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建立高压密闭消解原子荧光法测定酱油中总砷含量的方法,探讨了消解方式、赶酸方式对检测结果的影响。吸取酱油2.0 m L置于高压消解罐内罐中,加入8 m L硝酸、2 m L盐酸,室温预消解0.5h后补加高氯酸2 m L,120℃保持1 h,180℃保持0.5 h,冷却后超声赶酸脱气20min,加入预还原剂,定容至25 m L,放置30 min测试砷原子荧光强度。该方法线性相关系数r为0.9999,RSD为1.5%~2.8%(n=6),样品加标回收率为97%~99%。该法快速安全高效、试剂用量少、没有砷流失、环保卫生,满足食品检测要求。
A method for determination of total arsenic in soy sauce by high-pressure airtight digestion and atomic fluorescence spectrometry was established. The effects of digestion methods and catch-up methods on the detection results were discussed. Soy sauce 2.0 m L was placed in high-pressure digestion tank tank, add 8 m L nitric acid, 2 m L hydrochloric acid, 0.5 h pre-digestion after the addition of perchloric acid 2 m L, 120 ℃ for 1 h, 180 ℃ 0.5 h, after cooling ultrasonic degassing horsepower 20min, adding pre-reducing agent, constant volume to 25 m L, placed 30 min test fluorescence intensity of arsenic atoms. The linear correlation coefficient r of this method was 0.9999 with RSD of 1.5% -2.8% (n = 6). The spiked recoveries were 97% -99%. The method is fast, safe and efficient, with less dosage, no loss of arsenic, environmental protection and sanitation, meeting the requirements of food testing.