Document 2jJYLV9VyDeBqEqmLRDKNvEV5

E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK, NEW JERSEY Copy No. 1 Numerical File I >= \' NEWARK PLANT PIGMENT COLOR RESEARCH REPORT PROGRESS REPORT DEVELOPMENT OF A STRONG G-550 LINE OF CHROME GREENS Period Covered: JANUARY 1, 1948 t JUNE 1, 1949 FILE: 214 DATE: n/xf/42 N42216 Copy tot 1 - Nuaerical Pile 2 - Research Offlea <214) 3 * Library Fila <214) 4 V. Chalupski - Plant Files 5 - D. 1. Killian, Newark 6 - Extra 7 - Extra Strial So. KH-49-35 Copy So. 1 NEWARK PUNT PIGMENT C010R RESEARCH REPORT PROGRESS REPORT TITLE* DEVELOPMENT OF A STRONG G-550-D LISE OF CHROME GREENS. PERIOD COVERED* JANUAHX 1, 194$ JOSE 1, 1949. ClARGEt 1101-11-4 SUBMITTED APPROVED BX* DATE SUBMITTED* 7/26/49 DATE ISSUED* 11/15/49 -A DUP050067367 -2 i This report summarizes the progress made In ail attempt to improve the strength of our 0-550-D line to equal the strong lines of Imperial, Relchhold and Calco. Considerable difficulty was encountered in this problem, because of the complications arising from such factors as definition of objective,which frequently was changed, and obtaining of satisfactory tinctorial requirements without exceeding the blue content limitations regularly established in current chrome greens. CQHCLlfS IOSB i The use of sodium fluoride in place of sodium chloride in what is essentially a X-493-D process has provided a method for manufacturing chrome greens fully as strong as the strongest com petitive pigments, without an appreciable digression from the characteristics of the 0-550-D line. Prospective 0-550 and G-551-D standards have been submitted to the Sales Division for evaluation* SUMMARY 1. Proposed standards for G-550-D and 0-551-D have been submitted to the Sales Division for evaluation* These products compare (by H-108 linseed oil rubout) with our existing standards and competitive pigments as follows * CODS LOT 0-550-D* WJHS G-551-D* WJHS 0-550-D <x) G-551-D <x) Imperial's A-4442 90595 90596 SD-48494 SD-48486 m0# 50231 50256 5.84 10.37 5>*28 9.69 6*05 6*30 (x) See latter HAW * WPS, Oct* 15, 1948, for discussion of blue content of standards* m Iff L/F 90595 vs 0-550-D s*lt*,s*yel. 91*100 Std. vs.yel. vs Imperial A-4442 G# ~ v.blue 97100 0# blue better A-4462 C# 5' v.lt.,s.int., t ' we. blue vs.better al.clean :!W 90596 vs 0-551-0 s.dk.,s.yel., 88|00 Std. S.< vs 3W**rlal-^5 A-4443 G# 5156# v*vlt.,v.vyel A-4463 C# 51219 vs.lt*,s.yel*, 92=100 C# '* r" / . V. , .SvlfitW'-; C# 51356 s.dk.,s.blue, +92=100 - . int s.blue s.dull v.blue s.worze better ve.bettsr DUP050067368 Current standards compare with these competitive pigments as follows! STB. TIBT iff L/P 0-550 vs Imperial A-4442 C# 51273 s.dk^blua, 110=100 C# blue better A-4462 C# 51385 It.,blue, v.Int. 110=100 C# blue vs*better 0-551 vs Imperial A-4443 C# 51548 v.v.lt., v.v.yel. better A-4463 C# 50219 It* ,v* lnt 103=100 C# blue better 2* A Shading fellow coded Bf-561-0 - 90298. has been set up as a prospective standard strong f-493-D type Shading fellow* It compares as follows with recent f-493-0 standards by varnish drier rubout* 90298 vs f-493-B SD-(86721) Sp 7(48184) JBL It. ,gr. s.lt.,gr. Slit 97=100 95" 100 green rdd" n m better vs.worse 90298 vs f-493-P (48184) v.lt. O.K. fel* ,s. int. * 3. Pro-mixes designed for Muench mix manufacture of the following codes have teen set ups COPE 0-562-D Proposed Mix gal?glutJsa&aiiS H-108 Tinctorial Properties vs Standard Iff STft. TIBT Bf-561-0-90298-76*Of Y-442-D-60570- 2.5f B-269-0-89531-21*5f 20* 5f vs.blue 86=100 Std. s*blue COPB 0-S52-P Bf-561-0-90298-66.Of f-442-0-60570- 7*Of B-269-B-89531-27.0f 25*7f s.lt.,v.al. 91=100 v.sl.yel* blue,int* COPB a--p If-561-0-90298-532f B-269-0-89531-46*8f 44.5f 8.It., $9a100 s.blue,int* = DUP050067369 4. A single attempt to manufacture G-552-D ana Q-553-D struck greens st the 5 ol batch else was unsuccessful, the products being dark and dull when compared with standards* G-552-D and G-553-D. This was determined as being partly the result of the difference in quality of the 87-24 blue utilised in the struck greens as compared with the B-269-D standard utilised in the proposed *Muench Mixes *' A five percent reduction in blue content was found necessary and desirable when the 87-24 was compared with 8*269-8," 89531. 5. A modification of the fluoride content of the Shading Yellow process <50 lbs* in place of 64) utilised in the above batches was attempted in the plant* She Shading Yellow obtained was converted into a green in the laboratory with satisfactory results* Ho dullness of masstone was apparent* 6* A plant mix coded AG-6?6-D, lot 99450* was submitted to the Sales Division as a match for Imperial's A-4464, C 50441* By H-108 linseed oil varnish rubout, the product compared with the C# as follows* Mix vs C# m vs lt*^blue m* 3-4 str. tm yellow m ws worse fhls mix was rejected by "Sales" because of tinctorial variations from competitive products* 7. A board mix consisting of 42,8* a-552-Di 13.5/? 0-550-D,; 39*058 G-604-D, 4*7)6 Y-424-D SD-48418 SD-48494 SD-48054 SW-9361 was accepted as a basis for Sales Service laboratory work in an attempt to match W*P* Fuller's He.43 green, 00 50893. 8. The use of 1% "Sotex C" cationic agent in conjunction with 1% of "Hulsor 3 CWM was investigated briefly as ah anti-flooding agent* It was found to be effective when added to the yellow slurry before "bluing1* Greens prepared in this fashion flooded less than untreated controls as evaluated in H-108 linseed oil vehicle* Yhe effect was applicable to dry blended or struck greens* 0 9. An attempt was made, to standardise a strong G-604 line Shading Yellow, coded(GB^>7S-0* for use in matching Imperial's A-4464. this was dropped whi*en the necessity for Its use was discontinued* fhis product was originally ceded <A)Y-579-D. At the time ef issuance of the standard formula, the Quality Control Group requested that the product be eeaed (cJ#-572*8. DUP050067370 10* Several attempts sere made to manufacture more satis factory shading blues than SP-24, ''Potash blues", Nickel-containing blues", ferric chloride oxidised products, nitric acid oxidised, and air oxidised blues were studied without success* 11. A total mill cost penalty of $.40/100 lbs. results from the use of sodium fluoride In the BX-5613) process. Penalties of $.36/100 lbs. and $.34/100 lbs. art applicable to $0-550-9 and $0-551-9 respectively. (Assuming no blue cost penalty, see letter j.deh.K. - W.F.S., August 18, 1948). The possibility of patenting the use of sodium fluoride In Shading Nellow manufacture was considered. A review of the literature revealed no strictly analagous use of F*, although Earshaw patents British 416,744, Sept. 20, 1934, and 9,8, 2,044,244, June 16, 1936, suggest the use of hydrofluoric acid, fluoroboric acid, or fluorosilicic acid as solubilising agents during the manufacture of lead chromate from lead oxide end chromic acid or sodium bichromate. See letter AJ6 - NFS. July 22, 1948. Some use of Nat had been made at Newark but no product was manufactured using this agent as a standard ingredient. The patent situation la still under consideration. Chrome Greens have appeared on the market in the past three years manufactured by Imperial, Reichhold, and Calco, which are substantially stronger than our existing G-550-0 line. The Sales Givision reported significant competition from these products and requested that an attempt be made to match the best of the competitive pigments. No specific request to match any given competitive product was stated when the program was initiated, A review was made of the quality advantages of several of these competitive products end the "Vale" Green line of imperial's A-4442-4446 wtre determined as being the best of competition. Strength advantages ranging from 12j? Versus G-550-9, Si-48494, to 6% versus 0-553-9, $9-48483, were noted when the greens were adjusted to equal masstone depth. The competitive products were considerably yellower In masstone and tint than our existing G-550-9 line, being intermediate between the G-550-9 and G-604-9 lines. The strongest competitive products,regardless of manufacturer, contain higher percentages of iron bins than our existing G-550-9 line. Ths lightfastness of these products was, in ganaral, slightly inferior to that of our G-550-9 line standards. Attempts to match the masstones of the "Vale" Greene by mixtures of G-550-9 and G-604-9 lines, or by use f other means of obtaining olive masstones, were unsuccessful, S' DUP050067371 the mixtures being dull In masstone versus the competitive products* It was apparent therefore, that a substantial tinctorial modification of our X-493-D standard mould have to be made if a match for these competitive products was to be developed* Subsequently during this program, "frales* requested the matching of specific competitive codes such as Imperial's A-4462 and A-44&4, and W.P.Fuller's So* 43 Green <C# 50893). When it became apparent that no single Shading fellow would be satisfactory for matching the tinctorial properties of the various Imperial Greens, the matter was reviewed with the Sales Division and it was decided that the goal of this program should be the manufacture of greens similar to our current 0-550-D line, hut with strength advantages at least equal to the competitive products* The objective of matching specific competitive products was temporarily abandoned* ''Wet struck" 0-550, and 0-551 type greens wsre to be developed, along with a Shading fellow standard for use in manufacturing "fuenoh-mixed" 0-562-D, G-552-D, G-647-D. G-553-D. This program was well under way and standard formulas written when "Ifuench-mixed" greens were abandoned on hay 11, 1949* fork was then started on the setting up of struck G-552 and G-553-D standards to replace the formulated dry blended mixes Mtoptp.. M hatch Gmna ! Wr.ft Considerable effort had been spent by the Sales Service group in setting up a match for W.F. Fuller's #43 Green standard 10# 50190). A match (coded BG-663-D) composed of - G-605-D G-551-D G-552-D Y-442-D was submitted to "Fuller" and was accepted* When the plant was requested to make this material from typical production, they were unable to do so because of current strength deficiencies in the G-604-D line* The Seles Division requested ms to look into the matter of developing a practical match* Rubout work indicated that the use. of a strong Y-493- typo Shading fellow (Bf-5bl-D), in conjunction with a strong G-604-D type yellow both of which were under development at the time, would eWercooe the previous difficulties* The problem was then dropped pending the receipt of a new sample of "Fuller" standard end testing vehicle. DUP050067372 Upon receipt of the new standard <0# 50893) work was resumed, and a change in '`Fuller* standards detected, BG-663-D was no longer a suitable matcht and in addition was strong versus the competitive material* A mix consisting of 42.8# G-552-D. SD-48418 13*5# 0-550-D, SD-48866 39.: % G-604-D, SD-48054 4.7# V-424-D, SW-9361 was then presented to the Sales Division for consideration. This mixture was considered sufficiently close to the competitive pig ment to Justify returning the problem to the Sales Service Laboratory* Similar material coded 0-677-D was subsequently submitted to the Fuller Company and was accepted on a tinctorial basis, but was rejected because of cost considerations. REFERENCES: 1282-37. 45, #1* Inorganic Research Summary June, July, 1948* 2. At "Sales* request, the problem of matching this code was v started* A review of available samples of this competitive code was made, and exhibits versus our G-550-D standard and tha proposed fluoride matches were shown to the Sales Division* The Imperial Greens were much darker, yellower and duller than our G-550-D standard and approximately 12# stronger, the fluoride counter-offerings (of the time) were of comparable strength and much more intense compared to the Imperial product. "Sales* dropped Its request for this match on reviewing the above mentioned exhibits* 3. A match for this product was requested around 6/1/48. So specific 0# was mentioned and our examination showed a very considerable variation among the products available in our files* This was brought to the attention of the Sales Division representative who approved the goal of developing a match for 0# 50441 (received from Old Colony Faint Company) because of the possibility of develop ing business with that concern, and because it was somewhat closer in appearance to our existing G-55G-D line. So specific vehicles wars mentioned and the rubout evaluations and attempts to match were conducted in Varnish Drier (the vehicle in use at the time)* DUP050067373 Evaluation showed the product to he interned late in properties to our 0-550 and 0-604 line of Greens* At the Sales-ProductionResearch Conference of 8/12/48, the decision was made to attempt a match by dry blending, (Prior to this, wet struck greens had been considered satisfactory) It is interesting to note that nous of the components AY-561, 1-269,ov(C)iY-572f> mere standardised at the tine* loard mines utilised a strong 0-604 line yellow and 0-550 line green, and standardisation of this code was requested (Coded(C0f-572-D) At this sane meeting, H-108 linseed oil was established as the new vehicle for evaluating greens* These activities culminated'in a plant mix, coded 0-676-0 - 99450 (9/15/48), which was evaluated in H-108 oil, and subsequently rejected by Sales because of dullness of masatone* See letters - WPS - 8HP - 9/9/48^ JJ - AJH - 9/13/48 EPS - RHP - 9/22/48 RHP - WFS * 9/27/48 The Sales Division then requested that we attempt to match this code for the Armstrong Paint Company in their official vehicle of the time. Spencer Kellog's alkali refined linseed oil* Evaluation of the G-670-P mix - 99450, In this vehicle showed It to be considerably different from @#50441. andsoma time was spent in attempting to match the product in this vehicle by changing the percentages and nature of components* This culminated in a hoard mix approved by Hr* Shrewder consisting of - it was subsequently discovered by a Sales representative that A-4464 was not used by Armstrong and the problem was dropped around . 10/5/48* WllJMMi ! gjftiDlftmJBJlOt Because of the desirability of lowering the Kjeldahl nitrogen values of our greens (see subsequent discussion), an attempt was made to utilise blues different from our orthodox SF-24 type (dark masstone Milori Blue) for the purpose of producing shading blues which could be manufactured into greens containing lower nitrogen contents. The first attempt involved study of the use of potassium blues in place of ammonia blues. DUP050067374 9 Various experiments were run utilising potassium chloride, and potassium sulphate in place of ammonium sulphate, substituting on an equivalent basis in B-216-D type of process, Variables were studied for producing light or dark masstones. On an equivalent basis, the products obtained were very light in ma&stone and very weak in tint, When comparable mas stone depth products were obtained! a 10$ to 15% deficiency in strength of the potassium blues eras noted, Shis low strength/masstone depth relationship proved to be unsatis factory for this application, an actually increased quantity of blue * being necessary to obtain comparable masstone greens, with no strength advantage. See References - HB-1282-40, 41, the knowledge that so-called "under-oxidation" of blues, that is, less than one equivalent of oxidant per mol of sodium ferrocyanide, will produce stronger blues, is fairly well established. It was felt that the use of a stronger tint blue (like stronger shading yellow) might be reflected in the production of strong tint greens. Working with this hypothesis in mind, attempts were made to obtain blues stronger in tint than the B-216-D type. In addition to under-oxidation, variations in type of digestion, in type of oxidant (l.e., HNOq. NaCIO?, FeCl-j), use of nickel in place of some iron, reverse striking, and method of addition of oxidant, were studied. Son# of the products obtained were found to be significantly better than SF-24 (K-1487). It is apparent that for shading blue into greens, a specific relationship of masstone depth, strength, and blue is required. Increased strength blues. If redder in tint, are not desirable, making for duller tints which may bs weaker (depending upon strength advantage of the blue in question). Increased strength blues at correspondingly darker masstones are not particularly Useful since the masstone depth increase offsets any strength advantage* The ideal for this situation would be a stronger, greener tint blue of comparable masstone to that of our existing K-1487. This apparently Is a difficult goal to obtain. See N.B. 1282-42, 43, 44, 46, 49. i i mm MiMm (-57a-D) When work was started on the request for a match for Imperial's 4-4464, it became apparent that a stronger G-604-D (K-1735) type of Shading fellow would be useful. Previous work on a G-604-D sick list study,designed to increase strength of G-604-D line green, had indicated that a decrease in the amount of nitric acid in the strike (accompanied by a subsequent increase in the amount added after the strike) on the standard E-173? process, gave rise to stronger Q-604*X> DUP050067375 - xo line greens. This was accomplished thru the production of a slightly redder masstone, stronger redder tint Shading Yellow, Which required more iron blue to reach a given masstone depth green, these greens were stronger than those made on standard process.' A hatch of this type color coded AY-572 - 58132. made with an initial out of ljjr nitric acid (slth simultaneous increase in second nitric acid) had been found useful in hoard mixes for matching Imperial*a A-4464 Chrome Green, this was made the goal of a plant program designed to set up a standard for a stronger G-6Q4-D line Shading Yellow* A eode,(<i?*57!4>t was issued* the following hatches were made. Lot Humber mm&jtzM Standard 60132 SOSOS 60445 60446 160 lbs* 140 140 136 120 120 63 lbs. 88 8a 92 a the last two hatches were found to he comparable in strength at equal masstone depth to lot 58132* the poor reproducibility of these procedures may have been due to difficulties associated with the analysis Of the basic lead acetate liquor used* this seems to have been the ease in recent work on Y-524-D. See H*B 1281 and also 1305* Ho standard for this code was issued, since the necessity for it ceased when Sales dropped the request for a match for Imperial's A-4464 References! ff.B* 1274-2*30. BmiiiLm 1 CHROME 1 i* Mlgft..BhgBl?is.,gbaas-.l>,c,ad.,, fitowatt An early hypothesis concerning the obtaining of greater strength Chrome Greens was based on the assumption that the pro duction of smaller particle size rhombic phase crystals than that existing in Y-443-D would make possible the manufacture of the desired stronger greens* ?his was tested by adding Y-202-D or Y-524 <84577) K-1735 (G-604-D line Shading Yellow) to Y-493-S since the former are smaller particle size rhombic phase yellows* Unfortunately, the masstone of greens made at definite percentages of blue from the smaller particle size rhombic material are con siderably darker in masstone than greens of the same blue content made with Y-493-U as the Shading Yellow* this defeats the goal of obtaining greater strength greens (at any given depth) since the exdeamlve darkness of masstone requires a decrease in blue content In order to obtain the desired darkness, With consequent weakness of tint, the strength of chrome greens are very markedly affected by the content of iron blue as well as by the previously discussed effects of hue* %: DUP050067376 2. Use of Shading Yellows containing Substantial Percentages oftheMonaellni^Crystals An examination of Imperial's X-1945 light yellow (C# 48433) as a Shading Yellow led to several interesting conclusions. This material when examined by the electron microscope appears to be a mixture of the Khomblc and Monoclinic phases of leadi chromate and lead sulfate in solid solution. Comparing it with Y-493- as a. Shading Yellowy it consumes a higher percentage of iron blue to reach a given masstone depth greeny with the result that at equal depths the product was 15* stronger than our Y-493-D standard# Attempts to duplicate this effect by utilising blends of Y-493-D with Y-404-D, Y-405-D, Y-469} or Y-5Q0 were unsuccessful because of excessive dullness of masstones and tints# The successful manufacture of a yellow of the imperial X-1945 type might make possible a duplication of the Imperial ValeH line. 3. The knowledge that light yellows which are made with redder masstones and tints are usually strongex^well established. With this in mind, an attempt was made to apply variables that would produce such tinctorial affects in the Y-493-B process. In addition, the strong competitive greens were known to be yellower in masstone than our current G-550 line greens. Such variables as $ 1. Higher strike pH obtained by * A - increased sodium carbonate in white base. B - use of mixtures of sodium chromate and sodium bichromate. 2. Increased Chromate content. 3. Use of halogens to redden masstones. A - increased quantity of salt. B - use of sodium fluoride. were resorted to for this purpose. This work soon showed that the use of the sodium fluoride was the most effective strength improving agent despite the fact that some of the other variables gave 'ye^Osr*d1^h-'Wifer.fCOi3fflideiw^l|r redder. The quantity per mol uses is quite specific. In the laboratory maximum strength products were obtained when 15 grams of. sodium fluoride per mol of lead nitrate was Used (the fluoride being added to the bichrome solution). Quantities in excess of this amount produced dark, yellow and dull masstone greens# DUP050067377 The use of sodium fluoride In the laboratory yielded Shading Yellows which were slightly redder in mas stone and tint, and stronger than the control products made without the use of fluoride. They consumed Increased quantities of Iron blue to reach a given mas stone depth,grm&the tints are correspondingly stronger* This effect is directly proportional to the quantity of fluoride used (when evaluated as green of 20# blue or 1ess). Strength advantages of 18-20# were obtained In the laboratory processes (when blue contents wert disregarded), and comparable masstone depth products were rubbed out against the standard G-550-D line. The quantity of sodium fluoride necessary for optimum strength, considering also the hue of the masstone, was found to vary with batch size. In the semi-works, 10 lbs. of sodium fluoride per mol of lead nitrate was found to be comparable In effect to the 18 lbs* used in.the laboratory# The quantity of sodium fluoride used per mol in the plant (12-6/7 lbs./mol lead, nitrate) was a compromise designed to meet the requirements of effect of batch size, hue of masstone and tint, the necessity for strength advantage sufficient to overcome the strength discrepancies of our current G-550-D line versus competition, and iron blue content limitations upon which price ranges are set# Sales Division policy dictated that no blue increases above the maximum limit of 6# for G-550-D, 11# for G-551-D, etc#, would be tolerated# Electron micrographs do not reveal any visual effect upon particle size or shade resulting from this use of F* on Y-493-D* it is interesting to note, however, that F* can be detected in the Shading Yellow after its manufacture* mMmKuauM&afo After demonstrating in the laboratory and semi-works that the fluoride variable would provide a means of obtaining the necessary strength advantages, preparation of actual plant struck G-550 and G-551 products, as well as fluoride type Quench mixed*' G-562-D and G-647-D, was undertaken at the request of the Sales Division# (The latter were prepared in the Sjpmi-Works mixer)# These products were prepared and submitted to "Salas'* for evaluation* See - G-550-DNS - 88713 G-551-DNS - 88714 0-562-DSS - 9753 0-647-DNS - 9763 After reviewing the results of rubouts and alkyd grinds of these products, standardization of the fluoride type G-if^D line was requested around 2/20/49* See latter OHM - WFS, 2/14/49) DUP050067378 n Sines G-562-D, G-552-D and 0-553-D warn to be made by dry blending in the Muench mixer, a standard Shading Yellow (coded BY-561-D) was set up* An equal part mix (90298) of each of five lots of BY-561-8 - 64982, 65244, 65399, 65094. 65400, was approved by the Production Division as a prospective standard and was sub mitted to the Sales Division for their evaluation* This mix compares with Y-493-D standards as follows in varnish drier vehicle* JSL st b. fisf yy 90298 vs Y-493-D (48184) s.lt.,grn. 5% str* red vs Y-493-B (86721) It. | grn. 2-3Jf sir* grn. v.si.worse* better* *Iote 90293 and 86721 contains 755$ of tin crystals used in SB-48184. Proijtixas (previously tabulated in conclusion section) were developed utilising this Shading Yellow, B-269-D, and suitable "diving" agents for use by the Plant Development group in making Muench mixes for G-562-D, 0-552-B, G-647-P and G-553-. The promixes were approved by Sales. (See memorandum for files BHP 4/21/49 Strong Chrome Greens). These mixes were prepared by that group$ however, since the decision was reached about May 11, 1949 to abandon Muench mixing, they were not submitted as prospective standards. Simultaneously with the development of the Shading Yellow, struck batches of G-550-D and G-551-B were produced using the standard fluoride Shading Yellow formula and adding the necessary amounts of blue liquor to give a masstone approximation for tha G-550-D and G-551-D standards. The plan decided upon was to make light masstone G-55Q-P and dark masstone G-551-D from which the respective standards could be set up at the desired blue contents. Lots G-550-DHS - 65111* 65245 65411*** G-551-DHS - 65429** 65467 Used 140 lbs. blue liquor. Used 320 lbs. blue liquor. Considered out of line because of operating difficulty. These batches were approved for reproducibility by the Production Division and mixes of each code were prepared. 0-550-D* WJKS - 90527 G-551-B* fJHS - 90525 KCB-52 bine content 5*0% KCR-52 * 11.45^ DUP050067379 -- 3.4 * Suitable blende of each of these mixes were determined for matching the 0-550-0 and 0-551-0 standards# Q-550-D* WJNS (9059?) cone Isted of $7*6% 0-550-D* WJKS 90527 12.4^ 0-551-0* WJH8 90525 0-551-0* WJHS (90596) consisted of 17.2* G-550-D* WJBS 90527 82.8* 0-551-0* WJHS 90525 Readings of these final mixes versus current standards and competition have been previously listed under the section entitled Conclusions. Attempts to match 0-552-0 (66394) and 0-553-0 (66395) were limited to a single batch. A batch of struck yellow was made by scaling down the seven mol proportions (used in BX-561-D and struck 0-550, 0-551-0) to five mols. This was split in the vat and to each half of the slurry sufficient iron blus added to make a 0-552-0 and 0-553-0 depth green. (275 blue for 0-552-0 and 475 for 0-553-0 respectively)# The blue contents were determined from the Muench mixing requirements for these codes# The batches were unsatisfactory being very dark, and dull in masatone,and extremely strong in tint# An attempt to attribute this behavior to inaccuracies in blue liquor usage was found to be unfounded. However, a portion of the blue liquor utilised in these greens when dried out and compared with B-269-0 - 89531 (standard) as a shading component was found to compare as followst HT STR. TIHT 6o5 X-493-B (48184) blue liquor vs 405 Blue B-269-0 V.dk.| 3 str# s#blue. It was found that a five percent reduction in blue was necessary to compensate for differences in behavior between blue liquor and dry B-269-0. A second batch of Shading fellow was made decreasing the sodium fluoride used# (Because of the previously discussed effect of batoh size on fluoride requirements* and the belief that too great a quantity may have been used). See Sf-56l-P*RS - 66520# Struck greens of the 0-552-0 end 0-553-0 depths were made from this slurry in the laboratory* These products when evaluated against 0-552-0 and 0-553-0 were considerably lighter and more intense than those made in the plant at the higher fluoride level# The final comparison showed the 0-552-0 products to be intense and blue in masatone vs 0-552-0 at equal depth# The product made to match 0-553-0 was somewhat bluer and duller in masatone than standard 0-553-0* DUP050067380 She problem ess then transferred to Dr* Morrison with recommendations to modify the Ion fluoride formula in an attempt to obtain greater coreness of masstone* EllLffl' Work on this problem is being continued by DrMorrison. mmmm 1 *,KH-48-1 2 - DSH-49-31 3 - H.B. 1282-13, 14, 15, 17, 18, 20-26, 28-5?* 4 - M.B. 1319-1-3 DUP050067381 - 16 PMS03>2 NaF Ka2804 miaftiyyy^ 165*5 gr. iii 3.4 liters water at 4.6 pH 80F Add - Stir 15 minntea exactly 20 gr./200 oo Add la 20 minutes 62 gr. 7.5 gr* 5*0 gr. in 3 liter 4.6 pH Add with 2 minutes - Stir# SnClg.2HgO Ba2C03 to pH 1.5 gr./20 ml 13#6 gr./36 ml 5.1 5 gr./40 ml a i2(s o 4)3 s h 20 ' :i2 gr./-2 .ml Stir 10 minutes Flood to 8 1*8 - Draw 3 waters A12<S04>3 3 h 2 10 gr./lOO ml SaClg-aSgO to pH 1.5 gr./20 3.4 gr./30 ml 5-1 DUP050067382 B Humber H-3 N-8 H-10 H-15 H-26 llw to 8-33 N-41 N-?2 H-64 N-108 H-262 N-360 N-416 H-484 H-518 Na2C03 Na2Cr20^* 2H20 Na2Cr04 2<s>3 18 h 20 SnCl22H20 h mo 3* 2 Pb(H03)a m (Pb(0H^)2Pb(Ac)2 Ba^ H C| H302 Ha2S NaF Sodium Carbonate Sodium Bichromate Sodium Chromate Aluminum Sulfate Stannous Chloride Acetic Acid Hitrie Aoid head Nitrate Solution Tannic Acid Basic head Acetate Sodium Sulfate Acetic Acid Solution Sodium Sulfide Blue Liquor Para Soap Sodium Fluoride DUP050067383 Cost Group - 4 U.S. Pat. 2,139,753 [B] fl$50"D RODE: KJ-U\1 Q 501*0 - tinA). 2291# Ye l l o w r ip f - 7 Hot, D1AZO VAT: COUPLING VAT: STRIKE VAT: 260.261 .262.267 aSw SSh IY: JJs 8" 10-49 JOH: 8-10-4$ HA: 0-16-49 "r CWP* 8-1749,.! VAT PREP 1. v-ww; w w .... ......... ^..rss NAME: "HY-CAP" CHROME GREEN INSTRUCTIONS USE LBS. f. WEIGH AND HOLD AT VAT 36^ FOR STEP IS 2. WeipH AND HOLD AT VAT -j65 FOR STEP 3O 3. We ig h a n d h o l d a t s c a l e t a n k 36( f o r s t e p 20 4. We ig h a n d h o l d a t s c a l e t a n k 361 f o r s t e p 21 5. We ig h in w o o d e n k e g a n d h o l d f o r s t e p 39 6. We ig h a n d h o l d a t a t 366 f o r s t e p 35 7. We ig h d is s o l v e in 10 g a l l o n s w a t e r in k e g . a n d h o l d a t s t r ik e v a t f o r s t e p 46 280 40 90 9J 28 7 28 N. c o pe a Cc t . L! 3 280 40 90 108 91 K~ ~ 28 lar 7 ... 15 28 s.v, 2. 13. Ru n 30-401* (+3000G.) w a t e r in t o s t r ik e v a t . 9. Ru n in f r o m s c a l e t a n k 360 " Fe M .T Fe 1 M T ' *' % 10, Wh e n u s in g v a t s 261,2^2, o r 26?, s e t a g it a t o r a t 20 RfH, I I. Ad j u s t t o 65h (5655G.) a t 73-7rF. ^~ 12. Ad j u s t t o PH 4.6-4,8 w it h N-7 o r N-33, Re c o r d : p H W~ n. Ru n 35-45" (+ I76G.) w a t e r in t o 3* 14. Tu r n o n a g it a t o r a n d s t e a m. f*5, Du mp in N-3 w e iq h e o in s t e p 1. v at lo. Ad j u s t t o 55" 1242G.) AT 80-120^. 17. St ir t o d is s o l v e * 365. "" 41 2317 4l 361 T 18, Ru n 15" (2990.} w a t e r 19. To r n o n a g it a t o r . JO. Du mp in M-518 w e ig h e d in t o s c a l e t a n k 361, in s t e p 3, 21. Du mp in N-108 w e ig h e d in s t e p 4. 22. St ir JO min u t e s o r l o n g e r t o c o mp l e t e l y d is s o l v e . 23. Ru n in M 24. Ad j u s t t o 29" (479G.J a t 74-76*F. T ' 1' 25.Ad j u s t t o p H 4,6-4,8 w it h N-7 o r M-33. Re c o r d : p H ` .Ma in t a in a g it a t io n in t a n k 361 u n t il e n d o f s t e p 38. *1 t ' . M-_fi________ S.V. 5- 26. Ru n v a t ^65 in t o s t r ik e v a t in 4-5 min u t e s . 27. St ir e x a c t l y 14-16 min u t e s . W 6. 28. Ru n 10-15" (+ 55G.1 w a t e r in t o v a t 365. 29. Tu r n o n a g it a t o r a n d s t e a m. 30. Du mp in N-3 w e ig h e d ih s t e p 2. 31, Ad j u s t t o 25" (HOG.) a t 8o -I20*f . 32. St ir t o d is s o l v e . 3^ 7, 33. Ru n 10-15" (+ 20G.1 w a t e r in t o v a t ^66. 34. Tu r n o n s t e a m. 3*5. Du mp in N-368 w e ig h e d in s t e p 6. 36. Ad j u s t t o 25" (40G.1 a t 80-I20*F. 1 1 37. St ir t o d is s o l v e . . . . .... i ... t. . . .................... * c o n t in u e d o n p a g e 2. DUP050067384 VAT Pa g e : 2 .Co d e : jgj ^j^^Les: 2291# in s t r u c t io n s ' USE LBS. NCODE ACCT. LBS. S.V, 8. 8 27 * . Wh en s t e p 361s t ir r in g c o mp l e t e d , s t r ik e s c a l e t a n k at 7H-76F in t o s t r ik e v a t a t 74-76#F o n t h e s u r f a c e in 19-2! MINUTES. Re c o r d ; To t a l min u t e s Mi sc, 9. S.V. 10. 363-364 ii. 12. 3^ 13. T9. 46. We ig h a n d a d d t o N-26 w e ig h e d in Dis s o l v e N-26 t r e a t e d in s t e p T9 w at er an d h o l d at s t r ik e v at f o r s t e p *5-w it h -40 g a l l o n s s t e p 42. 2 Ul. Wh e n s t e p 38 STRIKE COMPLETED, WASH IN SCALE TANK 361 imme d ia t e l y . 42. Po u r in N-26 p r e p a r e d in s t e p 40 a t o n c e . 43. Ru n v a t 365 in t o s t r ik e v a t a t o n c e in .-2-3 min u t e s . 44. Us. 46. 47. Sa mp l e f o r p H a n d h o l d s a mp l e f o r s t e p 47. Ru n v a t 366 in t o s t r ik e v a t a t o n c e in 2-3 min u t e s . Po u r in N-15 p r e p a r e d in s t e p 7 a t o n c e . 10St ir min u t e s .Wh il e s t ir r in g , t e s t a n d r e c o r d s t e p 44: pH . NORMAL 4.6-5.0 48. Wh e n s t e p 47 c o mp l e t e d . Te s t a n d r e c o r d : p H . NORMAL 4.9-9.1. 49. If n e c e s s a r y , a d j u s t t o pH 4.9-9.1 w it h N-3 o r N-33. 90. Te s t a n d r e c o r d : s l u r r y 9i. Fl o o d t o 89" (73950.). 92. Dr a w 3 w a t e r s a t 9 h o u r Re c o r d : p H col or in t er v al s . . ` ... 93. Wh e n u s in g v a t s . 261, 262, o r 267, s e t a g it a t o r a t I2RB4 DO STEPS 94-66 ABOUT l/2 HOUR BEFORE DRAWING LAST WATER. 94. St a r t a g it a t o r o n v a t 36>3 o r 364 a n d s t ir u n t il 76c o mp l e t io n o f s t e p . 99, Ru n 29-30" (+ 1210.) w at er in t o v at 96. Tu r n o n a g it a t o r a n d s t e a m. 97. We ig h a n d d u mp in 98. Ad j u s t t o 40" (I7J at 80-I20f . 99. St ir t o o is s o l v e . 365. 60. Ru n 10-15" (20G.) w at er 61. Tu r n o n s t e a m. 62. We ig h a n d d u mp in 63. Ad j u s t t o 20" (320.) a t 64. St ir t o d is s o l v e . in t o v a t 366. 80-I20o F. 140 30 2$ 1 1*? 146" 3 30 Misc, 14. S.V. I5- 69. WE 1GH N-26 AND N-28 INTO KEG. DISSOLVE WITH 10 GALLONS ' w a t e r , a n d h o l d a t s t r ik e v a t f o r s t e p 69 %: 66. WEIGH INTO KEG, SLURRY WITH 10 GALLONS WATER, AND HOLD AT STRIKE VAT FOR STEP 74 67. Af t e r 3r d w a t e r d r a w n , t e s t a n d r e c o r d : s l u r r y c o l o r 68. Ru n v a t 365 in t o s t r ik e v a t in 3-4 min u t e s . 69. Po u r tN N-26 p r e p a r e d in s t e p 65 a t o n c e . . 70. Ru n v a t 366 in t o s t r ik e v a t a t o n c e in 2-3 min u t e ?. 71. St ir 5 min u t e s . (CONTINUED ON PA0E 3) 14 2 21 26 14 ?8 I W~ 21 DUP050067385 Pa g e : 3 J Co d e ; "55^l b s : 2291# (B) G-55I-D ' ,r in s t r u c t io n s 72. Te s t a n o r e c o r d : p H . n o r ma l `5.0-5.2. 73. Ip n e c e s s a r y , a d j u s t t o pH_{5.0-5.2 w it h N-3 o r N-33. Re c o r d : p H 74. Po u r in N-484 s l u r r y p r e p a r e d in s t e p 66. 75. St ir 3 min u t e s . 6176. If s l u r r y c o l o r o f s t e p w a s 4+ os b e l o w , r u n in f r o m SCALE TANK 363 OR 364 MT * NOTE: If Sl u r r y c o l o r o f s t e p 67 w a s r e d d e r t h a n 4+ u s e 162 LBS. N-4l6 AND PRESS BATCH AS 0-550-D (2453 LB.EST.1. 77. Fl o o d t o 85". 78. St ir 5 min u t e s . 79. Pr e s s w it h a g it a t io n . USE LBS. NCODE ACCT. CBS TIME START II II II It TIME FIN II f It It OPTR 1) CODE 41 G-550-D G-55I-D iPiTI 162 289 Go a l Yie l o 2453 2580 "NOliYl ISV Hllrt SS3UJ J'0001 ------- ------------syyvwaa------------ - W4.No X nU? X 48 ' .. "3X7g-- 11-38 Oi q OOt j SN3AVft N00|- X X X Al Avd DUP050067386 .5-550-1) (B) - STACMRU m&BU -HQfaS * This fom&& ropls-scn G~550~B (A) and was developed daring e program designed to find ways -cf increasing the strength of ar G-550-B' line of Chrosw Greens, iSx&sting '"A" processes yield products which ere weaker theft the competitive greens such c-s the ?al and Velvet line of Laperisl as well .as such products is Iieichkeld*s 3005 and Calico-a lO^tliOO* The previous ncn~Xuorids type 0-550-B has been reoodod 0>$90*>0* References: 03K-49-3X LH-49-35 1* A stepwise process has been written* 2 A decrease in -scdiuii fluoride will result in the production of weaker Shading ' Telle# which consumes less iron blue to reach a given msstoao depth and will giro weaker tints* The tinctorial effects will depend upon the extent of tiie reduction in quantity Of fluoride* Largo reductions will produce bluer Kasstone and bluer tint greens.* The converse cf this is also applicable up to a given maximum amount of sodium fluoride Above this quantity excessively dark, yellow and dull masstone greens result if tho marl*; amount pero&ssibl for a given process hag been exceeded* This has siot le=i datcr/vilaed in the pl?nt but in the laboratory 8.5 lbs>,/l655 Fb(i'0a)g way an excessive ^aeftni. 3* Attempts to reduce the iuoru-'sedhTua requirentente of this type Shading fellow, by such factors & an increase in sodium sulfide, era successful* However, the raasstones are somewhat duller, and the strength advantage *111 fall off proportionately to the decreased blue req.airer.ents* 4* Such factors as increased chromate content, higher initial sodium carbonate (whit base) produce similar effects to the use of sodium fluoride, but ar not fully equivalent. 59 The process has boon written with a stipulated amount of sodium carbonate (8-3) for steps 2 and 45* Plant history should be accumulated as to the desirability of continuing this practice Instead of. adjusting the pH to a given rang (4*95 - 5>05) before addition, of the K-3&8. This pH adjustment step was thought necessary because cf variable L'~3 reqxd.ronenis observed during the standardisation program* This adjustment procedure was considered undesirable by the Quality Control Group, Laboratory results indicate that a variable pH at the point of addition of T-:~368 is iwidcsirable since a lower pH produces a darker masstone green that that resulting froia higher pi! at that point* 6* No color values for yellow slurries were obtained.during the development program* At tho suggestion of the Quality Control Group, the standard formula includes a recording of this information (Stop 67) for future plant use as a possible control point* In addition, Quality Control has assigned a maximum value of 4+ to this point* All shading yellow with color readings above this value will be converted into 0-550-0 (see Step 76) * As plant experience is obtained on G550~B and G-55I-O, this value will be adjusted accordingly* DUP050067387 -2* 7 This process, with odjuBtesnt of bins liquor to 89 lbs*, s utilized in manufacturing a proposed G-551**D standard {G~55l~0 88, lot 90596)* Tbs sdx of five plant batches was rejected by the Sales Division, but a bland of thro of the five batch* gave an acceptable product, It is strongly rec<23sndsd that in the event of future plant production of this code* further attempts be made to nonufketure ths struck 8-551**^ f-W this process* &a General notes 'pertinent to th Y-"k$3^ (A) and 0-5SC-0 {A) processes- are applicable to the present process* GOAL HELD G.-55C-.33 (3) folia? 2291 Blue 162 Total tffc, 2453 & fella# 93*40 % Biro Complex 6*60 CALCULATED COMPCSITId; FbCrOe Other Pb Ccrapcumds Jnorg* " Organic 11 Moisture mIron I31xie Compl.;: 76*76 12*07 3*43 *41 *73 6*60 Blue Content by KCIW52 5*84 2293. 289 25 88*80 11*20 % 72,99 31*47 3*26 *39 .69 11*20 10,37 * Ca l c u l a t e d c o l p c s z t x o h Anhydrous Forrocyanidos Organic Agents Moisture BLUE COMPLEX G-550.DU 91.fe^ 3*2 ij-23- 5.0 xoooSS o*t>0 )o-5sa.o mh ****** 10*28 *36 3-U2D' Notebook Reference; 1096-56* j j *c o Signed J, JACKSOL - 8/20/49 Approved DUP050067388 1 :o>Sr' VAT PREP 1. SV<> 2. m 3- U/S. Pat. 2,139,753 c o d* k # (B) Y-56I-D APPROVCO BY: g o a l : 228.1# _snt. 7 Mot. j j j 8-io-Uo Cost Qrttp - 3 DIAZD VAT: COUPLING VAT: , CWO{ 8-19-49 _ STRIKE VAT: 260.. 26L26?, Z6l........ .......... .mil STD* HOURS NAME: SHADING YELLOW ' NON-BLEEDINQ JES: 10-19-1^ INSTRUCTIONS use iss. N. CODE ac c t . us. M kL0 ir yAT.M-r0R4Tkp.45.___ ________ _________ 46 3 3. WEIGH AND HOLD At SCALE TANK 361 FOR STEP 20 90 518 4. We ig h a n d h o l d a t s c a l e t a n k 361 reft s t e p 21 *91 108 5. We ig h in w o o d e n k e g a n d h o l d p o p s t e p 39 IB 26 6. WEIGH AND HOLD At VAT 366 FOR STEP 35 7 ' 3f 7. WEIGH.DISSOLVE IN l6 GALLONS WATER IN KEG. ANDHOLd AT STRIKE VAT POR STEpk ----... 11 ' "188------- - 40 9|.. L.. : 8:~ .... 7...... :... "W~* 8# Ru n 30-40" 3000a.U w a t e r in t o stRikt v a t . 9. RUN in f r orf m --Sc a-l e t a n k 360 .... - ......... .......... 10. Wh e n u s in g v a t s 261.262, o r 267. s e t a g it a t o r a y 0 r p m* ;i.i.;:Ao^u9T:TD;M"l tk5%i::S :::::::: 12. Ad j u s t t o pH 4.6~4.o w it h N-7 oft N-33. Re c o r d s pH 1 1fcfE fkBCtiP! MjTYTTnyfTV . 14. Tu r n o n a g it a t o r a n d s t e a m. 15. Du mp in N-3 w e ig h e d in s t e p 1, 16. Ad j u s t t o 55" (2420.) a t 80-120'F. 17. St ir t o d is s o l v e . .... 4f 41 . %' 18. Ru n 18" (2993*) w a t e r in t o s c a l e t a n k 361. 19. Tu r n o n a g it a t o r a n d s t e a m. 20. Du mp in N-518 w e ig h e o in s t e p 3. . 21. Du mp in N-ipS w e ig h e d in s t e p 4. 22. St ir 10 min u t e s o r l o n g e r t o c o mp l e t e l y d is s o l v e . ........ 23. Ru n in 1 "" 1 W 24. a d j u s t t o 29" 14790.) a t 74-70'P. T""~" " nr-" "Bar-- 25. Ad j u s t t o pH 4.6-4.0 w it h n -7 o r N-33. Re c o r o s pH Ma in t a in a g it a t io n in t a n k 361 u n t il e n d o f s t e p 38. . 1^ s.v. 5* 3S5 6. 26.Ru n v a t 365 in t o s t r ik e v a t in 4-5 min u t e s . 27. St ir e x a c t l y l4-i6 min u t e s . ........ 28.RUN I0-I5"_7+ 550.) w a t e r in t o v a t .365. 29. Tu r n o n a g it a t o r a n d s t e a m. _....... _... 30. Du mp in N-3 w e ig h e d in s t e p 2. * 31. Ad j u s t t o 25" (1tOQ.) a t 8o -120*F.^ 32. St ir t o d is s o l v e * ' w--1 33. Ru n 10-I5h 20G.) w a t e r in t o v a t 7. 34. Tu r n o n s t e a m. 35, Du mp in N-360 w e ig h e d in step 6.' 9 36. Ao j u s t t o 25" (40G.) a t 80-20*F. 37. St ir t o d is s o l v e . 365. 1 CONTINUED ON PAGE 2. DUP050067389 VAT J P6ii 5 Cool:(3)Y"561 -D Lb s ; 2281 In s t r u c t io n s use LBS. -70.. TtS-T-ANO _IC0ML J?iLr . , N0.RMAL 5.Q-'i.*k. '..................... -7-1___5,fe5JLv.i t h . .. . .._......... .................. -- 72. 43 &TIR... ...... _ ......BjEc.oRD.t_ pM .. ... ................................. _____ _ ,,....................... . ...... NCODE ACCT. LBS. \ 7k. Pr e s s uttHout a q u a t io n . .... ......... ..t ime s t a r t tt tt it ft *1 tt .............. M h < A ... t !) n o u v x io v Him fisaud *00011 *iviai j# xX ...... . uisfl .. .......X. .......... i# <* SMavW3U * AWO ....... m1. x ....... " rW'" ZfiSST".. oitWOM. iftfc JHBT O -------,------------------- : : , .....------- '"g'8STvaTf^lli"W"' DUP050067390 VAT Pa g e i 2, Co o b :(b ) Y-$6l*0 4b s i 2281# In s t r u c t io n s USE LBS. NCODE ACCT. LBS. s.v. J 8. 38. WMPN SYPP ?7 At 1 RftJNfl tOMPLETEOr_ STRIKE SC A it YAMRAT .,1,....jk-J&F INTO STiU.KE_.VA.fc. AT 4,.kr76*P ON TUB SU.St.Vt.B-..It} ......k, .....i^-SI MINUTES. ............... ........... ........ ....: ....... . . ......................_____ ..... ................. . .... ....... .... . ........... . RCCOROl. XQ.T.AL...ta.JNtlTEfi_^ .... ...... Mi sc. 9. 3p. WE 1 GH AND ADD TO N-26.i.6|lD .lN.J&tCJL .......... ...... . ..f,,.. - . 56. Dis s o l v e N-26 t r e a t e d j n s t e p 39. w iTk. 10 g a l l o n s _f.......... r. VATESAND HOLD AT STRIKE VAT FOR...STEP..4:2 Pfi I S ,Y. 10. 41 ... Wh e n s t e p 38 s t r i k e c o mp l e t Co ,. w a s h . in . s c a l e .. ?a.n k , ~ - ......- 36I . .IMMEDIATELY........................ ....,.. .... .................... . ................. ...r..... .42,. Po u r in N-26 p r e pa r e d in s t e p 4.0 a t o n c e... ........_______ 43. Ru n v a t 365 in t o s t r ik e v a t a t o n c e in ?-3 min u t e s . 45. Sa mp l e f o r 'pH a n d h o l d s a mp l e f o r s t e p .4.7I............. US. Ru n v a t 366 in t o s t r ik e v a t a t c n c s ; in 2-3 min u t e s . UfL Po u r ,l.jin M- p r e p a r e ^ in s t e p 7-a t o n c e .. .1,_..... .........: Uj. St ir 10 min u t e s . Wr i l e s t ir r in g , t e s t a n O r e c o r d s t e p ...... .......44:. pH,, ........... .n o r mal 4.6-5.O............... 48. Wh e n s t e p 47 c o mp l e t e d , t e s t a n d Re c o r d : pH ............ ........ No r mal 4.9-5-1...................... . . . ____ 49. If NFr.EssARv, a d j u s t TO pH 4.9-5-I WitN N-J oif.N^t........ ' ... . ................................... Rec o r d : pH ....~............ . B!0. Te s t a n d r e c o r d : s l u r r y c o l o r . ', 51. Fl o o d t o 85" <73950.). 352. Dr aw w at er s at 5 h o u r in t er v al s . 53. Wh e n u s in g v a t s . 261. 262. o r 267. s e t a g it a t o r a t 12 RPt ...... . .... n. W' ' 12. DO STEPS S4-64 ABOUT 1/2 HOUR BEFORE DRAWING LAST WATER. 54. Ru n 25-36" (+ l2lG.) w at er in t o v at 55. Tu r n o n a g it a t o r a n d s t e a m. 56. We ig h a n d d u mp in 57, Ad j u s t t o 40" (176G.) a t 8o -t |20,*F, *58. St ir t o d is s o l v e . 365. 59. Ru n 10-15" (20G,) w a t e r 60. Tu r n o n s t e a m. 61. We ig h a n d d u mp in 62. Ad j u s t t o 20h (326,J a t 63, St ir t o d is s o l v e . in t o v a t 366, 6o-l20`lFi, Pfo 30 ..... ,4,,,-, l4o 30 Mi sc. 64, We ig h N-26 a n d N-28 in t o k e o , o is s o l v e w it h 10 g a l l o n s 3- WATER; ANO HOLD AT STRIKE VAT FOR STEP 67# 14 ~W~~ t5 2 .. 1 S.V. l4 i%i f ,' 65. Af t e r 3r d Wa t e r d r a w n , t e s t a n d r e c o r d : s l u r r y 66. Ru n v a t 365 in t o s t r ik e v a t in 3-4 min u t e s . 67. Po u r in N-26 p r e p a r e d in s t e p 64 a t o n c e * 60'.'"RW"Va T 366 1 TN'TiiJ"''5,fBTf?i"'VXtl'1T"1>n c F^ col or 69# St ir 5 min u t e s . 0 , CONT1NUED ON Ptffi 3 - ' *T**" DUP050067391 <8)y-SUD ?oia:iLA mm fcmLlP, was developed for uso in Kaeneh nixing of the proposed strong fluoride type C*55C~D line of chrome greens* The existing **Art process (nen^fluorid typo) yields products vrbd.cli when forum.Ln.tsd into .greens an weaker than competitive products such a the Fnlo ami Valvet lift of Imperial, This material* will bo submitted to F & F for possible future replacement of Y4$M>(A) or T-561*0{A), Uaforenoos: DS1L 49~33. KhW>v35 X, A stepwise precoss has boor; written* 2* A decrease in sodium fluoride will result in the protetlon of weaker Shading Yellow which c c w bao s less Area biro to ranch a ^.w j msstone depth and vdll give weaker tints.. She tinctorial effects dll depend upon the extent of the reduction in quantity of fluoride. Largo 'reductions'will produce bluer masstone and bluer tint greens* Th converse of fcais la also applicable up to a given maximum amount of sodium fluoride,* Above this quantity excessively dark* yellow and dull masstone greens result if tho jm&dsanm amount permissible for a given process has been exceeded* This has not bean determined in. the plant but la th laboratory *8,5 Ibs*/I65*5 Pb<0s)s was m e&bossiye amount, 3, Attempts to reduce the inemss blue requirements of this type Shading Yellow, by such factors as an increase in sodium sulfide, are successful, However, the raasstones are somewhat duller., and the strength advantage will fall off proportionately to the decreased blue requirements*. 4 Such factors a increased chromate content, higher initial sodium carbonate (white base) produce sdailnr effects to the use of sodium fluoride, but are not. fully equivalent* 5* The process has been written with a stipulated amount of sodium carbonate (M-3) for stops 2 and 45. Plant history should be accumulated as to the desirability of continuing this practice instead of cdjustlag the pit to a given rang (4*95 - 5*05) before addition of the 11-368. This pH adjustment step was thought necessary because of variable .H-3 requirements observed during the standardisation progress. Tills Adjustment procedure was considered undesirable by the duality Control Group, Laboratory results indicate that a variable pll at the point of acldition of ii-368 is undesirable since a lower pll produces a darker masstone green than that resulting from higher pH at that point* 6* No color values for yellow slurries were obtained during the development studies. At the suggestion of the Quality Control Group, the standard formula includes a recording of this information (Step 67) for future plant use as a possible control point* 7, In conformance with th current practice in (A) Y-561-D the use of para soap has been discontinued, in order to decrease fire hazard, - DUP050067392 8* General notes applicable to '>493** (&) c-nd Gr-550-^ (A) processes are pertinent* CAI/0ULA.T3I) COMPOSXTIOi mxQfy if urn Other Fb Compounds 296 Inorganic " a Moisture 1 % 02.55 12.90 3,6t CSOfiL YTEU) 22mt Notebook Reference: 10.96-56* JJsCC Signed by J, JACKSON - 3/20/49 Approved by H AtttflHL * 8/20/49 DUP050067393 4 ikt PHSP 1 350 2 Cost Group - 3 NAftlS: C otio: (C)X-572-D k # Goals 1258sP*~~ Sizes Diaao*TatT^"~"^ Approved By: Coupling Vat: Strike Vats 260T2617262, 257 (2700) JUi INSTRUCTIONS USIi U3S.[ c d 5b ACCT. IBS in drum, and hold at strike vat for step IS z ( 12 16 Ul-Jj 12 aa-xza r2. Pump into scale tank 350 M T T Ratio 2r ,r afawuLiwojijftii a 1 J 1ST; use m mis g . 3 MX S77T 4 ') MISC. 5 "OT 6 361 7 _______________________________ 5. Run scale tank 350 into strike vat. 6T^^u^m tQt0r^etic*lLrid"cq^imt^to l^*at lo^T M nr k ^U^JfaigfcUULj^il.te atrUfl,.xatXor.jitgp..l7 M 11... Teat, 6*2, .6*5*. 12>. Ran into scale tank...361. M. -^JL X ^^dj.uatjtfl.pHL.6.O..r....6,>i.. j 6&~ 12L .262.J szc sxa: UJ1 J--JL-22L .19.__ ILJ&&. 177 Pom*1 |t > ^wmiodiateiy N-33 weil&ld la" step' ll ,A1y94n^w.^.*tMi,rri A..7.5?.* nIMrJirtttul toa,, 20* Tost and record:' rH Ib j bIo t .. ij... "ndrmal'g.l" ~'5',3? 21. foot and record: Back-water: must be 23*,^mzZM%smA,1 hfflg- totpxsala*. 24., After last-water, p0ur..,ia.Ma64 wnighod in atop 3 g^a^?Xto^g5,,.,(758pS*.)^ 257 Bress 'wiMoul aj^tatlgju DUP050067394 (c) Y-57S*J> FOIUtliLA HOT3S This formula docs not replace any previous formula, and is verysimilar to the {B)y572*D formula* This process is the outgrowth of a Sick list study on the G-6Q4-D line, tee object of which was. to obtain stronger groans*- Material of this type was found useful in attempts to catch Imperial's -*4464 green. The product was never standardized, because the request for the match was withdrawn by Sales, References: D5H 49*31 KN-49-35 1# The procsss has be established on a stepwise basis. 2, A decrease in initial nitric acid (H-33) followed by a simultaneous increase in second portion of El-33 results in the production of a stronger, redder aasstone, and tint, shading yellow* This yellow consumes a higher percentage of iron blue to reach a given msetoue depth g.-oen, than .does standard, and is therefore, correspondingly stronger in tint. Strength increases of the order of five percent were obtained to this fashion, 3, All notes applicable to the shading yellow portions of the (A) 3T-572-D process or <S5-604-d5 process are pertinent to this process. The following calculated composition and estimated yield apply: CALCULATED COl-ffPSITXCM FbCrOe PbSOft. PbO Organic Lead Salts IIS# 14 16 12531 94,55* 1,1 1,3 . 3.1 r GOAL YIELD 125# anhydrous HB, 951-19, # JJiCC Signed J* JACKS01I - 8/10/49 Approved H, AMPUL - #/16/49 DUP050067395