Determination of diphenylamine stabilizer and its nitrated derivatives in smokeless gunpowder using a tandem MS method
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Abstract:
A novel method for determination of diphenylamine (DPA) and its nitrated derivatives, which are considered as characteristic components in smokeless powder and gunshot residues, is described. A tandem mass spectrometric method is established and mass spectrometer parameters optimized for each compound to obtain higher sensitivity. Under optimum conditions, quantitative analysis was carried out. The linear ranges are 5.0–200.0, 2.0–200.0 and 5.0–250.0 ng ml−1 and the detection limits are 1.0, 0.5 and 2.5 ng ml−1 for diphenylamine (DPA), N-NO-diphenylamine (N-NO-DPA) and 4-NO2-diphenylamine (4-NO2-DPA), respectively. Intra-assay and inter-assay precision and accuracy of analysis of these three samples were investigated. Based on the regression lines obtained above, smokeless samples were analyzed. It was found that there are 0.952% DPA, 0.384% N-NO-DPA and 0.128% 4-NO2-DPA in smokeless powder. Recovery tests showed that using cotton swabs, 80.3 ± 4.9% DPA, 79.6 ± 3.1% N-NO-DPA and 83.1 ± 5.4% 4-NO2-DPA could be recovered from human hands.Keywords:
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Tandem
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Abstract α‐Farnesene was oxidised to conjugated trienes with an absorbance maximum at 269 nm and the oxidation was inhibited by diphenylamine both in hexane solution and in the natural coating of stored apples. The results suggest that superficial scald is caused by the oxidation of α‐farnesene and that the control of scald by diphenylamine is due to its antioxidant action. The mechanism of scald induction is discussed.
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Hexane
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Abstract A separatory funnel procedure is presented that separates diphenylamine (DPA) from Ext. D&C Yellow No. 1. The DPA is extracted from the color with isooctane and the amount of DPA is determined spectrophotometrically. Recoveries of 0.02–1 % added DPA ranged from 95.5 to 104%.
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Colorimetry
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Current sitation at home and abroad,production methods and uses of diphenylamine were described.It was suggested that continuous condensation of aniline be used,plant for production of diphenylamine be constructed as soon as possible to meet the increasing need of diphenylamine.
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Summary Dips of diphenylamine 1,000 p.p.m. in aqueous alcoholic solution controlled superficial scald on 11 varieties of apples, but not on Statesman. A similar formulation applied as a spray to fruit in cases was equally successful, but some damage occurred to the bottom fruit where drainage was incomplete. Paper wraps containing DPA completely controlled scald in Granny Smith apples. Oiled wraps did not give adequate control of scald in immature, early pieked fruit. Phenothiazine 1,000 and 2,000 p.p.m. did not control scald and caused damage to some varieties. Several other unsuccessful materials are noted. Diphenylamine does not aggravate other storage disorders, and there is some evidence that it may reduce both internal breakdown and core flush.
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