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Method improvement for determination of arsenic in vegetable oil by dry ashing-hydride generation atomic fluorescence spectrometry |
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KeyWord:vegetable oil arsenic dry ashing pretreatment improvement |
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Abstract: |
The operation details of dry ashing pretreatment of hydride generation atomic fluorescence spectrometry in the second method of GB 5009.11—2014 Food safety of national standard determination of total arsenic and inorganic arsenic in food were supplemented and clarified. The experimental parameters were optimized and the actual samples were determined. On the basis of ensuring the accuracy of the data, the effects of sample mass, dosage and adding form of magnesium nitrate, adding anti-boiling beads, carbonization process, ashing temperature and ashing time on the experiment were studied. The results showed that the optimal pretreatment conditions were obtained as follows: sample mass 4 g, adding 10 mL 400 g/L magnesium nitrate solution, adding anti-boiling beads, evaporating the water to dry at 90-110 ℃, carbonizing the sample to dry dregs at 180-250 ℃, adding magnesium oxide and heating the bottom of the sample to gray or white at 300-350 ℃, ashing temperature 540 ℃ and ashing time 8 h. The recovery rate of the improved method was 100.0%-106.0%, and the relative standard deviation was 1.88%-11.78%. The improved method could accurately determine trace arsenic in vegetable oil. |
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