Method for measuring selenium in food through combination of double cloud point extraction and hydride generation-atomic fluorescence spectroscopy
A technology of atomic fluorescence spectroscopy and hydride generation, which is applied in the directions of fluorescence/phosphorescence, food testing, material inspection, etc., can solve the problems of undetectable, solution entering, and low measurement results, and achieve good accuracy, detection precision and The effect of high enrichment factor and low detection limit
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Embodiment 1
[0046] Sample digestion:
[0047] Accurately weigh 0.5g sample into a 50ml conical flask, add 15ml HNO 3 -HClO 4 (4:1) Mix acid for wet digestion. When the solution becomes clear and colorless with white smoke, continue to heat until it is dried. After cooling, add 5mL of 6mol / L HCL, heat on an electric furnace to drive the acid to about 1mL, transfer to a 50ml centrifuge tube with stopper, and dilute with three distilled water.
[0048] Enriching selenium by double cloud point extraction operation:
[0049] Take the sample solution after the above treatment in a 50ml centrifuge tube with a stopper, add 1ml of pH 4.0 HCl-NaAc buffer solution, 1g / L APDC 1.2ml and 5% Triton X-114 solution 1.1ml, and dilute to volume with three-distilled water To 50ml, shake well, place in a constant temperature water bath at 51℃, heat for 15min, take it out and centrifuge for 10min (3500r / min) while it is hot, then cool in an ice water bath for 10min, discard the water phase, add 16%HCl+20%H 2 O 2 (...
Embodiment 2
[0053] Refer to the method in Example 1, the difference is that the pH of the HCl-NaAc buffer solution added to S22 is 1.0, the dosage is 1ml, 1g / L APDC 0.6ml and 5% (m / v) Triton X-114 solution 0.8ml , The temperature of the water bath is 40℃.
Embodiment 3
[0055] Refer to the method in Example 1, the difference is that the pH of the HCl-NaAc buffer solution added to S22 is 5.0, the amount is 3ml, 1g / L APDC 1.4ml and 5% Triton X-114 solution 1.2ml, the water bath temperature is 70℃ .
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