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柠檬酸的检测(Determination of citric acid)
柠檬酸的检测(Determination of citric acid)
2 the water used in the test is distilled water or ion exchange water.
2.1 differential test
2.1.1 reagents and Solutions
2.1.1.1 sulfuric acid (GB 625);
2.1.1.2 mercury sulfate: 5g Santar (HG3-1069), add 40ml of water, and then slowly add 20ml of sulfuric acid, stir, add 40ml of water and stir to dissolve;
Potassium Permanganate 2.1.1.3 (GB 643): 0.1N solution;
2.1.1.4 sodium hydroxide (GB 629): 4.3% (W/V) solution;
2.1.1.5 acetic anhydride (GB 677);
2.1.1.6 pyridine (GB 689);
2.1.1.7 sample solution: citric acid 5mg per milliliter.
2.1.2 test procedure
2.1.2.1 take a small amount of samples, with straight Huochi burning, which slowly decompose, but no odor of caramel.
2.1.2.2 take sample solution 2ml, with 4.3% sodium hydroxide solution to neutral, add 1 drops of dilute sulfuric acid, heated to boiling. Add 1 drops of 0.1N Potassium Permanganate solution, shaking, purple subsided. Add 1 drops of mercury sulfate solution to produce white precipitate.
2.1.2.3 samples 5mg, pyridine and acetic anhydride (3:1) about 5ml, which generates yellow to red or purple red solution.
2.2 content
2.2.1 reagents and Solutions
2.2.1.1 sodium hydroxide standard solution (GB 629): 1N solution, prepared and calibrated according to GB 601 standard solution preparation method;
Phenolphthalein 2.2.1.2 (HGB 3039): 1% (W/V) was prepared according to GB 603 preparation and product preparation method.
2.2.2 test procedure weigh 1.5g sample (referred to 0.0002g), adding neutral 50ml dissolved in distilled water, add 3 drops of phenolphthalein solution with 1N 1%, sodium hydroxide standard solution titration to pink end point.
2.2.3 calculation
V * C * 0.06404
X1 = - - - * 100....................................... (1)
M (1-0.08566)
V * C * 0.06404
X2 = - - - - * 100.......................................... (2)
M
Formula: X1 - citric acid content (by anhydrous),%;
X2 - anhydrous citric acid content,%;
V - the amount of standard solution of sodium hydroxide
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