LIBRARY OF THE UNIVERSITY OF CALIFORNIA. Class LABORATORY NOTES ON HEAT MEASUREMENTS BY CHARLES L. NORTON COPYRIGHT, 1902, BY CHARLES L, NORTON PRINTED BY THE SOUTHGATE PRESS T. W. RIPLEYCO., BOSTON, U.S. A, LABORATORY NOTES ON HEAT MEASUREMENTS BY CHARLES L. NORTON OF THE UNIVERSITY OF COPYRIGHT, 1902, BY CHARLES L. NORTON PRINTED BY THE SOUTHGATE PRESS T. W. RIPLEYCO., BOSTON, U.S.A. LABORATORY OF HEAT MEASUREMENTS The instruction in heat measurement consists of a series of lectures and laboratory exercises which have for their object the training of the student in such methods of heat and temperature measurement as will be of value in later scien- tific or technical work, and to furnish a foundation for research in thermal lines. Perhaps no portion of the heat measurement field is so fruitful, both to the scientific and to the technical investigator, as is the measurement of high tem- peratures, or pyrometry. Next in importance comes the measurement of the efficiency of fuels, the determination of their calorific power. To these two subjects the first portion of these laboratory notes is devoted, with the expectation that the additional notes on " thermometry," " thermal con- ductivity," and "electric-heating apparatus and methods" may soon be added. All reports handed in must be taken upon the proper blanks and Tegular physical laboratory paper and should be accompanied by the original records. All reports must be sent in within two weeks of the time the observations were finished. When sent back for correction they should be returned with all necessary corrections within one week. If not returned to the student within two weeks from their first presentation, the experiments may be assumed to need no correction, and they will not be returned to the student until the end of the term. THE LE CHATELIER THERMO-ELECTRIC PYROMETER The Le Chatelier thermo-electric pyrometer is based upon the increasing electromotive force which exists at a junction of two metals as the temperature rises. If we have a pair of dissimilar metallic wires, their junction becomes the seat of an electromotive force, and if they be joined at both ends, a current will flow through them as the result of the difference between the electromotive forces at the two ends of the wires. In general, this current is dependent upon the difference in temperature, though not directly proportional to it. In order to use this phenomena as a basis for a pyrometer, since there is no known relation existing directly between temperature and electromotive force in such a cir- cuit, we must expose the junction to known temperatures and note the current flowing, and in this way calibrate. It is usually customary to observe, not the electromotive force, but the current, keeping the total resistance of the circuit constant in order that this may be allowable. This pyrometer is by far the most important instrument for the measurement of temperature from the point of view of the engineer. It may be found described in detail in Le Chatelier's " High Temperature Measurements," pages 92 to 128 (Burgess translation). The apparatus consists : first, of a pair of platinum and platinum-iridium wires; second, of a galvanometer; ana third, a pair of suitable connecting leads. Leads. The lead wires connecting the galvanometer to the junction do not require any special care, other than that necessary to keep them well insulated. These wires should be of seme good electric line-wire, not smaller than No. 14, and they should preferably be of the so-called " rubber-cov- ered " type. LABORATORY OF HEAT MEASUREMENTS Junction. The junction to be used is composed of one wire of platinum, and one of platinum with ten per cent, of rhodium or iridium. This couple costs nearly ten dollars a foot and must be used with great care. The wires are some- what brittle, and they are easily attacked when hot by many of the baser metals. The junction in its simplest form is made by merely twisting the wires together at one end and then twisting each to the leads at the other end. It is desir- able, however, to be able to know the temperature of the junction of the couple with the copper leads, and it is there- fore best to inclose the joints in some receptacle in which a thermometer bulb can be inserted. For laboratory work, a FIG. I . Diagram of Thermal Couple. small bottle with a stopper perforated for the leads and ther- mometer serves to keep the junction at a fairly even temper- ature. Where greater constancy of temperature is needed the bottle may be wrapped with some insulating material, felt, magnesia, or asbestos. It is sometimes necessary to put the "cold junction," as the copper-platinum end of the couple is called, in a large block of iron to insure its chang- ing temperature only at a very gradual rate. The couple must be insulated from itself and from sur- rounding conductors throughout its length. The best insula- tion for the cool portions of the wires is a firre rubber tube, while the hotter portions may be insulated with asbestos string wound over and under, in figure-eight fashion, or they may be protected by means of small clay stems with a double bore. THERMO-ELECTRIC PYROMETER 5 To insure a constant resistance of the couple and leads it is, in all cases, best to solder the cold junction with ordinary soft solder. Resin, and not acid, should be used in fluxing this joint, or a slight electromotive force will be found to result, giving serious disturbance to the galvanometer readings. Unless there is a switch on the galvanometer there should be one inserted in the circuit, as it is necessary to open the circuit frequently for the purpose of reading the zero. Galvanometers. There are many galvanometers suitable for use with a thermal couple. Directions will be given for the adjustment and operation of those now in use in the Laboratory of Heat Measurements, and since the galva- nometers are of the same general class it is probable that no great difficulty will be found in applying them to others. All the galvanometers especially suited for this work are of the D'Arsonyal type, of medium sensitiveness. They oper- ate by the change in position of a coil of wire in a magnetic field, as the current in the coil changes in strength. This change in position is noted either by observing the move- ment of a pointer attached directly to the coil, or by noting the excursion of a beam of light falling upon a small mirror attached to the movable coil. Galvanometers which may be read by a pointer are made by Heraeus, and Hartmann and Braun. The galvanometers of Sullivan and Carpentier are the best of the instruments using a mirror and scale. The more important details of the procedure in setting up each of these instruments are given below. Carpentier galvanometer. This instrument is that most commonly adopted for pyrometric determinations. It will be found described in Le Chatelier, pages 108 to no. To set up the galvanometer one should select a place as free from vibration as possible, and screen it from any but a feeble light. - The galvanometer box should be firmly attached to the wall, taking care to see that it is plumb. The small bob inside the box is intended to assist this operation. Next slip the coil over the iron block between the pole pieces, with 6 LABORATORY OF HEAT MEASUREMENTS its mirror facing in the direction in which the lamp and scale is to be placed. The suspensions consist of short pieces of fine German silver wire with little balls of the same metal wedged on to the ends. The lower end of the upper sus- pension should first be inserted in its eye at the top of the coil. See that it is slipped well back in the slot. Next hook the upper end of the suspension in the eye in the flat spring near the top of the box. If the suspension is appar- ently too short loosen the tension of the flat spring by means of the thumb-screw. Next drop the lower suspension into FIG. 2. Carpentier Galvanometer. place in the opening between the magnets, and put its two ends in the eyes as before. The mirror may now be made to face in any desired direction by taking the ball at the lower end of the lower suspension between the thumb and finger and twisting it slightly. This is the most troublesome operation of the whole process, and must, moreover, be accompanied with the exercise of great care and patience, or the only result of a great expenditure of time will be a pair of broken suspensions. A small amount of adjustment of the light spot may be gotten later by means of the screw- feet at the bottom of the box. The lamp and scale should next be set up at a distance of about a meter. It is well to light the lamp and move it back THERMO-ELECTRIC PYROMETER / and forth, and up and down, until it is found that the image is well focussed, and at such a height as makes both the divisions and numbers of the scale visible. When its proper position is found the base-board should be firmly fastened to the wall. It is well to put in a strong screw at the middle of the board near the bottom, in addition to the screw r at the top. The oil lamp which is often used where the apparatus is to be carried about, often covers the lens with dew for a few minutes after lighting, and it is well to put off any attempts at focussing until this has disappeared, after the whole lantern becomes warm. As this lamp requires refilling at very short intervals, it should be used only when absolutely necessary. Either a small gas burner or an incandescent lamp .should be used whenever possible. Heraeus galvanometer. This galvanometer reads by means of a pointer attached directly to the coil. The coil must therefore move through a much larger angle than in the case of the.Carpentier instrument with its long beam of light. To make the galvanometer sufficiently sensitive to accomplish this, it has been necessary to use a very fine suspension wire, and to use only the upper suspension. The galvanometer is therefore more frail and must be handled with great care. There are only two adjustments neces- sary : first, level by means of the screw-feet and the circular level attached to the base ; and second, loosen the brass thumb-screw which projects through the side of the brass case. This removes the supporting spring which lifts the coil and takes all strain from the suspension. It is abso- lutely necessary to screw this thumb-screw firmly in, before attempting to move the galvanometer, otherwise the suspen- sion is quite certain to be broken. There are two scales upon the dial. The outer scale is intended to read in Centi- grade degrees directly, with an upper limit of 1600. The lower scale is in millivolts and it is intended to make the instrument thereby available as a voltmeter as well as a pyrometer. In several of the later galvanometers of this kind there is noticeable considerable " pivot friction," mak- ing it necessary to tap the glass of the galvanometer contin- 8 LABORATORY OF HEAT MEASUREMENTS ually to be sure of freedom from error due to the pivo* sticking. None of the joints in these galvanometers in the laboratory were soldered when they were purchased, and their variations in resistance made it necessary to solde* most of them. Sullivan galvanometer* This galvanometer is similar in many respects to that of Carpentier. It reads by means ot a mirror and has an upper and lower suspension. It is. however, more sensitive and it is so free from disturbance from jarring that it may be satisfactorily used on an ordinary- laboratory table. Further, the suspension is stout enough to allow the galvanometer to be readily handled and shipped without any unusual care. As set up in the laboratory, it is to be used with a telescope and scale. The scale must first be set up in front of the galvanometer at a distance of about a meter. The telescope should be focussed on the plane mir- ror and then gradually refocussed until the image of the number on the scale can be clearly seen. Some care is needed in placing the scale and telescope at the proper height, and also in a plane perpendicular to the axis on which the coil turns, so that the image may remain in the field of view as the mirror turns. Care must be used not to disturb the focus of the telescope after calibrating, as the axis of the telescope is not sufficiently constant in position to allow of even slight adjustments, without altering the appar- ent position of the cross hairs. Calibration. Having prepared the junction and having gotten the galvanometer set up and attached to the leads through the switch, the galvanometer may now be cali- brated. To do this we observe the deflection of the gal- vanometer which corresponds to a known difference of temperature at the two ends of the thermal junction. The most convenient temperatures to use are the boiling and melting points given below. The cold junction may be placed in a steam or ice bath, when desired, but it is usually sufficient to allow it to remain at the temperature of the room and read its thermometer at intervals of two to five minutes. THERMO-ELECTRIC PYROMETER 9 TEMPERATURES FOR CALIBRATION Substance. Boiling Point. Freezing Point. Water ioo. C. o. C. Naphthaline 218. Sulphur 444. Aluminum 657. Copper 1084. Gold 1063. Platinum 1760. The hot junction should be exposed to these several known temperatures while the deflection of the galvanometer and the temperature of the cold junction are noted, in each instance. A plot should then be made having the deflections as ordinates and the difference between the temperature of the hot and the cold ends of the couple as abscissas. If the Heraeus galvanometer is to be used with a couple of compo- sition similar to that for which it was originally graduated, it may be well to make the plot as a plot of corrections, hav- ing readings of the instrument as abscissas and corrections as ordinates. To obtain the galvanometer readings corresponding to the boiling points of water, napthaline and sulphur, it is best to put the junction directly into a small test tube of the boiling liquid. It makes no difference whether the junction be just above the liquid or well below the surface. Take care not to heat so vigorously as to superheat, or to cause the vapors to catch fire at the mouth of the tube. The highest steady deflection is, of course, the one to be recorded. To find the deflection corresponding to the freezing points of the metals, we may use either a small bit of the metal wrapped about the hot junction or a larger mass in a crucible. To heat the smaller mass, it is only necessary to use a Bunsen burner for the baser metals and an oxyhydrogen blow-pipe for the platinum. For the larger masses, a crucible furnace, similar to the small Fletcher furnaces in the laboratory, will be needed. The metal should in all cases be heated slowly, and the greatest care should be used to prevent heating more 10 LABORATORY OF HEAT MEASUREMENTS than a very few degrees above the melting point, as otherwise the platinum and platinum-rhodium will alloy with the melted metal, changing its composition and its freezing point, and the loss of a portion of the junction is also very probable. Especial care is needed when working with hot copper, as the fumes or vapor arising from the melted metal, if it be heated much above its melting point, cause the platinum to be alloyed at a distance of an inch or two from the surface of the hot copper. Since it is difficult to tell from its physi- cal condition, even when large masses are used, at just what temperature a metal melts or freezes, it is best to use the point at which the latent heat of freezing develops as the freezing point. To do this it is only necessary to note the point at which the galvanometer pauses in its swing as the melted metal cools. This momentary pause occurs when the latent heat of freezing develops and pre- vents for a brief interval the temperature of the mass from passing below the freezing point until all the metal has frozen. To find the platinum point it is best to use a long flame from an oxyhydrogen blow-pipe and draw the junction slowly down through it until the platinum wire melts. With care, a drop of melted platinum may be kept on the tip of the wire for several seconds, and the deflection can be read with a precision quite as good as in the case of the other metals. The eyes must be protected from the intensely bright light of the melted metal by very dark glasses, such as are used in examination of the electric arc. The junction wires may be protected from alloying with metals of low melting points by a fine hard glass tube, but in case this is done, larger masses of metal must be used to insure the junction being at the temperature of the melted metal. Reports. Each pair of students will be expected to set up their galvanometer and calibrate it, possibly omitting the platinum point from motives of economy. They will next measure several unknown temperatures, preferably the recal- escence points of two pieces of steel, and the melting points of several alloys. In case antimony is used it is necessary to perform the melting point determination under the hood. PLATINUM RESISTANCE PYROMETER II After having gotten the deflections corresponding to the points sought, they should be looked up in the calibration plot, not forgetting the necessary addition of the cold junction tem- perature. Bear in mind that the deflection is dependent upon, not the temperature of the hot junction, but the differ- ence in temperature between the hot and cold ends. PLATINUM RESISTANCE PYROMETER The platinum resistance pyrometer, or thermometer, of Siemens and Callendar may be found described in Le Chat- elier, pages 83 to 91. It is not always given place among the pyrometers, nowadays, because of the great difficulty of keeping the apparatus in proper condition if used at tem- peratures much above 500 C. Since, however, its preci- sion is very great at low temperatures, and, further, since in the hands of some exceptional observers it has yielded excellent results, it should be classed as one of the most important thermometers. The operation of the pyrometer is based upon the increase of the electrical resistance of a platinum wire as its tempera- ture rises. After calibration we have only to measure the resistance of the wire in order to determine its temperature. It will be apparent at once that the method is available for use at great distance and under varying conditions of pres- sure, and in many ways offers advantages over most other methods. Since it is not difficult to measure the resistance of such a coil as may easily be used in this work with a pre- cision of one-twentieth of one per cent., the method takes first place in the ranks of the thermometers in the matter of precision. The essential parts of the apparatus are, of course, a coil of platinum wire and a bridge with which to measure its resis- tance. Since the adjustment and subsequent care of a gal- vanometer and Wheatstone's bridge of the greatest precision would be so great as to call for a considerable outlay of time, it is deemed best to use a less sensitive measuring device and devote more time to studying the method of using and 12 LABORATORY OF HEAT MEASUREMENTS calibrating the pyrometer. Students will therefore use either the portable testing set or a similar simple bridge with a D'Arsonval galvanometer. The greatest precision sought is a single degree. Be sure and note the number of the coil used. Connect up the apparatus and measure the resistance of the coil at the room temperature. The blind leads may either be connected in the opposite side of the bridge circuit, or they may be measured separately and subtracted. Of course the object of this is to enable us to measure the resistance of the coil alone without the leads, and it is for that purpose that the blind leads are inserted. They are of the same wire and length as the true leads, and their position beside the true leads assures their being at the same temperature. Find the resistance of the coil in ice, in steam, in boiling sulphur, and in boiling napthaline. Take great care to keep the tube which protects the coil from too sud- den changes in temperature, as its breaking may cause the .breaking of the platinum coil, a rather serious matter, as these coils are difficult to wind. Having found the resis- tances, compute first the "platinum temperature" -pi for boiling sulphur. This temperature will be found to be some ten or twenty degrees below the true boiling point as ex- pressed in degrees centigrade (444). The formula for this deduction is 7P /? IOQ f ~ -j-pt (in platinum degrees). ^100 J?o To reduce the pt in platinum degrees to degrees centigrade we must make use of Callendar's second formula, in which / is the temperature in degrees centigrade and pt the platinum temperature as found under the assumption of the equation above, that the increase of resistance is directly proportional to the temperature increase. In this equation we may substitute the values of pt and / for the sulphur point and solve for D. This need not be rede- CALORIMETRIC PYROMETER 1 3 termined so long as the coil remains free from injury or contamination chemically. Next, with the aid of the first formula, find the platinum temperature of the boiling naph- thaline, and then substitute in the second formula, and find the boiling-point in centigrade degrees. The values of / are of course not known in the substitution in the second formula and -pt may be substituted instead for a first approximation. A second substitution should then be made with the values thus found. This second approximation will be sufficiently precise. Take care to leave the apparatus in the condition in which it was found, especially taking care to cut off all the gas and electrical supply from the boiling-point cans. CALORIMETRIC PYROMETER The calorimetric pyrometer, or, as it is often called, the specific heat pyrometer, of Siemens and Violle may be found described on pages 74 to 82 of Le Chatelier. The measure- ment of a temperature by the calorimetric method involves the measurement of the heat given out by the pyrometric substance in cooling from the unknown temperature to the temperature of the calorimeter in which it is plunged. If we know the specific heat and weight of the substance, we may compute the temperature, from the total heat received by the calorimeter. Unfortunately the specific heat of such substances as are available for pyrometry varies rapidly with the temperature. Let W= weight of the substance (platinum or nickel ball). w = weight of water in the calorimeter. 5 = the specific heat of the calorimeter and stirrer. t = initial temperature of the calorimeter. / 2 = final temperature of the calorimeter. T == ; unknown temperature to be measured. s r = mean specific heat of pyrometric substance (o to s t = specific heat of pyrometric substance (o to / 2 ). c = weight of the calorimeter and stirrer. 14 LABORATORY OF HEAT MEASUREMENTS Then when the substance is taken from the furnace, and is plunged into the calorimeter whose temperature thereupon rises from t, to t 2 the transfer of heat is shown by the fol- lowing equation : WTs T - Ws,i, = (t, _ /,) (TV + cs) and 7W^>n