滴定液的标定程序SOP

标准操作程序 Standard Operating Procedure 文件编码Doc. No.: SOP/QC/GEN/009/01 颁发日期： Issue Date: 生效日期： Effective Date: 替代： SOP/QC/GEN/009/00. Supersedes: 复审日期： Review Date: 页码：第1页共12页Page No.: 1 of 12 标题：滴定液标定程序 TITLE: PROCEDURE FOR STANDARDISING THE VOLUMETRIC SOLUTIONS 1.0 目的 Purpose: 阐述了滴定液的标定程序。 To describe a procedure for the standardisation of volumetric solutions. 2.0 范围 Scope: 适用于所有相关产品的反应过程物料、原料、中间产品、成品在检验过程中所使用的滴定液。 The Procedure applies to all the volumetric solutions used in the analysis of in-process, raw materials, intermediates and API. 3.0 定义 Definitions: 无 Nil. 4.0 责任 Responsibility : 滴定液标定的责任在于级别不低于初级检验员的 实验室 17025实验室iso17025实验室认可实验室检查项目微生物实验室标识重点实验室计划 职员。 The responsibility of standardisation of volumetric solutions lies with staff, not below the rank of junior analyst. 制定和批准该标准操作程序分别是实验室主管和QA负责人的责任。 The responsibility of preparing and approving the SOP lies with Laboratory in-charge and Head of QA respectively. 5.0 程序 Procedure: 5.1 1.0mol/L 、0.5mol/L、0.1mol/L的氢氧化钠滴定液的标定 Standardization of 1.0mol/L, 0.5mol/L and 0.1mol/L Sodium Hydroxide Solutions: 5.1.1 按下 表 关于同志近三年现实表现材料材料类招标技术评分表图表与交易pdf视力表打印pdf用图表说话 pdf 所列重量两人各精密称取三份基准邻苯二甲酸氢钾（预先在105ºC干燥至恒重）置于250ml的锥形瓶中。加50ml新沸过的冷水，振摇，使其溶解。加酚酞指示液2滴，用所要标定的氢氧化钠溶液滴定至溶液显粉红色。 Weigh accurately given below mentioned quantities of (previously dried at 105ºC to constant weight) of GR potassium hydrogen phthalate. Every person in triplet into 250ml conical flask. Add 50ml of carbon dioxide free water and shake well till dissolves. Add 2 drops of phenolphthalein solution and titrate with sodium hydroxide solution to be standardized till a permanent pink colour appears. 标定氢氧化钠滴定液基准邻苯二甲酸氢钾称取重量如下： Quantities of GR potassium hydrogen phthalate to be taken: 1.0 M : 6.0 g 0.5 M : 3.0 g 0.1 M : 0.6 g 氢氧化钠滴定液实际浓度计算 公式 小学单位换算公式大全免费下载公式下载行测公式大全下载excel公式下载逻辑回归公式下载 ： Calculate the actual concentration of sodium hydroxide as per the formulae given below: 邻苯二甲酸氢钾的重量 ------------------------------------------------------- 消耗的氢氧化钠滴定液的体积X 0.2042 Weight of potassium Hydrogen phthalate --------------------------------------------------------------- Volume of sodium hydroxide consumed X0.2042 5.2 1.0mol/L 、0.5mol/L、0.1mol/L的盐酸滴定液的标定 Standardisation of 1.0 mol/L, 0.5mol/L, 0.1mol/L hydrochloric acid Solution. 5.2.1 按下表所列重量两人各精密称取三份基准无水碳酸钠（预先在270-300ºC干燥至恒重）置于250ml锥形瓶中，加水50ml使溶解。加甲基红-溴甲酚绿混合指示液10滴，用所要标定的盐酸溶液滴定至溶液由绿色转为紫红色时，煮沸2分钟，冷却至室温继续滴定至溶液由绿色转为暗紫色。 Weigh accurately the quantity of GR anhydrous sodium carbonate anhydrous given below, every person in triplet (Previously dried at about 270-300ºC to constant weight) and transfer into 250ml conical flask containing 50ml of water and shake well till dissolves. Add 10 drops of methyl red-bromocresol purple indicator solution and titrate with hydrochloric acid until the solution turns from green to fuchsia. Heat the solution to boiling, cool and continue the titration until the solution turns from green to wine color. 标定盐酸滴定液基准无水碳酸钠的称取重量如下： Quantities of GR Sodium carbonate to be taken: 1.0 mol/L : 1.5g 0.5 mol/L : 0.8g 0.1 mol/L : 0.15g 盐酸滴定液的浓度 计算公式 六西格玛计算公式下载结构力学静力计算公式下载重复性计算公式下载六西格玛计算公式下载年假计算公式 ： Calculate the actual concentration of Hydrochloric acid as per the formula given below: 无水碳酸钠的重量 ------------------------------------------------------ 消耗的盐酸滴定液的体积X 0.0530 Weight of Sodium carbonate --------------------------------------------------------------- Volume of Hydrochloric acid consumed X 0.0530 5.3 0.5mol/L、0.1mol/L的硫酸滴定液的标定 Standardisation of 0.5mol/L and 0.1mol/L Sulphuric acid Solution: 5.3.1 按下表所列重量两人各精密称取三份基准无水碳酸钠（预先在270-300ºC干燥至恒重）置于250ml锥形瓶中，加水50ml使溶解。加甲基红-溴甲酚绿混合指示液10滴，用所要标定的硫酸溶液滴定至溶液由绿色转为紫红色时，煮沸2分钟，冷却至室温继续滴定至溶液由绿色转为暗紫色。 Weigh accurately the quantity of GR anhydrous sodium carbonate anhydrous given below, every person in triplet (Previously dried at about 270-300ºC to constant weight) and transfer into 250ml conical flask containing 50ml of water and shake well till dissolves. Add 10 drops of methyl red-bromocresol purple indicator solution and titrate with Sulphuric acid until the solution turns from green to fuchsia. Heat the solution to boiling, cool and continue the titration until the solution turns from green to wine color. 标定的硫酸溶液基准无水碳酸钠的称取重量如下 Quantities of Sodium carbonate to be taken: 0.5 mol/L : 1.5g 0.1 mol/L : 0.3g 硫酸滴定液的实际浓度计算公式： Calculate the actual concentration of Sulphuric acid as per the formulae given below: 无水碳酸钠的重量 ------------------------------------------------------------- 消耗的硫酸滴定液的体积X 0.0530 Weight of Sodium carbonate, g --------------------------------------------------------------- Volume of Sulphuric acid consumed, ml X 0.0530 5.4 0.1mol/L高氯酸滴定液的标定 Standardisation of 0.1mol/L perchloric acid Solution: 5.4.1 两人各精密称取三份基准邻苯二甲酸氢钾0.16 g（预先在105ºC干燥至恒重）置于250 ml的锥形瓶中，加入20ml无水冰醋酸使溶解，加结晶紫指示液1滴。用所要标定的高氯酸溶液缓缓滴定至蓝色。并将滴定的结果用空白实验校正。 Weigh accurately 0.16g of GR grade potassium hydrogen phthalate, every person in triplet (previously dried at 120ºC for to constant weight) into 250ml of conical flask. Add 20ml anhydrous glacial acetic acid, shake to dissovled. After the solid has completely dissolved, add 1 drop of crystal violet solution, titrate with perchloric acid solution to be standardized until the violet colour changes to blue.Correct the titration result with the blank titration. 高氯酸的实际浓度计算公式： Calculate the actual concentration of perchloric acid as per the formula given below. 0.1 mol/L高氯酸的实际浓度： Actual concentration of 0.1 M perchloric acid: 邻苯二甲酸氢钾的重量 --------------------------------------------------------------- （消耗的高氯酸滴定液的体积-空白）X 0.2042 Weight of potassium hydrogen phthalate --------------------------------------------------------------------- (Volume of perchloric acid consumed-Blank) X 0.2042 5.5 0.1mol/L的硫代硫酸钠滴定液的标定 Standardization of 0.1mol/LSodium thiosulphate Solution: 5.5.1 每人各精密称取三份基准重铬酸钾0.15g（预先在120ºC干燥至恒重）置于500ml的碘量瓶中，加50ml水使其溶解，加碘化钾2.0g，轻轻振摇使溶解，加稀硫酸40ml，摇匀，密塞；暗处放置10分钟后，加水250ml稀释，用所要标定的硫代硫酸钠溶液滴定至近终点时，加淀粉指示液3ml，继续滴定至蓝色消失而显亮绿色。并将滴定的结果用空白实验校正。 Weigh accurately 0.15g of potassium dichromate (previously dried at 120oC for to constant weight), every person in triplet and transfer into 500ml iodine flask, add 50 of water to dissolve. Add 2.0g of potassium iodide, shake gently to dissovle, add 40ml diluted sulphuric acid, stoppered the flask and allow to stand in the dark for 10 minutes. Rinse the stopper and inner walls of the flask and titrate the liberated iodine with sodium thiosulphate solution until the solution is yellowish green in colour add 3ml of starch solution and continue the titration to the discharge of blue colour to bright green.Correct the titration result with the blank titration. 硫代硫酸钠的实际浓度计算公式： Calculate the actual concentration of sodium thiosulphate as per formula given below: 重铬酸钾的重量 --------------------------------------------------------------- （硫代硫酸钠滴定液的体积-空白）X 0.04903 Weight of Potassium dichromate --------------------------------------------------------------------------- (Volume of Sodium thiosulphate consumed-blank) X 0.04903 5.6 0.1mol/L硝酸银滴定液的标定 Standardization of 0.1mol/L Silver Nitrate Solution: 5.6.1 每人各精密称取三份基准氯化钠0.2g（预先在110ºC干燥至恒重）置于250 ml的锥形瓶中，加50 ml水使其溶解，加糊精溶液（1→50）5ml，碳酸钙0.1g与荧光黄指示液8滴，用硝酸银溶液滴定至浑浊液由黄绿色变为微红色。 Weigh accurately 0.2g of GR sodium chloride (Previously dried at 110ºC to constant weight) into 250ml conical flask in every person in triplet and containing 50ml water. Add 5 ml of dextrin solution (1→50), 0.1 g of calcium carbonate and 8 drops of resorcinolphthalein indicator, and titrate with silver nitrate solution till color changes from yellowish green to brown light red. 硝酸银的实际浓度计算公式： Calculate the Actual Concentration of silver nitrate as per the formula given below. 氯化钠重量 ---------------------------------------------------- 消耗的硝酸银滴定液的体积X 0.05844 Weight of Sodium chloride ---------------------------------------------------------- Volume of Silver Nitrate consumed X 0.05844 5.7 0.1mol/L碘滴定液的标定： Standardisation of 0.1mol/L Iodine: 5.7.1 每人各精密称取三份基准三氧化二砷0.15g（预先在105ºC干燥至恒重）置于250 ml的锥形瓶中，加氢氧化钠滴定液（1mol/L）10 ml，微热使溶解，加水20 ml与甲基橙指示液1滴，加硫酸滴定液（0.5mol/L）适量使黄色转变为粉红色，再加碳酸氢钠2g、水50ml与淀粉指示液2ml，用碘溶液滴定至溶液显浅蓝紫色。 Weigh accurately 0.15g of GR arsenic trioxide (Previously dried at 105ºC to constant weight) into 250ml conical flask, every person in triplet, and containing 10ml of sodium hydroxide volumetric solution (1mol/L), heat gently to dissolve. Add 20 ml of water and 1 drop of methyl orange indicator solution. Add suitable amount of sulfuric acid volumetric solution (0.5mol/L) to turn the color from yellow to pink. Add 2 g of sodium bicarbonate, 50 ml of water and 2 ml of starch indicator solution. Titrate with iodine volumetric solution to turn the color to light bluish purple. 碘溶液的实际浓度计算公式： Calculate the actual concentration of Iodine as per the formula given below: 三氧化二砷重量 ----------------------------------------------- 消耗的碘滴定液的体积X 0.09892 Weight of Arsenic Trioxide --------------------------------------------------- Volume of Iodine consumed X 0.09892 5.8 0.1mol/L亚硝酸钠的标定： Standardisation of 0.1 mol/L Sodium Nitrite: 5.8.1 每人各精密称量3份0.5g的基准对氨基苯磺酸（预先在120 oC干燥至恒重）于150ml～200ml的烧杯中，加入水30ml和浓氨试液3ml，溶解后，加盐酸（1→2）20ml，搅拌，在30 oC以下用亚硝酸钠溶液迅速滴定，滴定时将滴定管尖端插入液面下约2/3处，随滴随搅拌：至近终点时，将滴定管尖端提出液面，用少量水洗涤尖端，洗液并入溶液中，继续缓缓滴定，用永停法指示终点。 Weigh accurately 0.5g of GR p-Toluenesulfonic Acid (previously dried at 120 oC to constant weight) in triplet and transfer into a 150 ml beaker, add 30 ml of water and 3ml of ammonia solution to dissolve, and then add 20 ml of hydrochloride solution (1→2). Stir, and titrate quickly with sodium nitrite solution, keep the temperature below 30 oC. Insert the tip of the burette to about 2/3 height below the water surface, stir while titration. When approaching the end-point, lift the tip of the burette to the position above the water surface, wash the tip with small amount of water, and combine the rinsing solution into the solution. Titrate slowly; use dead-stop titration method to indicate the end-point. 亚硝酸钠的实际浓度计算公式： Calculate the actual concentration of Sodium nitrite as per the formula given below: 对氨基苯磺酸的重量 ------------------------------------------------------------ 消耗的亚硝酸钠滴定液的体积X 0.01732 Weight of Sulphanilamide -------------------------------------------------------------- Volume of Sodium nitrite consumed X 0.01732 5.9 0.01667mol/L重铬酸钾溶液的标定： Standardisation of 0.01667 mol/L Potassium dichromate: 5.9.1 不需标定 No need to be standardized. 5.10 0.1mol/L高锰酸钾滴定液的标定： Standardisation of 0.1mol/L Potassium permanganate: 5.10.1 每人各精密称取三份基准草酸钠1.0g（预先在105ºC干燥至恒重）置于250 ml的烧瓶中，加新沸过的冷水250ml与硫酸10ml，搅拌使溶解，自滴定管中迅速加入高锰酸钾滴定液约25ml（边加边振摇以免产生沉淀），待褪色后，加热至65℃，继续滴定至溶液颜色显微红色并保持30秒钟不褪，当滴定终了时溶液温度应不低于55℃。 Weigh accurately 1.0g of GR sodium oxalate (previously dried at 105 oC to constant weight) in triplet and transfer into a 250 ml beaker, add 250 ml of newly boiled water and 10 ml of sulfuric acid solution, stir to dissolve. Quickly add about 25 ml of potassium permanganate volumetric solution to the beaker from the burette, shake while adding the solution, thus avoid forming the precipitate. When the color disappears, heat to 65℃, continue with the titration to make the solution gives light red and maintain the color for 30 seconds. The temperature of the solution should be not less than 55℃ when the end-point is reached. 高锰酸钾的实际浓度计算公式： Calculate the actual concentration of potassium permanganate as per the formula given below: 草酸钠的重量 -------------------------------------------------------------- 消耗的高锰酸钾滴定液的体积X 0.335 Weight of Sodium Oxalate ------------------------------------------------------------------------ Volume of potassium permanganate consumed X 0.335 5.11 0.05mol/L乙二胺四乙酸二钠滴定液的标定： Standardisation of 0.05mol/L Disodium Edetate: 5.11.1 每人精确称取3份基准氧化锌0.12g（预先在800ºC高温炉中炽灼至恒重）置于250 ml的锥形瓶中，加稀盐酸3ml使溶解，加水25ml，加0.025%甲基红的乙醇溶液1滴，滴加氨试液至溶液显微黄色，加水25ml与氨-氯化铵缓冲液（pH10.0）10ml，再加铬黑T指示剂少量，用乙二胺四乙酸二钠滴定液（0.05mol/L）滴定至溶液由紫色变为纯蓝色。并将滴定的结果用空白实验校正。 Weigh accurately 0.12 g of GR zinc oxide (previously dried at 800ºC to constant weight)in triplet and transfer into a 250 ml beaker, add 3 ml of diluted hydrochloride acid solution to dissolve, add 25 ml of water and 1 drop of 0.025% methyl red solution in ethanol, add ammonia solution to make the solution give light yellow. Add 25 ml of water, 10 ml of ammonia-ammonium chloride buffer solution (pH10.0) ，then add small amount of eriochrome black T, titrate with disodium edetate volumetric solution (0.05mol/L) to turn the solution from purple to pure blue. Correct the titration result with the blank titration. 乙二胺四乙酸二钠的实际浓度计算公式： Calculate the actual concentration of disodium edetate as per the formula given below: 氧化锌的重量 ----------------------------------------------------------------------------- （消耗的乙二胺四乙酸二钠滴定液的体积-空白）X 0.08138 Weight of ZnO ---------------------------------------------------------------------- (Volume of disodium edetateconsumed-blank) X 0.08138 5.12 0.05mol/L锌滴定液的标定： Standardisation of 0.05mol/L Zinc: 5.12.1 每人精确量取3份锌滴定液25ml置于250 ml的锥形瓶中，加0.025%甲基红的乙醇溶液1滴，滴加氨试液至溶液显微黄色，加水25ml与氨-氯化铵缓冲液（pH10.0）10ml，再加铬黑T指示剂少量，用乙二胺四乙酸二钠滴定液（0.05mol/L）滴定至溶液由紫色变为纯蓝色。并将滴定的结果用空白实验校正。 Transfer accurately 25 ml of zinc volumetric solution in triplet into a 250 ml beaker, add 1 drop of 0.025% methyl red solution in ethanol, add ammonia solution to make the solution give light yellow. Add 25 ml of water, 10 ml of ammonia-ammonium chloride buffer solution (pH10.0) ，then add small amount of eriochrome black T, titrate with disodium edetate volumetric solution (0.05mol/L) to turn the solution from purple to pure blue. Correct the titration result with the blank titration. 锌的实际浓度计算公式： Calculate the actual concentration of ferrous ammonium Sulphate as per the formula given below: （消耗的乙二胺四乙酸二钠滴定液体积-空白）X消耗的乙二胺四乙酸二钠滴定液的浓度 ------------------------------------------------------------------------------------------------------------------- 25 (Volume of EDTA-blank) X Concentration of EDTA ----------------------------------------------------------------------- 25 5.13 0.01667mol/L溴酸钾滴定液的标定： Standardisation of 0.01667mol/L Potassium Bromate: 5.13.1 每人精确量取3份溴酸钾滴定液25ml，置于碘量瓶中，加碘化钾2.0g与 稀硫酸5ml，密塞，摇匀，暗处放置5分钟后，加水100ml稀释，用硫 代硫酸钠滴定液（0.1mol/L）滴定至近终点时，加淀粉指示液2ml，继续 滴定至蓝色消失。 Transfer accurately 25 ml of potassium bromate volumetric solution in triplet into a 250 ml iodine flask, add 2.0 g of potassium iodine and 5 ml of diluted sulfuric acid solution, stoppered, mix well and keep it in the dark for 5 minutes. Dilute the solution by adding 100 ml of water. Titrate with sodium thiosulfate volumetric solution (0.1mol/L), when approaching the end-point, add 2 ml of starch indicator solution, and continue with the titration until the blue disappears. 溴酸钾的实际浓度计算公式： Calculate the actual concentration of ferrous ammonium Sulphate as per the formula given below: 消耗的硫代硫酸钠滴定液体积X消耗的硫代硫酸钠滴定液的浓度 -------------------------------------------------------------------------------------------- 25 Volume of Sodium thiosulphate X Concentration of Sodium thiosulphate ---------------------------------------------------------------------------------------------- 25 5.14 记录Recording： 5.14.1 所有滴定液的标定记录必须由级别不低于初级检验员的职员填写。Standardisation of all the volumetric solutions shall be recorded by staff of not lower than Junior Analyst. 6.0 相关文件 Related Documents: 无 Nil. 7.0 修订记录 Revision Record : 序号 Sl. No 版本号 Revision Status 修订 内容 财务内部控制制度的内容财务内部控制制度的内容人员招聘与配置的内容项目成本控制的内容消防安全演练内容 Details of Revision 备注 Remarks ******文件终结符END OF DOCUMENT 制定人 Prepared by 审核人 Reviewed by 批准人 Approved by 签名/日期 Sign / Date 名字 Name g 职务 Designation