中英文对照版微晶纤维素质量标准.doc

题目：微晶纤维素登记号：页数：1/13制定：审核：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.Characters1.性状2.IdentificationA.B.正文A white or almost white, fine or granular powder, practically insoluble in water, in acetone, in ethanol, in toluene and in dilute acids and in a 50 g/l solution of sodium hydroxide.白色或几乎白色，细粉或粒状粉末。不溶于水，丙酮，乙醇，甲苯，稀酸和50g/l的氢氧化钠溶液。Reagent:Zinc Chloride Solution, Iodinated：Dissolve 20 g of zinc chloride and 6.5 g of potassium iodide in 10.5 ml of water . Add 0.5 g of iodine and shake for 15 minutes, filtering if necessary.Store protected from light.Method:Place about 10 mg on a watch-glass and disperse in 2 ml of iodinated zinc chloride solution R. The substance becomes violet-blue.Apparatus: capillary viscometerReagent: nitrogen;Cupriethylenediamine Hydroxide Solution ： Use a 1M solution in which the molar ratio of ethylenediamine to copper is 2.00 0.04.Method:题目：微晶纤维素审批： 年 月 日登记号：页数： 2/13标题正文Transfer 1.300 g to a 125 ml conical flask. Add 25.0 ml of water R and 25.0 ml of 1M cupriethylenediamine hydroxide solution. Immediately purge the solution with nitrogen R, insert the stopper and shake until completely dissolved. Transfer 7.0 ml of the solution to a suitable capillary viscometer (2.2.9). Equilibrate the solution at 25C 0.1C for not less than 5 min. Record the flow time t1 in seconds, between the 2 marks on the viscometer. Calculate the kinematic viscosity 1 of the solution using the formula: t1(k1) where k1 is the viscometer constant.Dilute a suitable volume of 1M cupriethylenediamine hydroxide solution with an equal volume of water R and measure the flow time t2 using a suitable capillary viscometer. Calculate the kinematic viscosity 2 of the solvent using the formula: t2(k2) where k2 is the viscometer constant.Determine the relative viscosityrel of the substance to be examined using the formula: 1/2Determine the intrinsic viscosity c by interpolation, using the Intrinsic Viscosity Table (Table 0316.-1).Calculate the degree of polymerisation P using the formula:where m is the mass in grams, of the substance to be examined and b is the loss on drying as a percentage.The degree of polymerisation is not more than 350.题目：微晶纤维素审批： 年 月 日登记号：页数： 3/13标题2.鉴别A：B：正文试剂：经碘处理的氯化锌溶液（将20g的氯化锌和6.5g的碘化钾溶解于10.5ml水中，再加0.5g的碘，振摇15min，如有必要可过滤，避光保存）；方法：取约10mg的供试品于表面玻璃中，用2ml经碘处理的氯化锌溶液，供试品变为紫蓝色。仪器:毛细管粘度计试剂: 1M铜乙二胺碱溶液（乙二胺与铜的摩尔比为2.000.04）;氮气方法:取1.300g供试品于125ml锥形瓶中，加入25.0ml水和25.0ml1M铜乙二胺碱溶液，立即通入氮气，使溶液净化，塞上塞子，振摇使完全溶解。取7.0ml此溶液用合适的毛细管粘度计检查。在不超过5min内使溶液在25C 0.1C平衡。记录粘度计两个刻度之间的流动时间t1，单位s。按下列的公式计算动力粘度1:t1(k1) k1为粘度计常数。取适量1M铜乙二胺碱溶液用等量的水稀释后，用合适的毛细管粘度计测量流动时间t2。计算溶液的动力粘度2:t2(k2) k2为粘度计常数。计算供试品的相对粘度 rel：1/2照附表4.0计算固有粘度c照下列公式计算聚合程度: m为供试品的重量，单位g。b为干燥失重的百分比。聚合程度应不大于350。题目：微晶纤维素审批： 年 月 日登记号：页数： 4/13标题3.Tests3.检查3.1 Solubility3.1.1 Apparatus3.1.2 Reagent3.1.3 Method3.1溶解度3.1.1仪器3.1.2试剂3.1.3方法正文a sintered-glass filter (BS porosity No. 3)Copper Tetrammine, Ammoniacal Solution ： Dissolve 34.5 g of copper(II) sulphate in 100 ml of water and whilst stirring, add dropwise 13.5M ammonia until the precipitateproduced has completely dissolved. Keeping the temperature below 20, add dropwise 30 ml of 10M sodium hydroxide, shaking continuously. Filter the precipitate through, wash the precipitate with water until the filtrate is clear and stir the precipitate with 200 ml of 13.5M ammonia. Filter through a sintered-glass filter and repeat the filtration to reduce the residue to a minimum.Dissolve 50 mg in 10 ml of ammoniacal solution of copper tetrammine R. It dissolves completely, leaving no residue.垂熔玻璃滤器（英国标准3号孔径）四氨铜氨水溶液（取34.5g硫酸铜用100ml水溶解，搅拌，逐滴加入13.5M的氨水至产生的沉淀完全溶解。保持温度在20度以下，逐滴加入30ml10M NaOH，不断振摇。用垂熔玻璃滤器（英国标准3号孔径）过滤沉淀物，用水洗涤，直至滤液澄清。向沉淀物加入200ml13.5M氨水，搅拌。用垂熔玻璃滤器过滤，重复过滤操作，使残渣的量为最小）；取供试品50mg，用10ml四氨铜氨水溶液溶解。全部溶解，不留残渣。题目：微晶纤维素审批： 年 月 日登记号：页数： 5/13标题3.2 pH (2.2.3)3.2.1 Apparatus3.2.2 Method3.2 pH3.2.1仪器3.2.2方法3.3 Ether-soluble substances3.3.1 Reagent3.3.2 Method正文PH meterShake 5 g with 40 ml of carbon dioxide-free water R for 20 min and centrifuge. The pH of the supernatant liquid is 5.0to 7.5.PH计参照B.P.附录（2.2.3）。取供试品5g加入40ml不含二氧化碳的水，振摇20min，离心分离。澄清液的pH值为5.0-7.5。Ether, Peroxide-free ： Shake 1000 ml of ether with 20 ml of a solution of 30 g of iron(II) sulphate in 55 ml of water and 3 ml of sulphuric acid. Continue shaking until a small sample no longer produces a blue colour when shaken with an equal volume of a 2% w/v solution of potassium iodide and 0.1 ml of starch mucilage.Starch Mucilage ： Triturate 0.5 g of starch or soluble starch with 5 ml of water and add, stirring continuously, to sufficient water to produce about 100 ml. Boil for a few minutes, cool and filter.Produces a blue colour with free iodine in the presence of a soluble iodide.It must be recently prepared.Prepare a column using 10.0 g in a tube about 20 mm in internal diameter. Pass 50 ml of peroxide-free ether R through 题目：微晶纤维素审批： 年 月 日登记号：页数： 6/13标题3.3醚溶性物质3.3.1试剂3.3.2方法3.4 Water-solublesubstances3.4 水溶性物质3.5 Starch3.5.1 Reagent正文the column. Evaporate the eluate to dryness. The residue weighs not more than 5.0 mg (0.05 per cent).不含过氧化物的乙醚：取30g硫酸亚铁用55ml水和3ml浓硫酸溶解，取1000ml乙醚加入20ml上述硫酸亚铁溶液。加入等量的2%w/v KI 溶液和0.1ml淀粉粘液，振摇，至加入少量样品不产生蓝色。淀粉粘液：取5g淀粉或可溶性淀粉加5ml水研磨，不断搅拌，加水定容至100ml。煮沸几分钟，放冷，过滤。必须新近配制。取10.0g供试品加入直径为20mm的柱中，用50ml不含过氧化物的乙醚洗脱，将洗脱液蒸发干燥。残渣重量不超过5.0mg（0.05%）。Shake 5.0 g with 80 ml of water R for 10 min. Filter with the aid of vacuum into a tared flask. Evaporate to dryness ona water-bath and dry at 100-105C for 1 h. The residue weighs not more than 12.5 mg (0.25 per cent).取5.0g供试品加入80ml水，振摇10min。抽真空，过滤到抽滤瓶中。水浴蒸发至干燥，在100-105C干燥1小时。残渣重量不超过12.5mg(0.25%)。0.05M iodine：To prepare 0.05M iodine dissolve 20 g of potassium iodide in the minimum amount of water , add 13 g of iodine, allow to dissolve and add sufficient water to produce 1000 ml. Weaker solutions should be prepared using proportionately lesser amounts of reagents or by appropriate dilution.题目：微晶纤维素审批： 年 月 日登记号：页数： 7/13标题3.5.2 Method3.5 淀粉3.5.1试剂：3.5.2方法：3.6 Heavy metals (2.4.8)3.6 重金属3.7 Loss on drying (2.2.32)3.7 干燥失重3.8 Sulphated ash (2.4.14)正文To 10 g add 90 ml of water R and boil for 5 min. Filter whilst hot. Cool and add to the filtrate 0.1 ml of 0.05M iodine.No blue colour is produced.0.05M碘试液：取20g碘化钾用最少量水溶解，加入13g碘，溶解，加水定容至1000ml。取供试品10g加入90ml水，煮沸5min。趁热过滤。放冷后向滤液中加入0.1ml0.05M I2。不产生蓝色。2.0 g complies with limit test C for heavy metals (10 ppm). Prepare the standard using 2 ml of lead standard solution (10ppm Pb) R.参照B.P.附录（2.4.8）。取2.0g参照重金属（10ppm)限量试验C。用2ml10ppm铅标准溶液为标准溶液。Not more than 6.0 per cent, determined on 1.0 g by drying in an oven at 100-105C for 3 h.参照B.P.附录（2.2.32）取1.0g在100-105C的烘箱中干燥3h，不超过6.0%。Not more than 0.1 per cent, determined on 1.0 g.题目：微晶纤维素审批： 年 月 日登记号：页数： 8/13标题3.8 炽灼残渣3.9 Microbial contamination3.9微生物污染正文参照B.P.附录（2.4.14）取1.0g检查，不超过0.1%。Total viable aerobic count (2.6.12) not more than 103 micro-organisms per gram and with a limit for fungi of 102 per gram, determined by plate-count. It complies with the tests for Escherichia coli, for Pseudomonas aeruginosa, forStaphylococcus aureus and for Salmonella (2.6.13).参照B.P.附录（2.6.12）和（2.6.13）总的需氧微生物不超过 103 微生物/克。采用平板计数法，菌类的限量为102/克。参照大肠杆菌，假单胞菌，葡球菌，沙门氏菌的试验。题目：微晶纤维素审批： 年 月 日登记号：页数： 9/13标题4.附表正文题目：微晶纤维素审批： 年 月 日登记号：页数： 10/13标题正文题目：微晶纤维素审批： 年 月 日登记号：页数：11/13标题正文题目：微晶纤维素审批： 年 月 日登记号：页数： 12/13标题正文题目：微晶纤维素审批： 年 月 日登记号：页数： 13/13标题正文