OVERVIEW Reagent solutions VPA Combo 260624阳极溶出伏安法试剂配方要点.docx

1、OVERVIEW Reagent solutions VPA Combo 260624阳极溶出伏安法试剂配方要点Thursday, 26st June 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

2、same solutions, avoiding so cross-contamination.用于制备试剂的容器应该尽可能的干净，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 0.01MNitric acid (HNO3) and 3 times with Demineralized water.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

3、。The reagents used should be of highest purity regarding 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

4、measurements. Hence, it is advisable to test the used reagents 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 d

5、issolved gases (air) and microbes, so boil the water shortly and cool down to ambient temperature. This degassed Demineralized water will be suitable for reagent preparation. Obviously, clean vessels should be used for boiling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。So

6、me reagents may contain solid particles which may 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 preparat

7、ion ensures higher reliability regarding the purity 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。S Also refer to the word document RECOMMENDATION - Preparation Reagent solutions 1.1.PREPARATION OF CLEAN SOLUTION (0.01M HNO3)制备清洗液（0.01M HNO3）Ingredients成分: Water: demineralized water boiled and cooled d

8、own before use, 水：在使用前煮沸的去离子水冷却。 Nitric acid 65% (HNO3) 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 HNO3. 1.43ml的HNO3溶解在1000ml去离子水中。Adjust the volume to 2

9、L and mix the solution. 调整体积到2L并且混合溶液SNotes注意: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SREFERENCES REAGENTS参考试剂 Nitric 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.pdf HNO3G

10、R for analysis (max. 0.005 ppm Hg), ISO Mm 63.01 g/mol, d 1.41 g/cm3VWR no. 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

11、 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).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

12、溶解到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SNotes: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SREFERENCES REAGENTS参考试剂 Hydrochloric acid Fuming 37% GR for analysis (max. 0.001 ppm Hg)MSDS 113386_EN_EU.pdfH

13、Cl37% GR for analysis (max. 0.001 ppm Hg) Mm 36.46 g/mol, d 1.19 g/cm3VWR no. 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

14、%的HCl用于分析（max.0.001ppm Hg）(VWR/Merk). Triton X-100, GR for analysis (VWR/Merck),去拉通 x-100 Sodium chloride (NaCl) (VWR/Merck),氯化钠（VWR/MercK）Preparation of 5 L reagent solution R-315:配制5L试剂溶液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 w

15、ater in a 5 L vessel,溶解29.3gNaCl和0.85ml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。SShelf life（保质期）: 1 year.1年。SR

16、EFERENCES REAGENTS Hydrochloric 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/cm3VWR no. 1.13386 Triton X-100C8H17C6H4(OCH2CH2)nOH GR pro analysi Ph Eurd 1.07 g/cm3CAS no. 9002-93-1VWR no. 1.08643 Sodium ch

17、lorideMSDS 106404_EN_EU.pdfNaClGR for analysis, ACS, ISOMm 58.44 g/mol, d 2.17 g/cmCAS no. 7647-14-5EC no. 231-598-3VWR no. 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

18、),氯化钠（VWR/Merck） Acetic acid, 96 % (CH3COOH) (VWR/Merck),醋酸，96%（CH3COOH）(VWR/Merck), Sodium acetate, trihydrate (CH3COONa . 3 H2O) (VWR/Merck),三水醋酸钠(CH3COONa . 3 H2O) (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 CH3COONa . 3 H2O 68g醋酸钠30 mL CH3COOH 30ml醋酸in 5 L of

19、 water.在5L水中Some 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 r

20、eagent solution R-336配制2LR-336试剂:- 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2LPreparation of 5 L reagent solution R-336:准备5L的R-336溶液- Add 500 mL of the NaCl stock solution to a 5 L vessel,加入500ml氯化

21、钠储备液到5L的容器中- Mix the solution and adjust the volume to 5 L with water.混合溶液并且用水调整至5L。SShelf 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15-25C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温。

22、Sodium chlorideMSDS 106404_EN_EU.pdfNaClGR for analysis, ACS, ISOMm 58.44 g/mol, d 2.17 g/cmCAS no. 7647-14-5EC no. 231-598-3VWR no. 1.06404 Sodium acetate trihydrate MSDS 106267_EN_EU.pdf CH3COONa.3H2OGR for analysis, ACS, ISOMm 136.08 g/mol, d 1.42 g/cm3CAS no. 6131-90-4EC no. 204-823-8VWR no. 1.0

23、6267 Acetic acid 96%MSDS 100062_EN_EU.pdfC2H4O2GR for analysis d 1.05 g/cm3VWR no. 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 (KMnO4), Mercury-free (VWR/Merck).不含Hg的高锰酸钾 (VWR/Mer

24、ck) Nitric acid 65% (HNO3) 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 in a 1 L ves

25、sel.溶解0.032g（32mg）高锰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10-11ml65% 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SShelf life保质期: depending on temperature: between 2-4 weeks根绝温度：两到四周。SNotes注意:Avoid direct sunlight to the reagent.避免试剂被阳光

26、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。SREFERENCES REAGENTS参考试剂 Potassium permanganate (max. 0.000005% Hg)MSDS 105084_EN_EU.pdfKMnO4GR for analysis, max. 0

27、.000005% Hg, ACS Mm 158.04 g/mol, d 2.70 g/cm3CAS no. 7722-64-7EC no. 231-760-3VWR no. 1.05084 Nitric acid solution 65% GR for analysis (max. 0.005 ppm Hg)MSDS 100452_EN_EU.pdfHNO3GR for analysis (max. 0.005 ppm Hg), ISO Mm 63.01 g/mol, d 1.41 g/cm3VWR no. 1.00452PREPARATION OF THE STANDARD FOR As/H

28、g/Zn/Cd/Pb/Cu in 0.01M HCl配制As/Hg/Zn/Cd/Pb/Cu 在0.01MHCl的标准溶液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 Hydrochloric acid 37% (HCl) GR for analysis (max. 0.001 ppm Hg) (VWR/Merck).优级纯的37%的HCl（最大含0.001ppm的Hg） (VWR/Merck) Arsenic standard 1000 mg As Ce

29、rtiPUR1000mg砷标液CertiPUR Lead standard 1000 mg Pb CertiPUR1000mg铅标液CertiPUR Mercury standard 1000 mg Hg CertiPUR1000mg汞标液CertiPUR Copper standard 1000 mg Cu CertiPUR1000mg铜标液CertiPUR Cadmium standard 1000 mg Cd CertiPUR1000mg镉标液CertiPUR Zinc standard 1000 mg Zn CertiPUR1000mg锌标液CertiPURPreparation of

30、 1L STOCK II solution 10000 g/L As/Hg/Zn/Cd/Pb/CU配制1L储备液0000 g/L As/Hg/Zn/Cd/Pb/CU:Dilute accurately 1000 l (1,00 ml) of each of the 1000 mg As/L standard solution with demineralized water using a volumetric flask of 100 mL.用100ml的容量瓶精确稀释1000 l (1,00 ml)的1000mg/L的标准溶液SNote: Always prepare a new STOC

31、K 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：当准备新的校准液时候一般都配制一般都配制一次新的STOCK II 溶液，这样可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。SNote: 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 50 g/L As/Hg/Zn/Cd/Pb/CU:配制1L 50 g/L As/Hg/Zn/Cd/Pb/CU校准液Dilute accurately 5000 l (5,0 ml) of the 10000 g/L As/Hg/Zn/Cd/Pb/CU STOCK II