June, 1914
T H E J O C R N A L OF I N D U S T R I A L A X D ENGINEERING CHEMISTRY
tail here. The main reason for the long delay in securing d a t a of sufficient importance t o communicate formally has been due t o the difficulties encountered in devising suitable means for accurately determining the volatility losses suffered by commercial ware when subjected t o the temperatures, ordinarily employed i n laboratory operations. These difficulties have been,i t is hoped, overcome through the assistance of the Heat and Metallurgical Divisions of the Bureau of Standards, and it is expected, as opportunity permits, to accumulate data of value. There is, however, another more serious difficulty arising from the fact that the committee has been unable t o obtain reliable information on the composition of much of the ware which is a t its disposition, either through loan or purchase. Cntil exact d a t a of this kind are available it will be difficult, if not impossible, to determine all the causes of poor quality in ware or t o explain certain differences observed in the behavior of ware from different sources. This information. it is realized, is not t o be had from the makers, but can be gained only by carrying out an elaborate investigation involving the preparation of pure metals and of some of their alloys and also by the careful analysis of commercial ware. It is hoped that in time the Bureau of Standards may be able to take up such a n investigation, which i t is quite impossible for the committee to assume. This Division, or better still the Society, could lend most valuable support to a project of this kind by urging upon the proper authorities the great need for a thorough study of the platinum metals and their alloys, a study which will involve the expenditure of a considerable sum of money. The investigation should not he restricted to a study of the subject from the point of view of the chemist alone, but should be made comprehensive as t o the physical constants and physical behavior of the metals and alloys, so that all users of the platinum metals might benefit. In the meantime, however, Dr. G. K. Burgess, of the Bureau of Standards, assisted by hlr. P. D. Sale, has developed a method for determining with exactness and rapidity the total impurity in any platinum alloy in terms of iridium, which is the most common associate of platinum in commercial ware. This method depends upon the measurement of the electromotive force of the alloy against pure platinum at a given temperature. So far the method has shown itself very reliable for platinum containing known amounts of iridium, and its application will be extended, if suitable materials can be obtained, to other binary alloys of platinum and its common associates. At present it is not possible t o determine what other metal or metals may he alloyed with platinum, hut, as said above, their joint effect can be given in terms of iridium. The determination takes hut a few minutes. The method is printed in full in this issue (p, 452) in the form of a paper by Messrs. Burgess and Sale, with the results obtained on the various samples loaned t o our committee by American manufacturers of platinum ware, as well as upon articles of English, German and French make and some purchased specimens of American make. Since this work is a direct outcome of the activity of our committee, we feel that substantial progress has been made, notwithstanding that we have no experimental data of importance to present on our own immediate behalf, and we take this opportunity to express to 5lessrs. Burgess and Sale and t o the Director of the Bureau of Standards our appreciation of their efforts to forward our work. It was hoped that, after the publication of our first report, American manufacturers would furnish to purchasers commercial ware of decidedly hetter quality, as t o iron and perhaps other base metal content, than they had been offering in recent years. This hope has proved illusory as t o some a t least of the ware now sold, so far as we can judge from specimens recently submitted for test a t the Bureau of Standards, on request of one of
us.
513
In order that more information may be acquired as to the quality of ware sold from now on, the committee asks purchasers t o submit t o it one or two specimens (particularly crucibles) from each lot of new and unused ware. The committee is authorized to say that these samples will be examined-at the Bureau of Standards (for the present without charge) in such manner as not to injure the articles, and reports will be made to the senders. The tests will be directed, so far as can now be foreseen, toward the detection of iron or other base metal (as shown in part by the appearance of the surface of the ware after ignition) and to the determination of the sum of alloyed metals in terms of iridium by the thermoelectric method above mentioned. The determination of loss on prolonged heating a t high temperatures will not, for the present, figure in the tests. T h e Bureau will reserve the right to make such use of the results. of its examination as i t may find desirable. It is believed that the adoption of this course by a sufficiently large number of users of platinum utensils, during the next few years, will bring about speedy improvement in the quality of commercial ware. If not, the committee will probablv make other recommendations for the protection of the public. W. F. HILLEBRAND E. T. ALLEN PERCYH. WALKER AMERICAN CHEMICAL SOCIETY-49th MEETING, CINCINNATI, APRIL 6-10,1914 FERTILIZER CHEMISTRY DIVISION REPORT The meeting was called to order by hfr. J . E. Breckenridge, Chairman. After the transaction of the usual routine business, the papers were presented as published in the official program. An amendment to the by-laws was adopted, making a generaI Committee on Research and Methods of Analysis in place of the Committees on Xitrogen. Phosphoric Acid, Phosphate Rock and Potash. The meeting was very well attended considering the conditions which would enforce the absence of a good many of the members a t this season of the year. F. B. CARPENTER, Secretary REPORT OF THE COMMITTEE ON FERTILIZER LEGISLATION
The question of uniform fertilizer legislation having occupied the attention of this division for some time, the following resolution adopted by the Association of Southern Agricultural Workers a t the annual meeting in Montgomery, Ala., Feb. 26th, will be of interest: “%‘HEREAS, the wide variation in the requirements now existing in our Southern States for the branding of fertilizer packages are a source of confusion t o purchasers, a waste of time and liability t o errors in inspection, and an unnecessary expense to manufacturers, “THEREFORE, BE IT RESOLVED, that this Association endorses uniformity and simplicity in branding, and urges the officials in charge of fertilizer control in our Southern States to use their influence in securing such legislation as will bring about simplicity and uniformity in branding of commercial fertilizers.” Your committee was represented a t this meeting and participated in the discussion. I n the matter of new legislation there have been a few minor changes since the last report, but not of such a nature as to materially affect either the manufacturer or consumer. F. B. CARPENTER, Chairman REPOET OF COMMITTEE ON PHOSPHORIC ACID
This Committee has been asked to prepare a rCsumC of the work done since its organization, for the guidance of the Committee on Methods of Analysis. This Committee first turned its attention to the determination
T H E J O U R N A L OF I N D U S T R I A L A N D ENGINEERING C H E M I S T R Y
514
of insoluble phosphoric acid, since i t thought a method which would give more concordant results was needed. Since there are several factors which influence the determination of insoluble, such as the neutrality of the ammonium citrate, time required for filtering insoluble, etc., the best way of attacking the problem seemed t o be to vary one of the factors a t a time, keeping the others constant. The first question taken up was the preparation of neutral ammonium citrate. A solution of citrate was prepared by one of the members of the Committee and sent out with the samples. Those to whom samples were sent were asked t o prepare a citrate solution and run samples with the solution prepared by them and also with that sent out by the Committee. The results' showed that i t was possible to prepare a solution which would give results which were the same as those obtained by the Committee citrate, but results from different analysts showed great variation between them. One of the chief causes of this great variation was due to the great difference in time required for filtration. Another set of samples was prepared and together with these samples was sent a standard sample on which the Committee had determined the total phosphoric acid. The total in standard sample ran about the same as the highest insoluble. The instructions which accompanied were the same a s those sent out with the previous lot of samples, except t h a t t h e method of filtration was shortened by transferring the precipitate t o another filter in cases where filtration was difficult. The results2 showed some improvement in the case of goods difficult t o filter, b u t in the case of acid phosphate the variation between analysts was the same. The results obtained on the last set of samples are somewhat disappointing. The differences d.0 not follow any rule, hence it is difficult t o assign any reason for the variation. The most probable cause of the variations is due t o the failure, on the part of the analyst, to observe the details of the method closely. Analysts who have had considerable experience with the method think that much better results should be obtained where the details of the method are closely observed. [ J . Q. BURTON
V O ~6. , S O .6
The determinations as reported herewith were made on three samples which were prepared and averaged with the greatest care by hlr. G. H. Savage and t h e formulas used by him are given below in detail in as much as it has a direct bearing on the present report. The various ingredients which went to make up these three compounds were weighed with extreme accuracy and compounded with the greatest care in order that uniform average samples might be obtained. The vulcanized compounds were then ground according t o the requirements of the procedure under investigation, carefully mixed and placed in small vials which held the approximate amount required for the various determinations. These were sent by express to the various members and the analysis on the first determination started by each member within approximately twenty-four hours of the time of grinding the sample. These samples were re-analyzed a t intervals as indicated in the report. This Committee respectfully refers the members of the Rub6 , 75, for the complete method of ber Section t o THISJOURNAL, procedure of the Joint Rubber Insulation Committee as followed by this Committee in the analysis of the three samples prepared by Mr. Savage. The formulas of the three compounds, together with the analytical results obtained, are tabulated below. FORMULAS USED
IN
PREPARING COMPOUNDS ANALYZED
A Fine P a r a . . . . . . . . . . . . . . . . . . . . 297 Hard Paraffin,. . . . . . . . . . . . . . . 25 Ceresine.. . . . . . . . . . . . . . . . . . . . . . . 19 S u l f u r . , ...................... Litharge ..................... 70 Zinc Oxide.. . . . . . . . . . . . . . . . . . 350 Whiting ...................... 239 ~~
B 309
C 324
25 19 70 350 227
19 70 350 237
..
-
.. ..
__
1000
~
1000
1000
No corrections, additions or omissions have been made in reporting these analytical results. The analysts' numbers refer t o the following: I-E. W. Boughton; a-D. W. Whipple; 3-W. A. Ducca; 4-G. H. Savage; 5-J. B. Tuttle. SAMPLE A-FIRST
ANALYSIS
......
[ G. FARNHAM, Chairman =PORT
OF THE ANALYTICAL COMMITTEE-RUBBER SECTION AMERICAN CHEMICAL SOCIETY
,[The following report was presented t o the Rubber Section of the A. C. S.a t Cincinnati on April 8, 1914,and the Section authorized its publication for t h e purpose of bringing the results obtained t o the attention of those interested in the work and in answer t o the Joint Rubber Insulation Committee's request for criticisms. DORRISWHIPPLE,Secretary. I Your Committee begs to present herewith the third report of t h e investigations made by this Committee, together with the results obtained. The major part of the work of this Committee has been confined to certain methods of procedure as outlined by the Joint Rubber Insulation Committee for the analysis of materials used for insulating purposes. The results obtained on preyious work were presented t o the members of the Rubber Section at the Milwaukee meeting and at the Rochester meeting. The Committee has not included the previous work in the present report (although the same has a direct bearing on the present report) as some of the methods have been changed or revised. I n the time intervening between the Rochester meeting and the present day, this Committee has investigated the completed preliminary procedure of the Joint Rubber Insulation Committee and these final results are the ones tabulated below. 1 THIS JOURNAL, 3 (1911). 118. 3
I b i d . . 6 (1913). 956.
Analyst's No. 1 1 2 2 3 4 4 5 D a t e of Extraction with Acetone ...... 11/13 11/15 11/14 11/20 11/20 11/13 11/13 11/13 T o t a l Acetone Ext r a c t ( % ) . . . . . . . . 4 . 1 6 4.12 3.97 4 . 0 3 4 . 1 8 3 . 8 4 3 . 7 8 4 . 0 8 Free Sulfur (%). .... 0 . 8 7 0 . 8 6 0.80 0 . 8 2 0 . 9 0 0 . 7 0 0 . 6 6 0.82 Unsaponifiable M a ........ 2 . 9 7 2.70 2 . 7 6 3.29 2.71 2.69 2.69 terial (70) Waxy Hydrocarbon A ( % ) . . . . . . . . . . . 2.29 2 . 2 5 2 . 1 8 . . 2.27 2.39 2.31 2.40 Waxy Hydrocarbon . . 0.56 0.14 0.20 0 . 1 1 B ( % ) . . . . . . . . . . . 0 3 4 0 . 2 0 0.32 Total Waxy Hydrocarbon ( % ) . . . . . . 2 . 6 3 2.45 2 . 5 0 . . 2.83 2.53 2.51 2.54 B y Difference Organic Extract (yo) 3 . 2 9 3 . 2 6 3.17 3 . 2 1 3 . 2 8 3 . 1 4 3 . 1 2 3 . 2 6 Saponifiable Acetone . . . . 0 . 4 3 0 . 4 3 0.57 E x t r a c t (%) . . . . . . 0 . 3 2 0 . 5 6 0 . 4 1 Unsaponifiable Res0.18 0 . 1 8 .. ins ( 7 0 ) . . . . . . . 0 . 3 4 0 . 2 5 0 . 2 6
..
. . . .
SAMPLE A-SECOND ANALYSIS AnaIyst'sNo ........ 1 D a t e of Extraction with Acetone... . . . 11/20 T o t a l Acetone Extract(70). . . . . . . . 4.13 Free Sulfur (%) ..... 0.88 Unsaponifiable M a terial(%) . . . . . . . . 2.32 Waxy Hydrocarbon A (7") . . . . . . . . . . . 1.97 Waxy' -Hydrocarbon B ( % ) . . . . . . . . . . . 0.17 T o t a l Waxy Hydrocarbon ( 7 0 ) . . . . .2. . 5 5 B y Difference Organic Extract (%) 3 . 2 5 Saponifiable Acetone Extract (yo) ...... 0 . 9 3 Unsaponifiable Resins (%).. . . . . . . . . 0 . 1 8 Fillers (%) Sulfurfree
................
1
2
2
3
4
4
5
11/21 11/25 11/23
12/4
11/20 11/20 11/20
4.16 0.79
4.14 0.88
4.02 0.80
3.72 0.89
3.90 4 . 0 0 0.65, 0.65
2.75
2.82
2.81
2.54
2.41
2.51
2.60
2.31
2.31
2.37
2.32
2.11
2.32
2.51
4.20 0.91
0.24
0.25
0.19
0.49
0.10
0.10
0.11
2.64
2.56
2.56
2.81
2.21
2.42
2.62
3.37
3.26
3.22
2.83
3.25
3.35
3.29
0.62
0.44
0.41
0.29 0.84
0.84
0.69
0.20
0.26
70.7
..
0.25 71.6(a)
.. ..
72168 73.75
( a ) T h i s determination was not made b y the same analyst.
0.09
..
..
71. I
