精确称取试样约1.5g,溶于40ml新煮沸并冷却后的水中,冷至15℃,加酚酞试液(TS-167)数滴,用1mol/L硫酸滴定。在粉红色消失时,记录所耗的酸量,加甲基橙试液(TS-148)数滴,继续滴定至呈现持续不褪的粉红色。记录滴定所需酸的总体积。每mL 1mol/L硫酸相当于总碱量(以KOH计)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).
质量指标分析:
Quality index analysis:
1.碳酸盐:在含量分析中介于酚酞和甲基橙终点之间所耗的每mL 1mol/L硫酸,相当于碳酸钾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.重金属:取试样670mg,溶于5ml水和5ml稀盐酸试液(TS-117)的混合液中。加热至沸,冷却,用水稀释至25ml,后过滤。以此作为试样液,按GT-16方法测定。用含20μg铅离子的对照液(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%试样水溶液应无色透明。
3. Water insoluble matter: 5% sample aqueous solution shall be colorless and transparent.
4.铅:取试样1g溶于5ml水和11ml稀盐酸试液的混合液中,冷却。以此作为试样液按GT-18方法测定。对照液中的铅离子量取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方法测定。标准液和试样液按如下方法制备。
5. Mercury: determined according to ct-22 method. The standard solution and sample solution are prepared as follows.
(1)标准液的制备:按GT-22制各贮液和稀释液,使所得溶液每ml中含汞1μg。取该溶液1ml,放入-50ml烧杯,加水20ml、1:4稀硫酸溶液1ml和4%高锰酸钾溶液1ml。用表面皿盖住烧杯,煮沸数秒钟后冷却,备用。
(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)试样液的制备:取试样10.0g放入-100ml烧杯,加水15ml使之溶解,加酚酞试液(TS-167)2滴,在不断搅拌下用1:1稀盐酸溶液缓慢中和。加1:稀硫酸溶液1ml和4%高锰酸钾溶液1ml,用表面皿盖住烧杯,煮沸数秒钟后冷却,备用。
(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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