make Cr(NO 3 ) 3 . GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 AmOH Cr(OH) 3 j blue- \ green ( NaOH(ex.) 1 Acids Re-ppt. by hot AmCl or by boiling. 2 NaOH '* " NaOH (ex.) it a n tt 3 AmoCO; " " Na 2 C0 3 (ex.) tt tt tt it 4 Na-CO;: a tt u tt it tt n CO 2 formed. Slight ppt. 5 H 2 S Cr 2 2 Cr0 4 Reduces Cr vi to Cr'" in pres- ence of HC1. 6 Am 2 S Cr(OH) 3 u Acids Forms slowly if dilute ; H 2 S liberated. 7 HNaJ?0 4 CrP0 4 green M. acids 8 H 2 S0 4 +H 2 2 undeterm. blue (C2Hs)aO Blue liquid rises to surface with Cr vi only. 9 KCy Cr(OH) 3 ( blue- NaOH HCy liberated. ( green 10 KC10 3 , Cl, &c, Cr'" oxidized to Cr vi (yellow- red) with heat. 11 NazCOg+KClOa i K 2 Cr0 4 yellow H 2 Fused on Pt foil. 12 Na2C0 3 (bead) green V. Table G. 66. GROUP III.-Fe, Al, Cr. SEPARATION. DIRECTIONS. PPT. SOL. 1. Ppt. Fe(OH) 3 , A1(OH) 3 , Cr(OH) 3 . To sol. add AmCl sol., AmOH, (1) boil a minute, filter, wash. | Fe(OH) 3 , A1(OH) 3 , ( Cr(OH) 3 2. Dis. Fe(OH) 3 , A1(OH) 3 , Cr(OH) 3 in HN0 3 . (a) To (1) add dil. HNO 3 . (Fe(N0 3 ) 3 ,Al(N0 3 ) 3 , 3. Oxidize Cr(N0 3 ) 3 to K 2 Cr 2 7 . I Cr(N0 3 ) 3 Evap. (a) to dryness; when al- most evap. add 1 or 2 small crystals KC1O 3 . When evap. dis. in H 2 O ; decant on filter and add to res. a few drops HNO 3 ; pour on same filter. (Fe(N0 3 ) 3 ,Al(N0 3 ) 3 , i KoCr 2 7 4. Sep. Fe from Al and Cr. To (b) add excess strong NaOH (e) sol., shake, filter. (2) Fe(OH) 3 Na. : AL0 4 , K. 2 Cr0 4 5. Sep. Al from Cr. Acidify (c) with HC1, add AmOH, filter. (3) A1(OH) 3 (d) K 2 Cr0 4 6. Final test for Cr. Partly evap. (d), dil., acidify with HAc, add Pb(N0 3 ) 2 sol. (4) PbCr0 4 Supplementary. 1. AmCl prevents ppn. by AmOH of Mg, Mn, Zn, Co, Ni (Fe" partially), aids ppn. of Al, and does not affect Fe"' and Cr. Considerable AmCl is needed. AmO H at first ppts. Co, Ni, Zn, if present, all of which are sol. in excess. If only one of these Fe'", Al, Cr, is present, the color determines which. Cr(OH) 3 dis. in cold H 2 0, but is re-ppd. on boiling. Fe" should be oxidized to Fe'" by boiling with a few drops of HN0 3 . H 2 S must all be removed by boiling before adding AmO H, to prevent formation of Am 2 S and ppn. of Co, Ni, Mn, Zn. Cr"" is reduced by H 2 S to Cr'", and hence ppd. here. 3. Cr"' must all be oxidized to Cr or it will ppt. with Fe. 4. Fe should be tested in the original sol. for Fe" or Fe'" by K 4 FeCy 6 , K 3 FeCy 6 , KSCy. 6. NaO H dis. some SiO 2 from the containing bottles, and there may be a ppt. of H 4 Si0 4 , similar to A1(OH) 3 , small in quantity and sinking sooner than A1(OH) 3 . 6. A white ppt. of PbCl 2 will always appear if no Cr is present. The yellow color alone indicates Cr. 67. COBALT, Co". ANALYTICAL REACTIONS. BISECTIONS. PPT. COLOR. SOL. 1. Ppt. CoS (v. Ni, Mn, Zn). To sol. add AmCl sol., Am 2 S, shake, warm, filter, wash res. with hot H 2 O, adding to it a few drops Ani2S. (1) COS black 2. CoS insol. in HC1 (v. Mn, Zn). To (1) add dil. HC1, stir, decant. (2) CoS 3. Dis. CoS in aqua regia (v. Ni). To (2) add a few drops of aqua reg., stir, filter, evap. acid, dil. (S) (a) CoCl 2 4. Ppt. K 6 Co 2 0(N0 2 )i . To (a) add HAc, KN0 2 sol. (3) K 6 Co. 2 0(N0 2 ) 10 yellow Supplementary. 1. Am 2 S (colorless) must be used, not Am 2 S x (yellow). 2. CoS is sol. in strong, hot H Cl, and slightly in cold, as is NiS. 3. K 6 CoO(N 2 )io is broken up by alkalies, or HC1, but not by HC 2 H 3 O 2 . 1. CoS and NiS are liable to oxidize to the soluble sulfates if exposed long to the air, hence they must be filtered and washed at once. 4. Some ppt. may occur at once in 4, but to be sure all the Co is thrown down 24 hours is needed, and enough KNO 2 must be used. What sulfid in Group II was sol. in aqua regia only ? Why is not CoS ppd. by H 2 S with Group II ? (a) To Co salts add H 2 S, then AmO H. How is Am 2 S made ? (b) Make a borax bead by fusing with the blow-pipe a little Na 2 B 4 O 7 in the loop of a Pt. wire until it becomes clear. Dip this bead into a very weak sol. of CoCl 2 and fuse again. The blue color if the sol. was not too strong is very characteristic of Co. (c) Can AgN O 3 and CoCl 2 exist in sol. together ? Sep. (d) Co and Cd; (e) Co and Cr. GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 AmOH Co(OH) 2 red J AmOH (ex.), ' AmCl, &c. f Blue bas. ppt. first formed. 4 On stand, forms Co(OH),. i. Oxidizes to Co(OH) 3 . 2 NaOH u u " Insol. in NaOH (ex.). 3 Am 2 CO s Co 2 OC0 3 it Am 2 C0 3 (ex.) Violet or blue by heating. 4 Na 2 C0 3 " " Insol. in excess Na 2 CO 3 . 6 Am 2 S CoS black HN0 3 ,aq,reg. Oxid. to CoSO 4 , which is sol. 6 KN0 2 KeCojO(N0 2 >io yellow HC1 Ppts. only in pres. of HAc. 7 KCy CoCy 2 br.-wh. KCy (ex.) Dist. from Ni by hot HC1. 8 EUFeCye Co 2 FeCy 6 Grayish green. 9 KaFeCye CosTe.Cy. J brown (red fin absence of Mn", or Ni, 4 AmCl+AmOH+K 3 FeCy 6 (^ + Co" = blood-red color . 10 HNa2P04 HCoPO ; red AmOH, acids 11 Heat (on paper) blue Dehydrated. 12 Na2B 4 7 (bead) Blue bead in either flame. 13 Cl,Pb0 2 (warm) white Oxidizes Co" to Co'". 14 Zn Co a HC1 Also Cd, Mg. 15 B.B.C.C. i " u Magnetic. 68. NICKEL,, Ni". ANALYTICAL REACTIONS. DIRECTIONS. PPT. COLOR. SOL. 1. Ppt. NiS (v. Co, Mn, Zn). To sol. add AmCl, Am 2 S, warm, filter rapidly, wash res. with hot H 2 O and a few drops of Am 2 S. (1) NiS black 2. NiS insol. in HC1 (v. Mn, Zn). To (1) add little dil. HC1, stir and decant. (2) NiS a 3. Dis. NiS in aqua regia (v. Co). To (2) add at once a few drops of aqua regia, stir, filter, evap. acid, and dilute. (S) (a) NiCLj 4. Inaction of KN0 2 on NiCl and HAc. To (a) add little HAc, KNO 2 sol. ; leave 24 hours. (b) NiCl 2 5. Ppt. Ni(OH) 2 . To (b) add excess strong NaOH sol. ; boil if necessary. (3) Ni(OH) 2 ( apple- | green Supplementary. 1. Ni has not been wholly removed if the fil. is brown or has black particles in it. In that case acidify the fil. with HAc, boil, filter, and test for Ni. 3. In using aqua regia the smallest quantity (usually a few drops) that will suffice to dis. the substance must be employed. The sol. may after- wards be diluted. Note the color of Ni salts. Sep. (a) Ni and Co ; (b) Ni and Fe ; (c) Ni and Cu ; (d) Ni, Cu, Al ; (e) Ni, Bi, Sb. (f) Test Ni with borax bead (v. Co and Table G). GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 AmOH Ni(OH) 2 pale green i AmOH, ' AmCl, &c. Sol. NaOH re-ppts. slowly (violet-blue). 2 NaOH It u Insol. in NaOH (ex.). Un- changed in air. 3 Am,CO green Am 2 CO s (ex.) Sol. has blue-green color. 4 NajjCOs ** ' ' Xi ftjvOs \^) 5 H 2 S NiS black HN0 3 , aq. reg. From neutral or alk. sol., not acid. 6 AnijS u " u Sol. (si.) in Am 2 S (ex.). 7 KiFeCye NiaFeCyc green-white AmOH 8 KsFeCye Ni3Fe 2 Cyi 2 green-yel. AmCl+AmOH+K 3 FeCy 6 + Ni", boiled = red ppt. 9 HNa.PO, Ni3(P0 4 ) 2 green-white 10 ZCy NiCy 2 y el. -green KCy (ex.) Dist. from Co by HC1. 11 M,0x NiOx green Leave 24 hours. 12 Na2B 4 7 (bead) (V. Table G.) Co" obscures test. 13 Cl, Br, &c. Oxidizes Ni" to Ni'". 14 H 2 S, SO,, &c. Reduces Ni 1 " to Ni". 15 Zn Ni white Also Cd, Sn. 10 B.B.C.C. f " HNO Magnetic powder. 69. MANGANESE (ous), Mn". ANALYTICAL REACTIONS. DIRECTIONS. PPT. COLOR. SOL. 1. Ppt. MnS (v. Co, Ni, Zn). To sol. add AmCl sol., Am 2 S, warm, filter, wash in hot H 2 O and Am 2 S. (1) MnS salmon 2. Dis. MnS in HC1 (v. Co, Ni). To (1) add dil. HC1, stir, filter, boil to expel all H 2 S, NH 3 , &c. (test a little with PbAc 2 ). (S) (a) MnCL 3. Ppt. Mn(OH) 2 (v. Zn). To (a) add excess strong NaOH sol., warm. (2) Mn(OH) 2 Mn 2 2 (OH) 2 white brown Supplementary. 3. Mn(OH) 2 will not ppt. with NaOH if AmCl and AmO H are present. Mn(O H) 2 when pure is white, but it rapidly oxidizes to brown Mn 2 O 2 (OH) 2 (variable). This should further be tested by fusing it with a mixture of Na 2 CO 3 and KNO 3 , when bright green K 2 Mn0 4 and Na 2 Mn0 4 are formed, (a) See whether Mn(OH) 2 or MnS forms in preference to the other. Will these exist together hi sol. : (b) MnCl 2 + ZnS 4 ? (c) MnS O 4 + Cu(N 3 ) 2 ? (d) MnCl 2 + K 2 Cr0 4 ? Sep. (e) Mn and Ni ; (f ) Mn and As ; (g) Mn, Cu, Cr ; (h) Pb, Sr, Mn. GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 AmOH w _ SVTT Mn(OH) 2 white AmCl, &c. Quickly oxidizes to brown Mn 2 O 2 (OH) 2 ; insoluble in AmCl. 2 3 NaOH Am,C0 3 MnCOs u u U It U u 4 NazCOs it a 41 u . u u u 5 H 2 S MnS pink HC1, HAc MnS ppts. from MnAc 2 (un- less HAc is present). Not otherwise. 6 Am 2 S (t (t 7 ZiFeCye Mn 2 FeCy 6 white HC1 8 ZaFeCye Mn3Fe 2 Cyi 2 brown Insol. in acids. 9 HNaaPO* Mns(P04) 2 white Dil. acids From AnuMnCL. etc. , forms AmMnP0 4 . 10 KCy MnCy 2 u ZCy (ex.) Darkens in air. 11 M 2 0x MnOx " Acids 12 13 Na2B 4 7 (bead) NaaCOs+KNO,, 1 ignited on Pt [ foil Z 2 Mn0 4 | Na 2 MnO, ) amethyst green In o. f . In r. f . colorless (v. Table G). ( NajjCOg bead (o. f .), same { green color. 14 Cl, Br, &c. Oxidizes to Mn'". 15 (H,S), S0 2 , &c. Reduces Mn" to Mn", ppts. S. 16 Zn Reduces Mn'" to Mn" when rightly acidulated. 17 HN0 8 +Pb0 2 (boil) HMn0 4 (sol.) red Seen on settling of sediment. 7O. ZINC, Zn". ANALYTICAL REACTIONS. DIRECTIONS. PPT. COLOR. SOL. 1. Ppt. ZnS (v. Co, Ni, Mn). To sol. add AmCl, Am 2 S, warm, filter, wash with hot H 2 O and a few drops of Am 2 S. (1) ZnS white 2. Dis. ZnS in HC1 (v. Co, Ni). To (1) add dil. HC1, stir, filter. (S) (a) ZnClo 3. Zn(OH) 2 sol. in excess NaOH (v. Mn). To (a) add excess strong NaOH sol. (b) NaoZnO., 4. Ee-ppt. ZnS. Acidify (b) with HAc, add Am 2 S. (2) ZnS u Supplementary. I. ZnS is the only white sulfid, but it must not be con- founded with a white ppt. of S. 3. Zn(OH) 2 is not sol. in dil. sol. of NaOH, especially if boiled. 4. ZnS is ppd. by H 2 S if the sol. is acidified with HAc. Zn ppts. these metals from sols, of their salts : Pb, Ag, Hg, Bi, Cd, Cu, As, Sn, Sb, Co, Ni, Fe. State color of each sulfid in Groups II and IV (tabulate). What hydroxids are sol. in excess of NaO H ? Sep. (a) Zn and Al ; (b) Zn and Co ; (c) Zn and Mn ; (d) Pb, Fe, Zn. GENERAL REACTIONS. RK-AQT. PPT. COLOR. SOLVENTS. REMARKS. I AmOH ZnOH jgel. 1 white AmOH (ex.) Forms Am 2 ZnO 2 . Boil- ing re-ppts. 2 NaOH u u NaOH (ex.) All Zn salts are sol. in NaOH, except ZnS. 3 Am 2 C0 3 Zn5(OH) 6 (C0 8 )2 (( AmOH V 4 N^COs tt 11 u 5 H 2 S ZnS white From neutral sol. only, and in part only. 6 Am-jS K HC1 Insol. in HAc (v. Mn"). 7 K4FeCy fi Zn 2 FeCy 6 u 8 KaFeCye Zn3Fe 2 Cyi 2 yellow 9 KCy ZnCy 2 white KCy (ex.) 10 NaAfcOxMid) Hot, yellow ; cold, white. {As incrustation. On cool- 11 Na,CO.. / B.B.C.C. \ ZnO, Zn yellow ing becomes white. Co(NO 3 ) 2 makes green color on heating again. 71. GROUP IV. Co, Ni, Mn, Zn. ANALYTICAL REACTIONS. DIRECTIONS. PPT. SOL. 1. Fpt. CoS, NiS, HnS, ZnS. To sol. add AmCl, Am 2 S, shake, warm (not boil), filter rapidly. Pour on res. a few drops Am 2 S, then wash with hot H 2 O. (1) CoS, NiS, MnS, ZnS 2. Sep. Co, Ni from Mn, Zn. To (1) in e.d. add dil. HC1, stir well, filter and wash. (2) CoS, NiS (a) MnCl 2 , ZnCl 2 3. Dis. CoS and NiS. To (2) add at once very little aqua regia. Evap. acid, dil. , add HAc. (S) (b) CoCl 2 , NiCl 2 4. Sep. Co from Ni. To (b) add excess strong KN0 2 sol., leave 24 hours, filter. (3)KeCo 2 0(N0 2 ) 10 (c) NiCl 2 5. Final test for Ni. To (c) add excess strong NaOH sol., boil. (4) Ni(OH) 2 6. To separate Mn from Zn. Partly evap. (a) to concentrate the sol. and expel all NH 3 , acidify with HAc, add excess strong NaOH sol., shake, let stand, filter. (5) Mn(OH) 2 , Mn 2 2 (OH) 2 (d) Na 2 Zn0 2 7. Final test for Zn. Acidify (d) with HAc, add Am 2 S. (6) ZnS Supplementary. 1. Am 2 S (colorless), not Am 2 S x (yellow), must be used. CoS, NiS, etc. , oxidize to sulfates in air. Hence filter rapidly with H 2 having a few drops of Am 2 S. Group II metals, if not all removed, may ppt. here. 2. CoS, NiS are dis. by strong hot HC1, and slightly by cold. 6. ZnS, MnS will ppt. on adding XaO H if any H 2 S is present. Mn will not ppt. with NaO H if AmCl and AmOH are present. Zn(OH) 2 is sol. in excess of strong cold NaOH sol. only. Mn should be tested for by. fusing with Na 2 C 3 and K N O 3 . (a) What members of Group III will Am 2 S ppt. ? (b) of Group II ? (c) Group I ? 72. BARIUM, Ba". ANALYTICAL REACTIONS. DIRECTIONS. PPT. COLOR. SOL. 1. Inaction of AraCl. AmOH on Ba salts (v. Mg). To sol. add AmCl sol. , AmOH. (a) BaCl 2 2. Ppt. BaC0 3 (v. Sr, Ca, Mg). To (a) add Am 2 CO 3 sol., warm, filter, wash. (1) BaCOg white 3. Dis, BaC0 3 in HAc (v. Sr, Ca). To (1) add little HAc. (b) BaAca 4. Action o! K 2 Cr 2 7 on BaAc 2 (v. Sr, Ca). To (b) add K 2 Cr 2 O 7 sol. (2) BaCr0 4 yellow Supplementary. Has AmO H any effect on sol. salts of Ba ? (a) Sep. Ba and Mn ; (b) Ba and Fe'" ; (c) Ba and Bi ; (d) Ba and Hg"; (e) Ba and Hg 7 . (f) What numbers of Group IV will Am 2 C O 3 ppt. ? (g) Group III ? (h) Group II ? (i) Group I ? What Ba salt is insol. in HC1 (v. Exp. 100)? For what test i& Ba(OH) 2 used? BaCO 8 occurs free in nature. How can other Ba salts be made from it ? (g) Make several, (h) Test the Ba flame by dipping a Pt. wire (or a splinter) into BaCl 2 and holding it in the edge of a Bunsen flame. GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. I NaOH Ba(OH) 2 white 20 H,0, Acids Must be very cone. sol. 2 Am 2 CO- BaCOs u Acids Slightly sol. in AmCl, aided by XTrt OA AmOH and heat. 4 .Ma^lsUs HNa^O* HBaP0 4 u u Also AmCl (si.). Must be neu- tral or alkaline. 5 M 2 S0 4 BaS0 4 It 350,000 H.O One of the most insol. of salts. 6 Z 2 Cr0 4 BaCrO yellow j HAc (si.), ( HC1 (warm) Re-ppd. by AmOH. 7 K 2 Cr 2 7 (t u U it 11 8 H 2 SiF, BaSiF e white HC1, HN0 3 C 2 H 2 OH aids ppn., also stir- ring, standing and boiling. Sr not ppd. by H 2 SiF 6 . 9 AmjOx BaOx white Acids From cone. sols. 10 Flame test jyellow- 1 green Vis. through indigo sol.; blue- green through green glass. 73. STRONTIUM, Sr". ANALYTICAL REACTIONS. DIRECTIONS. PPT. COL. SOL. 1. Inaction of AmCl and AmOH on Sr salts (v. Mg). To sol. add AmCl sol. , AmOH. (a) SrCla 2. Ppt. SrC0 3 (v. Mg, Ba, Ca). To sol. add Am 2 C03 sol. , warm, filter, wash. (1) SrC0 3 white 3. Dis. SrC0 3 in HAc (v. Ba, Ca). Pour on (1) a little HAc. (b) SrAc 2 4. Inaction of K 2 Cr 2 7 on SrAc 2 (v. Ba). To (b) add little K 2 Cr 2 O 7 sol. (c) SrAc2 5. Ppt. SrS0 4 with Am 2 S0 4 . To (c) add Am 2 SO 4 sol., shake well, let stand, filter, test filtrate. (2) SrS0 4 Supplementary. (a) Test the Sr flame by dipping a Pt. wire (or a splinter) into a Sr salt, and holding it in the edge of a Bunsen flame. Sep. : (b) Sr and Ba; (c) Group IV and Sr; (d) Group III and Sr; (e) Group II and Sr; (f) Group I and Sr. (g) If HC1 were used instead of HAc (in 3), would the subsequent reaction take place just as well ? (h) See whether you can ascertain which is more insol., SrS0 4 or BaS0 4 . GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. fApirlo 1 NaOH Sr(OH) 2 white 60H 2 From cone. sol. 2 AniiCO: SrCOs " Acids From neutral or alkaline sol. 3 Na 2 CO;, ' ' ' ' 4 HNa 2 P0 4 HSrP0 4 " M. acids Partly sol. in AmCl. 6 M 2 S0 4 SrS0 4 " ( 500HC1, i 7000H 2 Let it stand some time. 6 Am 2 0z SrOx U ( HC1, HN0 3 , (AmCl Slightly sol. in HAc. 7 K 2 Cr0 4 SrCr0 4 yellow Acids From cone. sol. 8 Flame test crimson Best with SrCl 2 . 74. CALCIUM, Ca". ANALYTICAL REACTIONS. DIRECTIONS. PPT. COL. SOL. 1. Inaction of AmCl and AmOH on Ca salts (v. Mg). To sol. add AmCl sol., AmOH. (a) CaCL 2. Ppt. CaC0 3 (v. Mg). To (a) add Am 2 C0 3 sol., warm, filter, wash. (1) CaC0 3 white 3. Dis. CaC0 3 in HAc (v. Ba, Sr). Pour on (1) a little HAc. (b) CaAc 2 4. Inaction of K 2 Cr 2 7 on CaAc 2 (v. Ba, Sr). To (b) add K 2 Cr 2 7 sol. (c) CaAca 5. Action of Am 2 S0 4 on CaAcjj (v. Sr). To (c) add a little Am 2 S0 4 sol., very dil. (d) CaAc-j 6. Ppt. Ca with Am 2 0x. To (d) add AmOH and Am 2 0x sol. (2) CaOx u Supplementary. Sep. (a) Ca and Ba; (b) Ca and Sf; (c) Ca and Pb; (d) Ca, Al, and Bi. CaCO 3 is the most abundant source of Ca salts, (e) Make several Ca salts from it. (f) Test CaCl 2 with a strong sol. of Am 2 S0 4 , and compare with SrCl 2 . This will show why very dil. Am 2 S0 4 must be used to sep. Sr and Ca. (g) Test the Ca flame, as in the case of Sr, and compare the two. (h) See whether CaSO 4 or SrSO 4 is more sol.; (i) BaSO 4 or CaS0 4 . GENERAL REACTIONS. RB-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 2 NaOH Am,C0 3 Ca(OH) 2 CaCOs white u ( 700H 2 0, 1 AmOH Acids Solubility decreased by heat. Cone. sol. only. Slightly sol. with AmCl. Neutral or alkaline sol. 4 NasCOs HNa.PO* HCaFOi u u 5 MiSC-4 CaSO (i fH 2 0(sl.), \ Acids (si.), I Am 2 80 4 With dil. sol. use C 2 H 5 OH. 6 Am 2 0x CaOx II M. acids Insol. in HAc, H 2 0x. AmOH aids ppn. 75. MAGNESIUM, Mg ". ANALYTICAL REACTIONS. BISECTIONS. PPT. COL. SOL. 1. Prevent ppn. of Mg(OH) 2 and MgC0 3 (v. Ba, Sr, Ca). To sol. add AmCl sol., AmOH. (a) (AmCl) 2 MgCl 2 2. Inaction of Am 2 C0 3 on (AmCl) 2 MgCl 2 (v. Ba, Sr, Ca). To (a) add Am 2 C0 3 sol. (b) 3 A1(OH) 8 4 Acids 6 MgCl 2 Mg(B0 2 ) 2 < AmCl, acids 82. NITRATES, MNO 3 . TESTS. RESULTS. 1. Copperas test (v. MN0 2 ). Mix in a t.t. a sol. of MN0 3 , or sol. to be tested, with a fresh sol. of FeSO 4 . When cold, introduce into the bottom of the tube, with a glass tube used as a pipette, a little H 2 S0 4 . 2. Deflagration test (v. MNO 2 , MC10 3 ). Heat B.B.C.C. a very little pow- dered MNO 3 ; or mix with pow- dered charcoal, and put into an i.t. enough to cover a penknife point. Heat cautiously. 3. Red fumes test (v. MN0 2 ). Put into an i.t. very little MNO 3 , heat. Insert a glowing splinter into the tube while heating. 4. Free HN0 3 . (a) Add a little indigo sol. (b) Put a drop on the finger-nail, or dip a feather into it. (c) Pour a little on Cu and warm it. (FeS0 4 ) 2 NO. Brown ring or halo at junction of liquids. Vigorous deflagration ensues. N0 2 and N 2 3 (red) ; O (color- less). Splinter burns. Decolorizes, changing to red isatin. Turns animal matter yellow. Bed fumes (N0 2 ), green liquid, Cu(N0 3 ) 2 . Supplementary. If a ppt. appears on adding H 2 SO 4 , let it settle, then decant. H 2 SO 4 liberates HNO 3 from nitrates, and FeS0 4 reduces HN0 3 at the surface of contact to N 0, which unites with FeS 4 . Let it stand an hour or more if necessary. Heat decomposes this compound (FeSO 4 ) 2 NO, expelling NO. The depth of color indicates the strength of nitrate. Heat decomposes all nitrates ; from those of the alkali and alkaline earth metals are first formed MNO 2 and O, then M 2 O, O, N. Nitrates of Ag and Hg reduce to the metal, others to the oxid only. KNO 3 and NaNO 3 show faint fumes, best seen by looking down the tube to a white background. Indigo is also decolorized by Cl, Br, etc. Nitrates of Au and Sb are unknown. All nitrates are soluble except Bi(N0 3 ) 3 , which reacts with H 2 O and ppts. Bi(OH) 2 N0 3 (variable), and to a less extent Hg / , Hg", Sn", Sn iv . 83. NITRITES, MNO 2 . TESTS. RESULTS. 1. Copperas test (v. MNO 3 ). Apply this as in MNO 8 . 2. Bed fnmes test (v. MN0 3 ). To a little MN0 2 add a few drops of H 2 SO 4 . Test the HNO 2 formed with iodo- starch sol. Test it also with KMn0 4 sol. 3. lodin test. Add a few drops of KI sol. to 3 or 4 cc. H 2 O, then a few drops of dil. H 2 SO 4 ; finally a little MN0 2 sol. (or substance to be tested). Test yellow liquid with starch sol. 4. Nitrate test (v. General Reactions). Same result as in MNO 3 , but more readily obtained. N0 2 (red fumes) copiously evolved ; also HN0 2 . Starch iodid (blue) formed. Decolorized. HI first formed, then H 2 0, and I set free by MN0 2 (yellow color). Iodid of starch (blue). Supplementary. Indigo sol. is decolorized by nitrites, but not by nitrates except by the addition of H 2 S0 4 , which forms HNO 3 . Apply the test. All nitrites are soluble, but AgNO 2 and Pb(N0 3 ) 2 only slightly. Hence this test cannot be applied in dil. sols. GENERAL REACTIONS. BE-AGT. PPT. CO LOB. SOLVENTS. REMAKKS. 1 AgNOs AgN0 2 white \ Acids, i H 2 (ex.) This distinguishes MN0 2 from MNOg. 2 Pb(NO s ) 2 Pb(N0 2 ) 2 u it u it u a 84. CHLORATES, MC1O 3 . TESTS. RESULTS. 1. Oxygen test (v. MN0 2 , MN0 3 ). Heat a small quantity of the solid in at.t. Test the O with a glowing splinter. Dis. the residue when cool, and test for MCI with a drop of AgN0 3 sol. 2. Chlorin test (v. MN0 2 , MN0 3 ). To a very little of the powder in a t.t. add with great caution a few drops of H 2 S0 4 . 3. Deflagration test (v. MN0 3 ). Powder and heat B.B.C.C. 4. Bleaching test (v. MN0 2 , MN0 8 ). To sol. of indigo add MC10 3 sol. , and heat. Mix sols, of MC10 3 and H 2 S0 3 , and add to indigo sol., without heating. 5. Silver nitrate test (v. MAc, MN0 3 ). To sol. add a few drops of AgNO 3 sol. Melts, O escapes, MCI remains. Re-kindles vigorously. AgCl (white) ppts., sol. in AmOH. C10 2 (green-yellow, of charac- teristic odor) liberated with explosive violence. Deflagrates. Turned red (isatin). No effect if the MC10 3 is pure. Supplementary. All chlorates are soluble. Sb, Sn, and Au have no known chlorates. The deflagration of chlorates is greater than of nitrates, (a) Test this by scratching different kinds of matches. A few drops of HC1 added to a few crystals of MC1O 3 , and heated, give C10 2 and Cl, of characteristic odor. Heat liberates O with violence from chlorates, but the presence of certain oxids (e.g. Mn0 2 ) causes it to be liberated more regularly, and at a lower temperature. Dist. (b) KC10 3 and KC1; (c) KC10 3 and KNO 3 ; (d) KC1O 8 and KNO 2 . 85. CARBONATES, M 2 CO 3 . TESTS. RESULTS. 1. Lime water test, To the solid (or sol.) add a little dil. HC1. Test the gas with a drop of Ca(OH) 2 sol. on a s.r., or pass it into Ca(OH) 2 sol., or shake the lime water with the gas. 2. Barium hydroxid test, Apply this hi the same way as the lime water test, using Ba(OH) 2 sol. instead of Ca(OH) 2 . 3. Flame test. Put a burning splinter into the gas generated, as above. CO 2 gas (colorless) is formed, which ppts. white CaCOs with lime water. White BaCO 3 fails, ppd. by CO 2 gas, and dissolved with effervescence by HC1. The flame is extinguished. Supplementary. Any acid (except H 2 S, H Cy) will act on any carbonate and liberate C0 2 , but with varying intensity. H 2 CO 3 with a carbonate (e.g. Na 2 CO 3 or CaCO 3 ) forms the bicarbonate (primary or acid carbonate), as HNaC0 3 , H 2 Ca(CO 3 ) 2 . Most carbonates are insol. Heat breaks up many of them, forming the metallic oxid and C 2 . CaC O 3 requires a red heat, and the alk. carbonates are not decomposed at the temperature of the Bunsen flame (v. oxalates). Try the action of various acids on carbonates, as: (a) HAc; (b) H 2 Ox; (c) H 2 Tr. Na, K, Mg, burn in C0 2 , liberating C. (d) Pass C0 2 from a gen. into lime water till the ppt. clears, then boil. Dist. : (e) C O 2 and SO 2 ; (f) CO 2 and H 2 S ; (g) CO 2 and N0 2 ; (h) M 2 CO 3 and M 2 Ox. Some metallic salts with Na^C O 3 sol. give the primary carbonate, others the secondary, and occasionally a basic salt is formed, as 2PbCO 3 .Pb(OH) 2 . Carbonates are white in color. 86. SULFIDS, M 2 S. TESTS. RESULTS. 1. Acid test. To the solid (or sol.) add a little dil. HC1 (or H 2 S0 4 ), and warm it. Test the escaping gas (odor, PbAc 2 sol. on paper). 2. Coin test. Put a drop of water on a silver coin, and on this a soluble sulfid (if in- sol., first fuse with Na 2 CO 3 ). (V. M 2 S0 3 , M 2 S 2 3 , M 2 S0 4 .) 3. Ppn. tests (v. General Reactions). H 2 S gas formed, with odor of sewer-gas. Black, metallic PbS formed. Coin is blackened. by forma- tion of Ag 2 S. Supplementary. All sulfids, except those of the alkalies and alkaline earths are insol. in H 2 O. Most are sol. in dil. acids. A few (FeS 2 , HgS, CoS, NiS, etc.) are not acted on by acids, except aqua regia. In such cases H 2 S may be made by nascent H, with the addition of a little Zn. No sulfid of Al or Cr is known. Oxidizing agents with sulfids tend to form sulfates, or to liberate S and S0 2 . (a) Test several with HN0 3 , or aqua regia. Metallic sulfids (includ- ing Am 2 S) ppt. from sols, metals of the first four groups, except Cr and Al. H 2 S ppts. only the first two groups. GENERAL REACTIONS. RE-AGT. PPT. PPT. COLOB. SOLVENTS. REMARKS. With H 2 S : With. Am 2 S : 1 Pb(N0 3 ) 2 PbS PbS black HotHNOa(dil.) 2 AgN0 3 Ag 2 S Ag 2 S <( u u u 3 HgN0 3 Hg,S Hg 2 S u aqua regia Warming changes to HgS and S. 4 HgCl 2 HgS HgS u U i( First white, then yel- low, red, black. 5 BiCla Bi 2 S 3 Bi 2 S 3 u HotHNOaCdil.) CdCl, CdS CdS yellow (( It 11 7 CuCl 2 CuS CuS ( brown- f black u u u 8 AsCla AS 2 S 3 As 2 S 3 yellow ( Am 2 S 2 (ex.), 1 Am 2 C0 3 Alkaline sol. not ppd. with H 2 S. 9 SbCls Sb,S 3 Sb 2 S 3 ( orange- ( red ( Am 2 Sx (ex.), 1 HC1 (hot) Ppn. with Am 2 S is imperfect. 10 SnCI- SnS SnS j dark- i brown U 11 11 FeCls none FeS+S black Acids 12 CoCl 2 (t CoS u aqua regia AmCl aids ppn. 13 NiCl 2 NiS 11 u u <( U U 14 MnCl= u MnS pink Acids Turns dark -brown. AmCl aids ppn. 16 ZnCls (( ZnS white ii AmCl aids ppn. 87. SULFITES, M 2 SO 3 . TESTS. RESULTS. 1. Acid test. To the solid (or sol.) add a little HC1 (or dil. H 2 SO 4 ), and heat it. Test the escaping gas (odor, K 2 Cr 2 O7 paper). 2. Zinc test. To the original sol. add Zn and dil. H 2 SO 4 . Test the escaping gas (odor, PbAc 2 paper). 3. Coin test (v. M 2 S, M 2 S 2 O 3 , M 2 SO 4 ). Heat the solid B. B. C. C. with Na 2 C0 3 , also without. Put res. on Ag coin on which is a drop of water. 4. Oxidation test (v. M 2 S0 4 ). To some of the original sol. add a little euchlorin (or HN0 3 ), and heat. Test the product with HC1 and BaCl 2 sol. S0 2 gas is liberated, reducing K 2 Cr 2 7 to green O 2 (S0 4 ) 3 . H 2 S is liberated, forming with PbAc 2 black PbS. Na 2 S is formed, and on the coin black Ag 2 S. M 2 S0 3 is oxidized to M 2 S0 4 , and ppd. with BaCl 2 as white BaSO 4 , insol. in HC1. Supplementary. The alkaline sulfites are freely sol. in water. Most others are but slightly sol., or are insol. Sulfites are decomposed by acids (except H 2 C0 3 , H 3 B0 3 , H 2 S). (a) Ppt. BaS0 3 with BaCl 2 sol., dis. in HC1, filter if necessary, then oxidize fil. with aqua regia, and try to dis. ppt. in HC1. Heat changes sulfites to M 2 and SO 2 ; also to M 2 SO 4 and M 2 S. (b) Make the tests. Sulfites are reducing agents, (c) Test action of SO 2 on FeCl 3 sol., then test sol. for Fe" and Fe'". (d) Test HgCl 2 with S0 2 , then test sol. for Hg' or Hg". (e) Generate H in a t.t., and test the gas for H 2 S with PbAc 2 paper, then add a few drops of Na 2 SO 3 sol. and test again, (f) Bring together jets of S0 2 and H 2 S. (g) Test the bleaching action of S 2 sol. by putting in it a colored flower, or cambric, (h) Test with litmus sol. (i) Let some S0 2 sol. stand for a few days in an open rec., and apply the BaCl 2 and HC1 test, (j) Try the action of SO 2 sol. onCaCO 3 . GENERAL REACTIONS. KE-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 BaCl> BaSO; white HC1 (dil.) (V. M 2 S0 4 .) 2 3 AgN0 3 Pb(N0 3 ) 2 Ag 2 S0 3 PbS0 3 u u HN0 3 (dil.) u Boiling ppts. dark-brown Ag. Not blackened on boiling (v. M 2 S 2 3 ). 4 FeCla Fe 2 (SO) 3 red Boiling forms green FeSO 4 . 6 HgCl> HgCl white Boiling reduces to gray Hg. 88. THIOSULFATES, M 2 S 2 O 3 . TESTS. RESULTS. 1. Bulb-tube test. Heat the solid in a tube. 2. Acid test. Add to the cone. sol. (or the solid) HC1 (or H 2 S0 4 ), warm. Test S0 2 (odor, K 2 CrO 4 ). 3. Beduction test (v. M 2 S0 3 ). (1) To a sol. of starch and KI (made blue by Cl) add a sol. of M 2 S 2 O 3 . (2) To a sol. of starch and KI (un- colored) add M 2 S 2 3 sol. with which a little euchlorin is mixed. 4. Coin test (v. M 2 S, M 2 S0 3 , M 2 S0 4 ). Fuse B.B.C.C., put on Ag coin with a drop of H 2 O. 5. Precipitation tests. (V. General Reactions.) Sublimate of H 2 O and S, and liberation of S0 2 . S ppts. (white), S0 2 formed. Decolorized. Uncolored, as Cl has oxidized M 2 S 2 3 to M 2 S0 4 and HC1. Coin is blackened (Ag 2 S). Supplementary. Thiosulf ates, if mixed in a mortar with chlorates, explode violently. They are strong reducing agents. They are mostly sol. in water, except those of Ba, Pb, Ag. Dist. : . (a) M 2 S 2 O 3 and M 2 S ; (b) M 2 S 2 8 and M 2 S0 3 ; (c) M 2 S 2 3 and M 2 S0 4 . GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 BaCl 2 BaS 2 3 white Dil. acids Acids ppt. S (white). 2 AgN0 3 Ag 2 S 2 3 (t Na^Oz (ex.) Boiling forms Ag 2 S (black). Forms slowly on standing. 3 PbACa PbS 2 3 t( u u Boiling forms PbS (black). Forms slowly on standing. 4 HgN0 3 Hg 2 S 2 3 t( tt u Boiling forms Hg 2 S (black). Forms slowly on standing. 5 FeCla FeClo Acts as reducing agent. 6 CaCl 2 none Dist. from M 2 SO 3 . 89. FL.UORIDS, MF. TESTS. RESULTS. 1. Glass- etching test, (1) Put a little powdered CaF 2 into a small lead dish, and mix with enough H 2 SO 4 to make a thick paste. Cover the dish with a piece of glass (coated with wax if de- sired, and a design scratched on it) and let it stand in a warm place for several hours. Remove the wax by melting, and finally with a cloth wet with alcohol, naphtha, or tur- pentine. (2) Mix a little CaF 2 with HKS0 4 , put into a small t.t., and heat. 2. Turbidity test. Mix a little CaF 2 , Si0 2 and H 2 SO 4 , put into a t.t. and heat it, mean- time holding in the tube on a s.r. (or in the loop of a Pt wire) a drop of H 2 0. 3. Free HF in sol. Dip a brush into the liquid in a leaden dish, and mark out a design with it on a glass plate, going over it several times. Avoid getting any HF sol. on the flesh. The glass will be etched where exposed to the fumes of HF, SiF 4 being formed. The tube will be roughened (or etched) by the HF. The water is rendered turbid by the SiF 4 gas, forming H 2 SiF 6 . The glass will be etched as above. Supplementary. Several of the fluorids are soluble. The most important compounds of F are CaF 2 and HF. The latter corrodes glass, porcelain, and all metals except Pb, Pt, and Au. CaCl 2 ppts. CaF 2 (transparent, gelatinous). BaCl 2 ppts. BaF 2 (white). CaF 2 , which occurs in the earth as fluorite or fluor- spar and cryolite, Na 3 AlFe, a mineral found in Greenland, are the main sources of F compounds. 9O. CHLOKIDS, MCI. TESTS. RESULTS. 1. HC1 test. Add H 2 S0 4 to the solid in t.t., heat. Test gas (odor, color, NH 3 ). 2. Cl test. Mix the solid with MnO 2 , add H 2 SO 4 , heat. Test gas (odor, color, NH 3 , indigo paper). 3. Precipitation tests. (a) To sol. add AgNO 3 sol. Expose part to sunlight, add AmOH to the rest, then HNO 3 . (b) To sol. add HgNO 3 sol. ; then AmOH. (c) To sol. add Pb(NO 3 ) 2 sol. boil with plenty of H 2 0. 1IC1 is liberated. Cl liberated, green - yellow ; AmCl with NH 3 , indigo pa- per bleached. AgCl (white) ppts. ; blackens in light ; sol. in AmOH ; re- ppd. by HNO 3 . HgCl (white) ppts. ; blackened by AmOH. PbCl 2 (white) ppts. ; sol. in boiling H 2 0. Supplementary. Most chlorids are soluble. Except. : Ag, Pb, Hg', Cu'. SbCl 3 , BiCl 3 , SnCl 2 decompose water, forming SbO Cl, BiO Cl, Sn 2 O C1 2 . H 2 S O 4 frees HC1 from all chlorids, except HgCl and HgCl 2 (and not much from Ag, Pb, Sn chlorids). HgCl 2 sol. fails to ppt. PbCl 2 from Pb(NO 3 ) 2 sol. (a) Test the last statement. Dist.: (b) MCI and MC10 3 (cautiously); (c) MCI and MNO 3 . (d) Take 5& KC1O 3 and divide into 2 parts. Dis. one in H 2 O and add AgNO 3 sol. Heat the other a few minutes, then dis., and add AgNO 3 sol. Compare the results. GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 AgN0 3 AgCl white AmOH, etc. (v. Exp. 49.) 2 Pb(N0 3 ) 2 PbCl 2 u Hot H 2 (v. Exp. 48.) 3 HgN0 3 HgCl " HN0 3 (V. Exp. 50.) 91. BBOMII>S, MBr. TESTS. RESULTS. 1. Bromin test. Mix Mn0 2 with the solid, add a little H 2 SO 4 , heat. Test the gas by holding in it a paper dipped in starch-paste. 2. I o do- starch test. Liberate Br as above, and hold in it a paper dipped in a mixture of starch-paste and KI sol. 3. CS, test. To the sol. add a drop or two of 82 sol., and a drop of euchlorin, and shake it. 4. Silver nitrate test. To sol. add a drop or two of AgNOs sol. Try to dis. part of ppt. in HNO 8 , another part in AmOH. Br (red gas) is liberated. Colors starch yellow to orange. Br combines with K in KI, lib- erates I, which forms blue starch-iodid. Br is liberated and absorbed by 82, which is colored yellow. AgBr, yellow- white, ppts., in- sol. in HN0 3 , slowly sol. in AmOH. Supplementary. Bromids are soluble, except those of Ag, Hg', Hg", Cu', Pb. BiBr 3 and SbBr 3 need acidulation. Dilute H 2 S04 acts on bromids to form HBr; strong acid forms Br. (a) To a bromid sol. add euchlorin (very little), and note the color, (b) Dist. MBr and MCI. (c) Pour a little Br vapor into starch-paste, and shake., (d) Mix starch-paste and KBr sol. (very little), and add a drop or two of euchlorin. GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOL. REMARKS. I AgN0 3 AgBr pale yellow AmOH Only slightly sol. in AmOH. 2 PbAc2 PbBr 2 white Hot H 2 Less sol. than AgCl in H 2 O. 8 HgN0 3 HgBr yellow-white KBr 92. IODIDS, MI. TESTS. RESULTS. 1. Starch test. Mix Mn0 2 with the solid, add H 2 S0 4 , heat, and test with cold starch- paste (v. Exp. 40). 2. CS 2 test. Add to the sol. a drop of CS 2 [or (C 2 H 5 ) 2 0], then 2 or 3 drops of euchlorin (avoid excess), and shake it well. Violet I vapor appears, which colors starch-paste blue. CS 2 dis. the I set free by Cl, and is colored violet at the bottom of the tube. NaOH destroys the color, forming Nal and NaI0 3 . Supplementary. Most iodids are sol. , except Pb, Hg 7 , Hg", Au. Sb, Bi, Cu, Sn iv iodids need acidulation, as they react with H 2 0. The double iodids (KIAgI, etc.) are formed and dis. with excess of KI with salts of Pb, Ag, Hg. I may be liberated from an iodid by Zn and HNOs, HNO 2 being first formed. Euchlorin or bromin acts the same. Iodids are broken up by oxidizing agents more easily than bromids or chlorids. GENERAL REACTIONS. BE-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 AgN0 3 Agl yellow-white KCy, Na 2 S 2 3 Insol. in HNO 3 or ArnOH. 2 Pb(N0 3 ) 2 PbI 3 yellow NaOH (ex.) Dis. by HN0 3 . 8 HgNO s Hgl green-yellow HgN0 3 (ex.) u u u 4 Hg(NOs), HgI 2 yellow-red Hg(N0 3 ) 2 (ex.) u it . u 5 CuSCM-HjSOs Cul white H 8 (si.) Insufficient reduc. agent ppts. I. 93. ACETATES, MC 2 H 3 O 2 (MAc). TESTS. RESULTS. 1 . Charring test ( v. M 2 Tr, M 2 0x) . Heat a very little of the solid in a t.t. , take odor. 2. Acetic acid test (v. M 2 Tr). Add to the solid (or sol.) H 2 SO 4 , heat, take the odor, test with litmus. 3. Acetic ether test. Add to the sol. a few drops of C 2 H 5 OH and H 2 S0 4 , warm, and take odor. 4. Ferric test, To sol. add FeCl 3 sol. , boil. 5. Silver nitrate test (v. MNO 3 , MC10 8 ). To a dil. sol. add AgN0 3 sol. To a strong sol. add AgNOs sol. 6. Cacodyl test. Heat with an alkali and very little As^e ; take odor. Melts, expels H 2 O, turns black, gives odor of acetone, C 3 H 6 O (inflammable). HAc is formed, having characteristic odor, and acid reaction. C 2 H 5 Ac is formed, having characteristic odor. FeAc 3 (red sol.). Boiling ppts._ red-brown basic acetate of Fe'". No ppt. AgAc (white) ppts. Cacodyl oxid As 2 (CH 3 ) 4 evolved (intensely offensive odor). Supplementary. All acetates are sol., those of Ag and Hg' only partially. No acetate of Au is known. Dist.: (a) MAc and M 2 Tr; (b) MAc and M 2 Ox. (a) Try to make CH 4 in a t.t. by heating dry NaOH and an acetate, (b) Test the combustibility of the gas. (c) Test some vinegar for acetic acid, (d) Make some HgAc ; (e) AgAc. (f) See whether HAc will dis. Zn ; (g) Fe. (h) If so, test the product for Fe" and Fe'". 94. CYANIDS, MCN (MCy). TESTS. KESULTS. 1. HCy test. Add to sol. a little H 2 SO 4 (or HC1). Very cautiously take the odor by fanning the gas to the face with the hand. 2. Fe(CyS) 3 test. Put a few drops in an e.d., add equally Am 2 S x , evap. to dryness, dis. in dil. HC1, add FeCl 8 sol. 3. Prussian blue test. To sol. add equally a few drops of NaOH sol. and FeS0 4 sol., shake and warm it, add FeCl 3 . Dis. in dil. HC1 (excess). 4. AgN0 3 test. To sol. add a little A gN0 8 sol. Pour off liquid, and boil with HNOg. If not all dissolves, test liquid with HC1. HCy is formed (very poison- ous) ; odor of bitter aim onds. MCyS is formed, sol. in HC1, giving red Fe(CyS) 3 sol. with FeClg. FeCy2 (sol. in MCy excess), Fe(OH) 2 , Fe(OH) 8 formed, soluble in HC1, but ppg. Fe 4 Fe 3 Cyi8, deep blue. AgCy (white) ppts., sol. in hot HN0 3 , re-ppd. by HC1. Supplementary. Use great care in experimenting with cyanids, as they are very poisonous. Cyanids are insol., except HgCy2 and those of the alkalies and alkaline earths (BaCy 2 only slightly). The solutions are alkaline. The ppd. cyanids are often sol. in excess of the cyanids, forming double salts, (a) Make several by ppn., and then dissolve. Dist. : (b) MCy and MAc; (c) MCy and MN0 3 . In the Prussian blue test the following equations indicate the order of changes: (1) 2MCy+FeSO 4 = FeCy 2 +M 2 SO 4 ; (2) 4MCy+FeCy 2 = M 4 FeCy 6 ; (3) FeS0 4 +2NaOH=Fe(OH) 2 -f NaaSO 4 ; (4) 2Fe(OH) 2 +H 2 0+0= 2Fe(OH) 3 ; (5) 2HCl+Fe(OH) 2 =FeCl 2 +2H 2 O; (6) 3HCl+Fe(OH) 3 =FeCl 3 + 3H 2 O; (7) 4FeCl 3 +3M 4 FeCy 6 =Fe 4 Fe 3 Cyi8+12MCl. The vapor of HCy is a deadly poison, N H 3 or Cl inhaled being the antidote. As used in medicine the acid contains only 2% H Cy. 95. TABTKATES, (M 2 Tr). TESTS. RESULTS. 1. Ignition test (v. M 2 0x, MAc). Heat in i.t. Take odor, note res. 2. H 2 S0 4 test (v. MAc, M 2 Ox). Heat in i.t. with little H 2 SO 4 . 3. Mirror test. Add AgNO 3 sol. (to a neutral sol.). Almost dis. ppt. with AmOH, then heat gently in t.t. 4. Acetic acid test (v. MAc, M 2 0x). Add to sol. BaCl 2 sol. Dis. the ppt. in HAc. Add to sol. CaCl 2 sol. Dis. the ppt. in AmCl sol. 5. Potassium chlorid test. Add KC1 sol. and C 2 H 5 OH to the sol., stir with a glass rod. Evolves fumes (white, then brown), CO 2 , with odor of burnt sugar, and black resi- due, M 2 CO 3 , C. CO, C0 2 , S0 2 , C. Ag 2 Tr (white) ppts. Mirror of Ag collects on the tube. BaOx is sol. in HAc. CaOx forms, sol. hi NaOH, re-ppd. on boiling. HKTr (white) ppts. from strong sols. only. Supplementary. Only the alkali tartrates are freely soluble, and the bitartrates of the alkali metals are much less so than the normal ones (v. tests for K and Am). Dist.: (a) M 2 Tr and M 2 0x; (b) M 2 Tr and MN0 2 . (c) Make H AinTr. (d) Try the reducing action of H 2 Tr on K 2 Cr 2 7 sol. (e) See whether CaTr is sol. 96. OXAL.ATES, M 2 C 2 O 4 (M 2 Ox). TESTS. RESULTS. 1. Ignition test (v. M 2 Tr, MAc). Heat the solid in an i.t. Test gas with Ca(OH) 2 sol., also combustion of CO. H 2 Ox decomposes with very slight charring, and without res. 2. Acid test (v. MAc, M 2 Tr). Heat the solid with H 2 SO 4 (which absorbs the H 2 O). 3. Calcium suliate test. Alkalize the sol. with AmOH, add a little CaS0 4 sol. Try to dis. part of the ppt. with HAc, the rest with dil. HC1. CO 2 , CO, M 2 O form. On pass- ing the gas through NaOH sol. to remove C0 2 , CO burns with blue flame. CO 2 , CO, M 2 form. Dil. HC1, HN0 3 or H 2 S0 4 decomposes M 2 0x, forming H 2 Ox. CaOx (white) ppts. , sol. in dil. HC1 without effervescence, insol. in HAc. Supplementary. On igniting oxalates, carbonates and CO first form, then oxids and C 2 . Ag 2 Ox and HgOx (which easily decompose with heat) give the metals as a final product. Ag 2 decomposes with explosion, (a) Test several oxalates, first changing them to Ag 2 Ox. At moderate temperature H 2 0x sublimes unchanged, except to give off its water of crystallization. Most oxalates are insoluble, except those of the alkali metals and Cr. HC1, HNO 8 , or H 2 S 4 forms H 2 0x from its salts. Oxalates are reducing agents, (b) (test with KMn0 4 ), and are almost all white in color, (c) Make several oxalates. (d) vSee whether H 2 0x will react with metals, e.g. Zn and Fe. GENERAL REACTIONS. RE-A.GT. PPT. COLOR. SOLVENTS. I CaCl, CaOx white HC1 (dil.) 2 FeSO* FeOx yellow-white 3 AgNO, Ag 2 0x white 4 Pb(N0 3 ) 2 PbOx n NaOH, HNO S 97. SILICATES, M 4 SiO 4 , M 2 SiO 8 . TESTS. RESULTS. 1. Acid test. To strong sol. add HC1 ; then evap. Add HC1, boil, decant ; then add to res. NaOH sol., boil. 2. Fusion test (insol. silicates). Mix thoroughly 2 pts. dry K 2 C0 3 , 2 pts. Na 2 C0 3 , 1 pt. finely powdered M 4 Si0 4 (e.g. slate, etc.), fuse thor- oughly B.B.C.C. Pulverize, add H 2 O, boil, filter. To fil. add HC1, boil, evap. to dryness. Try to dis. in boiling HC1, then in boiling NaOH sol. The SiO 2 may also be tested with CaF 2 and H 2 S0 4 in a leaden dish (v. Exp. 28). H 4 Si0 4 (gelat., white) formed. Heat reduces to Si0 2 , insol. in HC1; partially sol. in NaOH sol. K 4 Si0 4 , Na 4 Si0 4 , M 2 O (M 2 C0 3 ) are formed. First two are sep. by H 2 O, and changed by HC1 to H 4 SiO 4 , and by heat to SiO 2 (gritty); insol. in HC1, slightly sol. in NaOH. Supplementary. Silicates are insol., except those of the alkalies, which are somewhat soluble. Some are dis. by acids, but many are not. SiO 2 is insol., even in acids (except HF), and is also infusible in the blow-pipe flame, but is fusible in the oxyhydrogen flame. There are two varieties of silica, the amorphous and the crystalline. The former is sol. in NaOH or Na 2 CO 3 , the latter not. In a bead of Na 2 C0 3 at very high temperature, B.B., SiO 2 and all silicates fuse to a clear glass. They will not fuse in a bead of HNaAmPO 4 . The best fusing mixture contains about half each of Na 2 C0 3 and K 2 C0 3 , the mixture melting at a lower temperature than either alone. Test Si0 3 . 98. FERROCYANIDS, H&FeCy* TESTS. RESULTS. 1. Ferrous test. Add to the sol. acidi- fied with HC1 a few drops of FeS0 4 sol. 2. Ferric test. Add to the sol. FeCl 3 sol. 3. Copper test. Add to sol. CuS0 4 sol. 4. Silver test. Add to sol. AgNO 3 sol. White K 2 Fe 2 Cye ppts., changing quickly to blue. Darkens by oxidation. Prussian blue, Fe 4 Fe 3 Cyi 8 , ppts., sol. in H 2 Ox (not HC1) to dark-blue liquid. NaOH changes to red-brown Fe(OH) 3 . Cu 2 Fe 2 Cy 6 (chocolate) ppts., insol. in HAc. White Ag 4 Fe 2 Cy 6 ppts. , insol. in HNO 3 or AmOH. Heated with HN0 3 the ppt. forms Ag 3 Fe 2 Cye (orange-red), sol. in AmOH. Supplementary. Ferrocyanids are mostly insol., except those of the alkalies and alkaline earths (Ba slightly). Ferrocyanids represent ferrous compounds, ferricyanids are from ferric salts. The most important of the former is K4FeCy, "yellow prussiate of potash." Make several ferrocyanids by the following table. GENERAL REACTIONS. RH-AGT. PPT. COLOR. SOLVENTS. REMABKS. 1 A1C1, FeCy 2 +Al(OH) 8 white NaOH Forms slowly. 2 SbCl, Sb 4 Fe 3 Cyi 8 u u 3 Bid, BuFesCyis (( u 4 CdCl, Cd,FeCy 6 (( HC1, NaOH 5 CaCl, EsGaFeCye u NaOH 6 CoCl, CosFeCye green (t Becomes grad. gray. 7 CuCl, CugFeCye red-brown u 8 FeS0 4 EsFeFeCye white-blue u Rapidly changes from white to blue. 9 FeCls K4Fe s Cyi8 blue u 10 Pb(N0 3 ) 2 Pb,FeCy6 white (4 11 MgCl 2 AmjMgFeCye U With ammonium salts. 12 MnCl, Mn 2 FeCy 6 u NaOH, HC1 13 HgN0 3 Hg 4 FeCy 6 u NaOH 14 Hg(N0 3 )2 Hg 2 FeCy 6 It u Changes to HgCy 2 and Fe 3 Fe 2 Cyi2 (blue). 15 NiCl 2 NiaFeCye green-white u 16 AgN0 8 Ag 4 FeCy 6 white u Changes to blue. 17 ZnClc Zn 2 FeCy u srn ^ t- ^ SITT. . FEBBICYANIDS, TESTS. RESULTS. 1. Ferrous test. Add to some of the sol. FeSO 4 sol. 2. Ferric test, Add to some of the orig. sol. FeCl 3 sol. Dilute if necessary. 3. Copper test. Add to some of the orig. sol. CuSO 4 sol. 4. Silver test. Add to some of the orig. sol. AgNO 3 sol. 5. Zinc test, Add to some of the orig. sol. ZnCl 2 sol. Turnbull's blue, Fe 3 Fe 2 Cyi 2 ppts. insol. in acids. NaOH decolorizes it. No ppt., but dark-green to brown color- ation. Yellow-green HC1. ppte., insol. in Orange Ag 3 Fe 2 Cy 6 ppts., sol. in AmOH, not in HN0 3 . Orange Zn 3 Fe 2 Cyi 2 ppts., sol. in HC1 or AmOH. Supplementary. Ferricyanids are mostly insol., except those of alkalies and alkaline earths. Alcohol does not ppt. the ferricyanid of Na or K from sol. , and this also dist. it from the ferrocyanid. Make the test. K 3 FeCy was formerly called red prussiate of potash. GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 AgN0 3 AgsFeCye red-brown AmOH 2 Bid BiFeCye brown 3 CdCl 2 CdsFe 2 Cyi 2 yellow AmOH, HC1 4 CoCla Co 3 Fe 2 Cyi 2 red-brown AmOH Blood-red sol. with AmOH and AmCl. 5 Cud; CusFezCyw yellow-green 6 FeS0 4 Fe 3 Fe 2 Cyi 2 dark-blue 7 Fed-, none Green to brown color. 8 Pb(NOs)* uncertain dark-brown In cone. sols. only. 9 MnCl 2 Mn3Fe 2 Cyi2 brown 10 HgNOs uncertain red-brown Turns white eventually. 11 Hg(N0 3 ) 2 none (V. M4FeCy 6 .) 12 NiCl 2 NisFezCy^ yellow-green 13 ZnCls ZmFezCyw orange AmOH, HC1 (V. M 4 FeCy 6 .) 1OO. SULFATES, M,SO 4 . TESTS. RB80LTS. 1. Barium test. To a little of the sol. add BaCl 2 sol, decant, and to the res. add dil. HC1. 2. Coin test (v. M 2 S, M 2 S0 8 , M 2 S 2 O 3 ). Fuse some of the solid B.B.C.C. (r.f.) with a mixture of Na 2 C0 3 . Place the product on a silver coin with a drop of water. 3. Insoluble sul fates. Fuse 1 part of the solid with 2 parts each of K 2 CO 3 and NaC0 3 (in Pt crucible, if no Ag, Pb, or S is pres- ent). Dis. what of the product will dis. in H 2 O, the rest, separately, in HC1. Test the former for SO 4 , the latter for M. 4. Free H 2 S0 4 , (1) Put a drop on paper, and evap. it high above a flame, or over a water- bath. (2) Put a few drops on sugar in an e.d. and evap. over a water-bath. (3) Evap. some H 2 S0 4 nearly to dryness, and add a little C 2 H 5 OH. BaSO* ppts. , which is insol. in HC1. is formed, which dis. in H 2 O and forms black Ag*S with Ag. K 3 S0 4 , NaaS0 4 , M 2 CO C are formed. The first two are sol. in H 2 O, the last in HC1. The former contains the radical, the latter the metal of the original. The paper is pulped, rotted, or charred. Comp. with HC1, HN0 3 . Greenish -black substance is formed. is liberated, which burns with a luminous flame. Supplementary. In the barium test use dil. HC1 unless considerable water is present for strong HC1 dis. a little BaS0 4 , and also ppts. BaClj from sol. What sulfates are insol.? (a) Prepare some PbSO 4 , and test it as aboT in 3. (b) Show that PbSO 4 exists in commercial H 2 S04 by diluting some witk its vol. of water, (c) Make CuS0 4 , and test it. (d) Test NasSOs for trace* of Na^S O 4 . Are most sulfates sol. or insol. ? GENERAL REACTIONS. KE-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 Bad, BaSO< white 400,000 pts. H,0 The only salt of Ba (exc. BaSLFe) insol. in dil. HC1. 2 Pb(NOs), PbSO* u NaOH, Am Ac C 2 H 5 OH aids ppn. 3 SrCl 2 8rSO t( 7000 pts. H 2 Ppts. slowly in dil. sol. 4 CaCl, CaS0 4 (( 400 pts. H 2 No ppt. in weak sol. 1O1. CHKOMATES, M 2 CrO 4 . TESTS. RESULTS. 1. Borax bead test. Make a bead of Na2B 4 O 7 or HNaNH4P0 4 with Ft wire, dip into sol., fuse in either flame. 2. Ppn. tests. Apply the first three tests below (General Reactions). 3. Hydrogen diozid test. Acidulate the sol. with H 2 SO 4 , and add a few drops of dil. H 2 O 2 sol. Then add ether, and shake. This will detect 1 part of chromate hi 40,000 of water. Glass, yellow-green when hot, emerald-green when cold. A blue compound is formed of uncertain composition, which the ether dis. and car- ries to the surface as a blue liquid. Supplementary. Most chromates are yellow, dichroinates are red. Bichromates are confined to the alkali metals. K 2 Cr 2 O 7 , etc., ppt. normal chromates, e.g. PbCrO 4 , BaCrO 4 from sol. Pb and Ba salts. In both the normal and the dichromates Cr is a hexad, in ic salts it is a triad, in ous salts a dyad. What other salts are yellow ? Acids change chromates to dichromates, alkalies reverse this. Reducing agents (nascent H, SO 2 , H 2 S) change Cr to Cr'" chromate to chromic salts. GENERAL REACTIONS. RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. 1 Bad, BaCrO, yellow Dil. acids 2 Pb(N03) 2 PbCrO* it (HN0 3 (sl.), f NaOH (si.) Insol. in HAc. 8 AgN0 3 Ag 2 Cr0 4 dark-red {f^n^' 4 HgN0 3 Hg 2 Cr0 4 " i HN0 8 (8l.) Ppt. ignited equals Cr 2 Og, Hg, 0. 5 HgCl 2 HgCr04 orange " 6 Bid, BiiCCrCWs yellow " 7 CdCl t CdCrO* u " 8 Acids M 2 Cr 2 07 red sol. Changed back by alkalies to M 2 Cr0 4 (yellow). 9 H 2 S+HC1 S+CrCls green sol. Warming forms S0 2 , ppts. Cr 2 O 2 Cr0 4 (brown). 10 Am,S Cr(OH) s green Acids 11 CAOH+Hd Crds tt On boiling. Odor of al- dehyde. 102. PHOSPHATES, TESTS. RESULTS. 1. Molybdate test. To 1 or 2 cc. of sol. add a drop or two of HN0 3 , then add 3 or 4 cc. Am 2 Mo04 sol. , and let stand. 2. Magnesium sulfate test (v. As, Mg). To sol. add AmCl sol. , AmOH, MgS0 4 sol., gently warm, stir, let stand. 3. Iron test. To sol. add a drop of HAc, excess of NaAc sol., and 1 or 2 drops of FeCl 8 sol. 4. Cobalt test (v. SiO 2 , Al). Heat the solid B.B.C.C., then on white infusible mass put a drop of CoCl 2 [or Co(N0 3 ) 2 ] sol., and heat again. 5. Silver nitrate test. To sol. add AgNO 3 sol. Am 3 P04.12Mo0 8 (var., yel.) ppts., sol. in M 8 PO 4 (ex.) or in AmOH. AmMgPO 4 (white, crystalline) ppts. FePO 4 (yellowish-white, gel.) ppts., sol. in FeCl 8 (ex.). Residue becomes blue. Ag 3 P0 4 (yellow) ppte., sol. in HN0 3 . Supplementary. All phosphates are insoluble except those of the alkali metals ; hence sols, of the other metallic salts ppt. phosphates. Most phosphates are somewhat sol. in HC1. If insol. in H 2 0, they should be dis. in dil. HC1, Am Ac (made from AmOH and HAc) added, then FeCl 3 till all the phosphate is ppd. The fil. will now contain a chlorid of the original metal. This test applies specially to phosphates of Ba, Sr, Ca, Mg. (a) Apply the test to each, (b) Test bone-dust in this way. (c) Test samples of fertilizers. Phosphates (and also oxalates) of Ba, Sr, Ca, Mg, if present, may ppt. with Fe, Cr, Al by AmOH. To separate them dis. the ppt. in hot dil. HN0 3 , cool and add excess NaOH sol., which ppts. only Fe and the phosphates (or oxalates). Dis. the ppt. in HNO, add H 2 Tr and AmO H, which in excess ppts. the phosphates and oxalates, die- solving the Fe. (For arseniates and arsenites, v. Exp. 58.) GENERAL REACTIONS. 1 2 3 4 5 6 7 RE-AGT. PPT. COLOR. SOLVENTS. REMARKS. Co(N0 8 ) 2 NiCl 2 BiCL Cn(N0 8 ) 2 HgNOs Hg(NOs) 2 Bad, C03(P0 4 ) 2 Ni3(P0 4 ) 2 BiP0 4 Cus(P<>4) 2 HgsPO* Hg 8 (P04) Ba,(PO) I red light-green white blue-white white (i it AmOH, acids n i< HC1 HAc HNO Acids, Am salts Dil. HC1 Insol. in HNO,. HgCl 2 gives no ppt. |o pipoi pnnojg r B* ^"aT Sflfe S*||1 jj|g'S!ajJ II II II II II II iff il ..S c-^5o-r TABLE B. Tube Reactions. Put into a small i.t. (or a bulb tube) a little of the powder, and heat it. liefer the results to this table. GASES. SUBLIMATE, ETC. FU- SION. RESIDUE. INDICATION. Red-brown, NO, MNO MNO, Yellow-gr. (rare) Cl (MCI) Red, Br MBr Violet, I Black MI Odor, NH 3 ; HC1 tests White NH, Odor,SO,;K,Cr 2 7 M,S0 4 , M 2 SO S> test M,S 2 0:: Odor,H,S; PbAc, test Yel.-red, brown drops X MsS Odor, Cy (flame crimson) (MCy) CO 2 ; Ca(OH) a test M,C0 3 , M,0x CO (flame blue) M 8 0x O (splinter test) MC10 3 , MNO,, MO, NjO " X All finally vaporizes AmNO Hot : yellow. Cold : white HgCl ; White X HgCU White, As 4 O Cryst. Heat and C = (odor) mirror AfcOe White, needles X Sb,0, O (splinter test) Metallic Hg Black, changing to red HgO Yel.-red-brown drops X 8 Hot : red. Cool : yel. As,Ss Red when rubbed HgI 2 Gray; white if rubbed Hg Black; red if rubbed HgS Black, tarry, burnt su- gar odor M 8 Tr Heavy white White cryst. H,0x Black; odor acetone MAc Hot: red-brown. Cold: light yellow Bi 2 s Hot: black. Cold: red Fe 2 8 Hot: red-brown. Cold: yellow PbO Hot:yel.-brown. Cold: yellow SnO, Hot: yel. Cold: white ZnO M 2 C0 8 , (M 2 0), (M) Org. cpds.ofNa, K,Am,Ba,Sr, Ca,Mg X No decomposition Cpds. of alka- lies, + Cl, NO 3 cpds. of alk. earths TABLE C. Action with H 2 SO 4 . Tut a little of the powder into a t.t., and add a few drops of H-jSO*. Ualess yiolent action ensues (as with K Cl O 8 ) heat it, and observe especially the gas. OOIOB OF GAS. ODOR. REFERENCE. REMARKS. GAS. INDICATION. Violet None Exp. 92 Dark crystal, sub- I MI limate. Yellow CIO, " 84 Substance deto- nates violently. C10 2 MC10, Red-brown NO, " 82, 83 N0 2 , N 2 3 MNO,,MNOo Eed Br " 91 Br MBr None HC1 " 90 HC1 MCI ti Stifling " 89 Etches glass. HF MF H,S " 86 In tube open at both ends gives SO 2 . H,S M,S White SO, " 87 S not liberated. SO, M 2 S0 8 ti ({ " 88 S is liberated. a M,S,0, None HAc " 93 HAc MAc HCy " 94 HCy MCy K CO "' 96 CO M 2 0x None " 10, 101 Kindles splinter. MO,, M,Cr0 4 ti K " 85 White ppt. with lime water. CO, M,CO, TABLE D. Heat on Charcoal (B.B.C.C.), With the round end of the forceps make a slight depression in a piece of harcoal, and put in a little of the powdered substance. With a mouth blow- pipe blow the flame against it, cautiously at first, afterwards strongly. RESULTS. INDICATIONS. 1. Substance melts and runs into the coal. 3. Leaves white, infusible residue. Add to this a drop of CoCl 2 sol. , and heat again. The color may be : Blue, Green, Pink. S. Coats charcoal : White, volatile, garlic odor, no globule. 44 " hard, brittle globule. 14 when cool, yellow when hot, no globule. 44 " " " " " globule malle- able, but difficultly formed. Yellow, globule easily formed, fusible, soft, malle- able. Yellow (orange when hot), globule hard, brittle. Brown or red, no globule. 4. Deflagrates. 5. Volatilizes. 0. Gives odor. Choking (SO*). Garlic. Salts of the alka- lies, and some alkaline earths Al, 810., Zn Mg As Sb Zn Sn Pb Bi Cd MC10,, MNO, Am 8 or M t S As TABLE E. Heat on Charcoal with Na2CO 8 (B.B.C.C., Blow the inner flame (r.f.) for some time against a mixture of the powdered substance, and dry, fine NaaCOs, using charcoal, as in Table D. METALLIC I GLOBULE. No GLOBULE. INFUSIBLE POWDER. | COLORED ! MASS. SOLID RESIDUE. INCRUSTATION. INDICATION. X White, brilliant, malleable, In strong o.f. red-brown. Ag non-oxidizable. X Hard, brilliant, oxidizable, B.B. volatile. Hot, orange; reddish-white. cold, lemon-yellow. Bi X Red, malleable ; oxidizes to black ; green flame. Cu X Easily formed, fusible, mal- Hot, lemon-yellow ; cold, leable, oxidizes to yel. sulfur-yellow; vol. B.B. ; O flame blue. Pb X White, malleable, difficultly Hot, yellow; cold, white formed, easily oxidized. near assay; non-vol. Sn X White, volatile; light-blue flame ; garlic odor. As X Red-brown (like peacock feather) ; vol. B.B, Cd X (x) White, brittle, oxidizable. Hot, yel. ; cold, blue-white; vol. B.B. pale green. Sb X Hot, yellow; cold, white. With Co(N0 8 ) 2 green. Zn X Infusible magnetic powder, white, gray, black. Fe X It It tt it It Co X tt It It It tt Ni X Yellow mass. Cr x Green " Mn TABLE F. Flame Reactions. Fuse one end of a Pt wire into a short glass tube. Hold the wire in the outer edge of a Bunsen flame till the latter loses the yellow color at first imparted. Moisten the wire with H 2 O or HC1, and dip it into a little of the salt, then hold it again in the flame, noting the color. Clean the wire with H Cl and the flame. FLAME COLOR. REMARKS. INDICATION. 1. Violet Seen through blue glass looks red- violet ; otherwise Na obscures it. E 2. Bluish As 3. Blue Pb 4. Blue-green Moistened with H 2 S0 4 . M 3 P0 4 5. First blue, then green. Cu, espec. CuCl 2 6. Yellow-green Moistened with H 2 S0 4 . MsB0 3 7. " HC1. Ba 8. Greenish Very slight color. Sb 9. Bronze-green " evanescent. MNO- 10. Orange-yellow Blue glass obscures the color. Na 11. Orange-red Obscured by Ba. Ca 12. Crimson " " " Sr TABLE G. Bead Reactions. Make a loop in the end of a Pt wire (Fig. 38, Exp. 45), moisten and dip it into some powdered borax, then hold it in the flame ; repeat till you have a glass bead filling the loop. Test a weak sol. (or the smallest bit of powder) by bringing the bead in contact with it, then blowing the flame against it with a blowpipe. OXIDIZING FLAME (o.f., outer). REDUCING FLAME (r.f., inner). INDI- CATION. Hot. Co/d. Hot. Cold. Blue Blue Blue Blue Co Yellow-red Green Green Green Cr Green Blue-green Colorless Red-brown Cu Yellow-red Violet Yellow Violet Bottle-green Colorless Bottle-green Colorless Fe Mn l( Red-brown Gray, cloudy Gray, cloudy Ni TABLE H. Acil Radicals Resume. SALTS. f w BaCl 2 +HCl. s AgNO 8 +HNO 8 . OTHER RE-AGENTS AND RESULTS. For further explanation, v. Exps. 81-102. Abbrevi- ations : b. black, bl. blue, br. brown, ch. chocolate, d. dark, g. green, 1. light, o. orange, r. red, v. violet, w. white, y. yellow. M 2 S0 4 w. W. (w.) Pb(N0 3 ) 2 : w. SrCl 2 : w. B.B.C.C. with Na 2 C0 3 on Ag: b. M 2 S0 3 w. w. BaCl 2 + HC1 + Cl : BaS0 4 . HC1 : S0 2 [odor, K 2 Cr 2 7 : g.]. M 2 S 2 3 w. w. BaCl 2 +HCl: S. HC1: S+S0 2 [odor, KoO 2 O 7 : g.]. M 2 C0 3 w. w. HC1: C0 2 [Ca(OH) 2 : w.]. Heat: (M 2 O, CO 2 ).^ ' M 2 Cr0 4 i-y. d.-r. Pb(N0 3 ) 2 : y. HgN0 3 : d.-r. HgClo: o. BiCl 3 : y. Cd(NO 3 ) 2 : y. H 2 S: y. Acids: r, which y. by alk. M 3 POi w. i-y. AmCl+AmOH+MgS0 4 : w. HN0 3 +Am 2 MoO 4 : y. B.B.C.C. +Co(N0 3 ) 2 :bl. M 3 As0 4 w. ch.- H 2 S, warm : y. AmCl + AmOH -f MgS0 4 : w. br. B.B.C.C.: As [garlic odor, white fumes]. M 3 As0 3 w. y.-w. H 2 S+HCl:y. CuS0 4 (neutral): g. K 2 Cr0 4 +heat: g. KMnO 4 : decol. C.C. + heat, t.t. : mirror. M 3 B0 3 w. w. H 2 SO 4 , Pt wire: green flame. Turmeric paper + H 3 B0 3 : br. H 2 SO 4 + C 2 H 5 OH : green flame. M,0x w. w. SrCl 2 : w. CaCl 2 : w. [sol. in HC1, insol. in HAc]. Heat: CO, CO 2 , M 2 C0 3 , M 2 O or M, no char- ring. H 2 SO 4 : effervesc., CO 2 . M 2 Tr w. w. CaCl 2 : w. [sol. in NaOH]. KC1: w. Heat: chars M: ; SiO, w. i-y. [odor]. AgN0 3 +AmOH: Ag mirror. HCl+heat: Si0 2 . Na 2 C0 3 bead: effervesc., forms glass. HNaAmP0 4 bead: insol. B.B.C.C.+ HC1, evap. : SiO 2 , sol. in NaOH. MN0 2 w. w. H 2 S0 4 : N0 2 . HAc+KMn0 4 : decol. HAc + AgN0 3 : w. HAc +KI+ starch: bl. MF w. H 2 S0 4 +heat: etches glass, makes H 2 turbid. HKS0 4 + heat : green flame. MCI w. W. H 2 S0 4 : HC1. H 2 SO 4 +Mn0 2 : Cl. AgNX) 3 : w. [sol. in AmOH, action of light]. Pb(N0 3 ) 2 : w. MBr y.-w. y.-w. PbAc 2 : w. CS 2 + Cl : y. H 2 S0 4 + Mn0 2 : Br [starch, KI+ starch]. MI y.-w. y.-w. Pb(N0 3 ) 2 : y. HgN0 3 : y.-g. HgCl 2 : y.-r. CS 2 + Cl : v. H 2 SO 4 + MnO 2 : I [starch test] . MCy y.-w. y.-w. CuS0 4 : y.-g. Co(N0 3 ) 2 : w.-br. NiClo : y.-g. H 2 S0 4 : HCy [odor cautiously]. KOH+FeSO 4 + HCl:bl. M,S b. b. HC1: H 2 S [odor, PbAc 2 ]. B.B.C.C. on Ag: b. M 4 FeCyo w. g-br FeCl 3 : bl. FeS0 4 : bl.-w. CuSO 4 : br.-r. M 3 FeCv fi 0. o. FeCl 3 : r.-br. CuSO 4 : g.-y. MN0 3 Heat,i.t.:O,NO 2 . B.B.C.C.: deflagrates. H 2 S0 4 : N0 2 . FeS0 4 +H 2 SO 4 : r.-br. H 2 S0 4 + indigo sol.: decol. MC10: HCl+heat: g.-y. Heat, i.t. : O. H 2 S0 4 (very lit- tle) : C1 2 4 [y. gas] . MAc Heat: blackens [odor]. H 2 S0 4 : HAc [odor]. H 2 SO 4 + C 2 H 5 OH : C 2 H 5 Ac [odor]. FeCl 3 , boil: r. TABLE I. Acid Radicals. Arranged according to convenient method of detection. 1. Flame { H 3 B0 3 (M 3 B0 3 +H 2 S0 4 ). f (with heat) { MN0 3 . 2. Gas J (with acid) { MN0 2 , MC10 3 , M 2 C0 3 , M 2 S, M 2 S0 3 , M 2 S 2 3 . i (with heat and acid) { MF, MCI, MBr, MI, MAc, MCy. o -a^ P j (with heat) { M 2 Tr, M 2 0x, e ) (with heat and acid) { M 4 Si0 4 (M 2 Si0 3 ). f (iron-cyanids) { M 4 FeCy 6 , M 3 FeCy 6 . 4. Precipitate 1 (insoluble) { M 2 S0 4 . L (unclassed) { M 2 Cr0 4 , M 3 P0 4 , M 3 As0 4 , M 3 As0 3 . COMPLETE ANALYSIS. In making a complete analysis, i. e. analysis for the metal and acid radical, the following order should be observed, and the pupil should begin with only a single substance, such as Pb(N0 3 ) 2 , FeCl 3 , etc., and should make a careful record under each head. 1. External properties: Color, luster, form (crystalline or amorphous), taste, odor, deliquescent, efflorescent, etc. 2. Heat in glass tube (v. Table B). 3. Heat with H 2 S0 4 (v. Table C). 4. Heat B.B.C.C, (v. Table D). 5. Heat B.B.C.C. NaaCO-j (r.f.) (v. Table E). 6. Apply flame test (v. Table F). 7. Apply Borax bead test (v. Table G). 8. Test solubility (v. Table A). 9. Test for Metals (aqueous analysis) (v. Exps. 48-80). 10. Test for Acid radicals (v. Tables H, I). 11. State conclusion as to composition. UNIVERSITY OF CALIFORNIA LIBRARY BERKELEY Return to desk from which borrowed. This book is DUE on the last date stamped below. < 2 1948 23May'58 D 100m-9,'47(A5702sl6)476