Report of Committee on Standard Specifications - Industrial

Ind. Eng. Chem. , 1911, 3 (11), pp 860–863. DOI: 10.1021/ie50035a022. Publication Date: November 1911. Note: In lieu of an abstract, this is the art...
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'order t o convey the meaning of the drawings more clearly to the pattern makers and to facilitate the arrangement in space of all the apparatus, complete models were made a t a scale of one inch t o the foot, and as a n example 3 pictures of the models for the column are given in the accompanying cuts. In the experience of the writer such models have been of great service to obtain the construction of chemical apparatus in conformity with drawings, particularly if they had t o be made in machine shops where the construction of chemical apparatus is new, or done only a t great intervals. I t also is thought that models similar t o the ones presented a t the meeting are highly instructive for students in chemical engineering. It is true that students even if they are highly advanced in manual training could not make such models themselves, since it takes the best of pattern makers to do that class of work. But it would pay well for any university t o have a shop and t o employ one or more

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pattern-makers steadily t o do such work. By so doing they might accumulate in time a stock of models, the manufacture of which will serve t o train the instructors, while the models themselves will be a lasting aid in the instruction of students. Two columns were actually constructed by these drawings and models. Each column was made up of I base, A; I bottom piece, B ; I bottom section, C ; 1 7 cooling sections, D, alternating with 16 center sections, E ; 35 dividing bottoms, F, cast together with perforated plates, one bottom being located between each pair of sections; 3 top sections, G ; and I cover H. The eqtire finished weight of one column was 177,570 pounds and it was constructed for 3 ' I r cents per pound of machined castings, the price being understood free on board cars a t place of manufacture. Specifications as actually used in construction of the apparatus were accompanying the drawings, and the paper gave a full account of the construction and cost of a ten-ton ammonia soda plant.

SCIENTIFIC SOCIETIES.

REPORT OF COMMITTEE ON STANDARD SPECIFICATIONS. I N D I A N A P O L I S M E E T I N G , A . C. S . , J U N E , 1 9 1 1 .

The Committee on Standard Specifications, appointed a t the meeting of the American Chemical Society held in Boston in 1909 and consisting of Frank G. Stantial, Robert Job and the writer, submits the following report : As has been noted in previous reports to the Industrial Division. your committee decided that the work could best be carried out by the appointment of a sub-committee for each of the materials selected as the subject of a specification, the personnel of these sub-committees to consist, so far as possible, of three members-two representing the consumers and one the manufacturers. The committee was further of the opinion t h a t inasmuch as other societies were working along similar lines, our efforts should be confined for some time a t least t o those materials of a strictly chemical nature. Nine sub-committees were appointed t o formulate specifications for the following materials : Alum, Soda Ash, Bleach, Solder, Caustic Soda, Sulphuric Acid, . Muriatic Acid, Turpentine. Nitric and Mixed Acids, The personnel of these committees is as follows: M . Booth, Chairman, Syracuse, Alztnz.-William New York; F. A. Olmsted, Willamette Pulp & Paper Co., Oregon City, Ore.; S. W. Wilder, Merrimac Chemical Co., 33 Broad St., Boston, Mass. Bleach.-W. P. Atwood, Chairman, Hamilton Mfg. Company, Lowell, Mass. ; Fred. W. Farrell, Emerson Laboratory, Springfield, Mass. ; Charles E. Acker, 97 Cedar St., New York City. Caustic Soda.-W. K. Robbins, Chairman, Amoskeag Mills, Manchester, N. H . ; James W. Loveland,

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Works Manager, B. T . Babbitt, Babbitt, N. J . ; J. D. Pennock, Semet-Solvay Co., Syracuse, N. Y . X u r i a t i c Acid.-Fritz H. Small, Chairman, Graton & Knight Mfg. Co., Worcester, Mass.; J. T. Baker, J. T. Baker Chemical Co., Phillipsburg, N. J . ; W. S. Williams, Arthur D. Little, Inc., 9 3 Broad St., Boston, Mass. hritric aud Nixed Acids.-Arthur M. Comey, Chairman, E. I. duPont deNemours Powder Co., Chester, Pa. ; Henry U. Walker, Maas &. Waldstein Co., Newark, N. 1.; Oscar W. Pickering, 4 2 Holden St., Malden, Mass. Soda Ash.-Henry TV. Hess, Chairman, Libkey Glass Works, Toledo, Ohio; Martin L. Griffin, Emerson Laboratory, Springfield, Mass.; A. F. Shattuck, Solvay Process Company, Detroit, Mich. Solder.-Carl F. Woods, Chairman, Secretary, Arthur D. Little, Inc., 9 3 Broad St, Boston, Mass.; W. M. Corse, Lumen Bearing Company, Buffalo, N. Y . ; George 0. Bassett, Western Electric Company, 463 West St., New York City. Szdphuric Acid.-Fred B. Porter Chairman, Chemist Swift Fertilizer Works, Atlanta, Ga.; W. M. Kelsey, Supt. Acid Department, Mineral Point Zinc Co., Depue, Ill. Tzwpentize.- J. E. Teeple, Chairman, Hudson Terminal, 50 Church St., New York City; C. H. Herty, University of North Carolina, Chapel Hill, N. C.; L. F. Hawley, U. S. Forest Service, Washington, D. C. The sub-committees on bleach and solder specifications have completed their work and have submitted the requirements of these respective materials. These have been drafted into a form agreed upon b y the main committee and are submitted to the Division for adoption or whatever action may be deemed proper. Bleach.-The specifications for bleach are, so far as we know, different from any others in use. I t

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seemed wise, in view of the variable composition of bleaching powder, that some provision be made for purchasing upon a unit basis, in much the same manner as is done in the case of other chemicals. Solder.-In the case of the solder specifications, no attempt has been made to cover special solders since their composition is necessarily dependent upon their specific uses and the total amount used is small as compared with the more common types. The requirements for fine solder were formerly and are now in many cases jo per cent. tin and 50 per cent. lead. Careful service tests carried out b y a very large consumer of solder have clearly demonstrated t h a t a solder containing 45 per cent. tin and 5j per cent. lead is entirely efficient for general service, while the cost is materially less. The composition specified for wiping solder is practically standard among all large users of this material. As specifications of this nature should be adapted t o the needs of the greatest number, a n attempt has been made t o insert such requirements as would guarantee a satisfactory product, but, a t the same time, not needlessly limit the method of manufacture. Copper and zinc have been entirely prohibited as the former affects the flowing qualities while the latter produces brittleness. Antimony, however, up t o a small percentage, is not detrimental and has not, therefore, been entirely prohibited. The other common impurities are not harmful if present in but small amounts. The requirements, therefore, allow the presence of metals other +an lead or tin (excepting copper and zinc) u p t o 0 . 5 per cent. I t is the opinion of the committee that this will allow the us%of old metal of a suitable nature, but will prevent careless manufacture or wilful sophistication. I t was deemed wise to include in these specifications methods of analysis, as i t is particularly essential in the event of controversy that all parties concerned should use the same analytical procedure. Caustic Soda.-The sub-committee on specifications for caustic soda has submitted a report, but there are several important considerations in connection with this upon which your committee desires further time. The majority of the sub-committee, and many others consulted, agree t h a t the so-callea New York and Liverpool test for grading b y the percentage of sodium oxide present is erroneous and t h a t a change should be made t o some system of grading according t o the percentage of NaOH present. The manufacturers do not agree t o this, but prefer t o retain the present system. The sub-committee, also, does not agree t o the necessity of incorporating in the specifications methods of sampling, but your committee feels t h a t this is of the utmost importance. Turpenti~e.-The sub-committee on turpentine has promised t o submit its report a t Indianapolis, and there will not be opportunity, therefore, for its consideration b y this committee. Incomplete reports have been submitted within the past few days by the sub-committees on soda ash, alum, nitric and mixed acids, muriatic acid and sul-

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phuric acid specifications, which your committee has not had the opportunity t o consider but which, in event of the continuance of this work, will be referred back t o the sub-committees for further action. The sub-committee on sulphuric acid specifications has been handicapped b y the difficulty experienced in securing a third member. Your committee has encountered considerable inertia on the part of the various sub-committees. The chairman of one of the committees reports: “ F o r ordinary purposes no one suffers from lack of specifications and any one using for special purposes enough t o be benefitted b y specifications would have the benefit of a chemist’s services and procure without difficulty the article desired.” A member of another committee writes that he has “ n o t been able t o gather very much information on this subject as the specifications appear t o be very simple. ” Your committee also finds that owing to the geographical distribution of the members it has been difficult t o make as much progress as we had hoped. In the case of nearly every sub-committee there has been a delinquent member who has delayed the work of his committee b y not attending to correspondence. I n one instance, a report prepared by a chairman was submitted t o the other members of the sub-committee on January 6th and no reply had been received up to May 18th. These are merely examples t o illustrate the difficulties encountered in committee work where members live a great distance apart. Any remedy for such conditions would greatly facilitate . the progress of the work. Respectfully submitted in behalf of the Committee, H. J. SKINNER, Chairman. STANDARD SPECIFICATIONS (PROVISIONAL) F O R BLEACH.

Definition of Terms.-The word “ Purchaser, ” where occurring in these specifications. shall mean the purchaser of the material hereinafter referred to ,or his duly authorized representative. The word “ Contractor,” where occurring in these specifications, shall mean the party accepting the order t o furnish the material hereinafter referred to, or his duly authorized representative. General Description.-The material desired under these specifications is bleaching powder or calcium hypochlorite, prepared b y absorbing chlorine in slaked lime. It must be white in color, fresh and dry. Requirements.-The bleaching powder supplied under these specifications must test as follows: I . It must contain not less than thirty-one (31) per cent. of available chlorine. z . It must settle readily and completely when mixed with water. If lumps are present, they must break down and leave no core. Basis o j Price.-The base price per ton-unit named in the contract shall apply t o bleaching powder containing thirty-five ( 3 5 ) per cent. of available chlorine and is represented in the table below as “ I . 0 0 ; ” for variations from thirty-five (3 j ) per cent. in the avefage of the whole shipment bonuses and penalties

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shall be applied as per the table, provided the strength may be rejected and returned, the contractor paying of no single package varies more than one ( I ) per freight charges both ways. cent. from the average of the whole and in no case S T A N D A R D SPECIFICATIONS ( P R O V I S I O N A L ) F O R S O L D E R . falls below thirty-one (31) per cent., otherwise the Definition of Terms.-The word Purchaser, ” where entire shipment is to be a t the disposal of the conoccurring in these specifications, shall mean the purtractor or accepted under such terms as may be chaser of the material hereinafter referred to, or his agreed upon. duly authorized representative. Containing not less than: The word ‘‘ Contractor,” where occurring in these 31 per cent. base price X 0 . 7 4 = price to be paid per specifications, shall mean the party accepting the ton-unit for whole lot. order to furnish the material hereinafter referred to, 3 2 per cent. base price X 0 . 8 2 = price to be paid per or his duly authorized representative. ton-unit for whole lot. General Description.-The . solder desired under 33 per cent. base price X 0.89 = price to be paid these specifications is a homogeneous alloy of lead per ton-unit for whole lot. 34 per cent. base price X 0.95 = price to be paid and tin, uniform in composition, containing no zinc or copper and as free from every other substance as per ton-unit for whole lot. possible. 35 per cent. base price X 1.00 = price to be paid Rosin flux solder shall consist of a shell of solder per ton-unit for whole lot. 36 per cent. base price X I . 04 = price to be paid in the form of a wire, containing a core of rosin flux. Mineral and other non-resinous fluxes shall not be per ton-unit for whole lot. used. 37 per cent. base price X I . o 7 = price to be paid The quality of the material used and the methods per ton-unit for whole lot. of manufacture shall be such as to insure for the com38 per cent. base price X 1.09 = price to be paid pleted solder the properties called for in these speciper ton-unit for whole lot. fications. 39 per cent. base price X I . I O = price to be paid Requirements.-I. The composition of the various per ton-unit for whole lot. solders supplied under these specifications shall be as inspection.-All shipments shall be inspected and follows: weighed upon arrival a t destination. A sample Maximum per shall be taken from every third or fifth package, accent. of metallic i m cording to the size of the shTpment, the number of Minimum purities other packages sampled, however, not being less than per cent. Per cent. than copper Quality of solder. of tin. of lead. and zinc. twenty ( 2 0 ) per cent. of the number in the shipment, Fine solder (bar solder). . . 45 about 55 0.5 and submitted to the tests described below. The Wire solder. . . . . . . . . . . . . 45 55 0.5 sample shall be taken by boring a one- ( I ) inch hole kosin flux wire solder. . , . 45 55 0.5 through the side of the cask, midway from the ends, Wiping solder. , . . . . . . . . . 40 60 0.5 or through the head near the center. The sampler, .2. The rosin core used in rosin flux wire solder shall which consists’of a stout iron scoop about threebe of commercially pure rosin and shall form not more fourths ( 3 / 4 ) of a n inch wide and eighteen (IS)inches long, shall be inserted €or two ( 2 ) or three (3) inches, than six (6) per cent. nor less than three (3) per cent. withdrawn, and the bleach removed discarded. The of the total weight of the finished product. Inspection.-Each shipment shall be inspected and ’ sampler shall be inserted again as far as it will go, weighed. Drillings taken from any portion of each removed, the bleach transferred to a glass fruit jar, and the jar closed until the next cask is sampled. lot of solder shall be analyzed and the results of the The hole in the cask shall be closed with a bung. analysis shall be considered t o represent the compoThe portions from the several casks shall all be mixed sition of the lot. Analyses shall be made in accordance with the together t o make one composite sample representing standard method attached t o and hereby made a the shipment. Analyses shall be made in accordance with the part of these specifications. Method o j Shipment.-The completed solder shall be method given in Sutton’s “Volumetric Analysis”, 9th edition, page I 7 5 , Penot’s Method, b y adding a n ex- furnished in such form and weight and with such cess of N / I O sodium arsenite solution and titrating marks as may be specified. Failure to Meet Requirements.-Any shipment which excess with N / I O iodine solution. Method o j Shipment.-All bleaching powder supplied fails to meet the requirements hereinabove specified under these specifications must be packed in strong, may be rejected and returned, the contractor paying tight containers, entirely protected from air and freight charges both ways. METHOD O F ANALYSIS SOLDER. moisture. Each package must be marked a t the factory with the gross, tare and net weights and a t Preliminary Examination.-Make a qualitative serial number t o identify it. Casks or drums which analysis of the solder t o determine what ingredients have been broken or the contents of which have been are present and to secure an indication of the amounts wet may be rejected a t the discretion of the purchaser. of impurities. Failure to Meet Requirements.-Any shipment which Note.-If any zinc or copper is found, further analyfails to meet the requirements hereinabove specified sis of the solder is unnecessary. If these metals are ( ‘



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absent, proceed with the analysis in accordance with the following method: Antimony.-Weigh gram of clean, bright drillings or clippings in a 450 cc. Erlenmeyer flask; add I O to 1 5 cc. concentrated H,SO, and heat until the alloy is thoroughly decomposed (this is generally accomplished in about 30 minutes from the time the fumes of SO, begin to come off). Cool the solution and add 300 cc. of water and 1 2 cc. of concentrated HC1; boil in order to drive off all SO,, cool the solution and titrate rapidly with KMnO, ( z grams t o the liter) which has been standardized against metallic antimony in exactly this same manner. The end point of the reaction takes place when a pink coloration is shown. After agitating the liquid, however, this pink will soon disappear Tin.-Weigh out I gram of clean, bright drillings or clippings into a tall 2 5 0 cc. beaker; cover beaker with watch glass and dissolve in 1 5 cc. of " 0 , (sp. gr. I . 2 0 ) ; evaporate the solution t o dryness on a hot plate, cool, add 40 cc.of HNO, (z per cent.), and boil until residue is completely disintegrated. Filter and thoroughly wash with HNO, ( 2 per cent.). Place filter and contents in porcelain crucible, smoke off the paper, ignite for 1 5 minutes in full heat of Tirre11 burner, cool in desiccator and weigh. iVote.-This precipitate contains the tin and antimony in the form of SnO, and Sb,O, and also a small quantity of lead. To determine the amount of lead retained b y the precipitate, proceed as follows: Fuse the above precipitate with a mixture of finely powdered sulphur and soda ash in the proportion of I part of precipitate to 3 parts each of the sulphur and soda ash in a covered crucible until the odor of SO, has disappeared. Cool' and dissolve the fusion in hot water. Add an excess of sodiuT sulphite to convert any polysulphides t o monosulphides. Filter and wash thoroughly the precipitate of lead sulphide. Note.-The tin goes into solution as sodium sulphostannate and the lead is quantitatively precipitated as lead sulphide. Dissolve the precipitate of the lead sulphide in dilute nitric acid ( I part of HNO, t o 4 parts of H,O), add 5 cc. of strong H,SO, (sp. gr. I . 84) and evaporate until the fumes of SO, are given off strongly. Cool and dilute with 2 0 0 cc. of water; boil, cool, add r o o cc. of alcohol and allow to stand in the cold for several hours; filter on weighed Gooch crucible, wash with 5 per cent. solution of H,SO, and then with a mixture of I part of alcohol and I part of water until the washings are free from acid. Dry to constant weight a t 105' C. and weigh as PbSO,. PbSO, X log factor 9.86681'= PbO. PbSO, X log factor 9.83449 = Pb. From the weight of the precipitate of impure tin and antimony oxides subtract the weight of PbO and Sb,O,. previously determined. Calculate the remainder t o metallic tin. Factors .Sb X logfactor I O . 1 0 2 5 1 1 = Sb,O,. SnO, X log factor 9.89657 = Sn.

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Lead.-To the original filtrate and washings from the precipitate of tin and antimony oxides, add 15 cc. of concentrated H,SO, (sp. gr. I . 8 4 ) and evaporate the solution until the fumes of SO, come off strongly. Cool and dilute with zoo cc. of water; boil, cool, add IOO cc. of alcohol and allow to stand in the cold for several hours; filter on weighed Gooch crucible, wash with 5 per cent. solution of H,SO, and then with a mixture of equal parts of alcohol and water until the washings are free from acid. Dry to constant weight a t 105' C. and weigh as PbSO,. Factor.PbSO, X log factor 9.83449 = Pb. To the weight of lead so obtained add the amount of lead previously determined in the tin precipitate. This will give the total percentage of lead in the solder. COMMITTEE oh' STAKDARD SPECIFICATIONS H J S K I N N E RChazrman ,

AMERICAN INSTITUTE OF CHEMICAL ENGINEERSREPORT OF COMMITTEE ON CHEMICAL ENGINEERING EDUCATION. Received July 3 , 1911

The Committee on Chemical Engineering Education was created a t the Pittsburg meeting, December, 1908,and under the leadership of its able Chairman, now our worthy President, has done a great deal of valuable work since t h a t time. I t has conducted a great deal of correspondence, compared the existing courses of study for chemical engineering students in several of the best American and European schools, and made two lengthy reports, one in June, 1910,a t the Niagara Falls meeting, and one in December, 1910,a t the New York meeting. Both of these reports led to animated and instructive discussions, to t6e preparation and presentation in December last of' the valuable papers of F. W Atkinson and M . C. TVhitaker, and to the sending out of a circular letter with a series of queries t o be answered by the membership of the Institute. Unfortunately, the election of Dr. Frerichs'to the presidency of the Institute made it necessary for him t o relinquish the chairmanship of the committee, and in reconstructing the committee a chairman was selected who has not had the opportunity to make the recent exhaustive study of the subject t h a t Dr. Frerichs has made, and must therefore apologize to the Institute for his inability t o cover the ground in the thorough way in which the former chairman would certainly have done it. However, we fortunately have our President in our midst and can count upon his participation in the discussion and his counsel in arriving a t a judicious conclusion to the same, and we have upon the committee several members who have already made valuable contributions t o the study of the problem and who will further aid us in arriving a t a solution worthy of the Institute. To review briefly the work t h a t has been done by the committee and t o note the results thus far achieved, we find in the Bulletin of the Institute, issued in August, 1910,the .text of a circular letter sent out b y Dr. Frerichs, a s chairman, under date of Feb. 4, 1910, which contained as a basis of discussion a synopsis of the course in Chemical Engineering of a typica

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