Document x9x699mE2wz8pnxVqYGNLzZJ

E. i. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK, NEW JERSEY Serial Ho. Copy Ho, KK`-53~33 / % \ xo' I NEWARK PLANT PIGMENT COLOR RESEARCH REPORT * of mumcm ac id m c pc m Tm s o l u t io n s mcmmmMme 1953 Period Covered 1101-11-20 U. o HJ 4407 FILEi PATE. 223*4 I Serial Ko. KH-53-23 Copy So* / Copy tos #1 - Bumarical File 2 - Besearoh CIffioe (223*4) 3 * X&mtmm* (223Jt ) 4 - <fH. Tinker>Jcluon Lab. robea, Him. 5 - D.C. Jftller-Deval. Section, Chanber* Wks. Orchea, Wil*. * Fbyelce Lab. 7 - J. I* Tully/A. Siegel 8 - H* S. Strure/Neeark Libras? 9 J* 8. Cooper 10 * Extra 11 - Extra 12 * Extra BSttBK PLAHT c b e h ic a l nmsioa - coucms titles ^EFFECT OF CBLOHWB IV CPC OH TVS CURVE OF SULFURIC ACID Period Corered: 1953 1101-11-20 d at s mmmm 8/13/53 OATS ISSUED: DUP050069295 Copper phtbsloeyanine blue end pol^ohlor green In sulfuric add solution give characteristic curves in tits new infrared. Tfa ehlor CPC lo different from that of CPC Blue then 6$ Cl. phth1neyan<n ' pbotcewirie for the poly- of a study involving the comparative differ* of polychlor CPC mde ty different processes, the preserve of lower chlorinated species of CPC was suspected. Maes the infrared ourva of the polychlor CPC has three sdnina mixture of two or sure epeoies present. The aost likely cendidatea would be CPCe containing somewhat loss than 16 chlorine atone, e.g. dodeeaehlor, octachlor, end tetrachlor CPC's. Although a sample of the dodeea* ehlor CPC was not available, curree have been run on staples of octa- chlor, tetrachlor, and diofalor CPC's which can be compared witii those of polychlor end Cl-free CPC's. Curves were also run on polychlor metal-free PC, polychlor A1PC, end several sasg&se of *jdgmentery erode'* polychlor CPC. II. 1. the two transaission minima asaooiated with Cl-free CPC shift to progreesively higher wavelengths as ths chlorine content of the CPC is increased up to the eetaehlor. the polychlor species, however, shows three minima, the strongest of which Is at 860 *>* (Sea figure 1.) 2. lower chlorinated specie* of CPC ware not found in uncontaminated polychlor CPC. the three sdnina in the curve of a nomad polychlor CPC are found only in that species. 3. the solubility of CPC in increases. decreases as the Cl content 4* ths odor of ths SggOj,, solution of CPC changes fra* a greenish has for the Gl-free, through saber for ths octachlor, to a reddish hue for the pelychlor. 5. A sensitive method for ths separation of low chlorinated CPC from polychlor CPC was developed. It is possible to detect the presence of CPC Sine ( 6% Cl) im* sample of polychlor CPC by welling use of the widely different selridldbies in 8(2804. A smell amount of CTO Hue was found in GT-674-D SJM21, using tide method. (See figure 2.) this is undoubtedly due to cai&aBlidtien in the plant, as a sample of lab extracted crude green showed no evidence of CPC Hue. 6. Polychlor AlPC end polychlor natal-free PC were found to be oasewbat unstable in B2S0^ solution, their epeotrephotawetric curves are similar in shape to those of polychlor CPC but the minima are at slightly higher wavelengths. (See figure,^.) 7. All samples of polyehlor CPC tested gave essentially the same spsctropfaotometric curve. DUP050069296 A* fh# following samples ware used is. this study. X) Chlorine-free CPC - acid-pasted 1226-74 (AJS) 2} Mchlor CPC - aolwanfc-mllled 1425-621 (TVS) 3) Tetrachlor CPC - acid-pasted 1425-36BP (flit) 4} Ootschlor CPC - acid-pasted 1425-25P (fFB) 5) Polyohlor CPC - solvent-milled 0J-674-D SB-121 6) Polyohlor ClPC - Grehsm Green (St Lot X sad Lot 2 7) Polyohlor CPC - "Green 25" (1454-294, fPS) 8) Polyohlor CPC - Gottlieb 3X3-69B 9) Polychlor A1PC - 1348-SOC (IPS) XO) Polyohlor Metal-free PC - Qrcbem J-59 - F-122 B. Procedure for Spectronhotcmatrlc Curves k tew milligTaae of each pigment was eoapletsly dissolved in C.P* concentrated %90|l at room temperature. The concentration was adjusted by adding sufficient %% to glee a transmission curve is tbs infrared having a minimum of about 10 to 20# transmittance. Tranamission curves were run on the Beckman Model DU speotrophotometer, using %S0^ as tbs hlank, from 680 a>to 1000 *y4. Readings were taken every 10 mm except in the vicinity of a minimum idlers tlBQr were taken every 5 . In tbs csss of the polychlor A1P0 and polychlor metal-free PC, which wars not vary stable in %3% solution, fewer readings were taken* C. Two grass of pigment was placed in a clean beaker and 10 wl concentrated H2SO4 added gradually* After the mixture was thoroughly pasted, it was poured into a clean, fins porosity, atstered glass crucible end suction applied* The first few drops wars collected in a test tube and removed from tbs filter flask. Sufficient B2SO4 was to glee a speetrophotanstrlc transmission curve having a minimum of about IQ to 20# trauawittanee. If any CPC Blue ..Is present in the CPC Green it will give a tranasdsaion curve In the infrared similar to that of CPC Blue* For comparison purposes, a curve may also be run on the hulk of the sample by using the pasts in the crucible. i?. mm The following table ahows the Ibea&ion of transmission atnine of the samples studied. Sanoli SSSBBSmSSSm a-free CPC l&eliior CPC Tetraohlor CPC Octachlor CPC Poa|i#W CPC Gt-6?4-D SD-121 Polychlor CPC-Gottlieb 313.69-8 Poljohlor A3.F6 Poljollier Metal-free PC TOO* m 710, 800 780, 805 820 730, 815. 860 2 730, 810. 860 730, 820, 860 ca 720, 820; 860 ca 840, 890* <ea 820; 880* * these samples ere not rery stable in concentrated eolation, consequently, only approximate curree coold be other sasples seemed to be stable in fl^SO^ solution. V. Beferences M62-7, 8 All VI. Patent Sltaatlop Cacpetitire Patents Patent Ppoteetion On Pont jfrientaaad Applications *!I|M M10** lone* this work has been feet finding in character. DUP050069298 DUP050069299 DUP050069300 DUP050069301