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1、题目:二氧化硅登记号:页数:1/6制定: 审批:颁发部门:质量管理部 年 月 日 年 月 日 年 月 日生效日期: 年 月 日分发部门:标题1.性状2.1 Apparatus2.2 Reagent2.3 Method2.鉴别仪器试剂方法正文A light, fine, white, amorphous powder, with a particle size of about 15 nm, practically insoluble in water and in mineral acids except hydrofluoric acid. It dissolves in hot solut
2、ions of alkali hydroxides.轻质,白色,无定形细粉。粒子大小约15nm,不溶于水和矿物酸,氢氟酸除外。可溶于热碱液中。a lead or platinum crucible; a copper wiresodium fluoride; sulphuric acidAbout 20 mg gives the reaction of silicates (2.3.1).In a lead or platinum crucible mix to a thin slurry using a copper wire the prescribed quantity of the s
3、ubstance being examined with 10 mg of sodium fluoride and 0.2 ml of sulphuric acid. Cover the crucible with a thin, transparent plate of plastic from which a drop of water is suspended and warm gently. A white ring is rapidly produced around the drop of water.约20mg本品能产生硅酸盐反应铅或铂坩埚,铜线氟化钠,浓硫酸取规定量的供试品和1
4、0mgNaF,浓硫酸,置于铅或铂坩埚中,用铜线搅拌成稀浆状。在坩埚上盖一片薄的透明塑料板,加一滴水使缓慢加热。在水滴的周围立即出现白色的环。题目:二氧化硅审批: 年 月 日登记号:页数: 2/6标题3.检查 pH (2.2.3)3.1.1 Apparatus3.1.2 Method值仪器方法 Chlorides (2.4.4)3.2.1 Reagent3.2.2 Method3.2 氯化物试剂方法 3.3 Heavy metals (2.4.8)正文pH meterShake 1.0 g with 30 ml of carbon dioxide-free water R. The pH of
5、the suspension is 3.5 to 5.5.pH计参照B.P.附录()。取本品,加入30ml不含二氧化碳的水,振摇后检查混悬液的pH值为。Nitric Acid, Dilute: Dilute 20 g of nitric acid to 100 ml with water . Contains about 12.5% w/v of HNO3 (about 2M).To 1.0 g add a mixture of 20 ml of dilute nitric acid R and 30 ml of water R and heat on a water-bath for 15
6、min, shaking frequently. Dilute to 50 ml with water R if necessary, filter and cool. 10 ml of the filtrate diluted to 15 ml with water R complies with the limit test for chlorides (250 ppm). 参照附录2.4.4;稀硝酸:取20g浓硝酸用水稀释到100ml,含量为12.5%w/v,约2M取本品,加入20ml稀硝酸和30ml水的混合液,在水浴上加热15min,不断振摇。如有必要,可用水稀释到50ml,过滤后放冷
7、。取10ml滤液用水稀释到15ml,参照氯化物的限量检查(B.P.附录2.4.4) (250ppm)。题目:二氧化硅审批: 年 月 日登记号:页数: 3/6标题3.3.1 Reagent3.3.2 Method正文Hydrochloric Acid: Dilute Dilute 20 g of hydrochloric acid to 100 ml with water . It contains 7.3% w/v of HCl.Ammonia, Concentrated :M).Ammonia R2, Dilute: Dilute 14 g of concentrated ammonia t
8、o 100 ml with water . The solution contains not less than 3.3% and not more than 3.5% of NH3 (about 2M).Lead Standard Solution (1 ppm Pb) Dilute 1 volume of lead standard solution (10 ppm Pb) to 10 volumes with water immediately before use.Lead Standard Solution (10 ppm Pb) Dilute 1 volume of lead s
9、tandard solution (100 ppm Pb) to 10 volumes with water immediately before use.Lead Standard Solution (100 ppm Pb) Dilute 1 volume of lead standard solution (0.1% Pb) to 10 volumes with water immediately before use.Lead Standard Solution (0.1% Pb) Dissolve 0.400 g of lead(II) nitrate in sufficient wa
10、ter to produce 250.0 ml.1 M hydrochloric acid; ascorbic acidSuspend 2.5 g in sufficient water R to produce a semi-fluid slurry. Dry at 140C. When the dried substance is white, break up the mass with a glass rod. Add 25 ml of 1 M hydrochloric acid and boil gently for 5 min, stirring frequently with t
11、he glass rod. Centrifuge for 20 min and filter the supernatant liquid through a membrane filter. To the residue in the centrifuge tube add 3 ml of dilute hydrochloric acid R and 9 ml of water R题目:二氧化硅审批: 年 月 日登记号:页数:4/6标题重金属试剂方法正文and boil. Centrifuge for 20 min and filter the supernatant liquid thro
12、ugh the same membrane filter.Wash the residue with small quantities of water R, combine the filtrates and washings and dilute to 50 ml with water R. To 20 ml of the solution add 50 mg of ascorbic acid R and 1 ml of concentrated ammonia R. Neutralise with dilute ammonia R2. Dilute to 25 ml with water
13、 R. 12 ml of the solution complies with limit test A for heavy metals (25 ppm). Prepare the standard using lead standard solution (1 ppm Pb) R.1M盐酸,维生素C,的氨水, 稀氨水(R2):取14g浓氨水用水稀释到100ml。氨的含量为3.33.5,约2M。稀盐酸:取20g浓盐酸用水稀释到100ml,含量为7.3%w/v标准铅溶液(1ppm Pb):取10ppm Pb标准铅溶液用水稀释10倍,临用前配制。标准铅溶液(10ppm Pb):取100ppm P
14、b标准铅溶液用水稀释10倍,临用前配制。标准铅溶液(100ppm Pb):取0.1% 标准铅Pb溶液用水稀释10倍,临用前配制。标准铅溶液(0.1% Pb):取b(NO3)2,用水配成。参照B.P.附录()。取本品加入适量的水制成半流体浆。在140C下干燥。当干燥物变为白色,用玻璃棒敲碎。加入25ml1M盐酸,缓缓加热至沸腾5min,同时用玻璃棒不断搅拌。离心分离20min,用薄膜滤器过滤。在离心管中向残渣中加入3ml稀盐酸和9ml水,煮沸。题目:二氧化硅审批: 年 月 日登记号:页数: 5/6标题3.4 Loss on ignition.1 Apparatus3.4.2 Method3.4炽
15、灼失重3.4.1 仪器3.4.2 方法4. Assay4.1 Reagent4.2 Apparatus4.3 Method正文离心20min,用同一薄膜滤器过滤。用少量水冲洗残渣,合并滤液和洗液,用水稀释到50ml。向20ml此溶液中加入50mg维生素C和的氨水。用稀氨水(R2)中和。加水稀释至25ml。取12ml参照重金属(25ppm)的限量反应A(B.P.附录)。用1ppm的铅标准溶液配制标准溶液。a platinum crucibleNot more than 5.0 per cent, determined on 0.200 g by ignition in a platinum cr
16、ucible at 900C for 2 h. Allow to cool in a desiccator before weighing.铂金坩埚;称取克放入铂金坩埚中,在900C灼烧2小时,在干燥器中放冷,残渣的减少量不得超过5.0%。sulphuric acid; alcohol; hydrofluoric aciddesiccator;water bathTo the residue obtained in the test for loss on ignition add 0.2 ml of sulphuric acid R and sufficient alcohol R to m
17、oisten the residue completely. Add 6 ml of hydrofluoric acid R and evaporate to dryness on a hot-plate at 95C to 105C, taking care to avoid loss from sputtering. Wash down the sides of the dish with 6 ml of hydrofluoric acid R and evaporate to dryness. Ignite at 900C, allow to cool in a desiccator and 题目:二氧化硅审批: 年 月 日登记号:页数: 6/6标题4. 含量4.1 试剂4.2 仪器 方法正文weigh.The difference between the mass of the final residue and the mass of the residue obtained in
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