Document BEmNmwwOQyeVEmXEgZN1rXjE

araramx h f mMiTTATTCB wo. PETyimrwmw or rm* nrp u a h c o w t f c t t In LITHARffi sm t ma Issued by Cleveland Tech. Service Dept, July 86th, 1923. The fallowing method Is nearly Identical with the procedure of tat African Society for Testing Materials and is one foond in general usage. Careful manipulation and strict adherence to the details of the tadare are necessary to obtain maximum accuracy. fi~r.T-rrs ATTD WATTPT1T3! 1. C.P. Crystallised Sodium Aocetate 2,. C.P* Potassium Iodide 3* H/lO Sodium-thiosulphate Solution. This solution is pre pared a9 follows: Dissolve 24.B3 grans of C.P. sodium thiosulphate, freshly pal prized and dried between filter paper,and dilute with water toons liter -t the temperature at which the subsequent titrations are to be made. The i'ui.tion is best mad with wall boiled water free from carbon dioxide, or allowed to stand 8 to 14 days before standnrStslng or using. Standardise with pure, re nub limed iodine as described in Treadwell-Hall, "Analytical Chemistry", Tol. 11, p.603 (1910),and also against purs, potassium iodate* The two methods of standardising should give results that agree within 0. 1 per cent iodine value* 4. tf/lQ Iodine Solution. 30-28 grams of C.P* potassium iodide are dissolved in as little water as possible in a liter flask, 12*7 grams of c'v.rjcsroiul iodine are weighed out roughly and added to the potassium iodide solution. The contents of the flask are shaken until the iodine is all dis solved. When this is accostall shed the solution Is diluted tothe one liter mark with water and standardised on the Jf/lO sodiunwthisulphate solution. 5* Starch Solution. Stir up 2 to 3 grams of potato Starch with 100 co, of ljf salicylic acid solution,and boil the mixture until the starch is practically die solved, then dilute to one liter* Weigh 3 grams of the litharge or gram of the red lead into a 200 cc, Erlenmeyer flask. Add a few drops of distilled water and ruib the airsVore with a flat rubber tipjed policeman to a smooth paste. Mix in a 3zs.ll beaker 30 grams of C.P. Tested Purity crystallzed sodium acetate, 2,4 grama of C.P. potassium iodide, 10 co, distilled water and 10 cc. of 50J& acetaic acid. Warm gently and stir until all is dissolved adding if nec essary 2 to 3 cc. water. Cool to room temperature and pour into the flask conzaliiing the lithaage or red lead annuls. Bab with the policeman until 000 '/ -SWP- 0000072 79 8ehsdule of Exaainatimj Ho. 6 * -3- July 26,1933 the litharge or red lead la completely .dissolved, add 30 eo. eater containing S to 6 grama of sodium acetate,and titrate at once with the N/lO sodiumthiosulphate, adding the latter rather slowly and keeping the liquid in con stant motion by whirling the flask.: When the solution has become light yellow, rub any undissolved particles up with the red until free iodine no longer forme. Wash off the rod, add the sodium-thiosulphate solution until pale yellow,then add 2 to 3 eo. starch solution and titrate until colorless. With deol-noraal iodine solution titrate back until the blue color is Just restored and substract the ec N/lO iodine solution used from the volume of sodium*thiosulphate that had been added,thus obtaining the number of pc. actually used. CALCTIATIQfll 7!hr inflat mine nf tie aciffsnw.iiirrtrpcaje auIaslXmi anlSfpriW by 0.94193 . Fbfrgj the iodine value: multiplied by 3.69973 . PbgO** th* ?W>3 value multiplied by 2.86616 PbgQ^ 0007-SWP-000007280 a Bulletin No. 23 Subject SCHEDULE OF EXAMINATION1 No. 15 " No. 16 30X21 U3M G20 3744 Feb, 16, ' 192 3 (Diet. 2-9-23) For Mr. C. S. Neal - Cleveland. We hand you herewith Schedule of Examination No. 15 for the estimation of Zinc in Zinc Oxide a, Leaded Zinca, idthopones, etc., and Schedule of Examination No. 16 for the estimation of Free Zinc Oxide in Lithopone. Please bring these schedules to the attention of all persons properly concerned in your organisation, and acknowledge receipt. Supt. Tech. Service Dept Materials Inspection Division DC:FMG Copies to: CSN CDH CLH HHC ALS *SS N Tech. Service File File li tn > \ 0007-SWP-000007281 N12904.01 SCHEOTIg OB* EXAMINATION Wo. 18 ESTIMATION OF ZINC IN ZINC 0X1183. LEASED ZINCS. LITHOFONSS. ta. SOLUTIONS? 1. Standard Potassium Ferrocyanids. 46 to 48 grams of the C. P, crystallised salt are dissolved in 1000 cubic centimetres of distilled water. 2. Uranium Indicator. a 5$ solution of uranium aoetate or uranium nitrate is made In distilled water slightly acidified with acetic acid. STANDARDIZATION OF THE FERBOCTANIDB: Neigh into 300 c. o. beakers several portions of c. p. sine, using about 0.3 gram. Cover with distilled water and dissolve in about 10 o. c. of hydrochloric add. Now add ammonia water till slightly alkaline, barely acidify with hydrochloric aoid, and add 3 c. o. in excess. Add sufficient water to bring the volume to about 200 c. c. and heat to almost boiling. Transfer about one-third of the solution to another beaker, and run the standard ferrocyanide solution into the main portion with constant stirring until a drop tested on a white porcelain plate with a drop of the Indicator, turns brown. Add nearly all of the . reserved portion, saving about 10 c. c., and again titrate till a drop turns uranium indicator brown, being careful not to add too large an excess. Now add the remainder of the reserved solution, rinsing the beaker out with a little water, and finish the titration, adding potassium ferrooyanide drop by drop till a drop tested with a drop of the indicator turns brown after standing one minute. A blank should be run with the same amounts of reagents and water as in the standardisation. The amount of ferrocyanide solution required for the blank should be subtracted from the amounts used in standardisation and in the subsequent titration of the sample. The standardization must be made under the same conditions of temperature, volune and acidity as obtain when the sample is titrated. CALCULATION: The number of cubic centimetres required (minus the number for the blank), divided into the weight of zinc taken, equal* the zinc equivalent for 1 o. o. of standard solution. This factor multiplied by 1.2448 gives the zinc oxide equivalent, and by 1.4906 the sine sulphide equivalent, PROCEDURE FOR THE SAMPLE: For zinc oxides and leaded sines weigh accurately 0.5 gram. Dissolve in hydrochloric add, make anmoniacal, reacidify, dilute to 200 c. c., etc., and titrate Just as in standardization, taking care that the same conditions of volume, acidity and temperature obtain. In the 0007-SWP-000007282 N12904.02 SCHEDULE OF EXAMINATION No. 15 . 3 ease of lithopone weigh 1 gram, dissolve In hydrochloric acid and boll till all hydrogen sulphide is expslltd. Dilute with water, and filter , off ths barium sulphate, than proceed as before. No. of e. o, of standard ferrocyanide multiplied by the correct factor, divided by weight of sample, multiplied by 100, gives the result. 0007 -SWP-000007283 .EAO&MA3,8Qg3.W g OF EXAHIHATIOH Ho. 23 Revised by Cleveland Teeh. Service Dept. January 22, .-1924, TESTS TOR COMPOTHTB Ilf LEAD CHROMATE T1LLOWS WHICH CAUSE THICKEHIKO WITH PAIKT VEHICLES. As It appears that Chroma Tallow* ara apt to contain impurities which eauss thickening or "livering" whan ground Into paint, tha following tasta have haan worked out to detect such impurities; isTHIC1CEKIWQ WITH (488): 4 ounce* of the sample ara weighed Into a 1/2 pint can; 3 liquid ounce* of (488), Wood Oil Bun Bobbing Tarnish, ara measured out and added with constant stirring. Tha mixture 1* thoroughly stirred, tha can than covered tightly, and allowed to stand 24 hours. Tha can Is than opened, tha mixture first stirred, and the consistency than noted by allowing it to ns 'off the spatula. It should not be appreciably thicker than whan it was first mixed. Ordinarily, tha foregoing will be the only test applied. In oase, however, it is considered desirable to determine the nature and amount of injurious Impurities, the following methods may be used: 2. ` DEPKHMIWATTQW OF UMB (Total) A 2-grom sample is weighed into a beaker, and dissolved in dilute nitric acid, whioh dissolves the oaloim compounds without reducing the chromium. The solution Is then made alkaline with ammonia, and acidified with acetio acid. Potassium bichromate solution is then added in excess, to precipi tate' the excess lead, and the solution heated to boiling. It is than filtered and the precipitate washed. 'Ammonium oxalate ie added to the filtrate to precipitate the lime, then ammonium hydroxide in excess. The precipitate is kept warm for about an hour, then filtered, and thoroughly washed with hot water. The calcium may now be determined either gravimetrleally or volumetrioally. If the gravimetric method ie followed, the precipitate Is ignited gently till com pletely charred, then with the full heat of a blast burner, cooled and weighed as Calcium Oxide. If the volumetric method is preferred, a hole ie punched in the'paper and the paper and beaker in which precipitation was made, treated with hot dilute sulfuric acid. The solution in the beaker (which must not con tain any'pieces of filter paper) is heated to boiling, allowed to stand two or three minutes, then titrated with tenth-normal potassium permanganate, added cautiously from a burette until a permanent pink color is obtained. One oc H/10 K lfe04 = 0.0033 0B. CaO. 0007-SWP-000007284 N12904.03 Haw Materials Schedule of Examination Ho. 23 (Con*d) - 2- 3. DEFFRMI1TATIOH OF WATER-SOLUBLE IMPURITIES; Among the impurities apt to ho present on account of insofflcient washing ore alkali chromates and sulphates. A preliminary test for their presence Is made by pouring hot water over some of the pigment In a beaker, stirring and filtering. A portion of the filtrate Is acidified with acetic add and tested by adding a few drops of lead acetate, which att'II precs'pfsacw any cilroaattr proutmO. jftnnhhir* purSjfJte * Aanhaf Sscsulphate by acidifying with H Cl and adding Barium Chloride. If only chromates are present, proceed as in paragraph (a). If only sulphates are present, proceed as In paragraph (b). If both are present, proceed as in paragraph (c). Procedure when only Chromates are present; (a) 5 grams of the pigment are neighed Into a 250 e e beaker. About 100 c c of boiling water are poured over it, and the mixture thoroughly stirred from time to time for a period of about 15 minutes. It is then filtered by decantation. The pigment remaining In the beaker is treated with 4 more portions of boiling water and filtered as before. The com bined filtrates are then acidified with acetic acid. 10 o c of 10$ lead acetate is added and the solution boiled 2 or 3 minutes. It Is then filtered through a Gooch crucible, the precipitate washed with hot water, dried at 100C and weighed as Pb Cr O4. This is calculated to Cr 0^ hy multiplying by tho factor 0.3097. Procedure when only Sulphates are present; (b) 5 grams of pigmsnt are extracted with 5 portions of boiling water as In paragraph (a), the combined filtrate acidified with 5 cc H Cl. The solution Is brought to boiling, 10 c c 10$ Ba Cl- are added, the precipitate allowed to settle overnight, filtered, washed, ignited and weighed as Ba SO^. Ba 80^ x 0.343 = SO^. Procedure when both Sulphates and Chromates are present; (c) ' 10 grams of the pigment are weighed into a 250 cc beaker. 90 c c of boiling water are poured over it, and the mixture stirred thoroughly from time to time for a period of abogt 15 minutes. It is then filtered by decantation. The pigment remaining in the beaker is treats! with 4 mors successive 90 cc portions of boiling water decanting through a filter each time as before. The combined filtrates are then transferred to a 500 c o volumetric flask, the solution made up to the mark and thoroughly mixed. This is then divided-into two portions of 250 cc each. For the determination of sulphates, one portion is acidified with 5 cc cone. H Cl, 25 cc of alcohol added, and the mixture boiled for 15 minutes. 10 c c of 10$ Ba Clg solution are added, the solution allow ed to settle overnight, filtered; washed with 2$ hydrochloric acid solu tion, ignited and weighed as Ba SO^. Ba SO^ x 0.343 = S Q-j . The other 0007-SWP-000007285 Ear? Mat arid a Schedule of Examination Ho. 23 (Con'd) -3- portion for the determination of Cr 0g, is acidified with 10 c o cone. H Cl, 25 c o alcohol ere added to reduce the chromium, and the solution toiled for 15 or 20 minutes, when the color should he a grass green. Ammonium hydroxide is now added carefully until the solution is alkaline to litmus and the odor of ammonia is barely perceptible. The precipitate is boiled for about 10 minutes, then a drop or two' of ammonia is added; the solution will then settle out clear. The chromic hydroxide is filtsred off and washed carefully with hot water. The well-drained precipitate le dried, ignited with the full heat of a Meker burner, cooled and weighed ae Cr^ 0^. Cr^ 0^ x 1,3158 = Cr 0^ . 0007-SWP -000007286 SAW MATERIAL SCHEDULE Off mMUTATIOT #38 Issued by Cleveland Ieoh. 8erTioa Sept. January 39, 1934. SETERMI NATION OF SULPHUR DlOXim IN LEADED ZINC PIGMENTS, 2IHC amgs. BTC, Weigh 6 grams of the pigment into a 250 ee beaker. Add 100 eo of freshly boiled distilled water, and 6 g o of concentrated sulphuric acid. Stir thoroughly. Allow to stand for 15 minutes, and then titrate With H/20 iodine solution, using starch solution as an indicator. Calculation:- No. of eo of N/30 iodine solution x 0.0016 (80. equivalent of 1 ce of 8/20 iodine solution) -r by weight of sample gramsj X lOO = jk of SOg. Be act ions: ZnS0,, H2S04 ZnS04 + HgO + S03 80g +31+3 HgO = H3804 + 3HI m 0007-SWP-000007287 \, HAW MACTBm S m SXA?U*A?IQH.J34_ I seuad by Cleveland Tech. Service Dept. January 29, 1924s, DgrmiWATrow OF z in c h t o ph a t h nrara oxipr. _ AWD mBSD awe PIQMEOTa, The following method is essentially the some at tba A. 8. T. U. standard msthod. Wslgh 5 grams of tho pigment into a 280 oo beaker, Add 180 oo of distilled water and 60 oo of alcohol, and beat the mixture nearly to boiling. Bold at a nearly-to-boiling temperature for 30 mlmites. Allow the pigment to settle, then filter, end wash thoroughly with 1 J 3 alcohol and water mixture. Beat the filtrate to boiling, expel most of the aloohol, and add 5 co of lo barium chloride solution, drop by drop. Boil for 0 minutes, allow to eottlo, filter through "aahless filter paper", wash, ignite precipitate, and weigh,all in the usual manner for this precipitation as barium gnlphate. Calculation:- Weight of precipitate x 0.6916 (sine sulphate equivalent), ~ by weight of sample x 100 = ?C of sine sulphate. \ 0007-SWP-000007288 '1 N12904.05 SCHEDULE gy EXAMIHATION HQ. 44 lamed by Cleveland' Technical Service Sept,, January 2, 1928. ANALYSIS OF YELLOW. OBAWSE. AW TEBMILIOH PAINTS ACT PIGMEBTS (This Schedule is derived from Chapter EXIT, of Sr. Holley's book, "Analysis of.Paint A Tarnish Products", edition of 1913) 1. COMPOSITION The lemon yellow chromes usually contain sulphate of lead, sometimes carbonate of lead. The red chromes, known by the various names of scarlet chrome, chrome red, Chinese red, American vermilion, and vermilion substitute, may be considered as basic chromates of lead. Often these basic chromes are brightened up by having precipitated on them an organic color; this may be tested for by treating a portion of the pigment with alcohol, which will dissolve the organic color, giving a strongly colored solution. See analysis of vermilions. 2. HTOBOSCOPIC MOISTURE Beat 2 grams at 105 C. for 3 hours. Lose in weight represents hygroscopic moisture. 3. BAHYTES. SILICA. AND CLAY One gram of the pigment la boiled for 5 minutes with 30 e.o. of concentrated hydrochloric acid in a covered beaker. While boiling 4d& half a dozen drops of alcohol one at a time. Fifty o.e. of water is added and the boiling continued for 10 or IS minutes. Filter, wash thoroughly with boiling water, ignite, and weigh. The insoluble residue is fused with sodium carbonate, and the barium, silica, and alumina separated as described under analysis of white painte. 4. LEAD The filtrate from the insoluble resfdtew fr uutrimr?seif *ttt dilute ammonia until the further addition of another drop would cause the formation of a permanent precipitate, diluted to about 250 o.o. to 300 o.c., and hydrogen sulphide passed in for 10 minutes. Solutions containing large amounts of chromium, if neutralised with ammonia until a permanent precipitate appears, seem to require an excess of hydrochloric add for their resolution, sufficient to prevent the satisfactory precipitation of the lead with the hydrogen sulphide. 0007-SWP-000007289 N12904.06 Schedule of Examination Ko. 44 2 1/3/35 Allow the precipitate to settle thoroughly, as it renders the filter ing much easier, filter, wash with hydrogen sulphide water. Soil, filter, and jvrcjyi tat# with dilute nitric add. until all of the lead has dissolved, filter with aid of suetlon,. washing thoroughly with hot water. Add 5 o.e. of concen trated sulpfanrio acid, diluted with an equal volume of water, to the filtrate. Evaporate on hot plate until the white fumes of sulphur trioxide appear. Cool, dilute with water, add an equal volume of alcohol, filter, washing with dilute alcohol. Ignite gently, and weigh as lead sulphate. Save filtrate. 5. CHHOMItW The alooholie filtrate from the lead sulphate is evaporatsd nearly to dryness to sxpel alcohol, and the filtrate from the lead sulphide heated until the hydrogen sulphide is expelled. The two filtrates are mixed, diluted if necessary, fund made just perceptibly alkaline with ammonia; boll, settle, filter, wash thoroughly, Ignite, and weigh as chromic oxide. Wt. chromic oxide x 1.3137 - wt. chromic anhydride. ' Occasionally these pigments contain a small quantity of iron, which should be tested for qualitatively in a separate portion of the pigment. If found to be present, the precipitate of ferric and chromium hydroxides it dissolved on .the-filter with hydrochloric acid, the filter washed thoroughly with hot water, 'and the iron and chromium in the filtrate reprecipitated with asnonia and treated with sodium peroxide to dissolve the chromium as da scribed under the analysis of chrome greens. 6. ' CALCIUM The filtrate from ths chromium is treated with atanonlum oxalate, allowed to stand in a warm place for an hour or so, filtered, washed thorough ly, strongly ignited, and weighed as calcium oxide. 7. MAcarcsiPif The magnsslum is estlmatsd in ths filtrate from ths calcium In the usual manner. 8. COMBITOD SULPHURIC AGIO The cosblned sulphuric acid may be estimated by either of ths two methods given in the chapter devoted to the analysis of white paints. In fact, the latter method may be used for the rapid analysis of a chroma lead, ths insoluble lead carbonate being filtered off, the chromium precipitated as ths hydroxlds in the usual maimer, and the combined sulphuric acid estimated in the filtrate from the chromium. Wt. barium sulphate x 0.3433 = combined sulphuric acid. 0007-SWP-000007290 Schedule of Examination Ho. 44 9. CALCULATIONS 3 1/2/25 If calcium is absent, or present as carbonate, the combined sulphuric acid Is calculated to lead sulphate, the chrend a anhydride to lead chromate, and excess of lead to lead oxide. If calcium sulphate and carbonate of lead are present, tbs carbon dioxide must be determined and the amount of calcium present as sulphate estimated by Thompson's method as described under analysis of white paints. Vt. comb, sulphuric aoid x 3.788 *= wt. lead sulphate Wt. chromic anhydride x 3.230 = wt. lead chromate Ht. lead chromate x 0.6406 = wt. lead Vt. lead x 1.0773 = wt. lead oxide ANALYSIS OF MIXED PAINTS CONTAIN!Ml CHROME YELLOWS AND OCHRES. 10. DABTPES. SILICA. AND CLAY are estimated as described under analysis of chrome leads. 11. T.Ti:tpr both as sulphate and carbonate, is estimated as described under chrome leads, the filtrate from the lead sulphate being eared ae before. 12. IRON The filtrate from the lead sulphide is heated until all of the hydrogen sulphide has been expelled and added to the filtrate from the lead sulphate from which the alcohol haa been.-expelled by boiling. A few drops of nitric add are added and the solution boiled for a minuts or two, then made Just distinctly alkaline with ammonia, boiled, settled, and filtered. Dissolve on the filter with hot dilute hydrochloric add, wash with hot water. Cool. Eepreolpitate with ammonia, avoiding excess, without waiting for the precipitate to settle, carefully add a sufficient quantity of sodium peroxide (l gram is usually sufficient), keeping the beaker covered meanwhile. Digest until all of the chromium and aluminum have passed into solution, adding more peroxide if necessary. The iron remains undissolved, while the chrtxnium and almlnom go into solution; filter, wash thoroughly, ignite strongly, and weigh ae fezrie oxide, or dissolve in dilute hydrochloric aoid and titrate. Tie treatment with peroxide is preferably performed in a porcelain evaporating dish. 13, CHRQMIDM The filtrate from the iron is made up to 250 c.c. in a graduated flask. An aliquot portion is rendered aoid with acetio acid and a slight excess of 0007-SWP-000007291 Schedule of Sxaalnatlon Bo. 44 * -4- _ 1/2/25 ./ load nitrate solution added, allowed to remain on the hot plats until thoroughly eettlsd, flltorsd onto a weighed Gooch crucible; washed, dried, and weighed as lead chromate. 14. 1LPMI1TOM An aliquot portion of ths 250 e.o. solution Is Bade Just add with hydrochloric add, and than Just distinctly alkaline with ammonia, allowed to settle, filtered onto a Gooch crucible, ignited, and weighed as alumina. 15. ZIBC The filtrate from the chromium, Iron and aluminas hydroxides, under Iron is mixed with the filtrate from the lead sulphate from which the alcohol has been expelled, and the mixed solution saturated thoroughly with hydrogen sulphide, boiled with the addition of solid ammonium chloride to render the precipitate less slimy, and filtered. The sine sulphide dissolved with hydro chloric add, boiled to expel hydrogen sulphide, and titrated with standard ferrocyanide of potassium as described under analysis of white paints, 16. CALCIUM. MAGNESIUM. AND COMBINED SULPHURIC ACID are estimated as described under analysis of chrome leads and the calculations made as there described. AKILTSXS OF VEHMILION 17. PROPERTIES Vermilion is a bluish scarlet powder, having a specific gravity of 8.2. It is insoluble in any single aoid such as hydrochloric or nitric add and in the alkalies. Heated in contact with the air, it burns with a pale blue lambent flame. Pure vermilion will burn away entirely or at least leave but a small fraction of 1 per cent of ash. This is a reliable teat for it, as other adulter ants would be left behind on heating. The most eomaon adulterants of vermilion are red lead, oxide of iron, lead chromes, vermilionette lakes, para reds, and allsarine redd. 18. DETECTION OF VERMILIONETTES. PAHA AND AIIZARINB HEXS (a). Boil a little of the dry color with water, settle, and filter. Vermilionettes give a deep red solution, para reds a pale brownish or orange, and the allsarine reds a eolorlsss solution, (b). Boil a little of the dry color with a mixture of methyl and ethyl aloohol, filter, heat, and settle. Vermilionettes give a bright red solution, usually having a yellow "bloom,* para reds an orange-red solution, alizarine reds a practically colorless solution. 0007-SWP-000007292 Schedule of Examination Ho. 44 0- 1/2/28 (o). Boll another portion of tha dry pigmsnt with toot freshly distilled aniline, settle, and filter. Vernd lionettea giro a purple-red, allsarlns lakes a pale brown, and the para reds an intense orange-red solu tion. (d). Boll acme of the dry color with a solution of caustic soda. Vermllionettes give a red solution with a green "bloom," para reds a bluish rod solution, while alizarine reds yield a characteristic deep violet solu tion, ' 19. BAHYTES. SILICA. AND CLAY Dissolve 1 gram in 30 e.o. of concentrated hydrochloric acid, 50 o.o. of water with the aid of 1 to 2 grams of potassium chlorate added in small portions and warming. Evaporate to dryness on water bath. Take up in 50 c.c. of water acidulated with hydrochloric add, heat to boiling to dissolve any lead chloride, filter, waah with boiling water, Ignite, and weigh any insoluble reeldue. Ease with sodium carbonate and estimate tha barium sulphate, silica, and alumina ae described under analysis of white paints. 20. LEAD ' If lead is present, oalcinm compounds being absent, the filtrate is treated with sulphuric acid, evaporated carefully to expel excess of hydrochloric add, diluted with water and alcohol, the lead sulphate filter ed off on a Gooch crucible in the usual manner. 21. MERCURIC SULPHiag (VERMILION) Tha filtrate from the insoluble residue, if lead is absent, or the filtrate from the lead sulphate, is heated with a little sulphurous acid to reduce any iron present `to the ferrous condition, made neutral with ammonia, and then just add to litmus with hydrochloric add. The solution is diluted to about 350 o.e. and hydrogen sulphide passed in for 10 minutes. The marcurio sulphide is filtered off on a weighed Gooch crucible, washed with hydrogen sulphide water, the crucible removed to another holder and washed with alcohol and carbon bisulphide to remove sulphur, dried in steam oven, and weighed. .22 ESTIMATION OP LEAD ADD ME \ CALCIUM COMPOUBIS PBBSgNT The filtrate from the insoluble residue from 19 is prsdpitatsd with hydrogen sulphide ms described under 21, collected on a weighed filter, and dried at 100^ C., weighed, and mixed uniformly. An aliguot part is introduced into the bulb of Fig. 10, (See Dr. Holley's book) a slow stream of washed chlorine gas passed through it, and a gentle heat applied to the bulb, increasing this gradually to faint redness. The escaping chlorine ie conducted into a flue. ^r***_*tt*?r*r chloride distills over, which decomposes with the water in E and * , ine mercuric chloride formed volatilizes, condensing partly in X, padtly in u. 0007-SWP-000007293 Schedule of Eundnatlon Ho. 44 6- 1/2/25 Cut off that part of the tubs, rinse, the mercuric ohloride into E, and mix the content s of ths latter with the water in 7. Mix the solution with excsss of ammonia and warn gently until no more nitrogen is evolved, acidify with hydro chloric acid, filter, and determine the mercury in the filtrate as under 21. 23. FEHRIC OKISB The filtrate from the sulphides is heated until all of the hydrogen sulphide has been expelled and the iron chromium and alumina precipitated with ammonia, filtered and separated as described under analysis of chrome greens. 24. ZIKC PETtE The filtrate from ths iron and alumina precipitate is made distinctly alkaline -with ammonia and ths zinc precipitated with hydrogen sulphide. The liquid containing the zinc sulphide precipitate is heated to boiling, and about 5 grams of solid ammonium chloride added, which renders the precipitate easier to filter. Settle, filter, wash thoroughly. Pierce filter, wash through into a clean beaker with water, dissolving the residue on filter with dilute hydro chloric add, and washing with hot water. Dilute, heat to expel hydrogen sulphide and titrate with ferrocyanide at previously described. If iron is absent in the paint, the zino say be estimated directly as described under analysis of whits pigments. 25 . CALCIUM dHD MAGNESIUM Estimated as usual In the filtrate from the zinc sulphide. 26. CALCULATIONS If chromium is present, it is calculated to basic lead chromate, and any excess of lead above that required to form the chromate is calculated to red lead. 27. AOTiMorrr v e r mil io n a n d p r ims These two pigments have the same composition, corresponding to the formula of antimony trisnlphi&e. They ere insoluble in dilute adds, but soluble in strong hydrochloric add. It is seldom necessary to soaks a complete analysis of thess pigments. Adulteration will be indicated by the pigment not being completely soluble in strong hydrochloric, though a trace of sulphur may remain undissolved, floating on top of the add* 0007-SWP-000007294 flGBgrora o p sacmm'Pioir w?. 4B Issued fey Cleveland, *' ' Technical 8erric Bspt., January 13, 1925. AMLT8IS CP BLACK FIGMENTS AND PAIBT3 (This Schedule is derived froa Chapter XXI of Dr. Holley's book. "Analysis of Faint A Varnish Products*, edition of 1912) 1. COMPCSmOW The ordinary black pigments -- lampblack, Tagstable black, bone black, ivory drop black, gas black, graphite, eto. -- contain carbon as their essential constituent, and while all of these products are said to bs of a black color, they vary greatly in shade and still mors so in tinting strength. lampblack and vegetable black are essentially soot blacks being the soot deposited from the combustion of oily bodies such as dead oil. lampblack has a distinct gray tint, as may be shown by com parison with ivory black. These blacks are apt to contain varying quantities of oil, owing to the nature of their manufacture; less than 1 per cent of oil often being sufficient to retard seriously the dry ing of lampblack paints. Vegetable blacks are more voluminous than lampblacks and are usually of a Jet black color. Carbon black is usually produced from the incomplete combustion of natural gas. While its tinting power is very great, its use has bean largely abandoned owing to its tendency to produce a streaky color when used in tinting paints. Bone blade is, as Its name indicates, obtained by the charring of bones in retorts. The carbon content Varies usually between 13 and 23 per cent, the balance consisting of moisture, phosphate of calcium, and carbonate of calcium. The best grades of bona black are made from selected sheep bones. An exceedingly Intense black is made by digesting selected bones in hydrochloric add until all of the mineral Blatter is dissolved, leaving the carbon in a floccoleht state. This black la often sold under the name of black toner, and is one of the highest priced blacks. black is a nans semetimes given to bone black but is also used .to designate a wide variety of blacks prepared in the same way as bone black from waste animal produots of all kinds, as leather scrap parings, horn trimmings, etc. Frankfort black, drop black, and German black are terms used to da si gnata blacks made from a variety of organic materials, such as vine twigs, refuse of wins making, peach stones, bone shavings, etc. These black# vary in hue from a bluish black to a reddish black. 0007-SWP-000007295 Graphite, while not used to any extant in house palate, is largoly used In bridge, elevator, and warehouse paints. It is rarely used by Itself for these purposes, silica, ealoltn carbonate and Iron oxide pigments, aino and lead being the other usual constituents. It nay he tested qualitatively in the extracted pignent by rubbing a portion of the sample between the pains, which soon assume the characteristic appearance produced by stove polish. Of all the black pignent* graphite alone gives this test. Charcoal black and vine black are produced by tbs charring of wood products, and contain bssidss oarbon the ash ingredients ooonon to wood. Charcoal blacks arc usually nads from napls, willow, and basswood, and vine blacks froa the charring of the grapevine. Paints containing considerable quantities of those blaoks are liable to saponify badly owing to the moisture and potash salts present. Mineral black, which is still occasionally used, is black slate finely ground. 2. MOISTPIS Dry 3 grams at 105 C. for 3 hours. Loss in weight represents approxi mately the amount of moisture present. 3. OILS Xxtract 3 grams with ether in a fat extraction apparatus. After remov ing the ether and drying, any increase in weight represents the amount of oily scatter present. 4. ASH Two grams are weighed into a crucible and heated over a Bunsen burner until all the carbon le burned off. If the ash constitutes only a snail per cent, it may be cooled and weighed directly. Otherwise the residue is moistened with a solution of ammonium carbonate, heated gently, and weighed. The object of this operation ie to restore the carbon dioxide which may have been expelled from the bases by the strong heat to which they have boon sub jected. 5. CAHBOW The carbon is usually estimated by difference, by adding together the moisture, oil, and ash, and subtracting from 100. 6. CALCIUM Digest the residue from 4 in a mixture of 33 c.c. of concentrated hydro chloric acid and 8 c.c. of concentrated nitric aold o_n >thue_ hot-- p* la*t e- *fork arW ore-half hour, dilute, filter, and make up to 330 e.o. in a graduated Any appreciable residue on the filter may indicate addition of barytes, 0007-SWP-000007296 Schedule of Zxas clay, or alumina. Determine tbs caldum and magnesium In an aliquot portion of tho solution by adding somonia in small quantities until a praaipltats is formed, then acatio sold in excess until rsdissolved, except for traces of iron which may be removed by filtration, Ammonium oxalate Is added, and tbe calcium precipitate treated in tbe usual manner. 7. THOSPHOBIC ACID Take an aliquot portion of tbs solution prepared above, neutralise with asmonia, and clear with a few drops of nitric acid, add about 5 grams of dry ammonium nitrate or a solution containing that amount, To tho hot solution add SO e.o. of molybdlc solution for every decigram of phosphoric acid that is present. Digest at about 65 for an boor, filter, and wash with eold water, or preferably asuronium nitrate solution. lest the filtrate for phosphoric acid by renewed di-' gestion and addition of more molybdlc solution. Dissolve the precipitate on the filter with ammonia and hot water, and wash into a beaker to a bulk of not more than 100 e.o. Hsarly neutralise with hydrochloric add, and add magnesia mixture from a burette; add slowly (shout 1 drop per second), stirring vigorously. After 15 minutes add 30 o.e. of atmonla solution of density 0.96. let stand for sons time; 3 hours is usually enough. Filter, wash with 3.5 per cent ammonia, ignite to whiteness or to a grayish whits, and weigh as magnesium pyrophosphate. Molybdlc solution Dissolve 100 grams of molybdlc add in 400 grams or 417 o.o. of ammonia. speoifie gravity 0.96, and pour the solution thus obtained into 1500 grams or 1350 o.e. of nitric add, specific gravity 1.20. Xep ths mixture in a warm place for several days, or until a portion hsated to 40 deposits no yellow precipitate. Decant the solution from any sediment and preserve it In glassstoppered vessela. Magnesia Mixture Dissolve 110 grams of crystallised magnesium chloride, 280 grams of ammonium ehloride, in 700 o.o. of ammonia of specific gravity 0*96, and sufficient water to make 3000 o.o. 8. MAGNESIUM She filtrate, from which the calcium has been precipitated, is evapor ated to a small hulk and made alkaline with ammonia. After standing several hours the magnesium precipitate is filtered, ignited, and weighed, and calculated sajmctaluw bv anltlnlvlby 21.88. 9. CALCPLATI0B5 The magneslum is calculated to.magnsslum phbsphate, and the remainder of the phosphoric add to calcium phosphate. Any calcium remaining is calculated to calcium carbonate 0007-SWP-000007297 Schedule of Examination 36. 45 4- 2/13/SS Genuine ivory 'black, made by carbonising waste fragments turnings of ivory, la often adulterated with bona black, which la somewhat alalia? la composition, but contains only a small amount of magnesium phosphate as compared with tbs Ivory black. JLMLT3I3 Cff MIXED PAIOTS T1STED WITH BLACK JBD anus cr am pig men t s 1&--SATO One gram of ths pi grant la dissolved in hydrochloric acid as described under shits pigments, and ths residue filtered through an ashless filter, that has been dried in ths hot-water oven and weighed. After washing ths residue with boiling water ths filter and contents are dried and weighed, then ignited until all ths carbon is burned off, and weighed again. Ths percentage of carbon is obtained by difference. Where the percentage of color is small, it is often esti mated by difference, adding together the determined constituents and subtracting from 100. If the filtrate from the insoluble residue is of an appreciable yellow color, it indicates shut tfifcr tfiTrt- hudr 3mur VnwrsMd spr* Ox t the -addition of -an ochre or oxide, in which case the lead le precipitated and estimated as described under analysis of whits pignsnts, the filtrate from the lead sulphide heated until all of the hydrogen sulphide has been expelled and the iron and alumina precipi tated with ammonia after having been oxidised by boiling with a few drops of nitric acid, filtered and ignited and weighed in a porcelain crucible, the residue fused with bisulphate of potassium, dissolved in water with the aid of a little hydrochloric acid, heated to boiling, reduced with stannous chloride; mercuric chloride and manganous sulphate solution added and titrated with permanganate in the manner described under analysis of Venetian reds. 12. ALUMINA The aimins is calculated by difference from ths data obtained under 11. 13, ZIITO 0XI71S The filtrate from the iron and alumina precipitate and the filtrate from the lead sulphate precipitate, the alcohol having been removed by evapor ation, are mixed, made distinctly alkaline with ammonia, and the sine precipi tated with hydrogen sulphide. The liquid containing the sine sulphide precipi tate is heated to boiling, and about 5 grams of solid ammonium chloride added, which renders the precipitate easier to filter. Settle, filter, and wash thoroughly. Pierce filter, wash through into a clean beaker with water, dissolv ing the residue on filter with dilute hydroohlorio acid, and wash with hot water. Dilute, heat to expel hydrogen sulphide, and titrate with ferrocyanide as previous ly dascribsd. If iron le absent in the paint the sine may he estimated directly as described under analysis of white paints. 0007-SWP-000007298 Schedule of Examination So. 1/13/26 14. GALcimt iTO mmcw Estimate as usual in tbs filtrate frets tbs sino sulphide. 15. HBSinre IK30LU3LE IS STDBOCBLOBIC ACID Ease with sodium carbonate as previously described. Dissolve in water and filter. Iron not previously dissolved will remain on tbs filter as ferric oxide along with any barium that msy be present. XMi residue after thorough washing is dissolved with the aid of a ssall fosntity of hydrecklerle add, the barium precipitated as usual, and tbs iron satlmatsd in tbs filtrate from the barium sulphate. The silica and alumina arc estimated as usual. 16. ISAD SULPHATE Determine the confelned sulphuric acid as described under analysis of whits paints and calculate to lead sulphate in the absence of calcium sul phate. If calcium carbonate and calcium sulphate are both present the nitric acid-alcohol separation should bo used. 1?. GRAPHITE PAINTS The term graphite ae applied to paints does not necessarily amen that such paints are eosposed of graphite wholly or even in part, In fact there is no accepted standard of purity for graphite Itself. Che paint msunfacturer may purchase a natural graphite for Me line of graphite paints which contains 20 per osnt of graphitic carbon, the other 80 per cent being silica . and various silicates; others may purchase graphites containing 80 per cent or more of graphitic carbon; and some purchase products which are very nearly pure graphitic carbon, prepared electrically. WMlo it ie a far from settled question, perhaps the majority of paint manufacturers and those who buy graphite paints under strict specifications are of the opinion that a graphite paint affords better service value when it contains in part something besides graphitic - carbon. 18. COLOURS GRAPHITE PAIWT3 Saving established Ms grapMte paint on the market, the manufacturer i soon has requests for colors other than black, and in order to meet the require ments of Ms trade he finds it necessary to add considerable amounts of tinting pigments, with the natural result that in time many of Ms formulas contain little or no graphite. Tbs following analyses will give some idea of the pigment combinations l to be found on the market: Graphitic carbon . . . ......................... } Calcium carbonate ......... Magnesium silicate and silicate . . Ochre ........................................................... Jerria oxide ............................................ I. Hatural Graphite. Par cent. 32.14 42.86 25.00 100.00 II. Olive GrapMte. Per cent. 21.89 19.16 58.95 ee 100.00 III. Indian Bed GrapMte. Per cent. 44.59 12.1? ee 43.24 100.00 IT. Seal Brown GrapMte Per cent 5.31 26.13 33.72 e * 34.85 100.00 0007-SWP-000007299 Scisdnl of Sxanination So. 45 ft 1/u/aC* Th pigment portion of on* sampl* analyzed by tb* author was nothing but Keystone filler*, another, carbon black, which wMli as erpensire * th* ordinary gradaa of graphite la nevertheless radically different. Graphlta paints which arc sold according to specifications for structural iron and steal work are -usually hig&>grade products. 0007-SWP-000007300 acaaouLL-OF, ummm j & - ' ' ; ^ - ^-Tr * IS' 'MM- crrsmiisATioi. OP THE TRUE LEAP CONTEIT , Pb3^ PAINT3 CONTA; ilVO CARBON AND OTHER MATERIAL* WITH THE T Hi- SULPHATE TITRATION WHEN THU ir;'-yg - t + V '**&* miLM. OP - Noigh out too grama of twhare a am*' . amount of Hal load is prwaaat a 350 ",o t- kir. Aid *rom 50 to 60 o.e of Acetic AC . containing Potaatium X elide 3041un Act* is (Saa oolutioaVNo,4). I__ * a x tly 35 0*0. of ff/XOrSodlu* Tb wad pli&oa on ho hot Plato or atwoa batb at about SO G :o 7u* 0* (Don't U41). Filtop^i a Oooch Crcc; >!- wash thoroughly with hot.'***** th# exoid t - oauiphata with EoCModina " ' C*i' 0. c. of N/iG Hml^| io a Thwraforwi -'"'** V;1' aquala tfc# pa sent of PbsO*, or Rad rapxasaat th- normality faotoxt Of th<$ Thi Olutioaa ras; aotiv#lyc * ^Httn aSMTI.aij 1* di,,% Solution - 8Mi,^ia SohwdiatiKPi^ o. c an Dwtorminatioa of True Bid Llthfe g# *.nd Rod Lead. :a*. Sell'- Thioaulpfaata 4?- tion -;0 a. 00 in 3, 3tarc ao-iuttoq - Sana aw in Schadubfc 4* |SJU ' A^il^^taojAyi-IgdAdA^ 3b41 300 k -as to#tod Purity Cryatalilaadu 24 .*33 O.P. PotaosluiR Iodide 150 c a, Wator 50 c .3* Oalaoial Aootid Acil War* ^-satly and ad-1 30 to. 30' c a* wf^ aary. If 000a of tha Sodium Aco upon .-oolinf It doaa not-of foot .*? . - Ottia? ~oat a rial* odino from P*:Saasitai odida, auoh at Oh with thio da termination but would not or A/ 0007-SWP-000007301 Schedule of Examination So. 75 , Shift 2 a railroad paint of this type. ' Small amounts of unextraeted oil does not Interfere with this determination. - This method gives th^ True Red Land content, PbaOs. only. For instance, T,f the r^d lead pigment used oontalne PSt True Red land, then thie method determines Only the 93$ which ie Ph^O^ and does not include, the other B$ which la Litharge, PbO. To calculate the total number of pounds of nuoh nod,Ljf^ud ..^ment used, (such as 302 dry), it is thus nacsasaryTo divilnThe weight of True Pe^^eac) determined as above by .93 or whatever is the true PbaO^ content of the Hi L>rv-i pl-yuent need. If AtlffiTAtSLXSIHQfi - Weigh out exaotly tso grams Ferrouf Amaon- iua sulfate, transfer to beaker, add 25oo dilute HOI and 78 cc water, and stir till dissolved. Then add exactly l grm of pignwnt (or a larger amount if only a small percentage of Pb?4 /* Prc3*nt7 boll for a few minutes, cool and titrate with H/S K3OX2O7, using Potassium Fwfrioyanide as indicator. The number of cc acquired for a blank of 3 grama fsrrbu* salt is doter.nlnod, , 2u. req'd. for blank - Wo.for sample x Pb^O* factor of KuCraOv x iwj ----------- -------------gy ------------------------- *-------------- x per cent of pbjO^ l co H/5 KgOr^ * O.OG85 g This method gives the True Red Lead content., FI-3O4. only* For Instance, if the Red Lead pigment ueed contains.93$ True Rod Lead, then this method determines only the 93$ which Is Pb^O^ n<l does not include the other 6$ whl oh ie Litharge, PbO^t To calculate the total number of pounds of suoh Bed Lead pigment used, (suoh at 303 dry), it is thus necessary toTlvide the weight of True Rod (.sad determined a above by .03 or whatever is the true PbwOa oonlent of the T.ed Lead pigment used. .` 0007-SWP-000007302 ` ' SCHEDULE OF SKAMBTATiaff Ho. 86 ; Issued "by Paint Besearch Division. Detroit, Michigan -July 15, 1932 STABILITY TEST LEADED ZINC ASP OTHER BASIC LEAD SULPHATE PIGMEHTS SEKERAL This test should he regarded as tentativeo This test is based cn the reaction which takes place when Basic Lead Sulphate pignents, such as Leaded Zincs and Sublimed White Lead, are rubbed up in Glycerine, producing a pinkish discoloration, more or less pronounced, depending on the particular pigment, grade of Glycerine, temperature and light conditions0 Some Basic Lead Sulphate pigments which develop this color-' ation rapidly show a similar tendency in certain vehicles when exposed in paste form to ultraviolet lighv-, and much more slowly on exposure to sunlight in a paint film*. This "Glycerine test" is easily performed, and serves to distinguish Basic Lead Sulphate pigments which are relatively light stable from those which are relatively unstable. In order to avoid misleading results the test must be conducted under carefully controlled conditions and against a standard of proven stability in various vehicles under ultraviolet light. GLYCERIHE FOR TEST Because of the sensitivity of this tea*, and variations in different Glycerines, a stock of tested Glycerine wi?i be kept a* the laboratory of the Ozark Smelting & Mining Co., Coffeyville, Kansas, and supplied -;o the different laboratories on request. TEST PROCEDDBB Jour grams of Leaded Zinc or other Basic Lead Sulphate pig3 ment is placed on a glass slab and 2-l/2 c.c. of Glycerine added. Thorough incorporation of the plgaent with the Glycerine is effected with a spatula. A portion of this paste is spread on a piece of plate glass approximately 2" x 12" to form a smear the width of the slide, and 2" in length (2" x 2" smear). A space of 2" is then left on the slide and then a smear t f the standard Leaded Zinc is put on. Dp to this point it is essential that the operations be. conducted in a dull light only, not bright daylight or direct sunlight.' The Glycerine is to be used at normal room temperature. The plate carrying the smear is then placed in an oven and maintained at 80 C for one hour. At the expiration of this time, remove from the oven and cool at room temperature for fifteen minutes* 0007-SWP-000007303 N12904.09 Schedule of Examination No;> 86 Sheet #2 A fresh paste of pl^aent and glycerine is now to ho made and laid down against the heated and cooled smear* This paste oast he freshly made and not a portion of the first paste held over* Examine-* tion is then made for change in coloration of the particular pigmentin the heating with Glycerine. Dae consideration mast he given the flatting effect- of the heat on the paste, the change in the coioi1 only is considered. Each pigment 1b examined against itself. The use of the . standard is a check on the test and not on the sample under test. If properly conducted there will he no change (or at most a faint apparent darkening due to flatting of vehicle rather than of the pigment) with the standard pigneat. The discoloration, if any, may he reported on a numerical system using the standard light sensitivity chart in . estimating- G - Fo change Gj; " Very faint darkening or pink G Easily detectable darkening or pink Q2 .. Decided darkening or pink q ~ Considerable darkening or pink q 5 Salmon red oz' fellow red A test result of between G and G2 on 412 dry or 1526 dry appears to represent a satisfactory pignent for general usage. Stocks on hand manufactured prior to April 1932 may require a tolerance of Gpo Unless the conditions above specified as to the degree of light permi tted during the preparation of the sample are strictly ad hered to, the results may be misleading. --G* --G3 -G2 0007-SWP-000007304 SCHEDULE OT BXAMIHATIOff Ho. 87 Issued 1)7 Paint Research Division, Detroit, Mich, January 4. 1933 TESTIKQ OP DHT COLOR SHIPMESTS (Federation of Paint & Tarnish Production Clubs revised 11-1 32) APPARATUS & MATERIALS . 1,, Oil - White Defined Linseed Oil (Acid Ho., approximately 4), 2, Balance > Regulation. Laboratory Balance' 3' Burette *> Accurate one cubic centimeter burette, graduated in tenths of a cubic centimeter, or the apparatus known as the Brown Burette* 4- Muller To hare rubbing face of from 23/4" to 3*. lace to be free from blowholes and flaws* 5. Bobbing Surface - To be lithographer7 s atone or Polished Plate Class Slab, that has been ground to a satin finish with a nailer and fine emery flour wet with kerosene* 6* Tinting and Strength Tests - (a) A standard Zinc Oxide paste in oil in --tabes for colored pignents , (b) A standard Ultramarine Blue paste in oil in tubes for white pignents* 7. Balanced'watch glasses or counter balanced weig&ng pans* 8. flexible spatula for mixing oil and plgnents (3* blade). 9. Trench scraper or body glass scraper * with true edge (3" to 4" wide).. 10* Bright tin panels or clear glass slides (for exhibition of color daubs) EXPLAHATIfiH. 1. Oil - White refined linseed oil with an acid number of approximately 4 is generally acceptable for white and colored pineats. Sons pineata particularly earth colors hare a slightly greater tendency to flood in refined oil than when milled in raw linseed oil. The use of two rather, similar oils would call for additional equipment and be the possible source of error, so for simplicity we suggest the general use of refined lia> seed oil. It is necessary therefore that all colors should be examined imaedi&tely after haring been placed on slides.- Oil should be changed frequently. The use of bodied oils or varnish is essential for sows trades. * This point is one that should" be arranged for between the indi vidual buyer and seller.- 0007-SWP-000007305 N12904.1 SCHEDULE Or 2XAMIHATIC Vo. 87....* 5HS3T 2 3. Balance ~ Should /be the regulation laboratory balance, sensitive enough to be accurate to three decimal places,- To be used In wei^ir^ dry plgaent,, oil and redaction or tinting pastes. * 3 Burettes Should be either standard one cubic centimeter burettes, gr^d' unted in tenths of cubic centimeter, (pet- cock controlled) or the apparatus known s the Brown Burette, which consists of n suall reservoir to supply the burette. Tills burette is - noted in tooths of a cubic centimeter and is stop--cock con trolled. Tie tips of all burettes should be ground optical1" flat-. Ko dropper3 or weighing bottles should be used. 4. Mullers Should be of the standard typo cn the market with grinding fees of from 2-3/4* to 3* diameter. The fo.es should be frc from blow ..boles end other imperfections. Hie use of "weighted" crullers is not recommended- 5 Rubbing Su-facea Should be lith.ogr&rhsr s stones or Ground Hate Glass Slabs., the surface of which are kept sharp by sand -blasting alien necessary. Different slabs or btones should be available for RED. YSLLCST, BLUE hHSSlf, BLASS and 'TOITB. if ot all possible to guard against contamination. 6. (&) Tinting *>nd Strength Te^te should be made "using (a) 2inc Oil Paste for colors. Secoixaended formulae for white Zinc Past*;-EJ ther 1- Sy?7 Green Seal Zinc Oxide 64? Poppy Oil 2# Calcium Stearate 1# Turpentine Ground Fine end placed in small collapsible tubes, This formula yields r. mart paste-, handy to use and which has little tendency to settle. or 2 90? Green Seal Slue Oxide 10? Refined Linseed Oil - 1# 4 hear cooked Linseed Oil (560P) Mixture placed in tubes. Tills formula yields & paste, that is sli^itly stringier than #1 and settles very little. Seme manufacturers prefer the use of Zinc Oxide ground in "G1or "000" lithographic nil. 6 (b) Tinting 4 Strength Tecta for shite pigments chould b sal# using (b) a blue paste in oil- Recommended formulae for ths . blue pastes- Zither 0007-SWP-000007306 SCHEDUL3 QT SUU1VATZOV STo. 87..................................................................... SBSST 3 lo 140# Ultramarine Blue ~ SO# Poppy Oil 3# Calcium Stearate 2# Castile Soap l/2# Turpentine Ground fine and placed la small collapsible tubes. This .formula yields a short paste, handy to use and which has little tendency to settle. or 2. 70# Ultramarine Blue 27# Refined linseed Oil 3# 4 hour cooked Linseed Oil (560J) This formula yields a paste, that is slightly stringier than #1 Blue formula. . .. iffhen running the tinting tests or strength determinations blue or drr white plgnent should po$ be added to a smiled sample under examination, as this calls for additional mulling, to incorporate the tinting pigpent. The objections to this method of procedure are as follows^- 1st > A waste of time and energy 2nd - Additional smiling may develop color that 1b unobtainable in the plant. 3rd This is coatrazy to geaezal plant practise of tinting- It is also considered a waete of time to weigh up and rub out portions of the contrasting dry pignenfcs-- for instance, a dry sample of a white shipment and dry blue. The shite has already been rubbed up for shade and is available on the slab in paste form for tinting purposes. Then again the hardness of each pigneat must be considered when dispersing color. 7. Balanced watch glasses or counter- balanced weighing pans * should be used in weighing out the samples of dry colors, oils and pastes. Tor regular control work we recommend the use of the burette in measuring the oil used Instead of the scale because of the simplicity, speed and tolerant accuracy of the buretts. In case of doubt and dispute over any color, all portions should be weighed. 8- -flexible spatula for mixing oil and plgnent should have a three inch blade. 9, Trench Scraper or Body dazing Scraper0 should be used in smoothing down the color daubs that are placed on the glass or tin. so that both Bhijmont-and standard ere seen on the came plsne.. Scraper should ha?e a blade that is about 33 or 4 wide wi'h a good straight edge* 0007-SWP-000007307 SCHEDULE GF2XAMIHATIGH Ho. 87 SHEET 4 10. Bright Tin or Clear Class Panels should be used for observing color matches. If glass is used rub outs should be observed from the top and not through, the glass for we are interested coinly in how colors look on top. Looking at the under side of rub -outs on a glass panel is useful if properly inter preted. It should sot permit to modify o&es judgement of a color as made from the top aide. HggQJ> JO BS 20J&CWEP IV HJBB.XIKJ Ogj PIGUEST3*. Carefully weigh out sample of pigment to be tested and counter--balance with the standard sample. If oil is to be weighed, add oil to the dry samples accurately. Transfer the mass to the rubbing slab. If oil is to be measured, transfer weighed sampleo of the pigments to the slab and add oil by dropping (slowly) frem the burette, working up paste with the small spatula all the while. Be-sure to allow enough time for burette to drain to its true level. When ell dry pigment is worked up by means of spatulaf the mass should then be mulled. The stoke should be from 3 to 4 inches widef and from 12 to IS inches in length. In counting rubs given a color, one stroke up and one stroke back is considered pne, - sot- two pubs. Muller should be allowed to traveler up'one side and back the other side, twisting xsuller slightly at the top and bottom of each half stroke t-o help work the pignent in. A pigment demanding 300 rube shall he "picked--up* after each 50 rubs w " 200 " w It NN 0 *40" " 100 " * ba H 26 M w 50 *w n IS " By "picking^np" we mean that face of auller shall be scraped with the spatula and the paste on slab gathered up in a daub once again. Then mull ing is started once more. When mulling is completed, shipment and standard samples are placed in juxtaposition*on a dean piece of bright tin or dear glass. Daub shall be about two inches long and at least an inch wide. Eie Trench "Scraper shall be lifhtly drawn down over the pastes to even off the ridge and so present both, daubs on an even plane. Mass tone should be judged immedi ately. Observation for floating, bronzing, etc., should be taken note of after 2 or 3 hours, if this fact is important to the consumer. Tinting Value or Seduction should he run ad follows:-- Weigh up the re quired amount of the mulled paste from dab and counter-baluice with the standard sample. Than add the correct amount of the "Seduction Paste" tr- ehipment and counter-balance. Best thoroughly Hi* the pastes on the watch glass or weighing pan and transfer samples to the slab miming them thoroughly with spatula only, till no more streaking is noticeable. 0007-SWP-000007308 SCHEDULE .OF 2XAKIHASIOH Ho. 87 SHEET 5 Transfer samples to the tin or glass, placing then in Juxtaposition, ds.nl> 'being about 2 inches long end at least an inch wide. Snooth down with the French Scrapvr and Judge color lmrediatelj. strength'tests shall he made in a similar raannei to the reduction teste except amaunts of reduction pastee ox mulled pastes of shipment'-re regivLatsd es ia necessary Color f% w* .fl. -' - i nci-sirr h u p- c u t s c h eme Grans of Color c.c.. of 9t\ thills or Pb*_ Be&uction .Grama of Deduction Tests to Grams of Mvxl C..F. Iron Blues C TP. Light * Medium Inra Toner r. C P IVrfc Para Toners 10$ Para Toners on Hhlting C P.. Toluidlne C P. Light Chrome Gresn C P Med. Chrome Grrm C P, Deep Chrome Green 25$j Grinder's Creen Light* 2Z4> Grinder" s Green Medium -25< Grinder's Green Deep C.P Chromium Oxide CP. Primrose Chrome Tallow C P- Light Chrona * Yellow C P. Med. Chro ir . Yellow C,P. Park Chrome Jellow C Pi Zinc X'Vl0* "English Yertail. VI .remttrine Blue Cobalt Blue nlrh Strength Carbon Black Bone Black 10 080 0.5 0 80 0 6 0.80 1.0 0 50 0.5 0 50 1 0 0-40 1 0 0 50 10 0 60 1.0 0 30 1.0 0,40 1,0 0.40 2,0 0 40 loO 0 20 10 0 50 1.0 0..30 20 0,40 1,0 0-40 2.0 0 50 1,0 0,00 1.0 0.50 0.3 2.80 1,0 0.80 300 200 3C0 50 150 100 150 200 50 50 75 50 50 50 50 50 50 ICO 150 150 150 100 5 . cl 5 .1 5 a 2 .-l 5 .i 2 - -i 2 .i 2 -i 2 3 i 2 -> a 2 * .i 2i ) , . s 2 > .1 e* 9* 2 -l 2 oV M k ,,l 2 v .1 p cl 2 - ..1 0007-SWP-000007309 qg* v t i> ) r*; ." S* ,s s:i' * *. - * SCEZDOLS QT JXiMJMSIQB Vo. 87seoeoooeoeoeo / . r-vfr' -Y: ^* -'p .- Color or Class . . * - Grams of Color C.C. Malls of or v* Bednctlon-Grams of Bednctlon Paste to Grans SOfe&lfiOfisla Leap Black Carbon Black Territe Tellow Trench Tellow Ochre Indian, Spanish;, Venetian, Persian and light Bed Oxides Baw & Bt. Sienna Baw it Bt. Umber White Leads Zinc Oxides 355* Leaded Zinc Titanaz Titaniun Dioxide Cryptone Lithopones v Zinc Sulphide 0.3 1.00 0.3 1.30 0.5 ' 0.30 * 1.0 0.50 100 iso 150 150 2 - ,1 2 - .1 2 ,1 2 - .1 2.0 0.60 1.0 0.60 1.0 0.80 2.0 0.40 2.0 0.60 2.0 0.40 2.0 0.50 2.0 0.90 2.0 0,50 2.0 0.50 2.0 0.60 150 2 - a 200 . 2-.1 200 2 -- .1 100 Per whites nse .1-4 100 Ultramarine Bine .1 - 4 - 100 Bednotion Paste .1 ~ 4 100 .1-4 100 .1-2 100 .1 -- 4 100 .1 - 4 100 .1 - 2 V 0007-SWP-000007310  V/.** &- ``*'i IfV -' -0; ' 2.Vwr5'*&+4t T- 8CHZDPL35 gy JernmnmrcM Wo. 9L'J r .4 ~ " ' ''- ;''?? ' - Issued By .-*%;. -*\< ' ' Resseeaarrcchh. UDivlistironla. l^o...yn,_ "- y V"-'': Detroit, Michigan ";'*'.&'.r%/^ '" ''* ' Jane 15, 1934 DRYING QUALITIES OT SiMI-lIgTIBG OILS vX STATSMEHT Because of lade of constant temperature, constant humidity and constant illumination facilities, drying tests - especially if pigmented are made on a comparative Basis using a standard oil. Drying tests made By pouring the semi-drying oil on a vertical strip of tin results in such thin films that important differences which would occur in a pigaented product, are difficult to evaluate. In order to spread the drying interval so that dif ferences in drying qualities Become more noticeable, a pignent was selected which retards normal drying, vis* ferrite Yellow Light, having no calcium or soluble iron sulphate salts. 2. MATffiTAT.S (a) - Soybean Oil standard, Preserved from contamination and oxidation. (B) - ferrite Yellow (Light) Standard* free from calcium compounds. Contains 86.5JC TegOg equivalent and not more, than 0.002/C soluble iron salts or l.OjC (803). (c) - Ground class plate or stone slab. +.<fc ' (d) - Glass mailer having a face of approximately 3 inches ; diameter and weighing about 1-3/4 IBs. .<s (e) - Burette measuring to tenths of cc*s. . (f) fin strips 6-1/2* x 3. '%[''[ " # *v (g) - Steel spatula. (h) - Prepared standard drier solution, 5 gallons of uhicih has the equivalent active metal Lead and Manganese content t of 2 gallons (31). 5 4 0007-SWP-00000731X N12904.ll 3. PREPARATION OT EBHB Any desired portion . _ formula can be accurately made upland preserved in, mall, _ ;r_ _ closed glass containers, kept in:ihe darks . .,yJHga^^ML.'w 1*55 lb. of metal Lead equivalent, obtained from Soligen or Buodex Lead Solutions. -><7? , 0.051 lbs. of metal Manganese equivalent, obtained from Soligen or Haodex Manganese solution. , w Turpentine balance needed bo complete cfoxmula onJ5 & m*VV X-, t X'tSi-L. 4. PBOPOBTIOBS' OF ESIEB IPD OIL '? A* Sr- .r .- .J&' *r . tvr^mmsme Tlve volumes ..measnred from a ' b-n. retAt*o* >'~ oAf above _ " m' ' are thoroughly mixed with, 95 voltmea of Uxe . oil^oLbe evaluated, imaediately before incorporation with the pigaeti>|;. : . ; -* *v> 5. SHTBDCTO PB0C3D0RB 'T" ? ' 1^3 13 co of the Oil-Drier mixture' are added to ;5 grand^' Ferrite Tellov Ligit and moiled 25 times irttk^oalj&a gentle rpressQse^i^l| 6. PAIHT..QPT AMD DHTIBO PSOCflDURE >; f . * The paini prepared' as above is spread, on a cleaned^^hjet^ of Ma 5-1/2 x 3" and spun on a rapidly rotatingjiisc ihfteuch'a^ftJ^^ ner as to` produce a film thickness of 0002 im&|.*i.If fsolli.ti.ea&^pg^^l-^f for spinning are not available then bruah out^^^^roajttatel^ti^'-^^l^^V ''* specified thicknesso Place the standard panel prepared au above vhidh seryep . as the etandardi for-comparison oL^dryiag'^l^^gSpf^^^bn^^pftiga * panels of the oils to be evaluated in a well lighted, well-vent .Mated, place,. free from excessive'.dust and note the time.: . -K,V'j- .'.j.S)&fr. 4i .. - . ^*^*A9*S 'M- '1^.. M :i;i lAj '.j , ; v. -3"& ,:4 ... *.. ; 0007-SWP-000007312