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【分享】刚把FCC里测铁粉中汞含量的方法翻译过来，喜欢的PK下【已搜无重复】
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Mercury—FCC iron powder Dithizone Stock Solution Dissolve 30 mg of dithizone in 1000 mL of chloroform, add 5 mL of alcohol, and mix. Store in a refrigerator in a dark bottle. Prepare fresh each month. 二硫腙贮备液 用1000mL氯仿溶解30mg双硫腙，加5mL酒精，混合，暗色瓶冰箱中储存，每月新制备。 Dithizone Extraction Solution On the day of use, dilute 30 mL of Dithizone Stock Solution to 100 mL with chloroform. 双硫腙提取液 在使用当天，用氯仿稀释30ml二硫腙贮备液至100ml。 Hydroxylamine Hydrochloride Solution Dissolve 20 g of hydroxylamine hydrochloride in sufficient water to make about 65 mL, transfer the solution into a separator, add a few drops of thymol blue TS, and then add ammonium hydroxide until a yellow color appears. Add 10 mL of 1:25 sodium diethyldithiocarbamate solution, mix, and allow to stand for 5 min. Extract the solution with successive 10 to 15 mL portions of chloroform until a 5-mL test portion of the chloroform extract does not develop a yellow color when shaken with a dilute cupric sulfate solution. Add 2.7 N hydrochloric acid until the extracted solution is pink, adding one or two more drops of thymol blue TS, if necessary, then dilute to 100mL with water, and mix. 盐酸羟胺溶液 用充足水溶解20g盐酸羟胺成约65ml溶液，转移溶液至separator，添加几滴麝香草酚蓝ＴＳ，然后添加氢氧化铵直至刚现黄色。添加10ml的1：25二乙基二硫代氨基甲酸钠，混合后静置5min。Add 10 mL of 1:25 sodium diethyldithiocarbamate solution, mix, and allow to stand for 5 min. Extract the solution with successive 10 to 15 mL portions of chloroform until a 5-mL test portion of the chloroform extract does not develop a yellow color when shaken with a dilute cupric sulfate solution.。添加2.7 N的盐酸直到提取液变粉红色，如需要可添加一滴至多滴麝香草酚蓝ＴＳ，然后用水稀释至100ml后混合。 Mercury Stock Solution Transfer 33.8 mg of mercuric chloride, accurately weighed, into a 100-mL volumetric flask, dissolve in 1 N hydrochloric acid, dilute to volume with the acid, and mix. Each milliliter contains the equivalent of 250 mg of mercury. 汞储存液 准确称量33.8mg的氯化汞，加到100ml容量瓶里，用1N盐酸溶解后用酸稀释定容混合。每ml含250mg Hg。 Diluted Standard Mercury Solution Transfer 2.0mL of Mercury Stock Solution into a 100-mL volumetric flask, dilute to volume with 1 N hydrochloric acid, and mix. Each milliliter contains the equivalent of 5 mg of mercury. 稀释标准汞溶液。2.0ml汞储存液加到100ml容量瓶，用1N盐酸稀释定容、混合。每ml含5mg汞。 Sodium Citrate Solution Dissolve 250 g of sodium citrate dihydrate in 1000mL of water. 柠檬酸钠溶液。 1000ml水定溶溶解250g 柠檬酸钠 Sample Solution Transfer 1 g of sample into a 250-mL beaker, add 20mL of 1:2 nitric acid, and digest on a steam bath for about 45 min. Add 5 mL of 1:3 hydrochloric acid, and continue heating on the steam bath until the sample is dissolved. Cool to room temperature, and filter, if necessary, through a medium-porosity filter paper. Wash the paper with a few milliliters of water, add 20mL of Sodium Citrate Solution and 1mL of Hydroxylamine Hydrochloride Solution to the filtrate, and adjust the pH to 1.8 with ammonium hydroxide. 样品溶液 1g样品 250ml beaker ，添加20ml 1：2的柠檬酸，蒸汽浴溶解45min。添加5ml 1：3的盐酸，继续蒸汽浴加热直至样品溶解。冷却至室温后过滤，如果需要，通过中间多孔性滤纸。用几毫升水洗滤纸后加入20ml柠檬酸钠溶液和1毫升盐酸羟胺溶液过滤，用氢氧化铵调整pH至1.8。 Procedure (Note: Because mercuric dithizonate is light sensitive, this procedure should be performed in subdued light.) Prepare a control by treating 1.0 mL of Diluted Standard Mercury Solution (5 mg Hg) in the same manner and with the same reagents as directed for the preparation of the Sample Solution. Transfer the control and the Sample Solution into separate 250-mL separators, and treat both solutions as follows: Extract with 5mL of Dithizone Extraction Solution, shaking the mixtures vigorously for 1 min. Drain carefully, collecting the chloroform in another separator. If the chloroform does not show a pronounced green color caused by excess reagent, add another 5mL of the extraction solution, shake again, and drain into the separator. Continue the extraction with 5-mL portions, if necessary, collecting each successive extract in the second separator, until the final chloroform layer contains dithizone in marked excess. Add 15mL of 1:3 hydrochloric acid, to the combined chloroform extracts, shake the mixture vigorously for 1 min, and discard the chloroform. Extract with 2mL of chloroform, drain carefully, and discard the chloroform. Add 1mL of 0.05M disodium EDTA and 2mL of 6 N acetic acid to the aqueous layer. Slowly add 5mL of 6 N ammonium hydroxide, and cool the separator. Transfer the solution into a 150-mL beaker, adjust the pH to 1.8 with 6 N ammonium hydroxide or 1:10 nitric acid, using a pH meter, and return the solution to the separator. Add 5.0 mL of Dithizone Extraction Solution, and shake vigorously for 1 min. Allow the layers to separate, insert a plug of cotton into the stem of the separator, and collect the dithizone extract in a test tube. Determine the absorbance of each solution in 1-cm cells at 490 nm with a suitable spectrophotometer, using chloroform as the blank. The absorbance of the Sample Solution does not exceed that of the control. 程序：（注：因为mercuric dithizonate是光敏感，本程序是在暗光下进行。）用1.0毫升稀释的标准汞溶液（5mg 汞）用与样品溶液相同的方式和试剂配置对照溶液。转移对照和样品溶液至250ml的separator中，按照下面方式处理两种溶液：提取5ml双硫腙提取液，摇动混匀1min。小心排水，用另一个separator收集氯仿。如果氯仿没有由于过量试剂导致的明显的绿色，添加另外5ml提取液，再振荡，排到separator中。继续用5ml比列的提取液，如果需要的话，在第二separator中收集每次过量的提取液，直到最终氯仿层明显包含过量双硫腙。添加15ml的1：3的盐酸，至混合的氯仿提取物中，振荡混合液1min，丢弃氯仿。用2ml氯仿提取，小心排，丢弃氯仿。添加1ml0.05M Na2EDTA 和2ml 6N的醋酸至水层。缓慢添加5ml 6N 氢氧化铵，后冷却separator。转移溶液至150ml的beaker，调整pH至1.8 用6N 氨水或1：10的硝酸，用pH计，然后返回溶液至separator。添加5.0ml的双硫腙提取液，摇动1min。允许层分开，塞上一团棉花之separator的颈部，用试管收集双硫腙提取液。测定每个溶液的吸光度，在490nm的条件下。用氯仿做空白。样品吸收值不应超过对照。 [ Last edited by signal023 on 2009-3-31 at 11:31 ] |
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