精確稱取試樣約1.5g，溶于40ml新煮沸并冷卻后的水中，冷15℃，加酚酞試液(TS-167)數(shù)滴，用1mol/L硫酸滴定。在粉紅色消失時，記錄所耗的酸量，加甲基橙試液(TS-148)數(shù)滴，繼續(xù)滴定呈現(xiàn)持續(xù)不褪的粉紅色。記錄滴定所需酸的總體積。每mL 1mol/L硫酸相當(dāng)于總堿量(以KOH計)56.11mg。
Accurately weigh about 1.5g of sample, dissolve in 40ml of newly boiled and cooled water, cool to 15 ℃, add several drops of phenolphthalein test solution (ts-167), and titrate with 1mol / L sulfuric acid. When pink disappears, record the amount of acid consumed, add several drops of methyl orange test solution (ts-148) and continue titration until it shows a continuous pink. Record the total volume of acid required for titration. 1mol / L sulfuric acid per ml is equivalent to 56.11mg of total alkali (calculated by KOH).
質(zhì)量指標(biāo)分析：
Quality index analysis:
1．碳酸鹽：在含量分析中介于酚酞和甲基橙終點之間所耗的每mL 1mol/L硫酸，相當(dāng)于碳酸鉀138.2mg。
1. Carbonate: 1mol / L sulfuric acid consumed between the end points of phenolphthalein and methyl orange in content analysis, equivalent to 138.2mg of potassium carbonate.
2．重金屬：取試樣670mg，溶于5ml水和5ml稀鹽酸試液(TS-117)的混合液中。加熱沸，冷卻，用水稀釋25ml，后過濾。以此作為試樣液，按GT-16方法測定。用含20μg鉛離子的對照液(溶液A)。
2. Heavy metals: take 670mg of sample and dissolve it in the mixture of 5ml water and 5ml dilute hydrochloric acid test solution (ts-117). Heat to boiling, cool, dilute with water to 25ml, and then filter. Take this as the sample solution and determine it according to gt-16 method. With 20 μ G reference solution of lead ion (solution a).
3．水不溶物：5%試樣水溶液應(yīng)無色透明。
3. Water insoluble matter: 5% sample aqueous solution shall be colorless and transparent.
4．鉛：取試樣1g溶于5ml水和11ml稀鹽酸試液的混合液中，冷卻。以此作為試樣液按GT-18方法測定。對照液中的鉛離子量取10μg。
4. Lead: take 1g of sample, dissolve it in the mixture of 5ml water and 11ml dilute hydrochloric acid test solution, and cool it. Take this as the sample solution and measure it according to GT-18 method. The amount of lead ion in the control solution is 10 μ g。
5．汞：按CT-22方法測定。標(biāo)準(zhǔn)液和試樣液按如下方法制備。
5. Mercury: determined according to ct-22 method. The standard solution and sample solution are prepared as follows.
(1)標(biāo)準(zhǔn)液的制備：按GT-22制各貯液和稀釋液，使所得溶液每ml中含汞1μg。取該溶液1ml，放入－50ml燒杯，加水20ml、1:4稀硫酸溶液1ml和4%高錳酸鉀溶液1ml。用表面皿蓋住燒杯，煮沸數(shù)秒鐘后冷卻，備用。
(1) Preparation of standard solution: prepare each storage solution and diluent according to gt-22, so that the resulting solution contains 1% mercury per ml μ g。 Take 1ml of the solution, put it into a - 50ml beaker, add 20ml of water, 1ml of 1:4 dilute sulfuric acid solution and 1ml of 4% potassium permanganate solution. Cover the beaker with a watch glass, boil for a few seconds, cool and set aside.
(2)試樣液的制備：取試樣10.0g放入－100ml燒杯，加水15ml使之溶解，加酚酞試液(TS-167)2滴，在不斷攪拌下用1:1稀鹽酸溶液緩慢中和。加1:稀硫酸溶液1ml和4%高錳酸鉀溶液1ml，用表面皿蓋住燒杯，煮沸數(shù)秒鐘后冷卻，備用。
(2) Preparation of sample solution: put 10.0g of sample into - 100ml beaker, add 15ml of water to dissolve it, add 2 drops of phenolphthalein test solution (ts-167), and slowly neutralize it with 1:1 dilute hydrochloric acid solution under continuous stirring. Add 1ml of 1: dilute sulfuric acid solution and 1ml of 4% potassium permanganate solution, cover the beaker with a watch glass, boil for a few seconds, cool and set aside.
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