A kind of detection method of chromium content in organic chromium
A detection method and technology of chromium content, applied in the field of detection of chromium content in organic chromium, achieves the effect of simple operation, good reproducibility and high accuracy
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Embodiment 1
[0021] 1 Reagents and solutions
[0022] 1.1 Sulfuric acid (1+1); 98% concentrated sulfuric acid and water are prepared according to the volume ratio of 1:1
[0023] 1.2 Silver nitrate aqueous solution: 10g / L;
[0024] 1.3 Ammonium persulfate;
[0025] 1.4 Diphenylcarbazide acetone solution: 5g / L;
[0026] 2.1 Chromium standard stock solution: Weigh 0.1415g of potassium dichromate baked at 105°C to constant weight, dissolve in water, transfer to a 500mL volumetric flask, and dilute to the mark. This solution contains 0.10mg of chromium per ml;
[0027] 2.2 Chromium standard solution: pipette 10ml of chromium stock solution into a 100mL volumetric flask and dilute to the mark with water. This solution contains 10μg of chromium per ml.
[0028] 3.1 Weigh 0.4000g of chromium pyridinecarboxylate raw powder (accurate to 0.0001), add it to a 150mL conical flask, add 20mL of sulfuric acid (1+1), boil on an electric stove for 2-3min, transfer to a 500mL volumetric flask after cooli...
Embodiment 2
[0037] Example 2 Determination of 9.9% chromium picolinate and 10% chromium nicotinate
[0038] 4.1 Weigh 0.4000g of the sample (accurate to 0.0001), add it to a 150mL conical flask, add 40mL of water, 20mL of sulfuric acid (1+1), boil on an electric stove for 5min, cool naturally, transfer to a 500mL volumetric flask, and constant volume, Shake well and filter. Draw 2 mL of the filtrate and add it to a 50 mL beaker. Another 50mL empty beaker was used as a blank.
[0039] 4.2 Add 2mL of sulfuric acid (1+1) to the two beakers, put it on the electric stove and cook on low heat until the sulfuric acid refluxes to 2 / 3 of the cup wall, take it off and cool, add 0.5mL of silver nitrate solution, 0.5g of ammonium persulfate, Dilute to 20mL with water, heat on a small electric stove until small bubbles emerge, then boil on high heat for 2min-3min (add water during boiling to keep the solution at 20mL), remove and cool, transfer to a 50mL volumetric flask, add 2mL Diphenylcarbazide ...
Embodiment 3
[0047] Example 3 0.1% Chromium
[0048] 5.1 Weigh 1.0000g of the sample (accurate to 0.0001), add it to a 150mL conical flask, add 40mL of water and 20mL of sulfuric acid (1+1), boil it on an electric stove for 5min, cool it down naturally, transfer it to a 100mL volumetric flask, and constant volume, Shake well and filter. Draw 2 mL of the filtrate and add it to a 50 mL beaker. Another 50mL empty beaker was used as a blank.
[0049]5.2 Add 2mL of sulfuric acid (1+1) to the two beakers, put it on the electric furnace and cook on low heat until the sulfuric acid refluxes to 2 / 3 of the cup wall, take it off and cool, add 0.5mL of silver nitrate solution, 0.5g of ammonium persulfate, Dilute to 20mL with water, heat on a small electric stove until small bubbles emerge, then boil on high heat for 2min-3min (add water during boiling to keep the solution at 20mL), remove and cool, transfer to a 50mL volumetric flask, add 2mL Diphenylcarbazide acetone solution, dilute to the scale ...
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