Document 6b89rDXEzjqE6e9mEkEye0vq6

E. I. DUPONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK, NEW JERSEY Serial No. Cop/ No. KK~44~G7 / ~^^ ^7 Period Covered: NEWARK PLANT PIGMENT COLOR RESEARCH REPORT Progress Saport XKGS5 BLUE - GOAL OF K-1661 JOKE - ATJGUUf 1944* FILE: DATE: 503 H-1S~44 Njeess N37934 < 2 /3 Serial 8* KS-44-67 apy 80* / epy tel #1 * taerieal File t - mmmrn omo Cau) l - ttMur file (snj 4I *- #$1*0SrulaliieCiahgcfFflieileel ' 9 * " 7 * 8 * Uv* F* F Beley, Wil*aingiso Ltd* e * . f o - V i" RWAI& FLABS piesffl c o l o r nm bs f o r f Progress Report ltlei SR08 SL01 GOAL fllLB Of K-1661 Period Covered* <T08E - AB6US7 1944* soBumo mi APPROVES M BASE SUBRITfEDi 11-1-44 BASES ISSOIBt H-15-44 DUP050149699 fids progress report covers two series of experiments which are run to establish o goal yield for &-ld61* Further esspeiintents are planned*, particularly to determine the effect of Increased concentration. The results will be presented im a seldHWEuent report*. Two basic formulas cere used in the present study,* one wim, IA$ g. (ltHA)2SQ, per mole YPS and a digestion temperature of Ifthe the# with 143i a digestion temperature of IS* In each ease* batches foie made both withou Saphthenic Add end with three different amounts of this agent*. She goal yield figures (per mole IPS) are reported below both m m "as is" and "anhydrous" basis* She significance of the results is discussed in the succeeding section* Weight of Saphthsnie Acid 195 igestlon field ___ field___ ISO Digestion - 8* (Wr.* Yield... Yield _ 0 g* 19*95* 3*4 39*9 31A.5 g. 330*0** 333.5 342.5 300. g. 311.7** 317.5 324.0 318.5g. 330.5* 333.5 345.0 301.0 g. 313.2"* 320*5 324.5 "Standard quantity* **Average of two determinations* fhe goal yield is observed to increase in proportion to the amount of naphthenic Acid approximately 60p of the agent being retained 1 all oases, BISCOSSIOBi The following formula was used In preparing the blue* The inert atmosphere technique was followed and all reasonable pre cautions ta&en to prevent loss of pigment. The "as is" weights are probably accurate to within a few tenths of a gram* DUP050149700 I 3** S0j.7B^ 115.2 *. .8 i (or 47*2} Volume 2310 e at VGf* AM is 30 aimstee ! 8*43P# <^6*10320 160 g. (lets 1) ------- Volume 1260 ce at 909?* Stir 5 minutes M heat in 60 minutes to 195 (or ISO0 with 47*2 g (HH^SO^) | H> Bj E04 71.4 Stir for 30 minutes at 195 (or I80t)* AM Sa2Gr2Oy2H20 15*9 (in small amount of water) Stir for 15 minute# at 195 (or 180) Add Kaphthenie Acid) Cone* jSa.OH 0 ) See below for plan of experiments and quantities used for this sis batch* Stir for 45 minute# at 195 (or ISO). Shut off agitation (Sote 2) and let stand overnight* Filter and wash with 20 liters water <ea. 150F*y* toy at U0F* Sote 1) Ferrous sulfate adjusted with hydrogen peroxide and sulfuric acid to 13 Fe*4"* (Ratio ?++/** a 0*01) and pH 2*0. Sote 2) An atmosphere of nitrogen is maintained up to this point* DUP050149701 She two gammed as follow#i soma* 1U5-XA Be s s wfr 8 8 180P 4#.@ * 8 4?. 2 0*0 g 10*08 0n 3m t Sot# 1 2 83 UX5-30 1 8 48*8 8*8 10*05 HA 8 (cheek on IB) i 8 (check o& 11) Bote 1 - Equivalent to 19*95 g Bapfcthentc Acid war mole XPS 2. J3O0^.4i. V 8 8 39.9 fixe products were compared (fey tight roller mill grinds) with K-1061, tentative standard lot 7303a for color and likewise with the standard quantity, 8.0 grams, of naphthenic acid (ca. 20 grams/ sol SPB) hut the samples with 10.05 grams were only a few percent weaker* % Omitting naphthenic add gave an increase la strength (10 vs IB, 30 vs 38) of about 10$. Xt is not likely that the strength advantage of the untreated products would be so pronounced under testing conditions involving less severe grinding. 0e attempt has been made In fable X to show the comparative strength of the various samples using 1115*11 as an arbitrary standard of comparison* Be quantitative adjustments were made but the estimated figures are reasonably dose to the truth* She samples are arranged for convenience in order of naphthenic add content* 4 high figure indicates higher strength,1 i.e., 10 is about 10$ stronger than IS* Xt will be noted that the temperature variable (with adjusted ammonium sulphate) has very little effect on color* She 180 digestion gave a trace darker masstone and possibly 2-3* increase in strength over that obtained by digesting the pigment at 195 She chief uncertainty involved in any goal yield figures for iron blues arises from possible errors due to variations in composi tion* . Shis has been given considerable study in the past but no simple and entirely satisfactory procedure has been developed* (Xn this connection, reference should be made to the following reports! KB-39-144, 39-230, 42-93 - files 213). DUP050149702 t . in the ease of'**afcr oeuteab* of bt pigment* no relly\ reliable method is available. 9b# toluene distillation mwhjicfchA\ls noeoOt raesaiedoielyllyfeupsereddbauetlbilet laand at boat Ismsibreieseubltsto fairly well tewa errors. In tbrproses* mir particularly puaaliag results ware obtained with samples treated with the larger quantifies of mpktfamte Mil* A much simple method. &eit the operating ^Sat of view ito oaf the Irabtmdor apparatus* There la no gaol: correlation m this and other methods (#* toluene distillation) sal the ft'M&ed vary considerably with the conditions used, " and time of heating haring c<s*aiderable effect*' While 90s e fairly good degree of precision and it was tb#re; ed to use the irabsader reeolts in reducing the ob- served to a comparable basis* She loss in weight Iron iron blues on heating (160c) in rapidly at first and wore slowly after 2-3 hours. Iren after 7 or 0 Mors samples continue to lose weight! It seems probable that this is due in part at least to actual decomposition of the pigment, in examination of the results indi cated that the best agreement between duplicate determinations was obtained using the figures obtained 'after 30 minutes heating end these are the values shesafor *per eent water* la fable X* fhe 3 hour figuros are about'O.TJS higher end would give correspondingly lower fteshydrous yield* figures, fhe choice between them in the litt of our present knowledge Is entirely arbitrary* In fact. It is possible that the *as Is" figures may be more useful and they have consequently been reported also* They represent the lump weights obtained after drying for several days at 110f and weighing the samples as rapidly as possible. It can be concluded that an increase in yield is obtained from the Saphthenle Mid approximately equal to 60J6 of the weight of the agent used. A slight Increase in yield is also obtained by lowering the dlgestion-b^firature from 175* to 180. The naphthenic Acid treated blues are weaker than untreated controls* using large amounts results in a further loss of strength. Details of the work are recorded in Sotebook 1115# Bxpt. 1115-1 & 3. / DU P050149703 a a gg s i i 1 ***M *o *a *c m &'S SSS3^S t-WSO'OHtO-* O' Of* O' O' O' O' O' sssuss 4 v! 4 4 4 ft 4 CM 1 i fir- fr- i O r* 33 rl e M* H CM I ** <> as I + 1 & O' S55j ft c> w> ^ w *0 s( 1 * >ft H -) O O' 'i 7 I I | | 8 I S H H H H H r-f r>l |hI HI H H * * +0o & VO* M> UO\ ot asssasa 3 8 <HHft*f # a &9 a DUP050149704