Aug.,
1920
T H E J O U R N A L OF I N D U S T R I A L A N D E N G I N E E R I N G C H E M I S T R Y
technical activity in this country along these lines. T h e proposed section would serve as a clearing house for papers and information on cellulose technology, and should also play a n important p a r t in promoting research on the chemistry of cellulose. T h e symposium at St. Louis wa? distinctly successful. The interest shown was so great t h a t it was voted t o hold a second Cellulose Symposium under t h e auspices of t h e Industrial Division a t t h e Chicago meeting during the week of September 7. At this time, the advisability of forming a permanent Cellulose Section will be considered. An interesting program is being arranged, and a large attendance of those interested in cellulose is anticipated. G. J . ESSELEN, JR. ARTHUR D. LITTLE,INC
81 j
Thursday, September 2 , will be given up t o mill visitations, followed by a steamboat excursion on Lake George in t h e evening. It has been arranged t o pay visits of inspection by automobile t o the plants of t h e International Paper Company, Finch, Pruyn & Co., Union Bag and Paper Corporation, Standard Wall Paper Co., and Sandy Hill Iron and Brass Works. On Friday a visit t o t h e works of the General Electric Company at Schenectady will show in the making the machinery and electrical apparatus used in pulp and paper mills. The visitors will subsequently be t h e guests of t h e General Electric Company at luncheon. In t h e afternoon i t is planned t o visit t h e felt mills of F. C. Huyck & Sons and t h e Albany Felt Compaw. THOMAS J . KEENAN,Secretary NEW YORK,N Y.
CAMBRIDGE, Mass July 6 , 1920
CALENDAR OF MEETINGS
TECHNICAL ASSOCIATION OF T H E PULP AND PAPER INDUSTRY
On September I t o 3, 1920,t h e fall meeting of the Technical Association of the Pulp and Paper Industry will be held at Saratoga Springs, N. Y., with headquarters a t t h e Grand Union Hotel. The program gives assurance of a most interesting and instructive meeting. Following t h e business session on Wednesday morning, September I , at 9:3 0 o’clock, papers on special subjects will be presented, an especially important one being on the “Washing of Felts.” In the evening members and guests will be entertained a t dinner by t h e paper manufacturers of the Hudson River valley and vicinity.
1
American Ceramic Society-Summer Meeting, LaSalle Hotel, Chicago, Ill., August 16-18,1920. American Institute of Mining and Metallurgical EngineersI m n d Meeting, Lake Superior, August 20 to September 3, .19zo. Technical Association of Pulp and Paper Industry-Fall MeetSeptember I t o 3, 1920. ing, Saratoga Springs, N. Y., American Chemical Society--Sixtieth (Annual) Meeting, Congress Hotel, Chicago, Ill., September 7 t o IO, 1920. Sixth National Exposition of Chemical Industries-Grand Central Palace, New York, N. Y . , September 20 t o 2 j , 1920. American Electrochemical Society-Fall Meeting, Hotel Statler, Cleveland, Ohio, September 30 t o October 2, 1920.
NOTES AND CORRESPONDENCE
UNCOVERING T H E PLATINUM THEFT AT THE OLD HICKORY POWDER PLANT, JACKSONVILLE, TENNESSEE Between 4 30 P M , March 1 7 , and 9:oo A h r , March 18, 1920, almost 2200 g. of platinum laboratory ware, mainly crucibles, crucible covers, and dishes, valued at nearly $I 1,000,were stolen from t h e chemistry building of the Bureau of Standards. During the first week in April, information was received of t h e arrest in New York of two men. giving their names as Robert E. Carter and Joseph Fredericks, who were attempting t o dispose of about 280 troy ounces of platinum sponge. Lots of 50 oz. and I O oz. had been left a t t h e offices of two concerns in New York who deal in platinum and the other noble metals. The remainder of the sponge was later found in two rubber hot-water bottles in a small grip checked a t the hotel where t h e two men were registered. Belween December 28 and 29, 1919,Roessler and Hasslacher Chemical Co., of Perth Amboy, N. J , had lost pure iridium sponge, platinum sponge, platinum sheet, and alloys of platinum and iridium containing I O and 15 per cent iridium, as well as a considerable amount of gold and silver. Carter and Fredrricks were arrested and detained under $5000 bail, t h e charge being t h a t the platinum in their possession was stolen from t h e Roessler and Hasslacher Company. Acting on the idea t h a t the platinum in question might include t h a t taken from the Bureau of Standards, the Department of Justice was asked t o investigate the matter. In the preliminary hearings, Carter stated t h a t his connection with Fredericks was merely casual, and t h a t he and a n associate named H. H. Brooks had obtained the platinum by placer mining on a n unregistered claim about IOO miles north of Parry Sound, Ontario. The platinum was brought into t h e country without declaration to the Customs.
Carter gave certain false references in Ontario, among them the name of the Maxwell House as a hotel in Parry Sound. It was known from statistics of t h e U. S. Geological Survey, subsequently confirmed by the Canadian Department of Mines, t h a t the total annual production of placer platinum in Canada did not exceed 2 5 ounces, and, furthermore, t h a t no placer mining of platinum was carried out in Ontario. I n a n interview with the representatives of the Bureau of Investigation and the Bureau of Standards, Carter described how “Brooks” had removed the gold from the crude platinum and had converted t h e remainder t o sponge by dissolving i t in aqua regia followed simply by drying and direct ignition of the chloride solution. This was done on t h e scene of the mining operations with reagents and equipment brought from Trenton and Montreal for this purpose. It was obvious t h a t a chemical analysis of t h e sponge would clearly distinguish between platinum t h a t had undergone even t h e simplest refining and the crude mixture of platinum, iron (IO t o 15 per cent), osmiridium, and sandy matter which would result from platinum ore treated in the manner described. It seemed probable, furthermore, t h a t a n exact analysis might help t o decide the real origin of the metal in t h e event t h a t Carter’s story should be completely overthrown. Most of the platinum stolen in Perth Amboy was alloyed with IO t o 15 per cent of iridium. It was estimated that t h e laboratory ware lost by t h e Bureau of Standards would contain a n average of about I per cent iridium with lesser amounts of rhodium and probably some palladium and iron. It was obvious that either of these lots of metal might be somewhat changed in composition through conversion into sponge. It was also possible t h a t the seized sponge represented several lots of stolen platinum. It was t o be expected, therefore, t h a t the results of the analysis would be of greater value in pointing t h e way in which t h e in-
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vestigation was t o be directed than as testimony in t h e argument of any particular case. The whole of Carter’s Canadian story was discredited without much difficulty. Since the .weight of platinum in Carter’s possession was very nearly t h a t of the platinum itself which had been stolen from the Roessler and Hasslacher Co., considering that all of t h e platinum had been carefully refined out of t h e platinum-iridium alIoys, and since no thefts of equal magnitude had been reported, Carter and Fredericks were held in the Tombs awaiting trial on this indictment. The U. S. Customs Service was prepared t o bring action against Carter, in the event of his acquittal, on the ground of his own statement that the platinum had been brought into the country without declaration. A suggestion was made by Mr. Schauwecker, of t h e U. S. Assay Office, t h a t the platinum in question might have been taken from one of the government munitions plants, certain of which used thousands of ounces of platinum in the manufacture of sulfuric acid by t h e contact process. The platinum used in the plants built during the war was refined by the U. S. Assay Office and converted t o chloride solution either by t h e Assay Office or by the company which operated the plant. The diluted chloride solution was used t o impregnate granular magnesium sulfate. Owing t o the fact t h a t some of these plants were in the process of being salvaged, an undetected theft might have been perpetrated. At the request of t h e Bureau of Standards an inventory was taken by the Bureaus of Ordnance in the War and Navy Departments of all t h e platinum in their possession, but this revealed no shortage. Owing, however, t o the fact t h a t most of the platinum held by the War Department plants was still in t h e contact mass, it was apparent t h a t the actual amount of platinum on hand could not have been determined without a very extensive series of assays or a complete recovery of the platinum in the mass. In the meantime, the analysis of t h e sample of Carter’s platinum had been completed b y the platinum laboratory of t h e Bureau of Standards, with t h e following results: Total platinum metals. . . . . . . . . . . . Loss on ignition in porcelain crucibl atile matter). ...
....
(vol-
........................
Per cent 99.20 0.67 __ 99.87
Analysis calculated on “non-volatile” basis, i. e., metals: , ; Iridiu Rhod Iron., . . . . . Platinum.
........................
IOO per
................... ...................
cent
Per cent 0.33 0.10
100.00
Gold, copper, and nickel were not detected. Spectroscopic examination revealed t h e presence of a trace of palladium, as well as small amounts, of aluminum, titanium, and magnesium. Traces of calcium and strontium, and possibly of silicon, were found. The sponge was apparently homogeneous except for t h e presence of small lumps of a yellowish brown substance which, on ignition, yielded platinum sponge, and gave off chlorine fumes. T h e brown lumps of incomp€etely ignited ammonium chloroplatinate revealed the fact that t h e conversion of the yellow salt t o platinum sponge had been carried out with inadequate facilities or in haste. The main thing t o be learned from the chemical analysis was t h a t t h e platinum was of unusual purity. The low iridium content was very strong evidence t h a t the platinum did not originate from the alloys taken from the Roessler and Hasslacher Co., or from the ware lost by t h e Bureau of Standards or any other chemical laboratory. It was known t h a t nearly all the other platinum of commerce contained from 0.5 t o I .o per cent of iridium, if not more. Nearly all the crude platinum which came into the country
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during the war was handled and refined by t h e U. S. Assay Office. Platinum 99.9 per cent pure and better was turned out in large quantities for the Nitrate Division of the Ordnance Department. (Most of this was subsequently alloyed with I per cent of iridium.) It was learned t h a t the 5,800 odd ounces of sponge prepared for use in sulfuric acid manufacture a t t h e War Department powder plant at Nitro, W. Va., and the nearly 13,800 oz. for the plant a t Jacksonville, Tenn., were also of high purity, except t h a t some of the platinum for use at Nitro contained about 0.5 per cent palladium. In view of these facts it was difficult t o banish the idea t h a t Carter’s platinum came from one or the other of these plants, especially in view of two clues which might otherwise have seemed irrelevant. It was found t h a t the “Maxwell House” was a well-known hotel in Nashville, which is about 15 miles from the powder plant at Jacksonville: and it was also learned that at the time of Carter’s arrest he had in his possession a cake of soap bearing the stamp of the Ruffner Hotel at Charleston, W. Va., in the immediate vicinity of t h e plant a t Nitro. The soap also bore t h e initials “H. H. B.” cut into it with a pocket knife. The photographic files of employees at the Nitro plant were unfortunately not complete, and Carter could not be identified. A visit of t h e Bureau of Standards representative t o t h e Jacksonville plant, however, met with sudden success. Carter was identified as one H. H. Brown, who had been employed as salvage foreman until his departure from t h e plant on March 27. While i t seemed t h a t Brown had had no possible means of access t o the platinum stocks of t h e plant, the manner in which he had obtained the 280 oz. found in his possession was explained by the next important development, which followed within a n hour upon Brown’s identification. This was t h e receipt by the Nashville office of the Bureau of Investigation of two letters, written by a man in the Tombs prison in New York t o his wife. The letters referred t o Robert Carter’s arrest, and spoke of “$20,000 worth of stuff” for which she should get $85 t o $go per ounce, and told her t o communicate with H. R . Crone, a t the Old Hickory Powder Plant. Crone’s arrest followed immediately upon Brown’s confession that the platinum in his possession was obtained from Crone, who had stolen i t from the reserve stock of platinum at t h e plant. Up t o the time of the present writing, Crone has denied any guilt in his handling of the platinum a t t h e plant. About the first of March, Crone, as chief chemist of the plant, was directed t o convert the reserve stock of platinum chloride solution, representing almost 2,300 oz. of platinum, t o sponge, and t o transfer it in sealed aluminum cans t o the custody of t h e accounting office, where i t was placed in a safe inside of t h e vault. About 75 oz. of platinum were handled at a time and the work was completed between the middle and the last of April. The safe contained 88 of these sealed containers, each bearing a label indicating t h e weight of platinum (about 25 02.) i t contained. After Crone’s arrest, the contents of these cans were examined, and only two were found to contain platinum. One of these was the first one placed in the vault, while the other represented a quantity of chloride solution which would only half fill one of t h e cans. T h e remaining 86 cans contained a mixture of mercury with ordinary moist dirt, the ratio between the two being carefully adjusted so as t o fill t h e can completely and give the correct gross weight t o the sealed can. One of the interesting and amusing phases of t h e case is t h a t Crone first proposed t o use lead filings as a substitute, but this meant a n amount of hard work entirely out of proportion t o t h e expected gains, and the scheme was abandoned in favor of t h e use of mercury and dirt. It is presumed t h a t Crone’s defense will be that Brown is shielding t h e real thief, who made the substitution in the vault. Brown disclaims any knowledge of t h e whereabouts of the platinum except t h a t which was in his possession, which is the total amount t h a t has been recovered to date. Crone and Brown
Aug., 1920
T H E J O U R N A L O F I N D U S T R I A L A N D EiVGINEERIlVG C H E M I S T R Y
had both worked in t h e Parry Sound, Ontario, region, and had agreed upon the mining story as t h e most plausible and easily supported account of t h e origin of t h e platinum. There was no evidence t o indicate t h a t Fredericks was implicated in t h e theft of t h e platinum or in t h e attempted disposal of it, except t h a t he acted as a guide for Brown in New York. It was learned t h a t Brown’s stop a t Charleston, while on t h e way t o New York, was in t h e nature of a visit and apparently had no connection with t h e stolen platinum or t h e government plant at Nitro.
DRAWINGS OF STANDARD APPARATUS Editor of the Journal of Industrial and Eizgineeriizg Chemistry: T h e work of t h e AMERICANCHEMICALSOCIETY Committee on Guaranteed Reagents and Standard Apparatus will necessarily be slow in regard t o reagents and apparatus which have been in use many years. There is, however, one line of work on which immediate results may be obtained if t h e editors of journals and authors of papers will cooperate with the committee. When a new piece of apparatus is described the committee would be glad t o recommend as standard the exact form w e d by t h e author who describes it. The makers of apparatus would be glad to furnish their customers with apparatus like t h a t of t h e author. One who has not given special attention t o this point would be surprised t o learn the small proportion of instances in which this is possible from t h e illustrations and descriptions published. In many cases there may be a wide range of dimensions which will prove entirely satisfactory. If the author considerr: this point he will know t h a t any chemist who may desire t o use the apparatus will know t h e proper dimensions, b u t makers who never have used such apparatus will be called upon t o make it merely from t h e published drawing, and even if they all succeed in making something which can be used there may be several sizes and shapes made for the same piece of apparatus. This causes unnecessary work for makers a n d frequently dissatisfaction on the part of their customers. A simple and obvious remedy would be for editors of journals to refuse t o publish descriptions or illustrations of apparatus which were not sufficiently complete t o enable any good workman t o reproduce t h e article described. Editors t o whom this sugge:stion has been made have expressed sympathy with t h e idea but have not been sure t h a t they could enforce such a rule. Some authors are n o t skilled draftsmen and cannot easily have such work done for them. T h e Association of Scientific Apparatus Makers of the United States of America is so interested in this question t h a t when t h e matter was taken up with t h e chairman of its Committee on Standardization he agreed t o take care of t h e drafting needed t o make proper drawings of apparatus recommended as standard by t h e Committee on Guaranteed Reagents and Standard Apparatus of the AMERICANCHEMICALSOCIETY.Of course this offer should not be taken t o cover t h e making of illustrations of every sort. It is intended primarily t o take care of the newly described apparatus which t h e two committees consider likely t o be used rather widely. If you will secure from authors complete dimensions, even on a rather rough drawing, the Association of Apparatus Makers will see t o it t h a t you have a suitable drawing for reproduction, provided t h e two committees think it worth while. Authors who submit complete drawings and specifications will save some time in publication of papers if you adopt this policy. Any delay in publication of their papers on this account will cost much less t o t h e interested parties t h a n t h e present common practice of publishing with nothing t o indicate t h e dimensions of apparatus described. W. D. COLLINS,Chairman, U. S GEOLOGICAL SURVEY Committee on Guaranteed Reagents WASHINGTON, D. c. June 16. 1920 and Standard Apparatus
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JOSEPH A. HOLMES SAFETY ASSOCIATION The Joseph A. Holmes Safety Association has recently announced the award of seven gold medals t o miners for spzcial deeds of bravery in th? saving of human life in the United States during the last three years. The Association was eqtahlished in 1916 in memory of Dr. Joseph A Holmes, the creator and first director of the Bureau of Mines, and is composed >f representatives of the leading technical and labor institutions of the United States, and receives its supp irt through voluntary contribirtions. In addition t o the awards for heroism, the Association plans t o recognize with awards the invention and application of safety devices in the industries concerned. It hopes in t h e future to devote attention t o imnrovement of health cond;tions and t o combating occupational diseases in mines and metal1 ~gical 1 establishments.
MACMICHAEL TORSIONAL VISCOSIMETER Editor OJ the Journal of Industrial and Engineering Chemistry: Referring t o the article in the Illarch issue of THISJOURNAL (page 282) on the MacMichael Torsional Viscosimeter, by Winslow H. Herschel, of t h e Bureau of Standards, I regret very much t h a t I was not advised t h a t this work was under consideration, as I would have been very glad t o furnish one of the late model instruments for testing. T h e machine actually used was one of the very earliest models, not even provided with heating coils, or with a number of other improvements found in the later models. Referring to the paper itself, my attention has been called t o the fact t h a t the term “poise” had been officially adopted as the name of the unit of viscosity in the C. G. S. system. I immediately wrote t o t h e manufacturers requesting them t o discontinue the use of t h e term “degrees M,” equal t o 0.1 poise, and t o graduate all future machines for direct reading in poises, which I understand has been done. It was never intended t h a t this machine should be calibrated according t o a mathematical formula, as this is obviously impossible, or at least impractical, from the very nature of the instrument. The method recommended is t o secure a sample of oil or other standard testing fluid, having a known viscosity nearly t h a t of the samples t o be tested. This sample should be tested by t h e Bureau of St.andards a t approximately the same temperature at which the machine is t o be used, as 60°, IOO’, or 210’ F. With such a sample i t is only t h e work of a mpment t o adjust t h e speed of the machine t o give t h e reading on the dial corresponding to that of the standard sample. T h e readings for other fluids of the same general temperature and viscosity will be found closely accurate, the results, of course, being expressed directly in poises. Where large differences in viscosity or temperature a r e dealt with, more than one standard testing sample is recommended, corresponding t o various conditions t o be met. I t is also suggested t h a t a large sample of fluid be procured, say, 0.5 or I gal., as there is always some slight loss in handling during tests. Of this, IOO cc. are t o be sent t o t h e Bureau of Standards for testing. T h e charge for this work is very moderate. It is not particularly difficult t o design a machine having a relatively simple mathematical treatment, giving primary readings for determining viscosity directly in poises. Such a machine would probably follow along t h e lines already laid down by Couette, using concentric cylinders, protecting end caps, etc. Such a machine, however, would probably not be well adapted t o ordinary commercial uses. The-present machine was designed t o fill a definite need i n t h e testing of colloids and suspensions, as well as true solutions. It is not intended t o give primary readings from which original data can be calculated, its function being t o compare the vis-
