Document NnzGG62JxdNBxZvOyNxoqnLb

3sr- */ar7 a*-- y & HE1SRK PLAIT' PICMEUT COLOR RESEARCH REPORTS BECEMEBR- 1935 N36973 DUP050316235 PIGMENT COLOR RESEARCH REPORTS DECEMBER -1935 I - CHROME ym.t.csm & (StABIEES light Yellow Y-1S0-D (JD>M) (November) .... * Da camber .... Study of Light Chrome Yellows (SCH) ............ Excelsior Yellow K-8021 (JDM) .......... Primrose Yellow K-8124 * .......................... Med. Yellows of Improved Strength (SCH) .. Medium Yellow Y-3I6-B (JDM) .............................. Medium Yellow Y-359-B * .............................. Chrome Orange Y0-34-B ............ .. Study of YO-38-B (HCM, SCH) ............................ page l^a 4-6 7-9 10-12 13-15 16-17 18-19 20-21 22 23-27 II - KGLYKBA.TKD ORANGE - YO-8074-D (JIM) ................... III - LEAD & LEAD MATERIALS Purification of Lead Nitrate (SCH) .............. Lead Nitrate Purification (JK) ....................... 28-30 31-33 34 IV - CHROME GREBES' Chrome Green G-389-B, Strong Type (JK) ... (ADR) ................................ Extended Green, K-8009 (Aim) ....................... 36-37 38-39 40-41 V - IRON BLUBS - Yield Studies on Iron Blues (HCM) 42-43 VI - PERMANENT RED 2B itho so 1* Red 2B Lake, EM-427-D (E JH) .... 44-45 VII- PIGMENT GEEBN B (AS) ....................................... .................. 46 VIII - VAT DYES PGR PIGMENTS - Vat Dye Lakes (AS) ... 47-48 IX - HEW ORGANIC PIGMENTS - Special Organic Pigments 49 X - PIGMENTS IN OIL Flushed PTA pigments (HBB) ................................... Flushed Lithol Red * ................................... 50-55 56-61 XI- PRINTING INK COLORS New Types of Printing Inks - Rotogravure Inks 62-65 ** ** Spirit Inks(AJS) 66-68 XII - PHYSICAL STUDIES - Dry Fineness of Pigments (RRD) 69-81 XIII - RUBBER COLORS Blue Lake for Rubber BP-168-D (K-8G47) (RJH) 82-83 XIV - ESC. ORGANIC PIGMENTS (a) Para Red - Blue Shade (JVS) .............. .. 84-91 (b) Lithol Calcium Lithol (FEE) ................................... 92- Ca Lithol Toners RT-379 & RT-300D (EJH) 93-94 Barium Lithol Toner RT-364-D (EJH) .. 95-96 (c) Hansa Yellow YP-324-D (J.W.Lang) (October) .............. 97 Hansa Yellow Lake YP-324-B (EJH) ____ 98-99 DUP050316236 2 XIV - use. ORGAHIC PIGMEBTES (Gout.) (#) Mists. Toners Red Toner K-763f (BP) .............................. Orange Toner K-tf84 (ADR) ............ (e) Bordo Maroons Maroon Toner RT-347-D(ADR) .................... * * RT-364-D * ................... * ST-363-D(BJH) .................... (f) Miso. lakes - Barium lake of range II (IBP) XV- SEMI-WORKS PRODOCTIOH (HA) ............ ................................. Page 100-101 102 103 104-105 106-107 108 109-117 DUP05 0316237 -ijgQHf f il e j tyaM&i.be.rr Following the developsment of a Titanyl-sulfete-treated T-309* witb superior late: properties, the seme method of attack was applied' to T-IBCM*'. After emccessfUliy prodnclag me improved yellow ia the laboratory the formulatiem was brought to the seal-works for mimt M w p v tmeimm . __ Jl batches of this color were made as checks on the laboratory formula, They were strong red and dirty against Y-1BQ-D standard with v.s. worse light fastness. The comparison against the laboratory product was similar* A smell decrease in the amount of soda ash added after strike gave a dirtier greener product with slight ly better light stability against standard. Fhe tint was weak against control, and the masstone much greener* A batch made on a smaller size (SW-7915) cheeking this variable was also green and dirty against standard but was a little silky and changeable. Strength was greater and light fastness was decreased as compared to the former batch. A number of other variables were tried without atmreciably improving the semiSworks products* These variables were: a) variation in development temperature, b} use of lead nitrate crystals instead of liquor e) slower washing cyele* i) omitting sodium sulphate after strike. Doubling the time of strike gave a product much closer to standard than any of the previous batches* This variable will be recheeked* >: EXFiaiMSHTAL DETAILS. Wotbook 4t5*gp,, 90 - 36* a DUP050316238 DUP050316239 DUP050316240 Si*..;- .VHv ?.V. V' a,.,: ,V- M- *; . .i > i- - ' -....t ` l-rn'mi . v>.' - \ iIPWWW Iwri -3?- ?*i IIIS: MTS: 3~./r*s- . ISXLOSS. 1938* The ;aeiiworks Study On the' 4eveXo$jet of a MthyX* sulfate-treated *iaCM8 with superior ink properties' was 'Continued during t!is month* 'trouble still feeing encountered with ittooasisteiit '`pfjStt.X'ts' at* took* pXI. ,iteBtiw#- /., " i- *r ' ' ' :; , ... - -.;' There were fen batches struck during' the month* nine feeing one tenth mol in size and the other one-fOurtietb. mol* This small batch was struck as a eheck on control to approach laboratory strike site* It was flatter and had somewhat better light stability than larger batches* The masstone was, flat and dirty against standard with an improvement in strength and light fastness* A number of variables were made to determine the effect of larger amounts of salt in the strike, and titanyl sulfate in the after treatment of the yellow* the resulting colors were all on the dirty, strong side of X-180-B with better light fastness* An increase of twenty-five percent in the amount of titanyl sulfate gave a red and dirty mass tone whereas a fifty percent increase produced a decidedly green flat one* the tint of the second batch was a little wekker than the first* These differences are probably of little or no significance* Doubling the amount of salt in the eontrol formula gaye material closer to standard* the masstone being slightly dirty apa the tint a little strong, red and dirty. Increasing the amount of titanyl sulfate in conjunction with the larger amount of salt gave a greener masstone, a tint practically equal to that of X-180-D and a v*v,s*improve meat in light stability over the former batch. An increase of fifty percent further in the amount of salt gave quite a similar product the masstone being v#v,s*rel* The tint was v*v,s*weak and green and lightfest- ness a trace worse* Increasing the amount of titanyl sulfate further also gave a similar product* These last two variables run in conjunction gave a dirtier psaker product with a little inferior light stability. Against standard this last batch was flat green and dirty with a v*sstrong red tint and v*e.better light stability* One batch combining the two most promising variables* namely, a longer time of strike* and the intermediate increases in the amounts of salt and titanyl sulfate, gave a very dark green flat dirty masstone compared to standard. This study will be continued in the semi-works and possibly in the plant* DUP050316241 'ft:... V 1 ,' '' .' r-: . , ' * Z '< ^{ .' ' ' "i?$' severs! variables have et times' shown 'Jappovep#^- ift tinetertal |'roe:rties.t<* , Stj increased" time of strike# b) increased amount of salt c) increased amount of titnnyl sulphate* lesuits, however, have been extremely inconsistent, indicating that the process is not yet a stable one. :|PotflhbOOlE #' ^1 DU P050316242 DUP050316243  fttfjNS.- teprovefi T480 process was renamed is Leveleprnant difficulties ia -the SihI*W6rks* 'M 'mmjoepm^ studies J nitrate, lieuer fronthe plant. an&vlehd nitrate crystals gave Bfo'isiaatially ":"~ 'Hi sitt* fcesdlt* JSAiftiif** tfti salt'in'the. strike' sdlutt&k -m&' m creasing As bitanyl suitat add** to Hie washed slurry both seateet to increase the .cleanliness Of. the jaasston very slightly* These variations a development teller stupe of BQOoF are to be studied is The effect of several other variables was studied but the results were negative* Increasing or decreasing the volume or tompAratur hat a negligible effect* A decrease in the pH of the strifes solution resulted" ia a lighter masstone weaker pigment* Sfverafc miscellaneous experiments were run to determine the effect of certain added ingredients* Replacing sodium sulphate with a mixture of rare earth sulphates (D-8Q44) obtained from the lithopone department resulted in a very dirty mas stone product* A similar result,was obtained by the addition of a small amount of diphenyl tffoarba6ii "twi ' attomth the stability of 481*880 formulation (Developing at sfpjfinstead of I8O0F) * Also make a run using the 4i3h semi^worfes procedure* versus 'S5f * all were clean* strong and much better in lightfastness tin standard* The product mad on the semi-works procedure was Somewhat red in mas stone versus the semi-works batch 8w*V48, but very close ia strength and tint* of increasing the salt in the strike; alsc second water to stand over rnm* also by increasing the percent of Titanyl sulphate DUP050316244 increasing tie sodium chloride gave a very slightly cleaner product acnflsipahlefi by a eiig&t deerease in strength and light ft.ability* Allowing the pigment t# stand over night with the second . wash Cater showed a trace i%rcvement lb lightfastmess* increasing the titamyl sulphate here favored an Improvement ia light fastness* Study striking at various temperature arranging fro 65I to 11QF (the control being 80^5 also study a fifty per cent increase in.yoi*** . . . ' . ` ` In this experiment the change in strike temperature did not seem to have any appreciable effect oh the pigment ; while an increase in volume showed a small increase in strength* Study lowering the volume of lead nitrate solution; study a one hour strike and the use of hydrochloric acid in the strike solution* Using hydrochloric acid in the strike and lowering the volume of the lead nitrate liquor both favored a decrease in strength* Striking in sixty minutes instead of twenty resulted ia a slight improvement in light fastness* Jfett___ Study the omission of salt in the strike and add salt after the soda ash* leplaee the chromate with bichromate; study developing for two hours* Substituting bichromate {SIB} for chromate gave products considerably weaker than the control* The use of salts in both the strike solution and after the soda ash (SIC) gave a much weaker product than using salt only after the soda ash {31-A}* pigment* Developing for two hours had little or no effect on the 481-32 Study increasing the bichromate in the SIB procedure; cheek 31A, and develop it for two hours* Again the use of sodium bichromate resulted in a weak product like in 31-B* Mo marked improvement was obtained by developing thd SI-A type for two hours* Study using Diphenyl thiocarbazoae in the lead nitrate liquor; also study the use of rare earth sulphates in the strike solution* DUP050316245 rf'. '. >* 'y $ 1 - : . . ^5?fc4 ti - ..a-'-VV.". -. J-r' . v i" -.-.r - V1.-!;; S>.,. "*f JMjlHMlft tfciaxba*M an# ***** Mgftate* ^aatat i* W7 pigats. 4 * V : i; ' ' >,* ,V,, ' ' > i, ,, v r .yv.;, . ."raL*' .: '^.,-.V'i: !** '* -. '' -Si >!': . ' * -y *'*' ?. ''''PV /$!.f * /' ^ DUP050316246 "-a >* ' . . : . v..i >f .' ' v- - ' . " - V- ' '* ,t I- . .; : : i. V /-i-.v'S ""V.*yV MSI W :-'.i ; r. SBBMXfTp) BY; . . , APFRBflfB BY* . //'/ wirnt cmmMm&m BA: BmOBSSBS-'WSS, \ ' _ ':v ': \ .. .: Flsspt production of this color was continned with the iwnfa#.ture of 'three b&te&es. during the month. .' ^sro-'S'eni-worWhetehe ware also made. maattwtmartai. la the ease of the first semi-works feateh, the washing period'was extended from a space of two hours to over night without a detrimental effect on the tinctorial properties of the color. Omission of the development and stirring period gave a very dart: dirty product* Plante The first plant hatch was run on the same formula as the initial"'batch made last month. Against 1-8031 it was a little dirty flat and changeable in aasstoae and on extension it was a little strong.,green,and clean. Light fastness was slightly worse than that of the 1-number. Sodium sulfate was added to the next batch to increase the yield. Against Y-300-B it was a little red, clean, and strong with somewhat increased brightness and better light fastness* It was a little cleaner then its control. Compared to 1-8031 it was some what red and strong with worse light stability. The sodium sulfate addition was found to materially increase the yield* tm alkalinity of the* chromate used in the f&ird hatch was abnormally high and, as a consequence* hydrochloric sold was added, to the striking solution with a corresponding decrease in the amount of salt used* This was a little green and dirty in masstone against the previous batch and scmewhst weak, red, and dirty in tint* Compared to 1-8021 it was a little red and dirty in masstone and on extension^!th slightly worse light fastness. The light fastness was better than that of T-309-B and the mas stone was a little green and dirty. The tint was on the strong, red, dirty, side of the standard* The three plant batches made during the month were tested on the ink mill to determine this behavior under such conditions* All thwfce mixed more readily than Y-309-B standard and showed a little less flow. Although the plant batches exhibited no superiority in resistance to lithographic tspeakdown using a zinc etch, they were distinctly better than Y-S5O0-B using a chromic acid etch. The plant DUP050316247 p - ;S<S* : . ' ' ': $ \ * <* w I * ' .*ff ;- : ft ' " Wv,: ^ .'v r' v*` * .*;; .< .' 4 ^tele sgtfhft a# -' iaproTaaeat mmt Y-JWNMr*a resisteaee -a- -iittle' Worse in mi respesf as m: v S::/v. :' '& hr#- ttix. 'off equal parts of the four batohes jaa#e in the plant up ta. the preseat tiiae was a little a the re# bright side of **30S>*B in amassttewia, % tint was slightly strong md a little.. re#* * v- is' beiKg- eisotiaws#. ua#r the mpuelTteii#.' of the;. ftprelo$n$itt' seshtba. -sSV' f## ir.i* :49a.,, "ip* i# & ii. k- if y- Oh? ' >:* Vv;.: -'l ' ' . 'v. ' . . :.. ./ \ .'A * . `i ;!* -..`Ik DUP050316248 DU P050316249 BmmTsm fits "' *S// t x m% o h ip mh imsxm SiTS: ISOfflilf? 1& 'M&mtsetter. of"till'd solar, fora#'ly imown.as 3*9886 we .continued du#in# seestbey* A mix f plant material ha been made and ' a#" i w ttaiidard,'ae-S*81&4* M3SWh\ "` total of fir batches' have been mad in th plant* fopr. of them were struck on identical ,fomuls cheeking'on a larger heal a semi-works batch (SW-7299J, throe of these batches were light, green, and clean in massten against T-305-B with ranch better light fastness* Intensions were a little strong and green* these three batches were a little redder than KV?888 with satisfactory strengths and s little worse light stability. The other one of the four went off color somewhat, being slightly dark, red, and dirty against the Knumbey, with very slightly increased strength and a little worse light fastness* It was, however, till very very slightly on the green clean side of T-305-D with better fastness to light* In one batch, the amount of bichromate was reduced five percent and the sodium sulfate in the strikes increased alike amount* This hatch exhibited a tendency toward instability on drying being only v.s.red against M>Vi@8 on press cake control and a little dirty and very reft on grind* It was a little weak against the K-mtaabar and li$kt fastness was equal. The aasstone was a little green and clean against Y-305-D and light fastness was much better* All five batch# were tested on the ink mill against ' Y-SOS-IS and a competitive primrose, G-8S349 (Imperial)* All of the plant batches and C-38349 mixed more rapidly than standard and gave similar inks with respect to body, length, and flow. Resistance to lithographic ireskftowa was satisfactory* Although the plant material wes somewhat superior in resistance to livering as compared to Y-305-P, it was all distinctly worse than 0-38349* Two batches were almost equal in this respect to Y-305-D, It was concluded that while the recent batches of KVV888 are inferior to the competitive yellow in color (i.e* greenness for a given strength) and livering resistance, they represent a decidedly worthwhile improvement over Y-305-* .v DU P050316250 wm . .wtT . .< s,s ;xtr?.-r _ __ __ of plant materiel asiag all of f&or , $*&& *' lto ;&ae:wltfe: "am adjustment in biebrnmat !*&' feaanaet up as a aew standard and boded as K~81B* / **** Itt'iq.ali&ny 110bt' green, and lean a aasitop, 'V4fe,M`aM**3*att * undertone, y.e.red, slightly strong and elem -ipy ^fc^aitaas} aftd -.better In- light atability* :-Bmntwca,`.aim-x - Sea notebook #48 - p* SO - 6S* V;'* , > * DU P050316251 u I? fH ?fc HP* g.3 H 4 P nS 3 < 8 B*S 4B b * &* * s> p P > ja P roH *H U fe* t* > # >>> no t* p p ,0 I 8 >> J* PH TO * *H no >m pi* tt 43 1 >* p t4 o P P 43 * t>% p ns -CJ id *4 U > U P P 43 * o ns u a A t 4/ if: uma f4 W c*n o t> pU *g # u p P S* *P * %n <3 > * 3a ?>>aJ u p Jh U IS 15 ,, u <&l &*% t s eo }> res > P it 8 "0 -*Hd Ubo 4*rda4 >H# ($*0* * -rH * rH 4<*o0JDr) Q b3 * od<P*Ho ^ rH s P d *a83y <& P raHi *+ # m Ot co tn 4*4 00 aI co trt O COOfli 1 Ii tff M > * H1 >* P rH *4 O *H rH o o nO *4 5i ttO tt t ns ** b * tn > * rH O rH p rH 08 <*? O rH * %0 g b2 %.b*5 u w 4i-1a fc* ns 2^ lb M -U xS ns tb fe 3 t*o tCeOoowoI no tWI*fI13t0o* 00 00 *? US a tn CO o o t> <0 CO d44 oJ g C& <359* tO - t-* II 44 pH H js tn If) TJs P. jH O > 03 <> n* Jb? 44 Al <Q H O' ct 44 * * n1$3 *4H4 O O CJH o 03 1 <e Hr 44 in w < trt tf> * a* 09 iH <0 09 10 oo g 09 5 ?. s4p s<^l s Vi 44 o o K <f 03 ' H- <0, ' <& DUP050316252 Ik j l /A/ .... Mfjts immsm ism. IJurtng an investigation at the Experimental Station of A the .relation \betweent particle size ant the strength of a Kedium brerae * ws found that last abrtestate prpared in a very dilute solution wSf abiut 50% -strong versus Y-SSS*, although dirty and changeable in (tmteWm A'aWdy 0f':tMs dilnie`itrifee pprroocess has been st. art.ed- at TlBftri-til-' |]fi{Bt~,;: ' :> '**'*7^ 'e*TM-'- * .; ,. m A number of samples of fcfome Yellows prepared at the ttal Station have been exaiaMned at Newark* These yellows were le by adding a 0*1 mol solution of lead nitrate to a 0*1 ol solution sodium chromate* The strongest produets which could be duplicated were 50$ strong vs Y-380-B* T6e only factor of importance aside from the pe"f a dilute solution appeared to be the use of a very small chrome excess* With a 8$ ehrbme excess weaker products with a slightly 01 saber masstone were obtained* These experiments were repeated at Hawark with similar results, A large size sample was prepared for evaluation in linoleum and asphalt* Hotjfeek.idSg*. 4Sa*S. - Preparation of strong lead chromate on which t make a drying iiwaSy* washing* chromate free* A part of slurry filtered without washing* B jp * * " 1 washed chromate free 0 part n * so as to form a thick cake without part * ** ** washed & BTo outstanding effect was observed from studying the above variations* ... of strike* mm - *-- of higher temperature and shorter time It appears from this experiment that the higher temperature trikesproduce a cleaner, but redder and weaker product than the 70F strikes. No great difference was obtained between a ten minute strike and a thirty minute strike* ^ .. ... 4BaSQ - ' Study effects of a high development temperature; a#rfche addition ofoarium chloride, molybdate and di-sodium phosphate* Heating to 140% after the strike resulted in a red and weak product* DUP050316253  / * 4. / *' >4* : ' -** ............... ' f * .- " X JfT ' : : --0 A i-STjg&U.-.. $ `.ehesasvei- By treating the'struck rey#ment was obtained By treating t*f:'fbe voiie , ' ,-'>V ' ' ' .: ' '' V ' ` ' ' s Study .a reduction la chromate, also a redaction end nitrate solution# A reduction in ahrornate gave a very large increase in Strength; this wee accompanied 9 ,:d||rty i9asstone#_ Seducing the volume of fl^vieM nltfats fiad\aittin';o"ne> btgeeb probably because bh 4^SjgaBig:r~ SNraliiaii^''Bf 'the lElehSls Surer slrenatft Helloes. 0&k aiteBeok ift sad '175for" details.'.''- Study .effect :of striking simultaneously. " The pigment made by striking the chromate and lead nitrate lifuors simultaneously was clean in aasstone, weak and red in tint, and better in -light fastness than the Control, 45a*S4 - Study a further reduction in chromate and an increase in volume on the 458*81A type# It appears from this experiment that only a very small Chrome excess is necessary to obtain maximum strength; an increase or decrease beyond the amount used in 8433 favors a reduction in strength. Too large a dilution of solutions does not favr an improvement in strength* f.i. r: -;< " : . ' -; f;- > ......-t* . -V DUP050316254 ft. tBmiTzm mt*. 41&FRWi. seua tr&%' &/// m$&i mQmmm xsss. The development seetion is continuing it sup02?It !sou of this color, trouble still being encountered with poor lighs&festaess* > ^ ^ . > " ; `..`i *, .. . '*&m bs't%hs .of this pigment were made during the month. The firet was ^jailer' t o the -previous hatefa made with a large base volume. It was h- little dark eQaC dirty against standard with a strong, green, and clean tint--and' slightly worse -fastness to light.* In the next batch, base volume end time of strike ware halved, the amount of nitric acid added to the base was increased seven pendent* and the amount of alum was out twenty-five percent. These changes gave a redder wealier product with a little better light fastness as compared to the former batch* The light stability was, however, still v.a.wors than that of standard. EXPERIMENTAL DETAILS - See Note book 492, p.&0~59* DUP050316255 DUP050316256 ^-S~- i. # '$*K jJsV % (f-^ ' .^t-.-v r-. i>. .& * ' ^l";.$v'*-> ;-.** ...' /->4SJ, +* , * t `* J$ ^/// BP:oa^%tsss. ot.'toiasmMsl? m& during the as attempt: being main t;'bfii. red*" weak material for shadtag 'K\>: green- .subat sa&ard. stock $r ` : '. ' ' - v::'xv :;!"** ; ,*'1 '.' ' V '~X' A total .of seven batched 0'mre male faring the scmth* .'.Shr first :*wo, $*- struck -w;..ffe;*ftRUK. prodnotieh ftomuls using titil-j0Ra amount hf-toriafio toid:" in $$ banto TI0y . !, dark, dirty side of standard ii* masstone to a small e^toto.with hllto#, ' grtom* m e^aa 'fiats* ;tft bftto^f attoiler U `mm*' ' fJ spaf ** batches contained a -told*' .f** ;fUtyV'. toem resembled tom material made -witif toe lower amount aT-told, toe tint*- however, being a little loses- t standard. The masstane of the second was slightly dark and dirty as compared to Y-3S*!> and the tint was a little .red# .Strength Was satisfactory and light fastness "soperior to standerd The next two batches were mad on the seme formulation as the last two ex apt for the substitution of ml trie aeid for muriatic in one of them* These two were aimed and gave a somewhat dark* dirty masstoae with vs. worse light stability and a slightly strong, green tint* , The last batch was struck with e further lnereato in the amount of muriatic acid added to the base* On press cake control the material was a little light,?green, and flat with a slightly strong green and clean tint* , Resistance to lithographic breakdown continues "to be Satisfactory with this color* ' Sor Ssperimentsl details see W*R* 448* pi T0 ;H * * to'-V' ' \ . /y S-V , ' fvto,;-.,! *!* h'A^u'-- * h-,*s vi: .*\*1 / '-I**' , "i-:-Ah ' '' '.: ?.' ** ,-v DUP050316257 DUP050316258 'i V 'U BTi f il e ? ei-eftaw DAIS: MB 1935* mj^s&uLu 0e . batch of color was struck on this cod during the month - .without attaining the. desired degree of brightness to justify Its Use- as she&ing imat r1 a I "for' substandard stock*. *& on batch made daring the month was struck on a formate based upon a research labora tory experiment * This formula differed considerably trm the usual dark orange being closely related to the light orange* YD~2S5*B procedure* A reverse strike**!** employed and the sodium bicsrbonatetj&m omitted. The lead liquor was struck into a mixture of sodium 0firornate end bichromattfgad acetic sold was added after the strike before bringing to a boil. The orange was light flat and yellow against Y0~344> standard. Board mixes of this material and current muddy* ohromy YQ-S8-B were made at Y0-34-b depth. The mixes were a little flat and muddy against the standard with somewhat less strength. EXPERIMENTAL DETAILS. See NB, 44:8* p, 159# m DU PO50316259 #. & pore intensive study of .than heretofore 'Mas fees taken: up in the laboratory* &. aw,-iaethd,..-@f investigation - - hsur been' adopted bated bn tie'aft'saatptloa bKai redent operating giffle&lties :#d iease by the presence of soma substance or substances not pr#~ vibusljr present in harmful amount* Ho definite information has yet . beeh..-obtained on' this point* Tie ntudy is being focussed on tie eeases for the Ieoh of brightness in pa astone* together with slight weakness, it being assented for the present that these offsets are independent of masstone depth- variations,* The possibility that impurities derived frost the chamber lead now used or from some other souree are the cause of present operating difficulties is being investigated and some preliminary results have been obtained* The presence in lead liquor of small amounts of titanyl sulphate, alum, sodium formats, sulphates, oppay, barium, vanadium, or iron apparently does not result la appreciably duller products* larger' amounts of oopper or bismuth result in a chrome orange with a muddy dirty mass tone. Several experiments on the preparation of 10-5SM) from a washed base gave negative results the products being similar to those obtained with an unwashed base* further attempts to obtain a dark orange by the TD-sse-I) type procedure were unsuccessful* Notebook #486* 486-40 - Study on Y0~34D plant formula the addition of Mearbonate in paste form, acetic acid in strike; striking at 80oF and Slf* Hone of the above variations gave any premising lead* All were too light and yellow tinetortally* 486*41 * Check 40 series, but use more bicarbonate {increased from 86*5# to 40#)* It appears from this series increasing the sodium bi carbonate had no effect on the shade; this, however, is contrary to any previous results, and will be cheeked* DU P050316260 , B ail## Using the bicarbonate in paste form gave a darker 'triage than. A, made 4al3ig the' bfrhiMfct ia the dry fora* fegeof the" above i#f0fet tie brlghteess-of ;tfc pigment# .. . ; -; V$r V ` ; '."'y y' '* ' '"'^i;^ ' ' 'Si > : "r . > '1 " ' : . " ~ ;sid$ vafiafien i temjte^Ure,. and use of aeetie seta aftea strlW (if' the rawerso presifi tab!oa method) * . . ' .fNrtking at. $80?jr gate imrkmr Mas sties' than striking hi SOF* Adding acetic acid to the 80F stfik gave a^brighter product than th4..eonirolf- a reverse. ffeetwas Mail!#-St ISGTF* ' .486*46 - C<mtihaatiaa of seals 486*44* 8tudy variation of alkalinity of chromate solution; study use of additional acetic acid in. lead,solution*: Mona of the variations showed any improvement. Being all chromate resulted in a muddy like mas stone* using more aeetie aeid in the lead liquor gave a lighter mas stone hut the figment was dull and changeable0 486*66 - Continuation of series 486*45* Study variation in chromate balance# Study a more alkaline strike* weak product# Adding soda ash to the chromate solution gave a dark Add soda ash after the strike resulted in a lighter masstonen Cutting the precipitant balance and adding acetic afld after the strike gave a muddy like and changeable mas stone* 486*47 * Continuation of 486*46 series* Study variation in temperature; uhe"f caustic soda after strike; also study direct strike* Striking at 180% and adding aeetie after the strike gave a darker product, than striking at 800?* Beplacing the acetic acid in B with sodium hydroxide resulted in a brighter color Making A (18043? strike) as a ||pt direct strike gave a pi@aent slightly darker in naestone than the A product* 486*48 , Continuation of 47 (using caustic soda iftor the strike) Study increase in caustic soda; use of molybdate; variation in acidity# increasing the Sodium Hydroxide (on the 180F strikes) t causes an increase in depth* file effects from using molybdate were not very marked# Striking the high caustic soda procedur e at 1860F resulted in an Increase in depth also* Mono of the variations improved the brightness of the pigment# 4B6*4f;* Continuation of 486*41 series. Study indreased amounts of bioarbe^Salo;'"use of aeetie aeid 1m strike* DUP050316261 4 increase lucres.: $ th# aapth jpr ^3| .** ^ " " .& * sadin.' Meailiosa't#,in. the lead liquor ' ' Vbut so is^rovsment In brightness strifem produced a lighter piaemt, ' -V' . V*. ifeieU of M aeries* Study former tereaet la SioirSouam Variation lb **1^**^ >-*' na*jik*'**timM tgio ifordmosi* Hi "arndtuli" hlosfhorna** em iiwres? *> i^romt_|a_tey^te.o a| iiS8* ** Beatles to a Sell la IS afcautea Cus _ ,& ,5****^ - 4&&r*m' - Omtiauablcm '''48#*4A Study use of OawebSe ;>#a before tfe^Wpel ase ff Sulphate; before the vtvtko* . All of thCfe o4uia'.'ipere ll;^t and Ae'we^ and brighter than - the stride imereas04 the depth but had no influence e., the. brightness* . study the use of sodiUm sulphate sulfuric acid and soda aSt to replaee .sodium bicarbonate* fhe additidhof sodium sulphate to the lead liqtpsr.ggye a very light and dull product. substituting soda ash for eU Of the bicarbonate resulted la a very Middy Ills masstone# cfsulphurie acid soda ash gave the darhest aad brightest pig^at of the seftes; even this product was dull-sad light versus 10-34*h* sadism - stfcdy washed base; variations of eoetto ir la washed base; fso of nitric aeld Using a Ihfge excess of sodium bicarbonate aad washing the base three waters did. hot aid in obtaining brightness. However, .pre cipitating more as lead carbonate gave the brightest pigment Of the series* " btmgnth M trJP5^ tk* etTeet * bahtaallintion with oopper, " M,, la t&is experiment the control was dirtier than 8Q~a and 3S-D. Using a large amount f copper k s eupri sttlpHgjfc. gave a very very muddy pigment. Bismuth used In the lead lisaor rfcsulted in a muddy dirty pigment. Iron added to the lead liquor gave a redder pigment than the control, and was somewhat cleaner In aaestoae* 48d~g * study the effect of adding sodium sulphate and sodium phosphate to the 'strife solution; study substituting ammonium salts for sodium bicarbonate, . ` 'S' > ` * , '* ' - 0- ^ _ ** additMaa of phosphate or sodium sulphate to the bichromate resulted in dirty dull pigments* Substituting bicarbonate for sodium bieerbonOt* gave a very very slightly dull pigment versus ^ - ' 'fo st; use of alius dud sodium formate in lead liquor; also s T tre. after the development with lead liquor < V.: DU P050316262 and ttbanyl sulphate* ' Adding lead liquor until m excess of lead was obtained produced a very flat and milky orange. Sodium formate produced depth, bat sot brightness; a very dirty undertone was also observed* Ai* added to the lead liquor did not increase the dirtiness of the pigment. In fact, practically no marked effect was noted* 486*57 - Study increasing the acetic and further use of nitric 5 studyr addlt ion of 10# of lead after washing the base* Splitting the leand adding about ten percent of lead liquor to the washing base produced a dull flat pigment. Nitric acid used in the bichromate reauiteyln a dirty pigment. Increasing the aceHc^aSid after the base had been washed increased the depth but added no Improvement to the brightness of the pigment. 486-58 - Check 486-54B with less copper* Study potassium bichrome; sulphate in strike solution. The series as a whole was dirty versus standard* Nevertheless, it appears that 0*1 gram of cupric per mol of lead oxide could be in the lead liquor without causing any appreciable effect on the pigment* No improvement was obtained by substituting the potassium salt of bichromate for the sodium salt* The addition of both acetic acid and sodium sulphate in the strike solution gave a dirty product* 486-59 - Study further the use of ammonium bicarbonate; titanyl sulphate im"''t]ae.base and in the strike. The use of titanyl sulphate, whether it be in the lead liquor or the strike solution tends to increase the depth of the mas atone. Ammonium bicarbonate substituted for sodium bicarbonate resulted in a light flat pigment. _________ 46~6 -Study the effect of iron and alumina hydrate In Y0-3S-D. Continue the study of sodium formate and ammonium sulphate* The use of ammonium sulphate in the lead liquor gave dept#, but no improvement in brightness. No marked improvement was obtained In mas stone from the addition of iron and alumina hydrate; an increase in strength was noticeable. 486-81 -Study contamination by barium chloride and copper nitrate* study use of sodium vanadate* In this experiment it appears that very small amounts of barium chloride, sodium vanadate and copper nitrate have very little effect on the pigment.obtained, when added to the lead liquor solution. DU P050316263 k - 486-63 - Continuation of 486-5?, Study variation in nitric acid; use of potassium bichromate; use of chromic acid* The use of chromic acid for bichromate resulted in a brown pigment Decreasing the acid and using potassium salt for the sodium bichromate resulted in changeable products, otherwise no marked dffeet was observed# & / DUP050316264 3*T- Y3 wrnmmz b bt sear o k bef o r e miSDATO 0BR0KE GRASG-B (fjjQffisnBMiTnro by : _ APFROFIB BT: J-/X 3 FIUS: MOLYBShffllSl gffltgMS' eBdHB BATE: DECEMBER 19S5. The study of this color was continued In the sssai-works during the month and the formula was taken to the plant for tax initial trial* smazm?' jam mmxamicm Eight semi-works "batches were mad during December, One run as a check on the K-Q074 formula was a little brigh ter in wosstone and redder in tint. Press washing color made on ap Idential formula reddened the masstone a trace end gave a slightly strong, yellow tint# light fastness on all the semi-works hatches averaged very slightly worse than that of standard, Striking et 60F instead of 50F gave a product that was a little dull. The extension was slightly yellow and w.v.s.strong. This batch was a little dull and weak against the press washed material, Chi one hatch struck on the control formula, the wash waters were drawn at three hour instead of at one hour intervals. The masstone of this batch was a trees yellow and dirty against K-8074 and a little blue and weak on extension. Hopper contaminated lead nitrate liquor was used in making one batch. The masstone was a little blue and bright and the tint was somewhat strong blue and dlrtj against K-8074. ^ Three batches were struck on a larger scale than that employed for the ones previously mentioned. The first was struck at 60rF iasteed of at 5GF* The messtone in this case was a little brighter and the extension slightly stronger than the E-number. A thirty percent cut in volume over this formulation gave a very blue and somewhat flatter masstone with a very week tint against JC-6074. Brcreaslng the temperature to 50F together with the low strike volume gave a product much closer to standard material, the masstone beinfr v.v.s.blue and the tint slightly yellow and strong. One batch of this color was made in the plant on e two and one half mol charge. The formula wes a check on the one for K-8074, The product was on the light, flet side of the K-numbsr with a weak yellow tint, and v.s. worse light fastness. It was found that the analysis of the sodium molybdate used in this formula was wrong, this error, in all probability accounting for the unsatisfactory tinctorial properties. One semi-works batch (8W-7571) was made-using the same molybdate and analysis as that used in the plant. This batch exhibited the same properties to a. somewhat more marked degree, indicating, in view of the satisfactory materiel made previously in the semi-works. DUP050316265 that til poor results are clue to a disrupted molybdate -sulfate ratio. Another seal-works batch will be made using the same molybdate on a new analysis and further plant work will be based on its results. IXPEHIim^TAL BITAILS see F.3. 4481 pp. 188-192# DUP050316266 Batoh - Bate Control Masatone 7496 M fie rfm shack SWa?462 hut 7459 Luiagj 7i*ada red press wash* 0*1 mol Pndertona = Strength T iat s.str* a *y e lj* Light S ta b ility v.s*worse v*w.s*worse * 7497 11/29/35 check Sf-7462 hut 7459 lump S,dull s trik e at 60 F* 7496 * f.S .d u ll v*v.s.str* s.yell* s.wk* Q.K* 00 <& IB 0 m & d> t* s- U 82 O O 9 * Sm 0 *t t* to CD > > m U o * ^H rO *S * > tJ r4 HI -P * rH p rO f-> r-4 *rt OQ >>43* t3 t1 u 0 H r--l > s M U U u > -P P to 'b* ta # it p # > & 0 H 8>> H -p ft -P 44 > 8 r-l > X> t * *H > T5 41 > * >> P <4J *P # H 43 . > H H H 4> >> 4 >* > > jS ? w r-J bI g CO H ,a 03 p cS * 03 f* H fft <5-2 P ja I o *o O o. iftt>- co i iaj t g SEo s*j-< a i 9~ O Af *W O *H 4o3 o J* t . * s}< t-l t~ m 03 | e 6 ou H o a, <a g bg~ Ch H> xH o o I C3 CO uto +> 5 o ** o 030* U9 m csi to o &o 1n H H -H &s tn TO ft- in m H ft- P00 . 44 II e rM > >> it rf > <0 t 43 09 2*> a ft* f7c4 cr *H H g s^ xa <gmi <N0 OjOo -*HCP llli 44 t> H* o <0 o Joa p* e4ga * P+ >* *P0 ptJ il P P & cS rH H Cm Cm * m # >> ** > (4{ H 0% CQ tr> 4* H fOe Eft2- <0 1 to t <; a XSI H ft* t-i :! 4frt-n*l 1 s If % CD >% * > 5* t 08 43 *P -P H r-| m >* >` 0% |I 1 CO 03 r-1 ?! 13 44 4to3 o m 40 o. IHWUMiwuWBBWia fggFjgxjteik DUP050316267 .a 3* V mm. UBSBUmBL freiflGAgm QJ-1142 Jimill;-- fAA/-/ mi; DATS: BEC1HB1H 1935. liMMail983031 A brief investigation has been made of She use of sodium ferroeyanide for removing copper from lead nitrate. It appears pomsssiible to remote copper quantitatively by this method and the resulting lead nitrate liquor Is satisfactory for the preparation of Y-359-B* A series of experiments ward made for the purpose of determining the effect of varying amounts of lead nitrite la lead nitrate when used in the preparation of Y-359-B, G-589-B, a molybdate orange, Primrose Yellow, and Excelsior ^eliow using laboratory pro cesses. In all oases no harmful effects were observed with 25$ lead nitrite, the largest amount used. A few experiments were run to determine the optimum conditions for the electrolytic removal of copper from lead liquor. > mmmj-m. commswm A study of the possibility of removing copper from lead nitrate by means of sodium ferroeyanide is required to obtain complete removal of the copper* The resulting lead nitrate liquor is satisfactory for the preparation of Y-359-B. The cost is approximately $1*10 per pound copper removed. T^e copper ferroeyanide formed does not filter easily* A series of experiments were run replacing 5, 10, and 25$ of lead nitrate with lead nitrite in G-389-B* Y-359--B, Y-180-B, a molybdate orange and in a Primrose Yellow. In no case was an appreciable effect obtained through the use of lead nitrite* Several experiments were run on the removal of copper from lead nitrate by electrolysis* The process is slow and even after two hours only about 90$ of the copper is removed. She best conditions ^ for removal of copper unaccompanied by lead seem to bexig potential difference of one volt at 160F. The difficulties encountered la the present system of copper flaking off the lead plates are also present in the eletrolytic process. Copper separates out cm both the lead and copper plates during the electrolysis* At en elevated temperature less lead appears to be deposited with the copper* The possibility of using lead powder to remove copper from lead nitrate was investigated. Copper can be removed by the use of lead powder and the resulting lead nitrate liquor is satisfactory for the preparation of Y-359-B* About 8 to 10 times the theoretical quantity of lead powder is required, and this material would probably be quite expensive* DUP050316268 m m assK sr - wmm Cbebook'#452* .#52*6? purification of lead nitrate lienor with yellow pruaslate of soda* The use of yellow prussiate of soda gave results equal t those mad from lead nitrate crystals,, hut was very difficult to filter lit the. laboratory,, ` '.l 4S%MK* study the effect of partially suhstituting lead nitrite for lead hitrot.; on Sfedltm Yellow, Y*339B# KO marked affeet was observed fro substituting lead nitrite for part of the lead nitrate. Cheek 452-6? series* Results obtained in this experiment were very similar to those obtained in series 462*6? 452*70 Study the effect of varying amounts of lead nitrite oa molybdate orange* Wo appreciable effect was obtained from substituting lead nitrite for part of the lead nitrate* 452*71 Study effect of varying amounts of lead nitrite on Primrose Yellow* Lead nitrite had little effect on the tinctorial properties or light fastness of the yellow* 452*76 Study lead nitrate liquor purification using powdered lead* The use of powdered lead to remove impurities in lead nitrate liquor gave material purified enough to give satisfactory f8SS0*E* 452*78 Study effect partial substitution of lead nitrite for lead nitrate in G~389D* Wo appreciable effect was obtained In this experiment from the substitution of lead nitrite for lead nitrate on the Glen Green type of Green* 452*76 - Check 482*710 fusing 9$ lead nitrite sub stitution for lead nitrate)* Substituting lead nitrite for lead nitrate has little or no effect on the Primrose pigment obtained* 453*77 0heok 452*75 (0-389*5 Green}* In this experiment a v*v,s,chalky and "si* weak product was obtained from the lead nitrite substitution (about 9%} for lead nitrate; this difference could have DUP050316269 'M7*. >: S' :; a* r- v^". .** 9t' * \bean' toe to experimental errors. 458*%jfr * study effect of lead nitrite on Y*18G*li* 3& appreciable difference was obtained from the lead nitrite substitution* 452*86 ~ To purify lead nitrate liquor by electroplating copper out of solution* The process is slow and even aftpr two hours only about 80j of the Copper is reacted* The best conditions for removal of copper unaccompanied by lead seem to be a potential difference of one volt at 160 P* AbouC ISOdp the solution takes on a yellow east after an electrical current has been passed through; it* **;* DUP050316270 rawm, HWiraPBl JLT- ^>2-- _TM_^ gPBMITTSB BY: / -------- APFROFB BYi ^/ HBtRQgqPTKT FUJI: / /*. / ~~s 'DATS: ESCHStBSR 1955. Work has'been conducted in the semi-works on the purification of lead nitrate by the precipitation of copper with sodium ferrooyanide# fitei..,...smbrnm. Five purifications have been carried out with a sixth in process# The variables studied have been temperature and time of precipitation. It has been found that precipitation et 110F brought about a subtly more efficient use of the *P*S. and the formation of a precipitate which was much more readily filtered than when the reaction was carried out at 60F. Slower precipitation gave a slightly easier precipitate to filter* The purification, as judged by the quality of Y-359-D made from the purified material, was quite satisfactory. Analyses of the solutions and residues have not yet been carried out* A batch is in process to determine the feasibility of gravity filtration* 1 DU P050316271 *8 w&mmmr&i, e b t a iia See notebook f49S pp. 100-10?* Batcti #Y.F.S./ Temp. #Fb(R0g)s Precipitation Time Filtration Press Cake Rat Yolume Sal/sq.ft./ cu.ft. bn* Lump Wt, of Res* 7549 7S55 7560 7565 7565 .0280 *0258 *0206 .0205 ,0218 0 60 P 80F 110F 110 F 60F 5 mins. 30 mins. 5 mins. 30 mins. 3 mins* 2*7 3*8 7.2 14*1 5.5 ** .173 .110 212 7 lbs. 9 6n 4-l/S " 6-l/s DUP050316272 :.n<mmT WM. mmmoM mpmv 3S~- </2JS SffffiBTTlDBT: a p mom b y ? inss-eOTB-fflwr^ DATS: BSeiMBE 1955. ! *am. Work lias been continued in the sent-works and plant on the study of tbs new laboratory formula, Sxp* 438-89-A, mentioned in tie Ho t ember report, to obtain a G-389-B type green with about 15$ additional strength* Strength, increases over the present standard have been obtained in the semi-works to about the same degree as in the laboratory* As compared to edmpetitiye samples, the new procedure gives material too blue and clean to allow of an accurate strength comparison. The best semi**works results appear, however, to be about equal to competition in strength* In an attempt to obtain more olive and strong material, a laboratory series (Sxp. 363-66} was run to study the effect of increasing the pH of the greening yellow and green slurries. Increased oliveness was obtained, but no additional strength* A board mix demonstrated that strength of the type shown by C-37984 can be obtained by mixing G-389-D standard with very small amounts (about 0*2$) of carbon bleok* The laboratory provision for the washing of the finished yellow was early eliminated from the semi-works procedure as being in convenient and doubtful as to its results* Washing the finished green appeared to have little effeot on the strength of this color either by semi-works test or by laboratory washing of plant or seml-worka slurries* (Experiments 383-64 and 363-65) Accordingly only standard washing was applied to the first three plant batches* These batches, (like some semi-works batches), ^ although superior in strength to standard, did not possess the full strength ? advantage obtained in the semi-works and laboratory. One plant batch made strictly according to the laboratory formula brought about no bettemment of the situation* The light fastness of all batches compared favorably with * that of standard. * restraining action of sodium sulfide was demonstrated by the dirtiness, oliveness and ehangeableness of one semi-works batch in which this ingredient was not used* Only very small amounts of sodium sulfide appear to be necessary, however, since no difference was noted between two plant batches, one containing 80$ and the other 40$ of the standard formula amount* i: DUP050316273 4* p a S3 c5 rl 5 Eh H rH H O 40 O a m M H rH | 43 in 4& b0 bq j3 2O 13 43 *h 49 +3 To 4 CO tn S3 O u p * O fe 43 * At O sP a 40 s! 0 40 0 rH *gcs * tiO S3 cd P rH cC iH O H i--t I <*$ t, O 1w A # -p 40 e Cl cn I CO ttl4 s * s *T5 S3 0$ <j> ty* u H 0$ 1 c O * to 15 W b- tISo. CO - A fc- O 2 I S E~ si W39 T 9H r-t m ,a 43 o --33 ^2 rH O .10 <*a Ai CO to * 4o4 P o o S* 43 49 1O3 4H S3 <a B (DO w <9 ri! U cd 7X 48 4> CO S"i 5* 03 0 g fe HI S3 pH c5 S3 f> 3 rH W H O m l> bO S3 O U 4 s4 0. ta fe O rH S H H > O >> l* 4 J4 H *ts S3 c5 r*H O S3 cti H tso S3 bD bp O 13 S3 U O hO O 4s U S3 Sh -P 49 Sh n 4 0 * to S3 rH rH O 43 a T3 fid S3 C ed cd * H S3 rH cd 3 rH rH 43 O I> a T" O bfl < P 49 tiO b0 0 S3 S3 u 0 O O 49 U * 49 p > b > V) > S3 d 75 HI H O 45 m tn & H O 0 tt H O 4 > 08 T9 *rt to A +> 2 fcD-l H .D js m> > t 43 o CW i 49 sl *X3 AS in H ' $4 ** s 8* H 4* -rl .0 n l <*l o sto to M CO CO p g* Oh j Q t- fc> o wM 44 u JU M o (9 410A j O 49 ` o O tO 43 3 to rH *CS p 08 td |o ^ O S3 & H 49 rH i. Q> H *H e 0 to w >* _ 49 * $4 H o 9 m . DO a> B > Cj H rl A OO M U g3 'tJ S3 O 5 rH H rH > O 5 0 HH rH >1 44 rH fid 43 it* s a s12 CM 6 *rl 44 5H P< ** 45 0 rH ns 0* * $> tt & O0 rH rH rH rH >1 p O rn H 43 s M rH 43 nd S3 g> 5 44 Ih %5t,, 0$ flJ rH Jh tJ * "S A . O 44 o o *5 49 23 **d tn 0 m# SP 0 m rH 3 8f 4* cJ 43 -H H 0 SD 0 bO CO Im 49 to 49 to 4? 0 rH in fc- * jrf *tt-r PQ d in P *- 2 44 u rH sd in p |f*r O 43 44 P 43 4> O O M 05 % J *3 45 o 43 ** O 30 c 13 oo to d to CJ O 63 CO 43 <2 40 ^ ttf>) ffl I(p Si 5 43 43 o rH iH I f*"' 4* ca S3 O to m tf- tr* to CM 0 rH CM CM CO tn in in m fe- fc* fc** t!-- fflHI * O PJ Cf> > CO 0 tO to wmww mmm DUP050316274 m i gjp. om&m mmm. g -589~b SUEMITTSB BTt APPHOTfB BTt <>,v Ell: KB8EMBSR 1955# imoBEGTie^ Greens of this line were kept under observation during the month. The difficulties previously encountered have been at least oartielly overcome as indicated in the ladt report# However, all the variations frcm standards persist to a slight degree and the blueness of mas stone, especially in the dark shade (5-39 8-E, had required further adjustment of the formula* mmmr jm eowazmicm G~389*i)# This is the most important member of the line and is in a fairly satisfactory position. Olive material for shading was produced by use of the full amount of soda ash {alum ratio 30:9) in the yellow treatment on standard formula. This produet was somewhat changeable but was used for blending. Omission of sodium sulphide resulted in an off changeable green. The restraining action of this ingredient is definitely established. Use of a double amount at this shed caused slight dirtiness in masstone and tint and in one case increased the tendency of the masstone to lighten on standing# Practically all of this shade is being struck at 75P and the bichromate is being varied from 580 to 595# per 5 mol charge to control blueness and yellowness of masstone* About 41,000# were blended during Beoember to date,, of which 28000# were for use in lacquer and the balance for paint. G-590-D - t this shade the 595# bichromate formula appears to be best although usually it gives too greet blueness. Use of higher alkalinity in yellow treatment gave a more unstable product than at 6-389-D resulting in a definitely changeable green, This shade exhibits more difference in flooding {greater lightening of masstone) as compared to its standard than do the other shades. It should be noted that the G-390-B stendard was a mix of G-389-B and G-891-B reground* G-391-B and G-392*>E The two dark shades are giving the most trouble at present in respect to blueness of masstone. The degree to which the yellow can be modified is limited because of the greater instability when shaded to these depths* Most of the present production is being graded very slightly or slightly changeable and variables which increase oliveness increase changeability. DUP050316275 Use of ./blue of redder types - SSS B-59-ID and red B-66-D liquor - has not been very successful oh G~39&2) Where olivesess is obtained by this means it is accompanied by loss in brightness * It is believed that with present known variables the best procedure is to make the type of yellow which is most stable but not too green, shade it with B-66-D of standard shad and bright ness and employ G-346-B in small amounts to match standard in. olive ness. The last mix of G*>392-B {8724#} was made up with 3.6# G-345-B and appears to be satisfactory although very slightly worse In light stability. Attention should be called to differences in standardi zation between rubouts and rubber tests. In order to obtain material satisfactory in rubber, it is necessary to shade considerably on the yellow side by rubout. New standard, (G-515-D and G-316-D) were set up for shades corresponding to G-390-B and G-391-B* EXPERIMENTAL DETAILS Found in Plant Control Book, Production for the month consisted of 24 batches of G-389-D, 4 batches of G-390-D 6 batches of G-391-L, and 16 batches of G-392-D, S DUP050316276 3~-9*s^ ElfflW OSM BBBBABCff REPORT SUBKITTBP BY: o&. a p p r o v e d BY: ^ gOTMtSBR '? KS069 oS/'^ FILS: qnnoME cmgara b a t s : BUCSMBSR 1955, INTRODTTCTIQHT One batch each of the ingredients for this improved extended green of G-X-S79-B type was made in the plant. The formulas need were previously developed in the laboratory for an extended green, K-8G14; extended B-.140-B, K-7959; and an jextended K-8008 SBMAFY AMD SdrQLtJBIOWS A 5700# mix was made up and is to he shipped to the customer, Armstrong Cork Go. This cheeked the laboratory sample, K-8G09 closely except for very slight dirtiness of tint, due to dirtiness in the green constituent which will be corrected on future manufacture. Some difficulty was encountered in washing the BX-7957-D because of the presence of sodium oleate in the formula. It is' possible to omit this soap without any harmful effect on the finished product* Part of the green was pressed out as G.p. color in order to reduce batch size. This portion took fire during grinding without any apparent cause* The fire occurred in the hopper instead of the mill, BXFfRXMEHTAL H5TAIL8 W*B, 457. K*-8014, 46298 - 2 mol charge, using G-409-B, yellow instead of K-7764 yellow given in formula* Fo copper hydroxide was used* Vs K-8014 - dark blue dirty; blue & dirty. Part of this batch pressed out as G-41Q-D lot 46541* E-7957__ 46S97 - 165# B-I40-B raw slurry extended using sodium oleate as in K formula. Washing very poor. Vs E-7957 - s.dark; strong. Greenish cast, K-80G8 46285 - 267# B-66-D raw slurry extended as in K*-#, Vw E>8QG8 - 3, dark, blue oast; v.s.str} s.strong; s,red dirty* DUP050316277 * K~8003 Lot 10865 - Mads up of above ingredients in formula proportions# with addition of china clay to obtain proper strength* Ys K-8009 - T.s.dk* & brtj v.-s .str , & dirty; 5~l/g% str; v*s,yellow and dirty, wt. 5?00ir * dp.Gr. r s,633 *w..y DUP050316278 P10MEKY COLOR RESEARCH REPORT YIELD STUDIES ON IRON BW SUBMITTED BY* APPROVED BY: FILS: *8GS~-Bi3S 2/^ V DATE: DECEMBER 1935. INTRODUCTION The yield study on Iron Blues was concluded during the past month. The results obtained during the entire study are summarized in the letter of a .m.E* to R.A.K. I218**35, SUMMARY AND CONCLUSIONS During the past month the goal yields of two additional blues were determined. The goal yield for B**147**D on an anhydrous basis per mol Y.P.S. is 507*4# The goal yield for B.15SD on an anhydrous basis per mol Y.P.S. is 352.5. EXPERIMENTAL DETAILS Notebook 463* B~I47D Standard Bme 468--55 - Series based On plant formula of B<*147~E> standard. 468-55A 55B 53C B*147 D SD-47148 B*.147~D* As is Yield H2O Anhydrous Houes dried at per 0*4 mol# Toluol Method Yield per 140F in Elec.ov* mol of _____________ Y.P.S*___________________________ 125 m 125 m. 127 * m 1.60 1.66 3.20 3.70 307*50 307.33 307*35 33 88 88 - Average yield per mol of yellow prussiate of soda 307*39 gm In rubouts all were on the red and strong side of standard B*152D Standard Blue 468*54 - Series based on plant formula.of B-152-D standard. DUP050316279 P*^f r! r*' ?i:.; , . ..: * ' ' V' B*1*M 8IMI8983 - ' ,S:>. Af is YXM& ',yrn S*4 'mdl. ^S0 Ankrdrons foliol Method BeM psr mol _ Qf.Y*?.g*....____________________________________________________ 3~:: Hours in fleet* drier at I40of* * , isaus . * 151*5 9*0 6,6 ?.2 11,6 3S1#78 554*45 351*35 ' m m 88 '=; u, Average yield per mol of Yellow Prussiate of Sofia 352*52* ' * Ail were on the brownI sh blfclc and strong aide of standard B152-B* # A r-iVi DUP050316280 ?!sgg? c o l o r mmm.CE b ip o r t "LITHOSOL* Hm SB LAKH, BM-417-D SUBMITTED BY: C. APffiOTO BY: ^ roiBi MISO..MS mi: BBCKMEIK- 1935 IKYRODTJCTIOB Production was started in the plant during the month on this color, two hatches being made with a total estimated yield of 722 lbs. Results on only one of these batches are available for report. SUMMARY & COBCLUSIOKS The first batch was made checking the standard K-7909 formulation and using "Lithosol* Red 2B* lot 5 which had given satisfactory results on test in the Semi-works using the K-7853 toner formula. (Bote that RM-417-D is K-7853 toner extended with a Gloss White base). Results on this hatch were fairly satisfactory, testing v.s. dark and muddy, slightly strong and v.s. blue and clean versus the standard. A toner control from this plant batch gave practically check results to the toner secured in the Semi-Works using *Lithosol" Red SB dye. lot 5. A 500 lb. batch of the lake is now in process, results on which will be reported next month. production is tabulated in Table 1 jjXBBRIMKETTAL RETAILS B.B. 457. page 150 DUP050316281 4 g C<H3O* C0M2 a rH lii rO m> Ho f*e* C3 fH rH & Sf3t*S!J Ak$4 ^*J33>-SP-. " IS *$>3 <r> S3 rH 02 ^ 3a*^68 "8 CO om O Gt*O" s&i f<-&. , I53 a.s ?! 0<p3& S3 aS rH r<H0 {H O > >a SO -P }> to *P *SGP* Vk 3 *iJ - & C<yO E> ,1 5X ts <OJJ3* 4fil * f-H ' 6 Afc4 rAH 4 1&3 ttoo. t*o* m < * DUP050316282 gpwppg n * i Uni i m n/fiiM mmwmTm .grt 4FBR0W mt "-- *2*?^. KHl!'4WaW*BHMr BATS: BS5EMBSR 193S* mmIMSiiimS Work on the Pigment Breen B problem in the laboratory was confined this month to studies on the preparation of dry colors for rubber and paper coating* zm~~ fari at lone in the lakiag procedures on the alumina hydrate lakes of Pigment Breen B and the use of diglyeol stearate has resulted in an improved fifty percent lake* The dry pigment when milled Into rubber is only approximately ten percent weaker than the latex dispersed Breen FB* Although further improvement of the dry color is possible, the additional work required does not appear justified at this time* Studies on the duplicability of the laking process and rubber dispersions are proposed, which, if satisfactory will be followed by the preparation of a large sample for testing and evaluation by the DuPont lubber Shemicals Division* Daring this month, the reason for the poor water wetting properties and the poor dispersion of lakes prepared by wet mixing G1-407-D with extenders containing alumina hydrate. Was uncovered* It was found that the responsible factor was the alumina hydrate possibly due to some chemical reaction between the hydrate and the sodium resinate in the green or to some physical effect of the hydrate upon the green* However, it was shown that GL-4Q?**D may be wet mixed with china clay before drying and then further dry mixed with hydrate without; obtaining any different results than a dry mix of all of the ingredients* Wet mixing seems necessary to obtain satisfactory dry appearance* The composition of the lake which is apparently satisfactory from the standpoint of full strength color by the brushout test is 20$ GL*409*>D, 70$ china clay, 10$ #3 Hydrate* The completion of this problem awaits the development of a satisfactory GL-407-D frcm the standpoint of water dispersion which is apparently dependent in turn upon suitable drum drying conditions* Lakes prepared from semi-works tray dried GL-407-B do not exhibit very good dispersion by the brushout test, especially when flinted EJFSRIMMTAh _BBTAI.L3-- Pigment Green B Lake for Rubber* Experiments 29, 31, S3 & 33 - H.B. 432, pp. 90,94, 98 and 103 respectively* respectively* Figment Green B toy dispersible lake for paper coating* Experiments 26, 8S5, 38 and 30 H*B* 482, pp* 82, 84, 92 DUP050316283 &sr~ PISHHf SOLOR RESEARCH REPORT StJBlIITTgB BY: iFEftQVBD BY: JL FILE: IW^HI-WWaflWWgDATE: DECEMBER 1936* mi mi p Laboratory studies on vat dye pigments this month, were divided into three distinct problems, as follows: (a) The preparation of a lake of "Ponsol" Jade Green Supra for latex, requested by the DuPont Rubber Chemicals Dept# fastness* (b) A Violet superior to rtPoasl" Vioxet AR in light (c) General Ifeking studies# SUMMARY AMD CONCLUSIONS Tests conducted by the DuPont Rubber Laboratory on 'Tonsor'Jade Green Supra resulted in pastel shades which closely approxlasted the shade of Guignet' s Green (chromium tetrahydroxide) However, latex dispersion of this green vat dye resulted in wide variations tinetorially from batch to bstoh of dye, these differences being caused presumably by variation in the dispersion of the dye. Pigments pre pared by first solubilizing the dye with rosin size prior to laking resulted in colored rubber superior to that obtained with the corresponding lake from untreated dye, in tinctorial and dispersion properties* The results of previous experience on the preparation of lakes from solubilized vat dyes indicated the possibility of controlling the dispersion of the dye and consequently also the tinetorlal properties of the lake in this manner, whereby variation in the dispersion of the original dye would have no influence* fork on this problem has reached a point where It is now necessary to check the duplieability of the laking process, using various batches of dye* Following this, the preparation of a large sample for evaluation by the DuPont Rubber Laboratory will be in order. Lakes of vat dye violets of better light fastness than "Ponsol"Violet aR have been prepared from^Ponsol" Violet SR(dichlor~iso~ dibenz anthrone) and from "Ponsol" Brillian%iolet 4RN (chlorinated brom-iso-violanthrone) However, the improvement in light fastness is not significant since both the 2R and 4 RtT Violet lakes are very much redder tinetorially than Violet AR ana the former less satisfactory for blending with blue lakes, etc* A lake prepared from "Ponaol" Red G SB (ethylateddi<* pyrazole-dianthrone) was a dull medium red of no apparent interest* A lake of ''Ponsol" Blue GL on Eailite, a silicous earth material used as a substratum, is Frantically similar to the DUP050316284 <Sf mi L '"* ' 4* '* *. :; **u ' ' ' ' *. * corresponding alumina hydrate lake timetortally and in llgbtfastnees* Kallite may be of interest as a substitute for alumina hydrats in colors for lacquer sad "Lulux" in which the alumina hydrate has a deleterious effect. The combined treatment of a 7W$ lake of "Fmsol* Blue #WL on Kallite with diglycol stearate and mineral spirits* and subsequent colloid milling resulted in an appreciable improvement in strength over the untreated alumina hydrate lake and work along this line appears to ' possess some promise* > Lakes of "Bonsai" Jads seen Supra for Rubber, Regular dyes paste* Hosin Sim dispersible dye* Bextrih dispersible dye# Biglycol stearate treatment* SO# alumina hydrate lakes* Bry ahd pulp colors in rubber* Mixed blano fixe-alumina hydrate lake* Experiments 487-40 and 44* N*B* 487* pp. 146 and 156* lakes of "Ponsol" Violet SB* "Ponsol" Brilliant Violet 4KK and "Ponsol" Bed G-2B* Experiments 477-5, EF.B, 477* p. 18* Lakes of "Ponsol" Blue QL da Alumina Hydrate and Kallite* Experiments 23 & 24, H.B* 470* pp-92-95* ... t DUP050316285 WXm% MBt A IS35 . - investigation of1 sow intermediate, dyes eta.was coo- 'M fined IMs month to only one iste:na8diate, namely 8:4 dicblor idl& ^ * MflnJUk M* '* ||^s and eora^amending pigigfiitii of tto llslt earth wrtsal a alto tare preiHired in the laboratory from AMsotissed 2*4 ifbier aa*ili* # ohlfcrei acid aitei with Cal iPfftf* (b) 2 aapittol 3 *rbe*yli acid. TIi barium and calcium. toners of the beta aaphthol c agination are very dail orange la color, varying only slightly in depth and shade. Both pigments art very dull in aaastoia. shad and tint compared -with Peraaten Orange XT-241~B, and both possess eonsMemhl oil solubility and poor lightrastness. Pigments prepared fro subject dye possess t o apparent farraise and warrant no further investigation. The beta-oxynaphthoic acid ablnatios possesses some interest# sine the alkali earth metal salts thereof vary in color fro very- light Bright yellowish red to sodium Bluish shad red* The harinn* strontium, and calcium tenors are practically insoluble in linseed oil but possess only fair light stability, being inferior to Llthol Rublaae pigments fBTSSA 902 da) Tha Calcium toner is bright but very wash lighter and yellower than Lithol Rubin in both lake and toner form. The ealeimt pigment closely approximates the general tinctorial properties of Toluidim Red RT-3B-, whereas the bar3ms and strontium pigments are lighter and yellower than the ealeita#* Altho pigments of subject dye are of interest, they apparently possess insufficient merit to warrant farther investigation* However, further investigation of other dyes of 0s 4 dioh1oranilIn 0 sulfonic acid appears worthy of ooxw iteration. sEmam&jsatBB, 2:4 dichlcsraniline Bxpt. 34, *.B. 487# 0 sulfonic acid --* p. 126 beta-naphthol ^Ba **^<Sa toner tenor 2:4 2 mpfctbol 3 carboxylic acid ypa toner tenor Bbtpt. 39, F.B* 487, p. 142 2*4 dichlaraniline 6 sulfonic aeid 2 naphfehol 3 carboxylic aeM Cal Bartua toner (b| strontium toner (o) Caloima toner It DU P050316286 3 S'- ** smsmm) 3t* awo,# W BYt c^^c-^ ** ITOOOTSflOS /&/ FIXE: P8W3-i~IL BATES BE0J8MBER 1935 The evaluation of flushed F.T*A* pigments has been continued by flushing experiments on the ink mill, with a spatula and in the vacuum mixer* smmmY am G&mmsiQm Flushed inks of ST**347* in #0 regular varnish show no advantage In tinting strength* body and length and slight advantage in texture and flow ever corresponding dry control inks* Duplicate experiments show that in hand flushing with a spatula, the apparent tinting strength of BT<*X0OBj #0 regular varnish inks increases if.the ink is left spread out on the board for a short time* Indications are that BT*100D flushed into #0 regular varnish in a vacuum mixer gives an ink with no advantage in strength over a corresponding dry control ink* Analytical results on the pigment content of all completed inks obtained by the ashing method and by the extraction method agree very well with the theoretical pigment contents of the inks* REVIEW OF PREVIOUS WORK GT*547*D has been flushed into #0 regular varnish by two different investigators {see 469* S, 3S) in the following manner. Various percentages (0, 50, 75, and 100$*} of #0 regular varnish were added to 0TM7*D slurries (either pi ant or laboratory slurries). The mixtures were stirred for 10 minutes, heated to the boil for 8 to 3 minutes and quenched* , There was no great difference in the rate of settling* After filtering, the samples were run over the iuk mill and the resulting inks compared* There was no advantage in tinting strength of the flushed inks over corresponding dry oontrol inks although there were some differences in other ink properties. The toner contents of these inks were checked by ash analysis. Therevwas only a trace of water in the inks* DUP050316287 DUP050316288 The results nu|i 3fe?>p obtained with otJr *fT#A* pigments ta.that the flushed inks have equal tinting strength, n^estone,, undertone, length*'tody and- lightfaatness but better texture and flow. as eompared to corresponding try control inks* These conclusions are based a three duplicate experiments eaeh of which gave the same results* Inhere was a consistent improvement is texture and flow for th fluked Saks although the differences were slight# It is considered that in regard to tintlag strength* this experiment confirms earlier experiments (see 469*S, S2) there the oil was. added to GT*347**B slurry which was subsequently boiled* he flushed inks produced by this method Showed no increase in tinting strength over corresponding'dry control inks# This experiment was carried out at the Berlin laboratory without having the optimum conditions so that at the end of two hours mixing there was still 18$ of water emulsified in the ink* This water was removed from part of this emulsion by six passes over the hot ink mill* The BT100"Bj #0 regular varnish flushed ink prepared ia this manner shewed no advantage in tinting strength over a dry control ink# In other properties it is similar to inks prepared by flushing on the ink mill* Evaluation of texture test for gTA pigment inks^ Tn order to evaluate the texture of iron blue inks# a set of arbitrary standard slides has been prepared* Similar slides of the inks to be evaluated are prepared by means of the texture wedge procedure an compared to the standards as to the number, size and distribution of specks on the slide* It has been found that an BT*389- flushed ink with am arbitrary texture rating of 19<fe is reduced to an arbitrary rating of IS by the addition of 1$ of"Aloxite 400" (on the basis of ink as 100$}. (400 alumina particles laid end to end equal one inch}* The visible particles ia P.T*A# pigment inks apparently are intermediate in size between "Aloxlte 400" and "Aloxite 600"* It requires a greater percentage (approx. m of"Aloxlte 600" to reduce 19* standard to 16 standard but it is difficult to make accurate comparisons when the particles are so small* ' On the basis of the above experimental evidence, it is apparent that an increase in tinting strength does not necessarily parallel an improvement ia texture# At least this Is true until further refinements ia the texture test are made including some correlation between size and number of visible specks Band flushing of BT*10Q~B with spatula^. duplicate experiments confirm that if a pulp is flushed on the board with a spatula, the time the ink is left on the board is an DUP050316289 important factor in the apparent tinting strength. If the ink is left spread out on the board for 1 to 8 hours, the yield of ink picked up from-the board is smaller and the apparent tinting strength is greater, which Indicates that some of the oil is probably partially oxidized and is not picked up from the board# Duplicate experiments with BT100D showed a 3$ apparent increase in tinting strength when the ink was left spread out on the board for 1*5'hours* flushing of Bf100<p into various vehicles _ BT1Q0D will not flush into Mazoot oil even when kadox is added but mixes to giro an emulsion* If sufficient blown castor oil is added, flushing occurs# BT*100**B will not flush into Kujol or petrolatum but mixes to give emulsions# Analytical results on pigment content of completed inks* fhe pigment contents of the various ink samples obtained by the ash method and the extraction in the centrifuge method are summarized in Table II* This analytical work was carried out by 3*W* Bumbel* DUP050316290 it*. I#, ....... r 8 * Sample code % Moisture % Asb $ Pigment i> Figment by <> Pigment __ __________ r.,,....... M.mkm__ ssteaa&agL.. by theory A i & '-ITS*. *4SAi -IBB? mg -80A1 *S03. *e o 4 -20B2 89Ai - msx -29Ag 29Bg 29AS iSV5g* * n n MV100-B ft tr BT-123-D It f G3*S47*D w ft It n f? 0*1 * *2 *1 1 *1 *1 2 1 1 *3 1 *1 *1 483-l?l> 18D BIB -to -to BT~3S9B BT-100-B t B-125B CT-347-B gBS.MJte,,,,Sag. 58309 210 211 213 230 232 Hllton-Bavia W ft ara-Fry Adeo Slierwin*%as. tt n 3*3 5*8 0*8 *5 .1 *8 32*7432*61 38*m 38*46. 31*74 31*8 88*19 87.96 19*87 29*08 19*96 19*64 36*01 36*25 36*23 34*90 35*01 35*20 ' 05*60 63*19 66*44 49*31 69*74 49*91 49*71 50*15 49*48 80*83 49.57 49*93 49*54 40*29 40*66 40*46 39.61 50*23 60*54 60*52 50*04 50*20 50*47 100*00 100*00 100*00 100*00 100*00 51.28 61*25 51*23 0*88 ' 52*83 61*86 61*98 51*31 40*91 46*30 48*67 41*67 50*01 50*02 50*00 60*00 60*00 50*00 50*00 30*0 80*00 60*00 40*00 40.00 40*00 40.00 50*00 50*00 50.00 50*00 50*00 100*00 100*00 100*00 100.00 100.00 ;'i '. s-J- DU P050316291 isaom ft ** i. See notebook $483*. J*=8. Evaluation of texture test wits. BT*100B* 48526 *> Flushing of BT100*D Into various vehicles* .MS8-S Flushing of MV1Q0*I> in vacuum mixer at Pari in* 483-29 * Quantitative evaluation of GT-347-B flushed and dry control -er inks Band flushing experiments of B3T-1Q0--B* Aj_# 3*70 g. BflGGD pulp was rutted three times, once every hour, in 2 g of varnish dryer over a large area# AS# Duplicate of Ax* Bj* 5*70 g BT-100-B pulp was rutted three times, once every half hour in S g of varnish dryer over similar area to Aj_> Bg* Duplicate of B^* "1 * 3*70 g of BT--100--D was rutbed three times as quickly as possible* Besuites Bi 5$ strong vs 01 Ox s Og Bg 3$ strong vs Og Bj g Bg A^ and Ag had livered badly and tints were weak# MSS L DUP050316292 'V 9** , 4/ ' " '>* / `.':?': >J SSKBpITTSD BY: 9/C maM*$ PJ>MWW& BY: /<&/ y il b j p-icagaKgg..nr 'Oiip BASS: BSG'EMBBB 19*5. A preliminary co~op#rative study with Philaaeildiia on the use of flushed Lithol Bet in "Bulux" and urea*femaldehyll'e formulations has been completed. Some improvement has been obtained through the use of flushed Lithol led in the urea-formaldehyde fomul at ion. ' ' Accurate evaluation of inks consisting of Lithol Red**#0 regular varnish (1:1) flushed on the ink frill against oorresponding dry control inks Indicate that the flushed inks are improved in textuBe but show no improvement in tinting strength, flow, mas stone, etc* &B7I5W OY PREVIOUS WORK The immediate effect of treating pigments with a vegetable oil under various conditions is summarized in Table I not only for Lithol Red but for other toners that have been treated with oil as recorded in the various experimental notebooks. IS r k I k DUP050316293 % Passes m ill e a s ily w ith 100# o il* HOrt r-i s%- ~( Av> (0 v> 3 60 fl gh-* <D *m r& H ow O r--i HOO 9 t ato H 33 so 4 4H r-i <QQ J O3 A r3-i ftei ro-i 4t3il r3-i fe. U r-i S +w> g~* la to Sfg rC4* 4O- r-l sm oo .3 ** 8 <5 3 r-i SO3 N ra+> + *oa 4 +> +3 j*d> P. CT 0r--f r-4 fH r-i & H p, P rr9--1>i P. 4 4p-< H--$' CO a 6C 1 d O fr* &O* ca 14 *r< t 2 iH s CO e 8wt JL e$ oa as* ? ' *?*? ** t* sse0a 59 Si noom4tfr CO 9 stlios os H1 Hto <4* ca ^ fr- c- ??r-JOS CtP C*?b *CHi 59 % 8 8 451-19 reen B <H*68P 1 cj OHI . * g i P *? 1 cr 1 i' ca co to t Ir0-i $ 4* 1 a Irt It*i r4 & o 5 00I2 i .. * a t f s 1 i t A f u fi -c pc; 4 OS I 34 g i OOP *4 p i ii jv-. DU P050316294 m , Is general, Mthol Bed toners flush successfully Sato a ^ vegetable oil on tbs ink mill a a t a "pellet* stage by .stirring-with oil. This ease of transfer makes .it impractical to aas litkoi 'Bad slurry throng a colloid mill with any more than a small amount of oil because of the tendency for the ink to gins up the mill* ithol. Bed-Blown Pastor Ml (H-lgQ) ..inks in.. Brea- lithol Bed-Blown Gastor Gil (itl) inks tested in a mres-forraaldehyae resin formula indicate that roller milling grinding of try color results in increased gloss over ball milling* (See Pigments in Gil report for 'September 1935J * Flushed, inks* in general, show better gloss, dispersion and fineness than a corresponding dry control ink ground on the ink mill but the difference is very slight* The maimer in which the ink is prepared seems to have but slight effeet on the quality of enamel produced* The methods of preparation of the inks are listed in the order of quality of gloss obtained: Best gloss: Slurry colloid milled with 12*5$ oil and then passed over the ink mill with 87*5$ oil additional* Second best gloss: Flushed on ink mill with 100$ oil* Third best gloss: Colloid milled with 12*5$ oil. Dried at 1401* Ground on ink mill with 8V*5$ additional oil* Poorest gloss: Dry color ground on ink mill with 100$ oil* It should be emphasized that the above differences in gloss are very slight. It is not known for odrtein where the "pellet** technique samples fit into the above rating as one sample of small uniform pellets gave better gloss and one sample of pellets of various sizes gave poorer gloss than a corresponding dry control ink* The Lithol Red-Blown Castor Oil (1:1) inks are suitable for testing but the ratio of pigment to total vehicles W8S increased from the usual ratio of 18:100 to 85:100 in order to make the test more sensitive* The inks were dispersed in the urea-formaldehyde solution with a "wizzer" which represented the best mixing conditions obtainable in the plant without grinding* There were 25 to 50 smell specks on the panels caused possibly by undispersed ink. The enamels were not felted* The urea-formaldehyde enamels produced with the flushed inks are satisfactory in every way indicating enamels can be prepared by simple mixing without ball mill grinding* DU P050316295 ...........Jii'' ''. ,J_.,,..> ..., ., srsn* *!P^WS5SSS,."ZL'W-iWfe iff. .u\f$n.;vM^i" Jfrjiis Lithol Refl flashed o r the Ink mill into 200$ of RC-8Q5 resin (resin end thinner) was badly skinned When tested and showed no improvement in the fineness test ofer a ballmillefi control. This flnshed sample'may have contained a considerable amount of water* Samples prepared by colloid milling Lithol Red slurry with 10$ of various resins, filtering and drying proved to be unsatisfactory since they gave poorer results than the untreated pigment even on grinding,, It is supposed that these poor results are due to the drying of the small amount of vehicle around the pigment protesting iVfrom the wetting action of the new vehicle rather than adding it, The following table shows the results obtained on grinding these pigments in small mills along with the untreated dry controls Sample 485*5A *50 5B *51 ~5F -50 *5H *51 XABfiUa GRIPPING Of "DUIHS" TREATED LITHOL BSD Flrujaess Resin 4 hrs. 44 hrs* Gloss oontrol 4 BE0*953*77 2 n 76 4 n 75 4 n 74 4 rt 73 4 79 4 ft 78 1.5 S <** 3 3 4 3 2*5 *# fair flat poor ft ft If t* The ebove table shows that although 483*50 and 483*51 (when examined on a glops slide) had apparently been ground fine enough after 4 hours, they did not make enamels with satisfactory gloss, indies ting that the necessary dispersion had not been obtained. The other samples at 4 hours were no better than the control and prolonged grinding had little effect on them, while the control ground in the usual time. Critical Evaluation of Flushed and Dry Control Lithol Red ilates* See Table III for e tabulation of the results obtained in three duplicate quantitative experiments when Lithol Red{?fO regular varnish (1:1) inks prepared by flushing the pulp on the ink mill are compared to corresponding dry control inks. For more information on the method of preparation of these samples for comparison, see the detailed procedure in the "Flushed PTa Pigments" report for November 1935, It is emphasized that these results were obtained by making duplicate experiments on a single plant batch of Lithol Red and might vary with other batches. DUP050316296 rH *T <S t to to i ** to* IE 5toO H H % H tn X> "8 < 4? r A *si 08 ?3I >* TG* I bd 0 AS a 4 d SJ to- HS-StrH rO 0 ta *W *0 I & HI .3 3 E0 O M S3 S3 l P 00 oo r-4 o H XJ *0 fw p o p H CQ 5* r4 Ato 0 o S3 <e > to* 0 S 5 ctf <e 0 jo M S3 m *8 < H c P M -P > a s <a O O.fl'ti cd 'g 4a sa .0 <4-c .0 *H bOHw> *i5 *h 11 H *H H *5 * 4k H hO H (0 ,0 r-4 **3 {0 ,0 H> -p ** *r* sg H ta H H 38 *ops4,, A in HI SH 0> H to H o Cvt m +9 H *M 0$ O Cl to *p O iH <3; e > !> -P tM H } H *} O -P U o 4 rs H *Q * S AS 4* < 1*4 o *p 4 'W. * a m U 8f 8 S Ok H 00 <0 o P H O C 1 ct*o 4 1. Si *4 IJ# tO - * %stl*3 >0.0 3 H ,C *8 Bj M HI << V. 10 00 1*3* *0s ne ^ p. fi . tsu ^ g. tS48 & Pt + *0 & # 44 M H *twJrt 4(D; O S3 rO m 4 m t, g* H O $4 O S3 O O o _ >* & Ute TJ ! ^ 38 o 8 &S> p 0H fi iH M JS H O -P O M OH <fiq O w> bO m p p 5 -a U 0 JS H 0 *H O 4> O O Q> 03 -P H H Hi U n* ^ 0 ft 0 . 0 f0i-GBi . fi Jjf *0 01 Pi c m f *1 O |l sgi| 0* I - fi ^ u + & + su 1! 0-:-t6 435 L 0 a**a 3MH- *4 o <s c< <2 % 01 % I e * 00 I o* oo> Oi> 4 09 R 4 a . p tO ia cn 4 3* # ' S& m $ o* vft ' - # : y gan idiswpiw DUP050316297 Strength of Tint The flushed ink Is consistently 4 pereent weak and bine' as eeicpSpea to a dry control ink prepared by the usual 1 procedure* i.s partially pulverizing the lump sample* with a spatula on the watch glass followed by grinding on the ink mill* However* the flushed ink is approximately 8 percent strong in tint as compared to a dry control ink prepared by grinding the plant ground dry color on the ink mill (483*316) or on the board in the ordinary rubout method (485-51D). These readings were made on the fresh tints and it is emphasized that the relationships changed radically on standing* the flushed inks gaining in strength against the dry control inks* Maaatone* The flushed ink is light and dull in mas stone against the dry control ink prepared in the usual manner, The flushed inks m^tch one another in mas a tone more closely than do the dry control inks* Undertone* The flushed ink is weak and blue in undertone against the dry "control ink prepared in the usual manner* ?Mp. There is no consistent difference in the flow of the flushedi and dry control inks according to the present testing method, Texture, The flushed inks have very noticeably better texture than the ' dry' control inks* Miscellaneous notes* The Lithol Rea Pulp did not flush cleanly on the ink mill* i*e, some water-wet pigment was left in the flushed water which necessitated running the ink over the mill until this water had evaporated* It is estimated, however, that at least 90 percent of the pigment transferred to the oil phase on the first pass. Some water became emulsified in the ink on the first few passes giving a crepe-like effect* DUP050316298 3f- - 3UBHXTX9S BY: a p p r o v e d Bf; imflBDfiftgBar JillSIL---. /&/\ // Fix,i: mmm^r^msL ursnsBS BATS: MSCJ5MBBR 1635. / ffae work on the Rotogravure Ink piles of th Hew Type Printing Ifik Problem lias been somewhat limited the past month due to the lack of fee ill ties for testing the inks as they haw been prepared. A number pf Inks have been prepared and it is hoped that they can be evaluated in the very near future. There has also been seme investigation of an organic brown to fill a need for such a color- In the rotogravure field* smmm? &m eomussicam Following the work of last month in which inks were prepared end- tested In cooperation with the Technical Laboratory of the Dyestuffs Division, similar inks have been prepared in our laboratory. Preliminary evaluations have indicated that our inks are somewhat lower in gloss and higher in penetration than those pre* viously prepared* A ready explanation for this must await a more \ complete evaluation of the inks but we believe it is probably a function of the solvent content of the ink. Inks have also been prepared from Cum&r resin and from East India Gina in an effort to determine the true value of RH-*35~D in relation to other resfn. Again we have preliminary evaluations which indicate that last India Gum gives an ink of superior working properties but of lower gloss than is obteined with Cumsr or with RH-35-D using similar resin contents. Brown pigments have been prepared by making the PTA of Basic Brown HR end also by making the Copper Complex of Para Bed, The former gave a very hard gritty pigment which is relatively poor in lightfastness and thus rather unattractive for the purpose at hand* Treatment with "BuPanal Wa Gone." and Diglycol Stearate resulted in mueh softer texture and better strength by rubouts but it was still poor in Mghtfastness. Even this soft product gave rather poor dispersion in the RH*35-D solution as a Roto Ink. The Copper Ocmplex of Para Red was also somewhat hard in the untreated form but it shows excellent light fastness with a barely perceptible break in 7S hours and a rather high order of strength. This pigment was given the following special treatments. 1. Treatment S. Treatment solution in solvent naphtha. 3. Treatment xylene and alcohol. with with with mineral spirits before heating. an equal weight of BH-35-D in BQfo ethyl cellulose in a mixture of I DUP050316299 ' The .^Jhoral .spirits gays an excellent texture ss judged . ..fcy the tenl - If ''tfee.'-pi^nb'-'ahd -by its bulk but. both. Ms and the untreated eontrl failed to show eoaplete dispersion after one hour itt a bail jaiU with Jffi>3&-D solution* On the other hand the RH-35-D tfeatment gave a very poor, dry appearance .and a rather harsh feel hut dispersed very well wen without milling in the resin solution. The ethyl cellulose treatment was done primarily with spirit inks in mind. It gave a peculiar cotton like feel to the dry produot. When i ah attempt was made to disperse it in the resin solution, the* ethyl cellulose swelled to a stiff gel which failed to disperse completely. It may* however, be worthy of further investigation. Some investigation was carried out to determine whether a 'better ink could be prepared by a short ball mill cycle- as,Compared with the simple pasting of the pigment as carried out by the. Technics! laborstory. It Is obvious that the ground ink shows distinctly less tendency to settle out of suspension. Otherwise the properties have hot been completely evaluated as yet# A series of inks have also been prepared using a typical rotogravure formula as given to us by Mr. S.L. Luhriag.* Ip uses a eumer resin varnish with a plasticizer and contains a large amount of alumina hydrate. It is obvious that the inks will give a very dull finish and dry quite slowly. A supply of rotogravure paper and a printing machine on which it is hoped that satisfactory tests can be made are both now at hand end we contemplate a more complete evaluation of these products in the very near future. BXPERIM2HT/X DETAILS See notebook #493; pp. 88-49* 493-5 Ibis series consists of a number of inks intended to duplicate some of those described in the November report and mad at the Technical Laboratory. Complete evaluations are not available but preliminary tests indicate that the inks as- preparid in this laboratory have higher penetration and lower gloss than that desired. This is probably a function of the amount of solvent present. Further evaluation of these colors will be made in the near future. The series also include a study of the effect of grinding in a ball mill* 493-6 Inks of Hansa Yellow (YT-891-D) and Barium Lithol were prepared in Cumar and last India Gum solutions with resin concentration similar to that previously determined as the optimum for RH-s s -d , The East India Gum inks appear on preliminary tests to have superior printing properties to the RH-35-I) inks but to be deficient in gloss. Further tests are contemplated* DUP050316300 2SCS 3SE 3* * m&L- '- P'.T.A. Toner of Basie Brown BR. ft. - Untreated Toner* B - "BuPonal WA Gone*" in the F.T*A. solution. G - As B but Mglyeol Stearate added at the end* D - As B but struck with BaGlg and then treated with B.0.S* basis* A - was very hard and weak* B - was also hard but stronger than A. C - was fairly soft and had good strength. J5 was quite soft and equal in strength to C on a color All show poor light fastness in ?2 hours* jg&flP. Bara Brown CGCpper complex of Para Bed) was prepared as in K-57S0 except for a slight change In procedure caused by an error in calculation* A - Untreated toner. B - Toner treated with Mineral Spirits before developing* G - Toher treated with equal parts of RH-35-B resin in solution in Solvent Naphtha* I) Toners treated with ethyl Cellulose (SCW In Xylene and alcohol. A is fairly hard in texture* B *> is softer than A and stronger tino tori ally* C - is very dark in dry appearance, is slightly stronger than B on an equal color basis. B - is rather hard and difficult to rubout arid is weaker than B and C All the products are stronger than K-5760 and all have good light stability with a barely perceptible break at 72 hours. 495-12 Inks in RH-35-B and solvent Naphtha. A - Ink of 90 - Poor dispersion after one hour on ball mill. B -- ** "10 %. * w n it * *t * C - " n10B - Dispersed well without milling. Required additional varnish to be thin enough to strain* X> - Ink of 1QG - Dispersed well without milling* Vary thick after milling. Required additional varniA. 1 ** Ink of 10D - Dispersed without milling but formed stiff ball of ethyl cellulose gell which refused to break up on long milling* DUP050316301 ; 5 So tests o? these inks are available* mm-": : Inks of X*S59*I>, Hsnsa Yellow, YTrSSl*53, Barium Lithol BT'*364-I) and la Gummay resin varnish by a procedure as given by Mr* B.L. DUhring* 1S*A is typical. 50 gas. Oamar Basin Varnish (55fl) 0 " Gteome Yellow, -4IS0*I> 25 * Al. Hydrate #100 25 * Blown Gestor Oil H^120. 5 n Ga Stearate* lis gives a very stiff paste which requires rntoljr more solvit to he thin enough to strain, ^h other inks wr similar hut used half as much color and were even stiffer drying* Preliminary tests show these inks as very dull and slow DUP050316302 ^ sir- & ' Fiamm mum- rnmErnom r e p o r t ........ ' ' mil, t ip is q w mmsim mm-- nunr /7 q /!----- 7/---- SUBMITTED BY: APPROVED BY* /<PA/ FIIS: j*nmTIHQ--'-IWr CfrhOftD BATE: DECEMBER 1955 lUTfiOBUoTioiE A start on the development of Pigments far use in spirit Inks has Been mad by attempts to incorporate ethyl cellulose in the pigments during manufacture* A number of inks from such products as well as typical controls from untreated pigments haw bees prepared hut no means of evaluation is now available* SUMMARY ATO COHCHTSIONS Inasmuch as the feature of the MRotalin Supra* colors which makes them distinctive is their content of ethyl cellulose which serves as the adhesive in the inks made from them, it was decided to attempt to incorporate ethyl cellulose in pigments during their manu facture in the hope that they would be much improved in their dispersion in alcohol. Ethyl cellulose is soluble in alcohol and to some extent in the aromatic solvents such as toluol and Xylol. In the letter type it swells very much and gives a viscous solution unless a small amount of alcohol is added. It was added to the colors (RT-564-B and BT-100-Dj before the final development using various combinations of solvents. When added In a mixture of aromatic solvent and alcohol, th ethyl cellulose seemed to be well incorporated and a soft product resulted but there seemed to be some loss in tinctorial strength. When added in alcohol solution, the ethyl cellulose was immediately thrown out as a fibrous mass and the final dry color had a cotton-like feel* It dispersed very poorly in varnish but showed little change tine torielly when finally rubbed out* All these products were dispersed in alcohol. They showed considerable evidence of dispersion without any milling but complete dispersion was obtained only with a short cycle in a ball mill* It is debatable whether the disparsi on By after milling is any better in the case of the treated inks than with untreated controls. Using the same solids content as is advised for "Rotalin Supra" colors a very heavy bodied ink is obtained which requires considerable thinning to be suitable for printing* The#e is evidence that the thinned out inks show very little tendency to settle out of suspension* Some inks of TiO,, in ethyl eellulose solutions in alcohol were prepared according to the Patent 435,818, but they were all very heavy bodied properly on the ball mill. and shellac examples in and did not British mill DUPO 50316303 Hone of these inks has been tested for printing properties sine we have as yet no equipment for printing the spirit inks* There is evidence, however, that the ethyl cellulose when present in amounts of about 20$ of the weight of the pigment has adequate adhesive powers to for an excellent printed film* The problem thus appears to be one of getting the pigment into such h condition that it can be readily dissolved or dispersed in alcohol without any grinding action* Bee notebook #495 ~ pp - 30-45 mm. lithyl cellulose (10$) was added to BT-IQG-B from solutions in various combinations of xylene, toluene and alcohol before the final development A * Treat with Toluene alone, B - Sthyl cellulose in xylene and alcohol. 0- n * " toluene and alcohol B- * " * toluene alone. E- " " " alcohol alone. B & E show good tinctorial properties by rubout. 0 end D are quite weak by rubout* Various inks were prepared from these colors* It is obvious that 10$ ethyl cellulose is not sufficient adhesive, hence otherrinkw were prepared in which additional ethyl cellulose was added to the inks during the preparations. Ho printing tests are available as yet. jgSsS. 20$ Ethyl Cellulose was added to a barium lithol before the strike with BaClg, A - Untreated control B' - Ethyl cellulose in xylene and alcohol C- " " " toluene and alcohol B~ * \n w alcohol slone. B & C are quite weak by rubout - also very blue. B is close to the^ control tinetorially. Inks from these products apuear to have sufficient adhesive but are very thick when milled 12,gms. to 100 oc alcohol* When thinned out and smeared on paper a very tenacious film results which appears to be somewhat opaque. Final evaluation must await actual printing tests. DUP050316304 This aeries was am attempt to prepare inks of TiOg in solutions of ethyl cellulose and shellao as described in the examples of British Patent 425*818* The proportions as given resulted in very thick pastes which ground very poorly in the bali mill* Further examination of the inks is contemplated when a method of printing becomes available* DUP050316305 BY? mmamo b y *. m ilg 33* Hill PHISIG&t STUDIES mmt marnsm* 1935 This i the third report on this problem, work on which was started some months ago and which has "been carried forward in conjunc tion with practical studies in the semi-works and plant directed towards obtaining a better dry fineness in our standard pigments* particularly the "Dry Dispersible Solars* for paper coating. She objectire has been to develop more reliable data on the dry fineness of our regular line as ordinarily ground, and of the improvemeats s&ich are possible by proper equipment arid operating conditions. In the same connection, a number of competitive products have also been examined . SDMM&HY & CPBglffSIOB Ti1 earlier reports outlined the methods of screen analysis used in the course of the work. These are still being used and give results which are satisfactorily reproducible. In view of the large amount of data now available, it has been felt wise to present it in tabular form for simplicity in future refer ence and, moreover, certain figures previously reported have been in cluded. The figures in the various columns have the same significance as before, namely the percentage held on the sereen in question but passing the coarser screen. Table I. * II. * III * I *y vi VII Standard Iron Blues * Chrome Yellows & Oranges * Chrome G-reena * Toners ** lake s Competitive Pigments Comparison of fine grinding with older type. DUP050316306 Pi r %s. s-VJ- " *> r i-': % Tttag&'x kviikTm&sm*&+*a*sxjirfnt?.rnr ...vj'Mgjryga.'P. ..m?fgiV`f-5Jec:,jr ' eade Held :a 80 meafe isa 800.. B-5-B SB-46735 . 21.2 B~6-B SB-46846 B-57-B SB-46810 1* 46.1 27.7 2-4.0 . B-63-B ttD-AdftU'} 13.7 .(Mp. SM*]0 ' X&-65-B SB-46053. 4.4 B-66-S S&r4?214. BX>7?-Ii SB-46363 20.3 3-7SHD SB-46X77 24.0 m80- SB-#6241 9.5 B-82-B SB-4624? 7.9 B-S3-B 8B-462S3 B&-87-B fSB-46370 10.3 # B--89-B SB-46382 17.6 B-98-B SB-46587 B-103-B SB-46948 7.8 26.1 * (earlier res .) 27.8 B-204-B SB-47082 1.3 "(earlier result) 1.7 B-1G9-B SB-47113 13.9 B-lll-B SB-46845 11.8 B-122-B SB-46643 B-119-D SB-46691 18.1 17.5 B-223-B SB-46934 11.7 (earlier result) 10.5 B-124-B SB-46730 .4 B-128-B SB-46760 1.6 B-ISO-B SB-46790 1.8 B-132-B SB-46799 24.1 B-133-B SD-47067 9.2 B-137-B SB-46840 B-13S-D SB-46842 B-139-B SB-46863 21.0 9.2 2.2 B-140-B SB-46944 17.1 B-141-B SB-46831 22.2 B-243-B SB-46878 24.0 B-146-B SB-46932 7.4 B-147-B SB-46936 29.1 B-X48-B SB-43952 B-152-B SB-46983 12.7 B-155-B SB-47021 1.6 - B-165-D SB-47152 .6 -26.8 S'X.l 2E.1 23.6 21.4 I0.6 86.1 26*2 23; 5 U7 8**7 . 12.4 30.2 36.7 25.3 15.3 15.7 25.9 17.9 25.6 26.5 23.8 22.3 9.7 6.9 7.2 22.6 27.7 23.3 24.8 18.8 23.8 25.2 13.4 21.7 23.4 7.6 28.1 10.1 2.8 15.5 8.7 13.3 11.9 15.3 - 11.5 11.9 15.2 15U3 15.1 14.4 1.3 7.9 14.5 11.2 15.4 17.5 15.4 15.4 13.5 12.9 13.3 15.0 14*3 13.7 7.5 8.9 13.0 15.0 12.4 15.6 13.3 15.1 13.1 6.4 12.6 11.7 16.3 15.9 12.0 6.6 325 16.4 Total aa 52 79.9 16.4 15-*' 21.6 18.2 7.5 10.4 16.5 14.3 15.6 3.1 11.5 14.4 13.5 19.8 10.2 16,2 10.3 7.3 17.2 17.6 16.1 14.3 13.7 14.8 15.4 .5 23.4 17.3 15.6 6.4 3.4 12.7 32.6 15.3 22.6 17.2 75.9 . 66.2 48.1 70*5 .*. 80.8 1.8 61.0 63.0 5.3 49*4 66.9 '81.5 53.9 65 *4 59.4 66.9 6446 67.7 41.4 32.1 32.2 73.6 63.7 72.2 50.1 51.7 75.3 76.1 50.2 45.1 76.9 56.5 66.0 46.2 27.2 7* ii DUP050316307 -48- .0ER II Code # Bald on if...pssb...... 180 ' 200 325 Total 325 Y-12'-J> 48959 YQ-27-B 48993 Y0-34-B 48994 TBfcHMt 48890 `OMft-D 41237 Y~17t-B '48558 Y-I0-B 46f56 Y-1S1-B 48892 2.3 32.3 1.6 1.1 .9 7.2 6.1 2*7 12.2 1*4 1.0 3.4 5.3 4.7 2.4 5.1 .8 .8 3.4 3*0 4.9 3.3 4.2 1.8. .8 5.8 4.8 3.2 8.6 10.7 53.8 5.8 3.7 12.5 18.7 24.3 Y-202-B 48738 Y-218-B 48267 Y-232-D 47163 Tills is tbs eurrent Y-232-B 47108 Y-240-B 48584 Y-240-D 47125 Y-253-D 46455 Y-260-D 46868 Y0-263-B 46994 Y-267-D 46534 Y-S87-D 46837 Y-203-D 46931 Y-299-D 46753 tt Y" 303-D Y-305-D Y"S09-D Y-315-B Y-326-B Y-318-B Y-329-B Y-328-D tt 46828 46920 46918 46717 47126 46922 46754 46907 H Y-347-D Y-359-B Y-366-D tt 46925 46989 47015 It Y-S73-D i(14009) std. Y-374-D (14010) 3.9 11.0 10.7 3.0 3.2 2.0 1.2 2.8 2.8 standard and represents 11.8 7.4 3.8 3.1 4.3 3.1 18.4 1.3 4.9 8.4 10.7 10.2 3.3 4.0 5.9 9.7 5.4 3.2 1.8 5.1 5.2 13.7 13.7 8.9 3.3 28.7 7.9 10.0 4.3 3.8 13.4 18.7 ' 6.3 7.3 18.0 avg,9 17.6 21.2 6.2 12.7 18.8 18.5 1.8 7.0 8.7 4.9 12.7 9.3 10.7 6.5 16.0 41.6 1.5 9.7 2.7 9.5 finely ground i 3.5 26.5 18.7 3.7 15.7 6.5 25.1 8.6 32.1 7.3 41.3 5.4 13.2 6.0 6.0 10.5 22.6 50.5 arfe. 8.5 44.8 .95 a-eer. 3.3 18.8 5.2 47.0 8.7 6.9 47.7 7.28 avg. 6.0 24.5 14.8 66.3 9.5 37.7 14.4 62.4 11.0 26.3 25.8 arg. 15.2 32.9 DUP050316308 0- .* <>& '*- . .;, ,^-f > . \.' ' ^*' " . Ci XII *7 T-' tele m z-&- a G-ISO-B 466Q2 G-ISI-B.. 46603 0-103*#. ~4ff6&7 G-18## 46862 -188*# 46087 &-XOO-3J 4$237 ROOTS' . oa 15.6 2.2 5.9 2.3 4.2 1.8 8.0 g x -s o ^b atee* 4|sto SX-ffte-B 4WHB1 GX-208-3) 40404 G-209-B 46902 e-8HHD G-21A-!) GX-227B 46889 372565 46947 @-g?G- 46376 S-280-D 46310 G-284-B 46152 GX-236-D 46114 0-291-B 46401 S-294-B 46547 1.2 1.9 1.0 7.7 .2 1.9 1.4 2.8 1.4 GX-309P 46316 {f~312-B 4631? G-SIS-B 46314 G-315-B 46338 G-316-B 46339 G-317-B 47001 G-318-B SB-46341 GX-319-B 46364 G-320-B 46351 G-322-B 46353 G-323-B 46354 G-3S9-B 46397 G-335-D 46458 G-340-B 46542 G-342-D 46539 G-343-3) 46546 O-344-B 46597 - G-345-B 46545 G-346-B 46562 G-352-I) 46656 G-355-D 46699 G-S6Q-B 46808 G-362-B 46814 G-S6IKB 46807 8.3 2.2 2.4 1.8 .7 8.5 1.2 1.0 2.2 7.6 7.3 1.5 2.0 1.3 1.8 2.0 20.7 .7 3.2 1.0 12.8 ' 150 11.4 . 5.3 5.4 7.3 8.8 10.4 >2.8' 6.8 6.6 5.1 10.6 3.0 7.4 3.2 11.9 7.7 9.4 6.6 7.6 6.0 6.2 6.0 7.1 8.1 11.8 17.1 12.2 5.6 8.3 7.6 9.4 11.8 9.8 3.1 9.1 6.0 11.7 ZOO 8.6 3.0 6.1 9.2 ss 11.7 9;2 7.0 7.8 7.2 7.0 6.1 7.2 3.8 11.9 10.2 10.4 6.0 8.2 7.2 8.0 4.3 8.0 10.4 13.2 11.2 8.8 6.3 9.0 8.4 11.8 12.0 5.4 4 b4 7.2 6.5 9.3 385 5.9 7.8 3.2 18.8 4.0 12.8 6>6 5. 15.3 1.9 14.3 14.2 A?X- 14.3 8.4 11.3 2.8 6.2 .8 8.5 17.6 9.7 1.2 15.8 12.0 7.0 11.9 6.7 .4 13.2 2.4 17.6 2.4 2.6 12.0 3.1 15.4 8.2 19.4 6.6 11.1 7.6 1.9 3.1 8.0 fotffcl oa ms 41.4 a'; 8 37.0 25.6 4Mr+ 36.0 29.3 30*5 17.4 29*3 20.6 19.3 14.6 35.1 36.9 37 .9 26.8 25.2 26.8 21.6 19.2 29*5 21.9 44*8 38.3 40*3 16.5 34.7 25.5 41.4 33.0 37.0 15.8 21.4 16.6 41.8 DUP050316309 j uj . 9MRPM 9- 40966 4696? 46914 46 09 40998 47003 0*39OB CHMNU* 0*392 5*694-2 *596* ~596*J> 404 MOM *406*B 58?~l> 6MBM OMOO*4> GM-401-D G*402 0*414# 40086 47089 47041 47184 47048 47643 47046 47077 47080 47099 47118 47116 47030 47090 47097 47096 47166 47164 9*0 5,8 1*3 0 *7 2.6 1*6 1*8 *1 *3 *4 1*6 18*4 4*0 8*6 8*8 11.6 1*5 1*3 4*6 *1 *3 1*4 *1 'Hi 7*1 0*9 6*4 -* 3*6 7*1 6*8 7*9 1*4 8.1 8*7 6*6 9*4 7*8 7*0 11*0 16*3 0*4 5*9 3*7 *7 1*2 4*1 8.0 9*0 1*6 6*7 6.8 6*4 .9*8 ' 8*5 4*4 4*1 6*2 6*6 7*0 7*1 10*0 13*4 3*5 6*2 3*7 1*5 1*6 7.4 2*0 7*8 4.8 S$9al aa 8*8 85.9 8*9 89.6 13*6 38*2 2*2 2.3 8*6 18*5 83*2 10*9 87*4 11*6 84*7 8*4 21*9 8*8 5*4 . 9*4 8*1 9*9 8*8. 16*6 9*9 26.2 3*6 33*4 18*1 31*6 10*7 27.4 17*9 48*1 11*8 58*6 18*8 50*6 8*7 82.1 6.7 18*7 2*6 8*9 5*0 4*5 7*6 .4 *4 11*4 10*9 87*5 9.6 15*6 - >.-$$; i<'- *`V ` DUP050316310 ry 4 BT*S08*B 46366 46311 .18*8904-46660' W*3l6*B 43333 R^*#68*B 46393 B&8444B 44713 *34?* 46685 R3!*363-.D 43771 affiMMI 4708 B306* 44884 SS*S96*B 47084 B30B 46751 1*1 16 7*7 80*7 3S.0 14*6 14*6 JB*B- *6 5*9 21*3 26*8 45*6 36*3 18*4 16*1 14*6 6*8 B*r<*96*D 48981 BT99* 46988 f*100*B 46SS8 23*6 10*4 7*4 B*1Q0*B 8M U 7*6 8*0 W101*J>' 48883 *T*102*B 4661? B^*116*D 48674 16*6 2*0 10*1 ' BN**** 48800 50*2 BMMMB * BS*08M 46783 48*6 17*7 B*18L8 46795 8*8 BT*150*B 46961 BM6S*B 4718? 7*3 $s >^BVb 16M Std*X5999 *02 G^<s530'* 46369 G^SS?** 46591 GS^M?* 46921 * <KW8B4*B 46648 *5 3*1 21*9 9*9 1MB4B 46393 1T**291 47135 4*5 6*1 4*2 58 16*0 10*6 18*1 lf#l 11*3 1*9 8*6 14*6 13*6 81*6 80*5 16*3 13*6 12*3 , 11*8 13*5 18*1 17*7 10*5 11*2 10*8 12*6 6*4 11*8 15*2 16*7 20*8 8*0 15*5 1*8 *6 4*4 8*9 17*1 11*2 9*2 8*0 6*0 *56 10*? 5*0 ?*8' 9*2 5*0- 6*6 3*7 7*5 ? ? 18*4 7*8 7*5 8*7 . 4*0 6*9 11*8 10*4 11*7 10*1 7*8 8*1 10*3 7*6 7*9 6*8 8*3 13*4 9*6 11*5 2*8 1*6 ?*4 11*7 9*8 8*6 6*7 3*9 8*5 *62 9*9 4*5 3*6 9*3 4*1 8*8" 4#?' ' 8*5 8*1 10*6 7*3 8*1 1*1 8*8 7*9 5*7 16*0 11*5 16*1 13*9 ,%al m 388_____ 19*8 1*5 45*1 40*8 61*7 58*2 35*0 34,6 11*4 36,1 50*7 67*4 81*0 32*6 31*5 41*2 *53 59*0 44*8 63*5 52*9 41*9 14*2 8*8 14*8 8*0 7*6 13*3 7*5 14*9 8*0 4*8 7.8 16,5 11*6 13*0 3*1 4*9 50*6 24*8 44*0 80*2. @1*1 65*2 27*9 49*2 12*6 6*8 19*6 60 *2 60*4 42*7 28*2 81*9 DUP050316311 ra**-*1*? 5Baaz~aaBaEtmam& -* lidlc'r IP # Pffrlfl @n 30 Mesh 4636 #6890 '46468.' 4mw" 46132 4*6 9*5 6*1; h i m- smm M*mi*- o&urs iS4^4} 99* 1#361 48654 88*4 .0*8 6*5 4- H*3S5 46784 B&ff&SM 46785 B3|w360 terns*at4 33686 . l&*86e* 46708- St 4* 86JM0 46808 #3 B*377*B 46853 Tt*380*D 40008 BB*994*I> 40084 B&*8&M 46057 HS^39C)*P 46030 - ' &M40*** 49*93 *1 BB38* 45810 ' B01* '. . 40118 BB60*B B1*7S* B*9M BP*70* BPS6 46484 46044 46344 47080 40013 4. BJI108 46686 W BB*114*B 46665 BP*iai*B 46015 . B*184*B '46583 33*135*1 46584 B3>1S6 46950 . 8B*143 46603 46064 11*145* 46990 @1*140*1 46934 ii0i3i*i 4mm Mrt&m# 40018 BB159 40068 19*6 10*8 *4 6*1 *8 85*8 3*9 4.8 83.9 5*0 *8 14*8- *01 8*7 81.4 4.3 ? -m *w* 180 9*5 8*0 8*0 800 0*1 3*0 3*6 5*5 11*8 14*8 0.5 1*1 3*8 6*6 4*8 1*1 .5 *7 *6 13.0 13*4 9*4 15*0 1.8 83*9 10*0 18.3 15*7 9*9 4*3 9.9 .3 10.7 84.8 1048 *3 5.9 9*3 10*6 10*3 4*3 9*6 0*4 9.3 5.0 0.1 6.3 7.9 *4 9*9 9*6 9*3 325 fetal on 385 11*4 38*6 8*8 aver* . 0*8 0*8 86*0 6*0 aver* 11*9 aver* aver* 6*8 31*4 8*0 30*8 4*6 ' 88*6 *3 aver* 1*0 1*3 aver* 1*4 aver* 1*0 aver* 3*0 1,0 8*9 *i 9*0 1*6 . 3*1 .6 8.5 1*5 0.3 9*0 13*3 15*0 0*1 9*9 15.0 15*4 *4 13*9 *0 #4 9*9 1*6 13*0 9*0 1*8 11*6 13*9 13*0 40*4 .49*3 93*0 49*1 18*3 70*3 45*0 41*0 59*3 31*7 84*6 39*9 8*1 34*6 69*1 36*8 ~?s~ DUP050316312 fffSWBM 69# IMIM 49072 m*290 46780 EelS <m m mm *8 w> 0 ^.aaaara^^e.s, 12*4 GI,~265**> GMBMG0?3Q3**D *55S* GE*559- g Mo m *36S-B <m*864*D aS-388-D 46000 46832 46326 469X9 49017 46813 46811 46825 47059 16*6 2 15*2 1 *0 6 *4 .1 10*1 1*4 19*0 2 *8 1*4 #8 5*2 5*0 2*2 9*4 3 2*2 1.8 1*0 1*2 . 325 5*0 . 6.5 8.3 1*8 8*7 1*5 3*6 8*8 8*1 3*4 Total 325 31*4 4*6 33.8 6*1 45*4 1*9 6*6 6*0 4*3 5*3 DUP050316313  1: . *> #':* ?7 - g* 'ofnwift........... - - 's' ..___________________so fearme Victoria Marom 16*3 , U y. 9otaX o b m,--888- m ` 10*6 11*6- 60*2 33902 imperial Sioux Marom u*s .. 13*8 14*0 39*0 % <WM* . .. 64765 Harmoa X**x Karoos imperial &#095 IF18 imperial m& Mth&X - M698 14*8 35*5 .36850 SarmeB VaJ^fcoa ISareCB . 36S1 8&rwl3BWillia Srapfcio la B #454 mmo Baperial Qeaoa foafr 3*3 24*6 12*4 1*1 : #9 20*5 9*4 25*1 . 11*9 1*1 7*4 11*5 9*3 12,& 8*4 19*1 10*6 16*2 10*0 64*3 4*7 63*2 71*4 24*7 34*1 36934 Sfcerwta*0illias lake Be CB #557 5*1 6*9 7,0 12*0 29*9 36965 imperial Medium LithoX - S-1096 37805 Imperial Seaeca Bfarooa #456 5 25 0 5*0 22*1 3*0 10*4 5*7 9*8 12*2 67*3 38240 imperial Karoos lake *4 1*8 3*1 7*6 18*9 38241 OBllob Scarlet lake mm 3*5 3*4 2*6 4*9 14*4 54100 as*Siegl Bermaaemt Purple 6*1 11*4 9*3 15*8 42*6 54629 Pope & Sray Milor i Blue 7*3 18*7 13*1 16*8 55*9 53451 Imperial 6 5*1 3*1 18*0 @0*8 . 35581 A&s*-Siegle Cascade Blue 49*6 23*4 3*0 6*4 4*4 39843 Keatueky Milori Blue 11*9 11*8 11*5 sas ' 56306 Imperial G*P* Blue Oaite Bronze Blue #1164 ';57808 Imperial GMaese Blue A**1835 1*4 *9 10*7 3*9 7*9 11*1 13*0 18*9 19*3 87457 Imperial 1*5 8*8 19*5 37651 lavey Milori Blue 3*9 16*6 14*3 57676 HaasmoB Gtoiaese Blue 58054 Eeatuaky 4*4 *5 13*4 18*2 17*8 47*8 58068 pam color & Oke* Milori Blue 2*7 7*0 8*5 14*7 $8*9 DUP050316314 '* 6*# omeetltar......... ..... ............. mum jnidLtoft chrome Green teglif :#*.....- wp. -.. 800 s*r. 13*0 10*4 .....- 38' 16.9 A'ipeAe W-Ow s7sn Waited Ofcroate 0t n Midiwa. 87**a moltea chrome Qa?e Bk* ^ 57780 ' Wmpxtsl. Glen Greea &od. 4*8 5*8 8*7 13*3 15*7 13*9 1S*1 ii8 12*9 16*6 17*0 19*5 46*8 49*1 49*8 88088 Imperial Xea Ore** 8fio Imperial Glen Green light 6*8 10*2 17*5 15*5 18*3' 15*8 ' ? * . 51*4 56*0 88107 ferial &lea Green ke 5*1 15*6 12*8 17*4 50*9 .mHML 35468 Kohastamm Med.Chroma fallow 8*8 7*5 6*4 7*5 24*0 3SS53 Imperial Idght Orange 87189 Imperial 18*7 9*6 9*9 7*7 6*9 5*8 6*0 5*7 36*3 26*8 37560 Imperial Med. Yellow A~548 6*3 11*8 11*0 10*1 58*6 88350 G#H* Morrill Ofarcaae Yellow #08385 3*0 6*0 3*6 4*9 17*7 # i- ri DUP050316315 Go$e RX>36*B|, #48055 Before H*S* #15533 After H*S* HSS56D #35719 Before H*S* 15586 After H*S* MMgMi 15421 Before H*S* BT*28l~B* 15482 After 3*S* BVaJMM* 15356 Before- B*8* BTg42.B,, 15944 After H.8* Rg*~283* 13346 'Before H.S* BT*883-B* 18111 After H*S* RE*390I>* 15811 Before H.S* 13946 After 3*6* RE~389~D, 14476 Before E.S* B~389** 15942 After H*8* RS~39D, 14472 Before H*S KS-S8S-B, 16197 After H*8* BB**68D, 14473 Before H.S* B5T.389wD, 16196 After H*S* RE~390*D* 15810 Before H*S* KE~390~B 16199 After H*S* RT**283wB 16192 Before Jl.S* BT~28S~D* 16196 After H*S. BT208*D 57507 Before H.S# BT*208D, 16286 After H.S* RT-544-B* 14501 Before H*S. JJT*544*B* 16287 After H.S. RT6?9~D* 15873 Before H#S RT3?9*B, 16888 After H.S* *n * 80 16 1*6 4.0 7 13*8 12*7 4*7 7*2 21*6 16*2 *4 2*4 4*7 6 1*7 11*4 3*6 1*4 8*4 1*0 18*4 18*5 11*8 2*4 15*6 14*6 7; 200 685 Total oa 325 3*6 1*5 6*6 4.2 9*8 2*9 6*7 2*2 6*8 6*5 *8 4*6 7*0 6*7 *6 6*0 4*6 *2 4.2 2*1 7.7 7.9 4*9 3*6 7*2 7.6 3*7 1*0 3*4 *4 12*6 4*2 69*3 22*4 48*1 10*5 *3 *02 1.S 02 1*2 *1 1*1 2 *6 *1 29*1 11*6 3*9 1*3 29*3 8*8 48*6 48*6 DUP050316316 16317. Before 8*8* 15517' After B#@ BHMM6* 15788 Before H*S* 15855 After B*3* 45488 Before H*S* BSS*148* W After HW8* * IW4 Before H*S* 236*14* >* 15786 After B*S# -15484 Before S*8* , lit After H*8* BS*1|NI*B* 158X8 Before B*&* BB^lfeB* 18986 After B*8 BS134&* 15220 Before 3*S* ---------~ 1, 16985 After S*31 BSX34B, 44505 Before ES BB*aS4*B* 15791 After H#S* >* 4155 Before S:*S# BB*1143>t 15857 After H*S* BB~ll4I>* 13129 Before K#S* BB*114* 15785 After E#S* BB1A4*D* 13078 Before K*8* BE*0L14**D, 16784 After E*S BB1S*1>* 14506 Before H*S* BB*136~B* 18797 After H*S* 15*1 '*1 18*5 3*3 24*1 2*7 26*4 9*0 . 1B.4 7*7 13*6 10*4 150 19*9 X5*S 30*4 73*5 *4 fX *84 1*6 3*8 11*0 *1 *7 1 1*8 *8 4*6 1*3 *08 GB*S58D 42532 Before H*S# 0M8M, 1570S After H*S* j)SE358B* 41920 Before H*S# GE~3S8-I>* 15707 After H*S* &B358*B 15458 Before H*S* SS58D 15712 After H#S* GE3S8*B 44397 Before H*8* GB**S88** -15718 After B*S* *4 *08 1*1 15 1*4 4 *7 8*2 3*4 2 DUP050316317 * 15 # 8# mim Before 'St#* imm mm?* h ** litwe-After h *s * SS69*D* X8p$M Before B@# Aftar 3*3* ^864*0# 1517 Before H## 3B<*664, 16078 After S*S* *287*B* 85786 Before H*S* Y*807*B* 15143. After B*S* YB-afO** 14389 Before H*S 1M90B 19368 After B*S* ' TeWMt 15387' Before 8*8* 1S852 After S*8* RBDiFG 1/88/56 *8 7*4 *7 I#1* 8*4 4*0 *8 8*8 8*0 5*7 1*3 66*9 38*9 DUP050316318 m&msts, earn mmmm r epo r t BHI LAKB FDR ROBBER RP-168-B fK-8047) mmiYms m Kpmovm b y : PILE* RBBBSR 601, S BATE: SBCSMKia- 1935 iimsgtreTiog Bevel opne nt work was started in the Semi-works the latter part of last month on a ne# Blue hake for rubber to replace Rubber Blue YD. A total f eight batches was made using as a basic formulation K-8047 which was developed in the Research laboratory. SUMMARY &COFC&TSIOKS Six batches were made using the E-8Q47 formulation. All of these batches were satisfactory in tint and averaged v.s. stronger than Rubber Blue YD on rubber test. Some variation in strength was noted from batch to batch but tint was uniformly satisfactory. The remaining two batches were made using an increase in barium chloride over the K-8047 formula, thus introducing more Blanc Fixe in the lake in order to weaken the product. Both of these batches were practically OK in strength and tint in rubber vs. Rubber Blue YD. Rubout results are not very satisfactory as an indication of quality on this color, the results indicating weakness on the part of material that gives satisfactory strength on rubber test. A composite mix consuming total production on this color is now in process and if the final test is satisfactory will be set up as BP-168-D standard. Results are tabulated in Table I DUP050316319 g H ) o ft** rH 03 S&>O * OCO 03 4 525 T3 rH *H 4* jx <a 4 *H CO X* rH I CO e 3 -p #H H 03 z$ m to* 03 1* & o i JU -P KO H *M MJO <s in 31 Cfl iH <o 4t* * m > *f* <0 > < rH V om CO n * M O t s* p isj VI O t lO feci 4t o 5b4 4 O CO O <o b- co <0 <J> Si o fcg o 5*3 1O 4 43 t &4 -P <0 i oa *P 5*3 O ! U -P it E > ** * feci. 0 l sp* to *P **5 0 t be* O 0 v J-* *p It . Jt to 5* DUP050316320  m-'\ . . 3S-- W7 fi SOTMliffe BTJ immmtm b y : t t s e x b a r a -r b b DATS: MOWBEl 1955 Investigation was continued along the following lines: A ~ Filtration; B - The incorporation of Hello Bordeaux BL, and 1-5 Acid; C Miseellaneous; B - Preliminary drying studies* mmmjm. . A* The most obvious single factor influencing the rate of filtration appeared to be the dispersing agent used. It was anticipated that (mission of the Para Soap should permit (1) flocculation of the pigment with an accompanying increase in the rate of filtration, (&) It should alter the nature of the dye, Para F, in solution, and (3} it should diminish the amount of Para F retained by the pigment. All three phenomena were observed* When the soap was added prior to coupling, very tedious filtration resulted, the Para F present in the bade water appeared under a aienoseope as long hairy needles, and a relatively high percentage of Para F was retained by the pigment. Adding the soap to the filter funnel after removing the reaction vehicle, approximately tripled the filtration rate, the Para F in the bleed crystallized in rectangular plates, and the m amount of Para F retained by the pigment was diminished, (The methods r of studying Para F retention are discussed in the November report, page 4, and have only been slightly modified). In this series the BN was pre cipitated from NaGH by the addition of NaHC0~. Obviously, addition of , Para soap prior to this precipitation - and consequently prior to coupling r would increase the rate of coupling. This was observed. While theoretically interesting this phase of the study was necessarily terminated* TFaiwarthe Para Soap is incorporated prior to coupling, as Is the usual case, the products are hard, brown in color, and the yields are poor. The diminution in yield is probably the result of many factors, viz,, decreased retention of Para F, Para Soap itself, etc, The hardness of texture and brownness of color may be due to alteration of the micelle. ?' M ; -a ; In the course of coupling both Para F and Para Red are w*** formed simultaneously, and the acid from the diazonium solution, interesting; with the alkalis of the BN component, produces NaCl which undoubtedly causes a "salting out" of Para F, increasing not only the amount Of Para F incorporated in solid solution with the Para Bed but also the amount of precipitated from the aqueous solution. From solubility studies of Para F, I m it seemed that this suiting out was incomplete and the pseudo solutions formed were responsible for the gelatinous films deposited which markedly retarded the rate of filtrstioiu On such a basis it seemed probable that salting beyond this threshold value, either gy NaCl or HC1, ought to increase the filtration rate* This was observed. In salting experiments produets were obtained Which did not bleed and filtered rapidly in the cold* When washed with cold water, the products than began to bleed and the rate of filtration was out down. It appears that Para F does not DUP050316321 disperse molecularly in eold water, but rather gives rise to pseudo Solutions of particles of greater than colloidal dimensions. Tinetorially the products suffered markedly, hence these methods of study were dis continued* It has been reported that development causes an increase in filtration rate, and it appears that development may be accompanied by a slight increase in yield* These two factors are not incompatible since it may readily be that development causes flocculation whieh not only increases the rate of filtration but inclusion of Fare ?, Para Soap, etc* The temperature of the wash water appeared to be another obvious factor which might be expected to influence the rate of filtration, and further this could be expected to be of aaaaetfeatB.. value* Heretofore, the product had been developed to 65C , filtered hot, and washed with cold water, and it was noted that the rate of filtration fell off, a smooth exponential curve (#490-20 in accompanying diagram) being obtained* By washing with hot water (at 65C) straight lines (490-21 A, B, C, & D) were obtained* It is obvious from the slopes of these lines and tangents of the curve, that the rates in series 490-21 are much greater than that of 490-20, and that the rates are reaennably constant, and may be duplicated* The overall rate in 21-D is approximately 100 ce/mlnute whereas after the first twenty-five minutes the rate of 20A settles down to approximately 22 oc/min. It is not to be inferred that the rate of the hot water wash is roughly five times that of the cold water wash, since the high initial rate of filtration in 20A increases the overall rate, to a greater extent the shorter the time, Extrapolating AC St D back to zero time shows a slight decrease In rate* This may be due to a small temperature drop on adding the slurry to the funnel, but more probably, it is due to the fact that whereas the filter paper is clean initially, it is not so after some minutes of filtration, and the Para F (whieh crystallizes readily with a slight temperature drop) can rush through initially, but soon after these extremely fine particles elog the pores of the paper and must then be dissolved out* This occurs at surprisingly constant rates (see curves for 65C and 15C, l*e. #21 and #20)* The advantage of the hot water wash thus appears to be due to nothing more than nn increased rate of solution of Para F. This hot water wash should be of control value since it is a means of removing Para F adsorbed to the surfac^pigment* It has been pointed out that surface adsorbed Para F/produoes hardness in texture, and probably bronze* These two properties, hardnesB and bronze, are attributes of. Para F itself and it was observed that as the Para F and particularly the excess surface adsorbed Para F content of the pigment was cut down, these properties were diminished* Since the in corporation of Para F is essential to the dark shade, it is planned at some future time to study coating of the particles with oil films as an approach to softer texture, but this is another phase of the problem to be taken up at some future time* Continuing with the control value of this hot water wash, it is evident that impurities may be more readily removed in this way, and further, this preliminary heat treatment may tend to stabilize the product to plant processing* The effect of processing seems to be primarily caused by heat and if it is concerned with vOlatili- DUP050316322 DUP050316323 zatioa of low melting substances, or growth, of particles, this hot water wash may be of value beyond that of simply increasing the filtration rata# The influence of Barium salt formation upon the rate of filtration is to be studied* B* The incorporation of Hello Bordeaux Bl offers promising possibilities. Dry mixing with RT-38*B is contraindicated, but with RT-70-B dark bright products with a clean blue undertone are obtained* Only 3*5 5*0$ of the Hello Bordeaux #3196 was required to improve markedly the depth and brightness of RT-7Q-B* This appears to be at least a good method of bringing substandard stock to par* Slurry mixing does not afford any improvement, but on the contrary appears to offer technical difficulties (see also part "B* for the influence of drying)* since there is a tendency for the Para Bed to settle before the Bella Bordeaux and layer cakes are obtained* The particles of the latter appear to be discrete* crystalline and considerably smaller than the agglomerates of the BT*70B type of pigment* Development of the mixed slurries does not increase inclusion of #3196* It was suggested that by incorporating the #2196 in the B,H, solution prior to coupling, enhanced effects such as obtained by Para F might be obtained* However, conditions are obviously widely different, since the #2196 is structurally different from Para F, and further it was not in solution* In an attempt to cause this Hello Bordeaux to be 0 0-precipitated, the B*N* was precipitated in the presence of the #2196 from caustic by NaHCOg prior to coupling* On addition of the di&zonium solution, the medium became a dirty brown In color* This was taken to indicate coupling other than FETA **BH* The products obtained whether mono acid F was included or omitted were brown and dirty* It is evident that coupling produces some effeot, physical or chemical, other than that of slurry mixing* Peculiarly, samples in which mono acid F was omitted, bled quite markedly, and since neither the Hello Bordeaux nor the Para Red bleed, it was hoped that the filtrate would furnish further insight into the nature of the change* It was thought that the bleed might have resulted from the displacement of the alpha-naphthylamine portion of the Helio Bordeaux by the P*N*A* giving rise to F.H,A. ** 1-5 Acid, This is possible since it is well known that media best suited to coupling are most satisfactory for such replacement reactions, and diazonlums with negative groups in the para position are most effective* Judging from the ease of diazotisatioi and rates of coupling, F.N.A* might readily replace alpha-naphthylamine, (See: Anllinokrasochnaya Prom, 5* 76 (1935): CA* 27,4677; 29* 5087)* However, the bleed did not give the expected color change with caustic and did not spot like P,F*A* - 1-5 Acid which was subsequently prepared. It is known (ibid) that these displacement reactions usually occur through bis-azo formation followed by displacement* Indeed, in preliminary test-tub experiments, the Helio Bordeaux appears to undergo reaction with P,U*A, diazonium. Insofar as the products obtained were undesirable, it was deemed unwise to devote further time to this interesting problem* Mono acid F was replaced by 1-5 acid and coupling carried out in the usual way, the B*N* being precipitated from the caustic solution by HaHCOg* Like Mono Acid F, the 1-5 Acid remained in solution. DUP050316324 and It could be 6bseated to couple mgr rapidly than the precipitated BBT by nature of the brown color of th P,B#a .-*> 1-5 .Acid* The reactions parallel those $a which the mono acid F Is used, coaly to a certain point* BiMnishiag the amount of 1-5 Acid incorporated increased the rate of filtration, and under a microscope the particles appear to b# amorphous* TOC pigments bleed badly, the filtrate being a distinct purple due to the fact that the F.M.A# --*-1-5 Acid changes in color at a loner pH than the PJ.i. --*Mon Acid F* Wnlike the Fare F, the sen dyestuff is washed out of the pigment by the hot water wash, leaving products of the RT-32-D type* As the P*H*A*~el-5 Acid is removed, the pigment particles can be observed as minute crystals* Although it is known that solid solution may occur in cases of limited miscibility in the complete absence of isomorphism (Walden & Cohen* JVA.Q.3# 59*85911. it seems not impossible that this phenomenon may be the result of the formation of a structurally different dye, ie, coupling may have occurred in the 4-position rather than the 8# Why this should result is difficult to understand. .On the other hand, the fact that the soluble P.H.A* memo, and bis-azo dyes of chromotropic acid were retained by the pigment renders it difficult to believe that spatial differences could have produced this effect only insofar as it is realized that the pigments containing the chromotropic acid dyes were not washed with hot water# Again the problem was discontinued with the accumulation of this empirical information# C TO use of B*0#H. in plaee of Mono Acid F was studied further* As in the ease the 1-5 Acid, the B*0#T remaining in solution coupled before the precipitated BR. After coupling, examination of the slurry at high magnification showed rectangular plates (probably Para Red) andaclusters of smaller crystals (probably FRA--#> Bo b ) This method of coupling is obviously not suited to the replacement of Mono Acid F by BOH since the FRA^BOH is insoluble, and couples before the HFA couples to BNa Consequently the product is little more than a dry mix* Crystals are obtained and they are larger than the agglomerates obtained in the true RT-70-D type Coupling with the EH in solution gave a more uniform product which filtered more rapidly than RT-ES-D, i.e. more rapidly than any products obtained heretofore. However, the products retained their brownuess in all oases. Coupling method 276-60C gave completely negative results, the product being of the RT-22-B type in color* Ho further attempts will be made to replace Mono Acid F by BOH* he incorporation of small amounts of the FRA bis-azo chromotropic acid dye gave brown produet3* It was therefore decided to drop this line of attaek# Heaations have been run to show that removal of excess nitrite by Brea treatment of the diazoniua has no appreciable effect on the tinctorial properties of the dark Faras being obtained* A more quantitative measure of average Para F bleeds in consistency series has demonstrate? as anticipated in previous reports, that Para F retention is higher when the dye is incorporated as such, then when Mono Acid F is used. This phase of the problem has been suspended pro tempers but probably should be studied further# It was suggested that series be run in which the amount Of EH present was out down. Bronzing decreased slightly, and there was a slight increase in brightness. These effects go through a maximum# DUP050316325 products th'O. become light ant flat in mas stem* .-There an s many variables in such series that it is extremely difficult to interpret the results# It is obvious that cutting * down the amount of BN used -will alter the Bara lei. Para F ratio* and " from previous work, this appears to be of considerable significance* The tread has already been indicated* Further* an excess of the diazonium will 'be present* this may have some effect* On development, the myriad thermal decomposition produets of the diazonium may exert some unknown and consequently difficultly controlled influences* These decomposition products would probably be preponderantly yellowtoorange solids, and the incorporation of these could readily be expected to produce the light flat mas stones observed* It has frequently been suggested that these decomposition products might exert a dispersing action upon the pigment particles* but it is difficult to understand how the resultant phenol, oxazo, hyirazo, etc# compounds could do so* Another variable, introduced by reduction of the amount of BIT present* is concerned with the isolated effect of the removal of the excess B from the pigment* When a more' stable procedure is developed* it is planned to study this effect separated from the concomittant variables of these series, slate it is felt that inclusion of this dirty gray colored substance cannot aid in the brightness of masstone of the pigment* Indeed* since fluoresces In caustic media* it is believed that excess BN may be a contributing cause of bronzing# B* Preliminary work on the drying of Para Bed confirms established data* RT*22B, practically a pure organic compound, becomes dark and bright in mas stone, weak and blue in tint on heating to 105C for 12 hours* This appears to be most readily explained by a change in particle size. RT**70-I), on the other hand, becomes light in masstone, weak and blue in tint* This again may be due to a simple change in particle sine but it is possible that the Para F in solid solution with the Para Red may be responsible for inversion of the heat effects upon the masstones. Apparently it makes little or no difference if the pigment is initially dried at a low temperature and then baked at 1G50C or if the wet cake is dried initially at the high temperature* Grinding produces the same effects, only to a more marked extent* presumably* through the heat produced in the grinding process* Preliminary observations indicate that cake thiekness probably does not influence these phenomena* although press cakes of plant size have not been studied, and caimot readily be studied in the laboratory# It is at present impossible to predict the influence of drying. Plant samples of R?*70l) when laboratory dried are dark, brown and muddy in masstone versus plant processed material. Dry mixing of this standard BT-70-D with Hello Bordeaux BL produces darkness and additional brightness* The same ingredients when slurry mired are similarly dark and bright when dried, but become light and flat when baked. Further, the loss in depth is not as great as when an RT?0*D cake is baked alone. These observations are additional evidence contra**indicating the slurry mix of R1V70-D and Hello Bordeaux BL* It appears to be much better to dry mix the two substances and very fine colors are so obtained* In the course of the filtration study, an unusually dark bright color (49G--2GB) was obtained, which from probability data appeared to contain a small amount of moisture* This sample on further drying under similar conditions (c* 10$ humidity and 60C) become light and flat in masstone versus the original* It was therefore decided to study extreme case* A portion of a press cake was thoroughly dried and another portion f8 flushed on a rub**out board (representing, it was hoped. DUP050316326 m&m w<rrjib w ib moisture content in ink formation). The flushed sample formed * a thick emulsion of pigment and water is oil, whisk respired rigorous mulling to remora the remaining water, This teaaeioue retention of < moisture may he taken to indicate some type of conjugation or saturation of the secondary valeaees forces of the polar atoms of the Para F. It so happens that the flushed sample was light and flat versus the dried * sample, fits seems to he the inverse of the usual ease, and appears to indicate that trades of moisture may he of considerable tinctorial H significance* It may be assumed in this instance that the largest possible W amount water is present and this produoes undesirable mas stones. In the case of the thoroughly dried sample a superior product is obtained, hut the two extremes need not necessarily he connected by a straight line. Possibly somewhere between these two points, the influence of adsorbed moisture exerts a maximum desired tinctorial effect, and 490-2OB lies somewhere near the pea|. However, data are by far too limited at the present timO to justify more than suggesting such a trend. Since baking experiments produced effects somewhat like plant processing it was assumed that in such preliminary work it might be sonsidered an index of what to expect in processing. It is planned to carry on a more extensive study of this phase of the investigation. SXEEBIMEHTAL DETAILS See notebook #490. 490-19: filtration study, the influence of "salting out" by HaCl and BCl. Hello Bordeaux Bl dry mix with RT-22-D. 490-SO: Filtration study, wash temperature. The in corporation of bis-azo-chromotropic acid dye. Incorporation in coupling method #276-600. 490-21: Filtration, consistency in 490-SOB and comparison with consistency series involving replacement of Mono Acid F by Para F* Study of bleeds-. 490-22: Effect of decreased Bn on bronzing. Omission of Brea treatment. Para Soap. 490-83: Filtration and texture. Points of addition of 490-24: Replacement of Mono F by low. The influence of diminishing the amounts of BN. 490-23: As in 24 but FaOH - HagCOS coupling medium* 490-26: Drying studies. 490-27: Incorporation of Helio Bordeaux BL #2196. Dry mix and slurry mix. The influence of drying* 490-23: Replacement of Mono Acid F by #2196. 490-29: Replacement of Mono Acid F by 1-5 Acid in DUP050316327 m m UataisMag enomts# The prefaratim SffA - 1-5 Acid, ?f DU P050316328 ygj&8tT-1 ciiHni FIIS: KraSBAT!* ISS&BMBBB 1935* laboratory work on the dark mas stone Calcium Lithol was ' completed during this month with, the stabilization of the U0B, reg# 9 BW-M<im-aQid S' formula. aquas* arc Buplieability studies on the latest formula for the dark Calcium Lithol (472**61<*S) were satisfactory. Studies of variables auoh ,ae rate of strike and increased temperature of strike were found to hare no appreciable offset on tinetorlal properties. Variations in digestion time in the range from 30 - 90 minutes has only a very slight offset on the tinctorial properties* However, the digestion time of 60 minutes seems to secure maximum depth. A composite mix of the latest check runs on 472-610 formula * was set up as K-81G8. This material is superior to BT-579~D in depth of masstone, strength (over 15$ stronger) cleanliness of tint, and is^j^e bleeding in oil {RT-379D bleeds slightly). A composite mix was made of 472-55Ag Be, Og* the blane fixe extended Calcium Lithol for Rubber and set up as K#8109. This material ground in Rubber is equal in shade, dispersion and light fastness to RL-4Q8-D, Semi-works trials are now in order on both K--8108 and 8100, NB* 472, page 156--161# m DUP050316329 'efciciini e iy h o i, .- v BY* ^hCuLf*^- A#*A .// FEES ; SdattHB BAYS* 1935 Complete results are available on four batches of BT-379-B which were made in the plant under Bevelopment Section supervision. Eight and strong material was desired for shading purposes. One batch -of RY-3G0-;D was made with .material satisfactory for rubber being required. The first batch of RT-379-B was made on a formula that was ad justed to give very slightly dark material, fhe following variables were used* 75$ TOB - '25$ YGBW, low amount tef calcium chloride (ISO# per mol), struck in development volume, and developed at 140CJ?.. The results were satisfactory, the resultant c olor being s.dark, v.s. bright vs. the RT-379-1) standard. The next three batches were made to secure light and strong material for shading. Thesd batches were all made onthe same formula tion, the variables used being as follows* 80$ TOB - 20$ TOBW, low amount of calcium chlor M e (160# per mol), struck in development vol ume, and developed at 160 I '. Satisfactory light and strong material was secured in the caseof the first two batches, but the last batch was v.a.weak and dirty vs. the standard. In the case of this last batch, however, a high coupling volume and a high coupling temperature (703? instead of 35F) were used because of an error made by the oper ator in making up the beta naphthol solution. Results on these batches are tabulated in Table I The RT-3O0-B batch was made on the K-7038 standard formulation to give satisfactory material for rubber. Results on this batch were unsatisfactory vs. the rubber standard^being 5$ weaker. This is the first batch of five made on this formulation that has been unsatis factory for rubber. Results are tabulated in Table II mSBinBHTAL B38TAIES See tabulations DU P050316330 C4 * rH l H ta fcffl & cn co * <33 52: W &* ffl ffl p c ft T3 ft >4 H rl Jx -Pi Si tn o CO P ST < P, X n ou t> p CO 3 { h ft* S$ ffi -p d!S J3' <a o, f<r5f +S3 to 8 rH O > ft P 03 rH & P ft ^3 I -p rH 33 ffl g) >B-- <3 e>; Q oM ft O <sH H b9 *04H3 ft H H rH ft* 0 ft p> 0 0 CO O 00 p 0 rH b0 rH ft ffl r *rl m ffl P ft ft s 1= rH rH f*f*l 5J ffl rj fa fto ft O O tffl rH O 00 >* rH P CD (4 s % * <0 *0 ft P rH 0 s> rPH ^f3t m > ft *o ft p > rH p ffl >. > <*$ p> %4 T3 CQ S* p 85 ffl O H ft ,o * P to H P ft p P H rH p, to iS% C4 rH sa o * H H sal t>- m da p p rH I r<H0 to v? <o CO ov rH HI o C* t & Cfc H H fc* p or 4: in e- to h S<r4 <> CO ** O CO ^00 a' to co oo C tionCO\ 3* <0 <H t* *& ffl 2 It 91 ft I--I Hi ffl H JM p| ffl ea O a> ffl uo O CO p v rt SK so to fr- u +> SS rH nci: 43 S <B. I 5 g OS! to < tn 1 co CO 00 CO * u H > *t3 g t* t o M Hf =a a 43 9 cc ag t>s> O T3 "S ua 43 #1 H#% Xt PP H c< rH S3 <H ilfl i, IS ss o o N JN O ffl SB ffl in Hf a C0 8 S A52 e rH| WoIH- f**f*l 2 3d *ri SP Pa 41 cn to <0 DUP050316331 i b s ~- fy m%mrm& mt Ar%^ m&mm'tr* ^hu^^ IMTH' im matt &fmm iskTSt mcmsm- 1935 Production on this color was continued in the plant under Development Section supervision. Considerable difficulty has been encountered in Securing OK top. sireng material to build up standard stool. Besults on only two batches are available for report. smmmr & The two batches reported this month were made on the standard K-7290 formulata on except for a 33-1/3$ out in the Para Soap used (32#/raol instead of 45#/mol). Both of these batches gave unsatisfac tory results grinding out s.dark vs. the standard. This undesirable depth of asfesstone is no doubt partly due to a high temperature of dry ing (160P) which has been used because of lack of space in the dryers set at 140feF. Arrangements have been mde to dry all batches now in process at 140F, There are three batches in process at present in which the para soap has been cut to 24#/raol in an effort to secure lighter material for shading. Keaults on these batches will be reported next month. A satisfactory 605 lb. mix has been mde consuming 411 lbs. of current production material. Sub-3tandard stock on this color remains high. Production is tabulated in Table I and the mix in Table II. DUP050316332 m 09 ** nr> co 8 0 > P HP 0 >> -P g* s 1> a t (> CO J * frj r* > ur> <10 H 0bD *w 0 ot ** to tcros CO tn& r4 m 43m at %P, 00 0O 0 a* tO eo 8AO I a* & -03? 09 t? rH C" rl 1O WJI -t 0 ** 0 CO sO A tn tfc S to * CO 0 H0 S23 o 4o5 00 -P r* * m OL P3 aS *o iO M VS <ts & 0' & CO AH W Q 0 3 += e-* 1M BH H H 43 e8 mOt c*o- 2 rl * && 4 *0 to ?* 5 ggj sn <o tn <rf* +*, 1 o tc?o** 4* fcft *rt 0 0 tS 00*3 0CO c% o* to o% *& ,4 0 #SP IO tPP >1 0 23 9 0 i .a DUP050316333 ;-s; :'..ri.;-,r%UiW'' "* v ' -- -?? u-ms*w <m*f ' *<"- ? .rwrur ~m' I! ** 'J&ttfcfc 5r^fJ *mWT7&B Bfs i|4 &Sf VSfcffs nt*& fl&i&yra ?,>as* t* jarasias&ML.. --Ais feesrii** ^a&aaS*- it*** f Sferift & Ham &$m Wite *r;.a*u;.- tt ytajasH".* xv .:.af&- ?** *u.i i . **?.* * ,,&* F-:a'i*5 :mZ ar a*o.i3r s&y 'sw* &i?>.tyi~M #'s l&fe Ids?* *>?&. n ?< miXs .$Nh;t ttiw?'&&%,*& * 2>. -i.#;ft.l"$8 ` 'll; .> *.-.< tfc& M^i *$? Wiffi assa&swts# fctfr:-;? *$ <3;s?lte;3 aM &$ ? ^ imrmmm t&twv&xtMF turn?*?*# ::.a ^ouislfe^ ntc? eT *j \*tm* t`m 'Zim l*#& in a^reai&SH *u%s* JTJir% i* a^-toi***'* * O* '-'W &assj* S * **e?3.? V;-i..?f;3 ;--i Xv: . >!. 0 &-4t i* n' , 4 :;^VVfp :?vyt.;.y; leas aflJA ..'a'W#**'* # Ifa^.-UPiS y?3*..ris y, ^:;xaaga M -a^ns ?0*3iKfc* j* . -few S^ Sssrte Viv Kd \ .->:, &&& ,>. stlrlda a jyiM'w* ;>? -mi;! v:??v;s ^i^tc???*: rvi -;c:un?<: rje<sv;.j#<s Tm~ iVA Sniaturty?*)* si**? *&* 3^`.;v: -> <mx& jul&tv* t-a x^i;x'fc"x.-': ' vu.n.\ :1> TV:.'.<'S? S3? XY.-i'-'f... kU -:^sU-:: -'-I, .- ,:a v;-j ;<..' ' :wW5P J'' * ;*+ '?f':; ' J Tut?.,- A ',"' r--'<`'ns '.'" ''.Mr.VT. ;.'?:!...:; . ,,,s. '- .: -r^1- as.X'vti . :"";'.v.--i< ;v".X. :;--.i';. -,r:' < i *u.-; ;T/-.r:v^ ';*w oi* 4o^ ?ms? n&%$xz*dj DUP050316334 visimiT c o l o r mmmcs r e p o r t mm& jmjm 1P-524& BY* C.&yfa-* msa p p r o v e d A t*/-^ PILEi B4SSA-^MfWBATE: DECEMBER- 1935 imoDuenoF Production was started in the Semi-works on this color to build up standard stock. Five batches were made with a total estimated yield of 600 pounds. SUMMARY & OOKC&gSIOHS All five batches were made on the same formulation checking SIT-7208 which had given satisfactory material on previous production. All five batches were fairly satisfactory, average results being slightly dark in masstone, OK in strength, v.s. green and clean in tint and slightly more transparent versus YP-324-D standard. It was not thought necessary to introduce a lower sodium resinate variable on these batches in order to lessen the transparency because of the fact that there is a 150 lb. lot of material in sub-standard stock which is less transparent than standard. A mix has been made consuming all of current production together with thi3 150 lb. sub-standard lot to give 735 lbs. of satisfactory material. Results are tabulated in Table I and the mix in Table II. BCESRIMSHTAL RETAILS N.B. 430. page 32 DU PO50316335 Jft! <0 a> co <8 D s* 69 P <SDC 1<Q * H I 1, 35 8 3 8 &b CD 1 cfcflj O t H 1 3 Ml tn * & <D r4 $ &* *t ts o* st <o s .( * na ufOs fc- -cs 1S %_ It a_ uw> '. * <ft0! $3 erf l o *1 3 I O t -J&p30 t u t l XQ > *>f3 n > a I cf~t oU) H OcS- o o iu~4xtfnt* fc-- frr ii U * * DUP050316336 * y- : *y ' ^ . 3~~ tf*3 /*& .f SUBMITTED BY! APfKQTll- BY! v yTT-ff! H-t-g&r2^**&&& mmmm 5.935. srnmmm. Work; was started on Bed Toner, E>7699 (Meta-sitroparaaaisidine - M) with the object of duplicating the original sample and ebtaia'lalditioaal material for evaluation* ^ai^Y: Mjwam. Material of Mb ta~nltro**para-anisidine B-8234) was tested oh E-7609 fomnia versus a sample of M.N.P.A* of Jackson laboratory, lie toners were close to each other hut v.s. brown versus Y-7699 and of lower oil**ab sorption. Investigation was started with the object of stabilizing the method in order to obtain consistent results. The variables sueh as alkalinity of coupling, rate of coupling, heating development of the dye and pigment/ and variation in the amount of B.N* were studied. So far no appreciable improvements have been obtained* High alkalinity as well as rapid coupling results in brown mass tone material. A large excess of B.N* has a tendaney to lighten and dull the mass tone* Isomers of Meta-nltro-para-anisi&ine were studied* The coupling of 4 nitro 2 amino anisole - B.N. resulted in an Orange Toner, which is dark, red, slightly inferior in light fastness as a straight toner versus Permatone Orange YT-241-D. The coupling of 5aitro-2**aminoanisol - B.N. resulted in a red toner which is much lighter, brighter, yellower and superior in light stability and less soluble in oil than K-7699; and darker and equal in light fastness to RT-364-B* The 5 nitro-2 amino-anisole - B.N. pigment ranges in shade between a Barium and a Calcium Eithol. SEPAL PBTAILS 487-36 A, B. Meta-nitro-para anisidine D-2834 resulted in a pi^aent a* close to material made with the new Jackson lab. sample. The purity of M.N.P.A. - D-2234 seems to be, however, lower as less sodium nitrite was taken up during diazotlzation. aasstone. 0 - All Caustic coupling resulted in a dark brownish I) - Caustic and bicarbonate coupling (eliminating the aoetie acid) had a tendency to lighten the masstone. Caustic and soda ash coupling resulted in a light and bright masstone. 487-38 A - Control on 36*B did not check. Heating after coupling had no appreciable affect upon the tinctorial properties. All alkaline coupling neutralized with acetic acid after coupling showed no improvement and resulted in dark, brownish material. 487--42 - Variations in rate of coupling - 5 mins,, 15 min., 30 mins., and 60 rains* The results of this series are not quite in line. However, there appears to be a tendency toward slightly darker and stronger products with decrease in rate of coupling. DUP050316337 2 48?<*43 - series variation in the amount of B.N. - theoretical amount M$>> and 6$* A smaller excess of B*N* seems to give a darker mas stone. A considerable excess of BH. was obtained by using the theoretical amount of B.K* which indicates a low purity for the M.K.F.A.B* 8234* B#B* 38? page * DUP050316338  ' . ,-./!' .. :j * '" " V ? v ,'i- ' ` gs---vr*/ jd ^ '' ,.^m.,.,lgl*,;;fe.l-....: mBWlWED .BY* & <&- APBROtlD BY; ^/ * %2^'T TXlMt 'ToWCRS B&TSt REGSMB2R 1935* One batch of this toner was made la the Semi-works to test the dye and the formula. This type of color Is mad from IKd' tho' sOl Fast 'Grange R Obtained " in dry for fro the ByWorks* SU1IMRY MJ> COWOLDSIOMS The product obtained was muddy in messton and dirty and weak in tint as compared to the Kstandard* This result was cheeked, in the laboratory. It is believed that the inferior products are dufc esithei to contamination of the dye or to the fact that it was dried out instead of being used in pulp form. Ho further work is being done in the semi* works* IXFgRIMMTAL BBT AILS !?*B. 455, p. 81* a 140 F* blue. SW?537 * l/soth of K-T984* Bye solution clear at Spotted clean* Grading ws E-T884 s,dark, t .muddy; wk, &. s.blue, wk., '-I DUP050316339 3iT~ ***' mmivMB BY: AFFROYET BYf mmm j&RQOK ?OfeK RT*gm~W fie^t^ac^ J Fills BQRPO MAROON *'>V BAfl; ESOEMBEB 1936. - iwmomoTiQM Three batches of this Maroon were made employing the higher alkalinity of development used in Works series in August of this year* In other reports was the same as previously used la the plant* in the plant the last Semithe formula ' 1*01'&RY MD CONCLUSIONS Two batches were much darker than standard in lacquer and the third was slightly dark* A delay in running in diazo is the only likely cause for the difference that wqs noticed* A total of 975f SSS was consumed in mixes of lacquer and paint material. Special attention was given to speed of processing, no unnecessary stirring periods being made* An increase was made in amount of caustic soda used in the development so as to give a positive test on Brilliant Yellow and a rH of about 8*2 after boiling. This is believed to give greater depth. On the basis of this series, a new standard formula, F-8110 wee written. 3 'CPYRiafYFr ? b PET/1 IS F.B. #385, p. 180. All three batches were made on same fojmula - 0*75 mol charge as in 44518 except increased final ceustio soda in development from 60 to 62#. Based on SW-7^45 - Lot 46540 - Lacquer test - dskk wt, 406# w 46672 n 46689 - " n * dark wt* * 411# " s.dark, v.s.bright wt, s 404# I ,y/ DUP050316340 .< J' V;r;,\ ts r . , ' ' v . >" j-jr-y'5% /&*/ mtO^y BYs JS FILE; >>"h DAIS: PBSEMBSR 19256* MROXSTCTIOH Twelve batches of this Maroon were mate la the semi* . wearies chiefly for production of standard material. Severe! variaisrions were tried in an attempt to obtain standard depth with enual brightness* In the plant one batch of BT*130**iP was made tm Pari in. s u mmar y mn mmmsiam Standard formula with a 50$ inereas in calcium chloride (T0BW lot 34} is giving the most satisfactory results in the seM^works, five batches on this formula being equal to erdarker than standard with satisfactory brightness* (These batches should consume nearly equal weight of lighter material}* The reduction in amount of B.0*N. which has been found helpful in the plant in obtaining brightness* resulted in rather light masstones. Pei&her increase in ealeium chloride nor reduction in final caustic gave any improvement on this formulation* Lot 33 of TOBW gave abnormally light products and it will be necessary to make additional experimental runs before this lot, of which a considerable supply is on hand, c.sn be used in production. This series has been started* The batch of BT-130-P, made on the formula used last month but with a total inorease in calcium chloride of 50$, was of satis factory depth on slurry control. DUP050316341 Pto t e-4 < n to 4* p 0) t St B p , H o'SC .ta eo *4 > 43 60 p PP 43 43 60 tc <S4 *c4c <CS p ! i~i o M 413M * *x > (M CL` t> t> *& MU 04 <ci cS a to Od * a* a* it * * a# * a#1 to a ata* to to to to to a*a S o o a C6 0> 0 o> 0 o C& CB 0 a(S' to 3p P0i <0 0 Eh o >i PQ wl PC CO OP PM 03 gr gp rf 3 P& ga X s s s>> PC (Q s j Cp c >* , hS pm P t>.HP(B iD, IS ts t: ga tt) >i s m cs 43 a * Wet Q )M ra to p s m p e to * p m f* Po M fXt O rH fit EKS iH- m p> p OHH P PtCO t> 3 ss tP wo 15 29 O 5p s=5 U J2 CR to MB* 3 * o ce *~ X SM 0 * 1 a o to *rH p p fM s> <0P *g S3 *2 P JM p P.4*t ft ,, "* O 0 #. O > i*'l s 8**1! W*o 1. IS P X3 (4 P$ < P e*s*H JoM xS g o 8 P- X* to Bo C- P X P' t gs 03 M0 iJ * 8 43 43 SS 2 *< ii y*0 3 43 * 6010 V* s3 <$ p p a p j 3 *y*s ig CO B- PS ti x to I M0 om g to P- I ja a &e= s ! ICO B- Oto a^# IS e* (O CO A. *. a p DUP050316342 PIGMBffT COLOR RlSBAEiCH mvmT ssr xfS 7 /& SUBMITTED BY: APEROTffiB BY: >>*- > *p iLit- wm&^isMQ&mmTEi 3KGMBIR- 1935 IKTROMJCTIOM Some difficulty has Been experienced by the plant in obtaining products consistently of satisfactory depth and brightness. Three batches were made in the plant during the month under Development Sec tion supervision in an effort to determine the reason for these varia tions in quality. SUMMARY & GOHOhUSlOHE All three of these batches were made on a formula cheeking present plant procedure. The first batch ground out vvs dark in lacquer but was unsatis factory because of a slight bleed on over stripe bleed test. On check ing back* a possible reason for this bleed was discovered. When this color is developed, it is necessary to split the coupling in two parts and treat each part separately because of the high development volume used. These parts are, of course, eventually mixed in the filter press. A vat control from the first half of this batch shewed a distinct bleed on lacquer test, while the second half was satisfactory in this respect, and the first half of the batch was s.lighter than the second half. Mixing of the satisfactory material with the sub-standard half of the batch produced the unsatisfactory bleed secured, from these results, contamination would seem to be the obvious reason for the difference in bleed although the vats used were scrubbed out thoroughly. Another possible source of contamination is in the pipe lines running from the coupling vat (which is on the third floor) to the developing vats (on the first floor). The possibility that these lines were not thor oughly clean would seem to be borne out by the fact that the first half of the batch which was run through the lines first gave unsatisfactory results while the second half was OK. Before making the next two batches, special attention was paid to cleaning of all the equipment including pipe lines used in making this color. Lacquer results on these two batches were satisfactory, both batches being dark, OK in brightness and OK in overstripe bleed vs. the RT-363-D standard. Results are tabulated in Table I DUP050316343 p H O P CttooO d rH <D H >-* P m rH63 pn 2U3 CO to a cn erf <DP erf SO3' M 0 fit 0 03 * p 0 6* 0 2 ** *j ^24 0 "& H 03 > & to 6- 5 m tn pHaI ,fc.gj UO 4> ., u M O rM ir3HA no fe~ t P O* W r *_t_3 2FAr,Hfl 3 rH tO CO J> <0 CO <*} HUtrj *1{4 rH *>t1J Pi d H -> lS PPSa grf g <3* O *dcmo 3 Cl t CO V <0 >> 0 r& 0 08 P S4 P *et3rf CO co sto bSir bO<0 rl r-i 03 o* in o CO 0 0 j H! CtO do85 & f^c P CO CO CO CO 525 *3 o gm |H *> <0 d 6 m to R CO > Ct0O A 'V*'* DU P050316344 1 STOUXSW6 APPROVER Y: JdJU^v4>&j mc ' ji^aDTTGTION f ^ PILE: M*CErTSnS MTS? SOTBSR 1935# The ppobleit of matching 0-258058 a barium lake ofi Orange II ( with admixtareof Chrome Yellow) was successfully concluded during this month* i|i&liOaMlity test# on ^57-24 formula were satisfactory and material was obtained whtOh by dry mixing.with blane fixe and Y-299-B gate a perfect match tot O-?802I8 The formula for the straight lake 587-24 was set up as E-8098 and the dry mixture as K-8099* Evaluation was made in rubber of a straight toner of Orange II and the lake 387-24. Both dispersed well in rubber, were equal to Orange in light fastness but weaker than the latter. The colors exhibited no migrations* E*B. 387 page 70*$} 72* j**DUP050316345 > StJH&ITTSnD BYj APPROVED BY*. ramtan* c o l o r r b s b a r c h r e p o r t /? , . , duct^f- gag-WORKS FRODtrCTTOH // / FILE: '** 800BATS: DECEMBER 1935. IHTHOBirCTIQH 69 batches of 16 different colors and 6 lead nitrate purifications were made during December; these included 15 batches of RT-354-D, 5 batches of YP-324-D* 5 batches of BP-16S-B, 6 batches of G-389-B, 10 batches of Y-18Q-D, and 7 batches of molybdated oranges* A second 12* mikro Pulverizer was purchased and installed during December on MO ir*481. This pulverizer will go into service the first week in January and be used as a High Speed mill, as well as being used for experimental grinding on a wide range of colors# RT354~B, Maroon Toner - Fifteen batches were made in production of shading material and in testing T.O.B.W* RT7853*D# Permanent Red 2B Toner - One batch was made to test another lot of dye* YT-7984-D, Llthosol Fast Orange R Toner - One batch was made in a trial of the formula and of the dye. Y180*D, Light Yellow - Ten batches were made in con tinuation of development work on this new formula* Y-359-D, Medium Yellow - Six batches were made in testing lead nitrate purifications# Y0-8074-D, Molybdated Orange - A total of seven batches were made in continuation of development work on this improved product. YF-524-D, Hansa Yellow Lake - Five batches were made for production of stock# G-389-D, Light Green - Six batches were made in development - - work on a stronger product, y* GT-337-B, P.T#A# Toner - Five batches sere made for production of shading material# ' GL-407-D, Treated Pigment Green - One batch was made to obtain material for drying experiments* BL-164-D, Peacock Blue - Two batches were made to obtain shading material* BE-149-D, Dry Dispersed Color - one batch was made to fill an order* DUP050316346 //^ BP*16'8"Da Extended P.*T*A* - Plhre batc&es of this Victoria Blue B Lake were aads in Sereloppeut of a nee sbafte for BbHiber * *$ ' DUP050316347 c 53 /// ' Lot* Material Transferred Boring Peoamber 1955 Researefr 3W CB**20Q Color coa Lbs. Gronp Coot Unit Total Coat 4393 4396 4397 4398 4399 4414 4413 4416 4417 4483 4433 4424 4485 4486 4430 4431 4433 4433 4338 4405 4406 4407 4400 4401 4403 4403 4404 4418 4419 4430 4431 1 RT-554D 1n 1n 1 tt 1 ft 1n 1n 1 if 1 rt 1 n 1 ft 1 ft 1n 1 t 1 1 tt 1 ft 1 ft 3 Y-299-D 5 Y-359~D 3 Y-180-D 3 Y*509--D 4 Q-389-D 4 ft 4 4 tf 4 ft 4 ft 4 tt 4 rr 4 ft 115 119 117 120 120 117 120 120 116 117 119 120 118 60 59 57 59 59 779 466 644 441 173 173 183 172 90 167 169 170 175 3 2 2 2 2 8 2 2 2 3 2 B 3 2 2 2* 2 2 2 2 3 3 3 2 3 2 2 2 2 2 2 #115*13 . 8*58 8*88 8*01 8,39 11*40 11*40 4437 10 YP-324-D 734 1 124,51 4409 4394 4428 11 125 125 BL-164*D RL-4G7-D BP8G47**B 139 303 418 1 2 1 45,70 46.15 145,51 4408 151 TO*8074~D 360 2 13,88 DUP050316348 #10 BM. fSOBtrCSIOF BEPOBT FOB EESBKBSR 1905 iisMROH swm*wms .* o Bate& G@8 15s* Struck lbs* Packed $> Yi#ia A $$01 0# os 05 "B 08 89 10 7S11 18 15 14 15 7510 17 18 19 20 7521 28 28 84 25 life ,, 7586 27 88 29 50 7531 32 58 84 35 7536 57 38 39 40 Y-180-B *3S9-D b p --b BY-S54-B Y-180-B ' .fQ*00OM MMP8SM Ef-i54-B Y*180'*B BT-334-B 10-8003-0 Y-180-0 0-389-0 . Y-180-B 10-8003*5 <5-389-0 10-8074-0 RY-354-0 YP-324-B Y--180--B 10-8074-0 0*389-0 BL--164--B Y-180- YP-384-D 6-389-0 BP--168-0 ft Y-100-0 6*389-0 YP-324-B Y-180-B YP-324-B BP-168-B YP--384--B BL-164-B RY-7984-0 Y-80S1-B BP-168--B Y0-8074-B 30 196 69 109 8 30 88 *8 109 180 30 176 30 180 176 50 109 180 30 ISO 176 90 30 180 176 6@ 68 30 176 ISO 30 180 68 120 90 39 ISO 68 30 30 185 65 117 8 m SO 118 38 119 125 31 170 31 185 165 32 114 116 31 186 170 87 31 119 171 70 67 38 176 118 31 116 67 116 76 33 156 65 89 100*0 94*4 91*3 107*3 100.0 103*3 90*9 108.8 106*6 99*2 . 104*1 103*3 96*6 103*3 104*1 93*8 106*6 104*6 96*7 103*3 105.0 96*5 96*7 103*3 99*1 97*8 102*9 98*3 106*6 100*0 98*3 103*3 96*7 98*5 96*7 84*5 84*6 97.S 94*8 96.7 DUP050316349 ' ...... . - i' ' ' , < ' / . ' ! Bateft- Oede Lbs< Otruek Lbs* Paeked. , 7BS ' 45 * 45 7545 4? 48 49 SO 7651 58 53 54 55 7556 87 58 59 60 7861 68 63 64 65 7566 67 68 69 70 7571 72 73 74 75 RT-354-B 03?*33?**B Y8Qgl**B RT**354*D m 109 34 150 109 n 109 Y-180~B 30 QX*337I) si Lead Nitrate Purifloatioa RM54*B 109 0L*4@7*B n 24 ft T*.337<B 34 Y~359~B 81 Lead Nitrate PurifleatlOB y*559**B 51 RT*354~B 55 OT537*I> 34 EXV354-B 55 Lead Nitrate Purifloatioa Y*359~D 31 GT3S7B 39 Lead Nitrate Purifloatioa RT~354~D 55 Lead Nitrate Purifloatioa Y-359-B RT*3B4*.B BB-149--B RT-354-D Y~3S9-B 31 55 300 55 31 Y06074-D 30 Y5S9~B 31 RT-354-B 55 Lead Nitrate Purification RT~354B 55 5258 180 35 185 118 120 31 36 ' 118 24 ft 35 30 31 60 35 58 32 40 57 31 59 290 60 32 30 31 58 61...... 5306 % Yield 116.0 102.9 103.3 108.2 110.0 108.3 105.8 m 108.3 100.0 ft' 102.9 96.3 a 100.0 109.2 102.9 105.5 103.2 102.6 M 103.6 100,0 107.3 96.7 109.1 103.2 100.0 100.0 105.5 110.8 101.3 DUP050316350 smmmT ow #10 b l d g , p r o d u c t io n r e p o r t f o r De c e mb e r 1955, RESEARCH SEMIWORES Cote __________Lbs* Struck RT~354-D R*7858 RT~7084f> X*180~B Y*0O214) t 70-8003-B IO~8074B YP3S4*D 8*388 GT*337B GL<*40?-B RL*164*0B B1*149*D BF~168~B 1287 m m 278 300 188 270 310 600 1076 175 24 180 500 -341... 5258 LbBPacjce6 1357 30 33 388 511 187 381 217 585 1037 181 24 165 290 332 5306 & Yield 108*0 80*9 84*6 103*6 103*7 100*5 10410 108.3 97*5 9.6*4 103.3 100*0 90.5 96*7 97*4 98*7 DUP050316351 DUP050316352 BOBOAPITOLATIQF '< COLORS TRANSFEREES FROM SEMI-WORKS JliT DECEMBER 19 35 Toners ** Yellows Greens Oranges - "HP" Lakes * "RL" " Total 185# 2359 1471 850 1158 342 7387# DUP050316353 *0 m m x U.xb!^xv..<iiiiLv<:xuCrJu //7 * ISO grinds of dry abler* 4 grinds of pulp color and 17 mires were made in the Beseareh S*W* for the plant during 9 Beoember 198*' War Orlads Green Boll: lake a 'Bed loners C*P.Blues Blue Bulk Bakes Charge 737*8 n 748* . 737*8 Batches 14 5 10 "W" Lbs* . 11*489 1*848 6.586 w^m-- Bale Grinds Bed Boner C*P*Yellow Oharge 737-s If Batches . 3 1___ Bbls* Lbs, 250 1005 Mires Gharge Blue P,T,A*Toner Red Boners 0*PBlues C.P*Yellows CUP. Greens Yellow Toners Green P.T*A*Toser 751*S ft 756*8 753-S 758*8 75X-S rt Batches 3 4 S 3. 5 1 lT" Lbs* 578 918 310 700 070 77 M- DUP050316354 -V) ^^ ^ A SUBMITTED BY: APPROVED BY: FIGMENT COLOR RESEARCH REPORT RAW MATERIAL TESTING / ^ c- FILE: -RAW-MATEBTAPS-DATE: DECEMBER 1935* There has been no change in the status of the items K indicated as outstanding in the November report# This month 123 shipments of raw materials were received and have the following status: 58 Vested in the laboratory and found to be satisfactory; 4 satisfactory when previously tested; 13 used before test could be carried out; and 44 reported without test. Four shipments of M*N#P,T* frcm the du Pont Dyeworks proved to be unsatisfactory when tested in the laboratory on the RT-386-D formula, ^he main trouble appeared to be in the flatness of masstone produced by this material. The matter was made the subject of an Investigation and it was found that the to#N*F.T* had been running comparatively low in purity. The Dyeworks have since taken steps in an attempt to remedy this condition* Raw Material Samples Eleven samples were received this month. RMS-1473 - T*0*B, from Garclay Chem.Co* Satisfactory, RMS-1474 - R-salt C*P. 325 from Sherwin-Mllisms. Unsatisfactory, RMS-1475 - Sod* Acetate from du Pont Rayon, Unsatisfactory* RMS-1476 - Azo Bordeaux S*S. Cone* from National Aniline* Unsatisfactory, EMS-1477 RMS-1478 RMS-1479 RMS-1480 - R-Salt GP-325 ) - R-Salt GP-264 ) " *) -" ") Sherwin-Williams* Unsatisfactory* BMS-1481 EMS-14B2 Soap Treated Biane Fixe 388) i* #n 389) Grasselli /f BMS-1483 390) Unsatisfactory* DUP050316355 r t l f. I / k f ,* .'M & -2f(h 2 f;i DU P050316356