Method for detecting total selenium content
A content, sodium selenite technology, applied in the direction of material analysis by observing the influence of chemical indicators, and analysis by chemical reaction of materials, etc., can solve problems such as errors and complex preparation of standard samples, and achieve difficult measurement. Error, accurate measurement results, simple preparation effect
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Embodiment 1
[0040] The glassware used in the laboratory was soaked in (1+1) HCl for more than 4 hours, rinsed with distilled water, and then dried in an oven for use.
[0041] Put 0ml (no selenium salt, use toluene as a contrast), 2ml, 4ml, 6ml, 8ml and 10ml of selenium standard working solution in a separatory funnel, add 1ml of EDTA-2Na, adjust to neutral with 5% NaOH, Add dropwise 2mol / L formic acid to adjust the pH to 2, add water to 35ml, then add 5ml of 0.5% 3,3-diaminobenzidine (DAB) each, shake well, react in the dark for 30min, and the reaction forms a stable Se-DAB complex, then use 5% NaOH to adjust the pH to 8, add 10ml of toluene, shake and extract for 1min, after standing and layering, take the toluene layer, and measure its pH value at 420nm in the system complex Absorbance value, taking toluene as blank, the results are shown in Table 1, and a standard curve is made simultaneously (see figure 1 ), get the R of the curve 2 =0.9912>0.99, obviously this curve can be used as...
Embodiment 2
[0046]Put 0ml (without adding selenium salt, use toluene as a contrast), 1.2ml, 2.4ml, 3.6ml, 4.8ml and 6ml of selenium standard working solution in a separatory funnel, add 1ml of EDTA-2Na, adjust with 5% NaOH To neutrality, add 90% formic acid dropwise, adjust the pH to 2, add water to 35ml, then add 3ml of 0.5% 3,3-diaminobenzidine (DAB), shake well, react in dark for 30min, react Form a stable Se-DAB complex, then use 5% NaOH to adjust the pH to 8, add 10ml of toluene, shake and extract for 1min, after standing and layering, take the toluene layer, and measure its presence in the system complex The absorbance value at 420nm is blank with toluene, the results are shown in Table 1, and the standard curve is made simultaneously (see figure 2 ), get the R of the curve 2 =0.9909>0.99, obviously this curve can be used as the determination of selenium content, and proves that this method is practical simultaneously.
[0047] figure 2 Colorimetric results at a wavelength of 4...
Embodiment 3
[0051] Preparation of digestive solution: Weigh 10g of sodium molybdate, add 150ml of deionized water to dissolve, slowly add 150ml of concentrated sulfuric acid, cool to room temperature, and add 200ml of perchloric acid.
[0052] ①: Weigh 0.1g of the yeast selenium sample (dried) and place it in a flask, add 5ml of digestion solution, connect the condensing device, condense and reflux on the electric furnace to digest until colorless, transfer the digested sample into a 200ml beaker, and use a small amount of Rinse the flask with water, and transfer the rinsing solution into a beaker and set the volume to 50.
[0053] ②: Take 10ml of digestive juice, add deionized water to 40, add 5ml of 5% EDTA-2Na, add 2ml of 5% DAB, shake well, and adjust to neutral with 5% NaOH. Add 4ml of toluene, and make a blank solution in the same way.
[0054] ③: After standing and stratifying, put the water phase in the pear-shaped funnel into the beaker, and then pour out the toluene phase from ...
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