OVERVIEW Reagent solutions VPA Combo 260624阳极溶出伏安法试剂配方.docx
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OVERVIEWReagentsolutionsVPACombo260624阳极溶出伏安法试剂配方
Thursday,26stJune2013
REAGENTSOLUTIONS
Thevesselsusedforthepreparationofthereagentsmustbeascleanaspossible,preferablymadeofTeflon,PEorPPmaterials.Thebestistousethevesselsalwaysforstoringandpreparationofthesamesolutions,avoidingsocross-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。
Ifusedvesselsareapplied,cleanthevessels3timeswithPotablewater,3timeswith0.01M
Nitricacid(HNO3)and3timeswithDemineralizedwater.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。
Thereagentsusedshouldbeofhighestpurityregardingthecontentofmeasuredspecies.EspeciallygreatcareisneededifsomecommonelementssuchasZn,Pb,Cu,Fe,Mn,etc.havetobemeasured.Mostcommercialreagentsmaycontaintracesoftheseelementsandmaybethereasonofdeterioratedmeasurements.Hence,itisadvisabletotesttheusedreagentsforpurityfirst,thebestbyICP-MSorsimilarsensitivemethod.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。
Demineralizedwaterusedforpreparationshouldnotcontaindissolvedgases(air)andmicrobes,soboilthewatershortlyandcooldowntoambienttemperature.ThisdegassedDemineralizedwaterwillbesuitableforreagentpreparation.Obviously,cleanvesselsshouldbeusedforboiling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。
Somereagentsmaycontainsolidparticleswhichmaynotdissolveinwater.Filtersuchsolutionsthroughacleanpaperfilter(rinsethefilterdeviceandfilterpaperwithdilutedNitricacidandwaterfirst).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-freeenvironmentduringreagentpreparationensureshigherreliabilityregardingthepurityofthereagents.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。
SAlsorefertotheworddocument‘RECOMMENDATION-PreparationReagentsolutions1.1’.
PREPARATIONOFCLEANSOLUTION(0.01MHNO3)制备清洗液
(0.01MHNO3)
Ingredients成分:
Water:
demineralizedwaterboiledandcooleddownbeforeuse,
水:
在使用前煮沸的去离子水冷却。
Nitricacid65%(HNO3)GRforanalysis(max.0.005ppmHg)(VWR/Merck).
65%的优级纯HNO3用于分析(max.0.005ppmHg)(VWR/Merk)
Preparationof2L0.01MNitricacid制备2L0.01M硝酸:
Dissolvein1000mLdemineralizedwater:
-1,43mLHNO3.
1.43ml的HNO3溶解在1000ml去离子水中。
Adjustthevolumeto2Landmixthesolution.
调整体积到2L并且混合溶液
SNotes注意:
Preparethereagentsolutioninareliablefumehood!
在一个可靠的通风柜准备试剂溶液
Usesecurityglassesandgloves!
使用安全眼镜和手套
SREFERENCESREAGENTS参考试剂
Nitricacidsolution65%GRforanalysis(max.0.005ppmHg)65%的优级纯HNO3用于分析(max.0.005ppmHg)
MSDS100452_EN_EU.pdf
HNO3
GRforanalysis(max.0.005ppmHg),ISOMm63.01g/mol,d1.41g/cm3
VWRno.1.00452
PREPARATIONOFDILUTIONSOLUTION(0.01MHCl)制备稀释液(0.01MHCl)
ForpreparationofCalibrationsolutionsandTestSolutionsPb,Cd,Cu,Fe,NiandZn.
制备校准试剂个测试Pb,Cd,Cu,Fe,NiandZn.
Ingredients成份:
Water:
demineralizedwaterboiledandcooleddownbeforeuse,
水:
使用前将煮沸的去离子水并且冷却
Hydrochloricacid37%(HCl)GRforanalysis(max.0.001ppmHg)(VWR/Merck).
37%的HCl用于分析(max.0.001ppmHg)(VWR/Merk).
Preparationof2L0.01MHydrochloricacid:
配制2L0.01M的HCl溶液:
Dissolvein1000mLdemineralizedwater:
-1,67mLHCl.取1.67mlHCl溶解到1000ml去离子水中
Adjustthevolumeto2Landmixthesolution.调整体积到2L并且混合溶液
SNotes:
Preparethereagentsolutioninareliablefumehood!
在一个可靠的通风柜准备试剂溶液
Usesecurityglassesandgloves!
使用安全眼镜和手套
SREFERENCESREAGENTS参考试剂
HydrochloricacidFuming37%GRforanalysis(max.0.001ppmHg)
MSDS113386_EN_EU.pdf
HCl
37%GRforanalysis(max.0.001ppmHg)Mm36.46g/mol,d1.19g/cm3
VWRno.1.13386
PREPARATIONOFTHER-315REAGENT配制R-315试剂
Ingredients成分:
Water:
demineralizedwaterboiledandcooleddownbeforeuse,
水:
使用前将煮沸的去离子水并且冷却
Hydrochloricacid37%(HCl)GRforanalysis(max.0.001ppmHg)(VWR/Merck).
37%的HCl用于分析(max.0.001ppmHg)(VWR/Merk).
TritonX-100,GRforanalysis(VWR/Merck),去拉通x-100
Sodiumchloride(NaCl)(VWR/Merck),氯化钠(VWR/MercK)
Preparationof5LreagentsolutionR-315:
配制5L试剂溶液R-315
-Add29.3gofNaCland0.85mLofconcentratedhydrochloricacid(or10mLof1.0mol/LHCl)to
1Lofwaterina5Lvessel,溶解29.3gNaCl和0.85ml浓盐酸(或者10ml1.0mol/LHCl)至1L水中在一个5L的容器中。
-Adjustthevolumeto5Lwithwater,用水调整体积到5L
-Add1.0mLofTritonandmixthesolution.加入1.0ml去拉通并且混合溶液
After1-2hoursmixthesolutionagainandnowitcanbeused.1-2小时以后再次混合溶液并且现在可以使用了。
SShelflife(保质期):
1year.1年。
SREFERENCESREAGENTS
HydrochloricacidFuming37%GRforanalysis(max.0.001ppmHg)
MSDS113386_EN_EU.pdf
HCl
37%GRforanalysis(max.0.001ppmHg)Mm36.46g/mol,d1.19g/cm3
VWRno.1.13386
Triton®X-100
C8H17C6H4(OCH2CH2)nOHGRproanalysiPhEur
d1.07g/cm3
CASno.9002-93-1
VWRno.1.08643
Sodiumchloride
MSDS106404_EN_EU.pdf
NaCl
GRforanalysis,ACS,ISO
Mm58.44g/mol,d2.17g/cm³
CASno.7647-14-5
ECno.231-598-3
VWRno.1.06404
PREPARATIONOFTHER-336REAGENT配制R-336试剂
Ingredients成份:
Water:
demineralizedwaterboiledandcooleddownbeforeuse,
水:
使用前将煮沸的去离子水并且冷却
Sodiumchloride(NaCl)(VWR/Merck),氯化钠(VWR/Merck)
Aceticacid,96%(CH3COOH)(VWR/Merck),醋酸,96%(CH3COOH)(VWR/Merck),
Sodiumacetate,trihydrate(CH3COONa.3H2O)(VWR/Merck),三水醋酸钠(CH3COONa.3H2O)(VWR/Merck)
NaClstocksolution(5L)氯化钠储备液(5L):
Dissolve溶解:
580gNaCl580g氯化钠
68gCH3COONa.3H2O68g醋酸钠
30mLCH3COOH30ml醋酸
in5Lofwater.在5L水中
Somereagentsmaycontentsuspendedsolidparticlesnotdissolvinginwater.Filtersuchsolutionsthroughacleanpaperfilter(rinsethefilterdeviceandfilterpaperwithdilutednitricacidandwaterfirst).
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)
Preparationof2LreagentsolutionR-336配制2LR-336试剂:
-Add200mLoftheNaClstocksolutiontoa2Lvessel,取200ml的氯化钠储备液在2L的容器中
-Mixthesolutionandadjustthevolumeto2Lwithwater.混合溶液并且调整体积至2L
Preparationof5LreagentsolutionR-336:
准备5L的R-336溶液
-Add500mLoftheNaClstocksolutiontoa5Lvessel,加入500ml氯化钠储备液到5L的容器中
-Mixthesolutionandadjustthevolumeto5Lwithwater.混合溶液并且用水调整至5L。
SShelflife保质期:
3monthsifstoredinaclosedvesselat15-25°C.Ifstoredintherefrigerator,letthesolutionconditiontotheambienttemperaturebeforeuse!
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温。
Sodiumchloride
MSDS106404_EN_EU.pdf
NaCl
GRforanalysis,ACS,ISO
Mm58.44g/mol,d2.17g/cm³
CASno.7647-14-5
ECno.231-598-3
VWRno.1.06404
SodiumacetatetrihydrateMSDS106267_EN_EU.pdfCH3COONa.3H2O
GRforanalysis,ACS,ISO
Mm136.08g/mol,d1.42g/cm3
CASno.6131-90-4
ECno.204-823-8
VWRno.1.06267
Aceticacid96%
MSDS100062_EN_EU.pdf
C2H4O2
GRforanalysisd1.05g/cm3
VWRno.1.00062
PREPARATIONOFTHER-365REAGENT配制R-365试剂
Ingredients成份:
Water:
demineralizedwaterboiledandcooleddownbeforeuse,水:
使用前将煮沸的去离子水并且冷却
Potassiumpermanganate(KMnO4),Mercury-free(VWR/Merck).不含Hg的高锰酸钾(VWR/Merck)
Nitricacid65%(HNO3)GRforanalysis(max.0.005ppmHg)(VWR/Merck).65%的优级纯硝酸用于分析(max.0.005ppmHg)(VWR/Merck)
Preparationof1LreagentsolutionR-365配制1L的R-365:
-Dissolve0.032g(32mg)ofpotassiumpermanganatein500mLoffreshlyboiledandcooleddowndemineralizedwaterina1Lvessel.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
-Add10-11mLof65%nitricacid加入10-11ml65%的硝酸
-Adjustwithwatertothe1Lmark用水调整至1L
-Stirthesolutionfor1hour.搅拌溶液一个小时
SShelflife保质期:
dependingontemperature:
between2-4weeks根绝温度:
两到四周。
SNotes注意:
Avoiddirectsunlighttothereagent.避免试剂被阳光直射
Theconsumptionofthereagentisusuallylow,soitisbettertostorethereagentinarefrigeratorandtakeasmallervolumetotheanalyzeronly.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。
SREFERENCESREAGENTS参考试剂
Potassiumpermanganate(max.0.000005%Hg)
MSDS105084_EN_EU.pdf
KMnO4
GRforanalysis,max.0.000005%Hg,ACSMm158.04g/mol,d2.70g/cm3
CASno.7722-64-7
ECno.231-760-3
VWRno.1.05084
Nitricacidsolution65%GRforanalysis(max.0.005ppmHg)
MSDS100452_EN_EU.pdf
HNO3
GRforanalysis(max.0.005ppmHg),ISOMm63.01g/mol,d1.41g/cm3
VWRno.1.00452
PREPARATIONOFTHESTANDARDFORAs/Hg/Zn/Cd/Pb/Cuin0.01MHCl
配制As/Hg/Zn/Cd/Pb/Cu在0.01MHCl的标准溶液
Ingredients成份:
Water:
demineralizedwaterboiledandcooleddownbeforeuse,水:
使用前将煮沸的去离子水并且冷却
Hydrochloricacid37%(HCl)GRforanalysis(max.0.001ppmHg)(VWR/Merck).优级纯的37%的HCl(最大含0.001ppm的Hg)(VWR/Merck)
Arsenicstandard1000mgAsCertiPUR®1000mg砷标液CertiPUR
Leadstandard1000mgPbCertiPUR®1000mg铅标液CertiPUR
Mercurystandard1000mgHgCertiPUR®1000mg汞标液CertiPUR
Copperstandard1000mgCuCertiPUR®1000mg铜标液CertiPUR
Cadmiumstandard1000mgCdCertiPUR®1000mg镉标液CertiPUR
Zincstandard1000mgZnCertiPUR®1000mg锌标液CertiPUR
Preparationof1LSTOCKIIsolution10000µg/LAs/Hg/Zn/Cd/Pb/CU配制1L储备液0000µg/LAs/Hg/Zn/Cd/Pb/CU:
Diluteaccurately1000µl(1,00ml)ofeachofthe1000mgAs/Lstandardsolutionwithdemineralizedwaterusingavolumetricflaskof100mL.用100ml的容量瓶精确稀释1000µl(1,00ml)的1000mg/L的标准溶液
SNote:
AlwaysprepareanewSTOCKIIsolutionwhenpreparinganewcalibrationstandardtoensureagoodcalibrationstandardsincecertainmetalsmayprecipitateonthecontainerwallandthereforeresultinalowereffectiveconcentration.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STOCKII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:
Alwaysuseplasticvolumetricflasksandcontainers.注:
经常用塑料容量瓶和容器
Preparationof1LCALIBRATIONsolution50µg/LAs/Hg/Zn/Cd/Pb/CU:
配制1L50µg/LAs/Hg/Zn/Cd/Pb/CU校准液
Diluteaccurately5000µl(5,0ml)ofthe10000µg/LAs/Hg/Zn/Cd