REACTIONS OF OXIDATION DYE INTERMEDIATES 867 Standard Curves ß ß ß ß ß ß •. * I I I I 21o 250 X (m•) ß ß *** ***, ß ß ß : ß ß ß : : ß ß ß ß ß ß t• ** ß ß I I i i 300 Figure 4. Quinonediimine and resoreinol in ether. QDI, , (265 mu), 24,000. ... Resorcinol, , (275 mu), 19,600
368 JOURNAL OF THE SOCIETY OF COSMETIC CHEMISTS Table 'm' OXIDATION DYES, AMMONI^ EVOLUTION % of Theoretical Reactants* Average ñ St. Dev. No. Expts. PPD 0.26 2 No H202 BB 0.97 2 m-Aminophenol 0.47 + 0.39 5 PPD 4.92 + 1.49 8 PPD: Resorcinol 4:1 0.97 + 0.66 11 PPD: Resorcinol 1:1 0.40 + 0.80 4 With H=O= PPD: Resorcinol 1: 4 0.26 + 0.14 4 PPD: m-Aminophenol 1:1.3 2,33 + 0.80 11 PPD: Resorcinol: m-Aminophenol 1:1:1 2.92 + 1,O1 10 ß 1 g. PPD in 100 mi. 1% Na2CO3 which may be 3% in H202, pH 9.6, I hr. A predetermined amount of QDI was weighed immediately after preparation into a 250-ml Erlenmeyer flask. A preweighed amount of a second component, as desired, was added. An appropriate amount of pH 9.6 (0.05 _/F/Na2COoPborax) buffer was added and quickly mixed to effect solution. Addition of the buffer was considered zero time of the reaction. Aliquots (5-ml) of this reaction mixture were taken as quickly as possible and added to separatory funnels containing 25 ml of anhydrous ether. Extractions were performed, and the ether layers were decanted into 100-ml volumetric flasks and brought to the mark with ether elapsed time was one to three minutes. The ultraviolet spectra of these solutions were examined for the presence of quinonedi- imine (Fig. 5). In the run in which only QDI was mixed with the buf- fer, 0.0251 g QDI was weighed into the reaction and 0.0064 g was found after 3 minutes, a 25% recovery. Oxidation Pigment Preparation of Pigment For preparing a large quantity of oxidation pigment from PPD and resorcinol (1: 1), the following procedure was used:
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