对含锌铝合金中氢分析的取样量、取样方法和加热释氢功率等方面进行了探索性试验,建立了脉冲加热-热导法测定铝合金中氢含量的测定方法.经过条件试验和对比试验,确定了最佳取样量为2.0~4.0 g,表面氢加热功率为850~900W,体积氢加热功率为1250~1350 W.试样9次重复测定结果的相对标准偏差小于6%.用该法对标准物质GBW( E)020030进行测定,测定结果与标准值相符合.%The sample was extracted with methanol for 15 min ultrasonicaly. After being centrifuged and filtrated with 0.45 μm film, Agilent ZORBAX Eclipse XDB - CN analytical column was employed for separation and analysis, DAD detector was used to test directly. External standard method was used for quantification. Linear relationship was found in the range of 7. 920 -79.920 mg/L for hydroquinone, 9. 696 - 96. 960 mg/L for phenol with correlation coefficient of 0. 999 99. The average recoveries ranged from 99.05% to 100.05% at addition levels of 15. 840-63.360 mg/kg for hydroquinone, 19.392-77.568 mg/kg for phenol. The relative standard deviation was less than 1% (n =5). The detection limit of hydroquinone and phenol were 0. 049, 0. 126 mg/L respectively. The method is suitable for detection of hydroquinone and phenol in whitening, spot - removal cosmetics and shampoo.
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