OVERVIEWReagentsolutionsVPACombo260624(阳极溶出伏安法试剂配方)

1、thursday, 26stjune 2013reagent solutionsthe vessels used for the preparation of the reagents must be as clean as possible, preferably made of teflon, pe or pp materials. the best is to use the vessels always for storing and preparation of the same solutions, avoiding so cross-contamination.用于制备试剂的容器

2、应该尽可能的干净，最好用聚四氟乙烯，聚乙烯或聚丙烯材料。最好同一个容器装同一个试剂，以避免交 叉感染。if used vessels are applied, clean the vessels 3 times with potable water, 3 times with 0.01m nitric acid (hno 3) and 3 times with demineralizedwater.如果容器已经使用过，最好用饮用水清洗三次，用0.01m的硝酸2清洗三次，去离子水清洗三次。the reagents used should be of highest purity regardin

3、g the content of measured species. especially great care is needed if some common elements such as zn, pb, cu, fe, mn, etc. have to be measured. most commercial reagents may contain traces of these elements and may be the reason of deteriorated measurements. hence, it is advisable to test the used r

4、eagents for purity first, the best by icp-ms or similar sensitive method. 所用的试剂应纯度最高的含量测定。 如果一些共同的元素如zn, pb, cu, fe, mn等需要非常谨慎。大多数商业试剂可能含有痕量的这些元素，并可能是影响测量的原因。因此，检测用试剂的纯度，通过 icp-ms或类似的灵敏 的方法最好。demineralized water used for preparation should not contain dissolved gases (air) and microbes, so boil the

5、water shortly and cool down to ambient temperature. this degassed demineralized water will be suitable for reagent preparation. obviously, clean vessels should beused forboiling配制试剂所用的去离子水应该不含气体或者微生物。所以煮沸的水应该冷却到室温。去除气 体的去离子水应该适用于试剂配制。显然，清洗容器也应该用煮沸的水。some reagents may contain solid particles which ma

6、y not dissolve in water. filter such solutions through a clean paper filter (rinse the filter device and filter paper with diluted nitric acid and water first).有些试剂应该含有不溶解水的固体颗粒。应该用清洁的滤纸过滤试剂(过滤装置应该用 稀硝酸和水先清洗) dust-free environment during reagent preparation ensures higher reliability regarding the p

7、urity of the reagents.在死机配制过程中无尘环境和试剂的纯度可以确保高可靠性。also refer to the word documentrecommendation - preparation reagent solutions 1.1.3）制备清洗液preparation of clean solution (0.01m hno (0.01m hno3 )ingredients 成分:water: demineralized water boiled and cooled down before use, 水：在使用前煮沸的去离子水冷却。nitric acid 65%

8、 (hno 3) gr for analysis (max. 0.005 ppm hg) (vwr/merck).65% 的优级纯 hno3 用于分析(max.0.005ppm hg ) (vwr/merk)preparation of 2 l 0.01m nitric acid制备 2l0.01m 硝酸:dissolve in 1000 ml demineralized water:-1,43 ml hno 3.1.43ml的hno3溶解在1000ml去离子水中。adjust the volume to 2 l and mix the solution.调整体积到2l并且混合溶液notes注

9、意:prepare the reagent solution in a reliable fume hood!在一个可靠的通风柜准备试剂溶液use security glasses and gloves!使用安全眼镜和手套references reagents参考试齐1jnitric acid solution 65% gr for analysis (max. 0.005 ppm hg)65% 的优级纯 hno3 用于分析(max.0.005ppm hg)msds 100452_en_eu.pdfhno3gr for analysis (max. 0.005 ppm hg), isomm 6

10、3.01 g/mol, d 1.41 g/cmvwrno. 1.00452preparation of dilution solution (0.01m hcl)制备稀释液(0.01m hcl )for preparation of calibration solutions and test solutions pb, cd, cu, fe, ni and zn. 制备校准试剂个测试 pb, cd, cu, fe, ni and zn.ingredients 成份：water: demineralized water boiled and cooled down before use,水：使

11、用前将煮沸的去离子水并且冷却hydrochloric acid 37% (hcl) gr for analysis (max. 0.001 ppm hg) (vwr/merck).37%的 hcl 用于分析(max.0.001ppm hg) (vwr/merk).preparation of 2 l 0.01m hydrochloric acid:配制2l0.01m的hcl溶液：dissolve in 1000 ml demineralized water:-1,67 ml hcl.取1.67mlhcl溶解到1000ml去离子水中adjust the volume to 2 l and mix

12、 the solution.调整体积到 2l 并且混合溶液notes:prepare the reagent solution in a reliable fume hood!在一个可靠的通风柜准备试剂溶液use security glasses and gloves使用安全眼镜和手套references reagents参考试齐1jhydrochloric acid fuming 37% gr for analysis (max. 0.001 ppm hg)msds 113386_en_eu.pdfhcl37% gr for analysis (max. 0.001 ppm hg)mm 36

13、.46 g/mol, d 1.19 g/cmvwrno. 1.13386preparation of the r-315 reagent 配制 r-315 试剂ingredients 成分:water: demineralized water boiled and cooled down before use,水：使用前将煮沸的去离子水并且冷却hydrochloric acid 37% (hcl) gr for analysis (max. 0.001 ppm hg) (vwr/merck).37%的 hcl 用于分析(max.0.001ppm hg) (vwr/merk).triton x-

14、100, gr for analysis (vwr/merck), 去拉通 x-100sodium chloride (nacl) (vwr/merck), 氯化钠(vwr/merck )preparation of 5 l reagent solution r-315: 配制 5l 试齐u溶液 r-315- add 29.3 g of nacl and 0.85 ml of concentrated hydrochloric acid ( or 10 ml of 1.0 mol/l hcl) to1 l of water in a 5 l vessel,溶解 29.3g nacl 和 0.8

15、5ml 浓盐酸(或者 10ml 1.0mol/l hcl )至 1l 水中在一个5l的容器中。- adjust the volume to 5 l with water,用水调整体积到 5l- add 1.0 ml of triton and mix the solution. 加入 1.0ml 去拉通并且混合溶液after 1-2 hours mix the solution again and now it can be used.1-2小时以后再次混合溶液并且现在可以使用了。shelflife (保质期)：1 year.1 年。references reagentshydrochlori

16、c acid fuming 37% gr for analysis (max. 0.001 ppm hg)msds 113386_en_eu.pdfhcl37% gr for analysis (max. 0.001 ppm hg)mm 36.46 g/mol, d 1.19 g/cmvwrno. 1.13386triton ? x-100c8h17c6h4(och2ch2)nohgr pro analysi ph eurd 1.07 g/cm 3cas no. 9002-93-1vwrno. 1.08643sodium chloridemsds 106404_en_eu.pdfnaclgr

17、for analysis, acs, isomm 58.44 g/mol, d 2.17 g/cm3cas no. 7647-14-5ec no. 231-598-3vwrno. 1.06404preparation of the r-336 reagent 配制 r-336 试剂ingredients 成份:water: demineralized water boiled and cooled down before use,水：使用前将煮沸的去离子水并且冷却sodium chloride (nacl) (vwr/merck), 氯化钠(vwr/merck )acetic acid, 96

18、 % (ch 3cooh) (vwr/merck), 醋酸，96% (ch3cooh) (vwr/merck),sodium acetate, trihydrate (ch 3coona . 3 h 2o) (vwr/merck),三水醋酸钠(ch3coona . 3 h 2o) (vwr/merck)nacl stock solution (5 l) 氯化钠储备液 (5l):dissolve 溶解：580 g nacl 580g 氯化钠68 g ch 3coona . 3 h 2o 68g 醋酸钠30 ml ch 3cooh30ml 醋酸in 5 l of water.在 5l 水中some

19、 reagents may content suspended solid particles not dissolving in water. filter such solutions through a clean paper filter (rinse the filter device and filter paper with diluted nitric acid and water first). 有些试剂可能含有一些不溶于水的悬浮颗粒物。通过干净的滤纸进行过滤(过滤设备和滤纸应当用 稀释的酸溶液和水进行清洗)preparation of 2 l reagent solutio

20、n r-336 配制 2lr-336 试齐u:- add 200 ml of the nacl stock solution to a 2 l vessel, 取 200ml 的氯化钠储备液在 2l 的容器中- mix the solution and adjust the volume to 2 l with water.混合溶液并且调整体积至2l加入500ml氯化钠储备液到5l的容器中 混合溶液并且用水调整至 5l。preparation of 5 l reagent solution r-336: 准备 5l 的 r-336 溶液add 500 ml of the nacl stock

21、solution to a 5 l vessel, mix the solution and adjust the volume to 5 l with water.shelf life 保质期:3 months if stored in a closed vessel at 15-25 c. if stored in the refrigerator, let the solution condition to the ambient temperature before use! 如果储存在密封的容器中并且在 15-25 c 可以 保存三个月。如果储存在冰箱中，在使用前将其至室内并且达到室

22、温。sodium chloridemsds 106404_en_eu.pdf naclgr for analysis, acs, isomm 58.44 g/mol, d 2.17 g/cm3cas no. 7647-14-5ec no. 231-598-3vwrno. 1.06404sodium acetate trihydrate msds 106267_en_eu.pdf ch3coona.3h 2o gr for analysis, acs, iso mm 136.08 g/mol, d 1.42 g/cm cas no. 6131-90-4 ec no. 204-823-8vwrno

23、. 1.06267acetic acid 96%msds 100062_en_eu.pdfc2h4o2gr for analysis d 1.05 g/cmvwrno. 1.00062preparation of the r-365 reagent 配制 r-365 试剂ingredients 成份:water: demineralized water boiled and cooled down before use, 水：使用前将煮沸的去离子水并 且冷却potassium permanganate (kmno 4), mercury-free (vwr/merck).不含 hg 的高镒酸钾

24、(vwr/merck)nitric acid 65% (hno 3) gr for analysis (max. 0.005 ppm hg) (vwr/merck).65%的优级纯硝酸用于分析(max. 0.005 ppm hg) (vwr/merck)preparation of 1 l reagent solution r-365 配制 1l 的 r-365:- dissolve 0.032 g (32 mg) of potassium permanganate in 500 ml of freshly boiled and cooled down demineralized water

25、in a 1 l vessel. 溶解 0.032g (32mg )高镒酸钾在新鲜煮沸并且冷却 的500ml去离子中在1l的容器中- add 10-11 ml of 65% nitric acid 加入 10-11ml 65% 的硝酸- adjust with water to the 1 l mark用水调整至 1l- stir the solution for 1 hour.搅拌溶液一个小时shelf life 保质期:depending on temperature: between 2-4 weeks 根绝温度：两到四周。notes注意:avoid direct sunlight to

26、 the reagent.避免试剂被阳光直射the consumption of the reagent is usually low, so it is better to store the reagent in a refrigerator and take a smaller volume to the analyzer only.试剂消耗量很低，所以最好储备试剂在冰箱中并且取一部分供分析仪使用。references reagents参考试齐1jpotassium permanganate (max. 0.000005% hg)msds 105084_en_eu.pdfkmno 4gr

27、 for analysis, max. 0.000005% hg, acsmm 158.04 g/mol, d 2.70 g/cmcas no. 7722-64-7ec no. 231-760-3vwrno. 1.05084nitric acid solution 65% gr for analysis (max. 0.005 ppm hg)msds 100452_en_eu.pdfhno3gr for analysis (max. 0.005 ppm hg), isomm 63.01 g/mol, d 1.41 g/cmvwrno. 1.00452preparation of the sta

28、ndard for as/hg/zn/cd/pb/cu in 0.01m hcl配制 as/hg/zn/cd/pb/cu 在 0.01mhcl 的标准溶液水：使用前将煮沸的去离子水并ingredients 成份：water: demineralized water boiled and cooled down before use,且冷却优级名勺37%的hydrochloric acid 37% (hcl) gr for analysis (max. 0.001 ppm hg) (vwr/merck).hcl (最大含 0.001ppm 的 hg) (vwr/merck)arsenic sta

29、ndard 1000 mg as certipur ? 1000mg 碑标液 certipur lead standard 1000 mg pb certipur ? 1000mg 铅标液 certipur mercury standard 1000 mg hg certipur ? 1000mg 汞标液 certipur copper standard 1000 mg cu certipur ? 1000mg 铜标液 certipur cadmium standard 1000 mg cd certipur ? 1000mg 镉标液 certipur zinc standard 1000 m

30、g zn certipur ? 1000mg 锌标液 certipurpreparation of 1l stock ii solution 10000g/l as/hg/znd/pb/cu配制 1l 储备液 0000 g/las/hg/zn/cd/pb/cu ：dilute accurately 1000l (1,00 ml) of each of the 1000 mg as/l standard solution with demineralized waterusing a volumetric flask of 100 ml. 用 100ml 的容量瓶精确稀释 1000 |l (1,

31、00 ml)的 1000mg/l 的标准note: always prepare a new stock ii solution when preparing a new calibration standard to ensure a good calibration standard since certain metals may precipitate on the container wall and therefore result in a lower effective concentration.注：当准备新的校准蔽时候一般都配制一般都配制一次新的stock ii溶液，这样可

32、以确保好的校准标液因为一定含量的金属可能会沉淀在容器壁上因此会导致测试值偏低。note: always use plastic volumetric flasks and containers.注：经常用塑料容量瓶和容器preparation of 1 l calibration solution 50g/l as/hg/zn/cd/pb/cu: 配制 1l 50 g/l as/hg/zn/cd/pb/cudilute accurately 5000l (5,0 ml) of the 10000 g/l a s/hg/zn/cd/pb/cu stock ii solution withdemi

33、neralized water using a volumetric flask of 1l. 用 1l 的容量瓶加入去离子水准确稀释5000 m(5,0 ml)的 10000 闻/l as/hg/zn/cd/pb/cu stock ii 的溶液add 0.83 ml of the concentrated hydrochloric acid 37% and f川 with demineralized water until the 1l mark.加入0.83ml37%的浓盐酸并且加入去离子水至1l。note: always use plastic volumetric flasks and

34、 containers.注：常用塑料的容量瓶和容器references reagentsarsenic standard 1000 mg as certipur msds 119773_en_eu.pdf1000 mg as (h 3aso4 in hno 3 0.5m) d 1.013 g/cmvwrno. 1.19773lead standard 1000 mg pb certipurmsds 119776_en_eu.pdf1000 mg/l pb (pb(no 3)2 in hno 3 0.5m) d 1.02 g/cmvwrno. 1.19776mercury standard 10

35、00 mg hg certipurmsds 170226_en_eu.pdf1000 mg/l hg (hg(no 3)2 in hno 3 2m) d 1.054 g/cm 3vwrno. 1.70226copper standard 1000 mg cu certipurmsds 119786_en_eu.pdf1000 mg cu (cu(no 3)2 in hno 3 0.5m) d 1.014 g/cm 3vwrno. 1. 19786cadmium standard 1000 mg cd certipurmsds 119777_en_eu.pdf1000 mg cd (cd(no 3)2 in hno 3 0.5m) d 1.013 g/cmvwrno. 1.19777?zinc standard 1000 mg zn certipurmsds 119806_en_eu.pdf1000 mg zn (zn(no 3)2 in hno 3 0.5m) d 1.02 g/cmvwrno. 1.19806preparation of electrolyte solution (saturated) 配制电解液(饱和的)ingredients 成份:water: d