催化剂中银含量

1、EXHIBIT1TOANNEXB图示1附件BSILVERANALYSIS专艮分析SDANALYTICALMETHODT5分析方法-SD(Revision2)(修订2)EXTRACTABLESILVERINALUMINASUPPORTEDCATALYSTBYNITRICEXTRACTIONANDSODIUMCHLORIDETITRATION银催化剂在氧化铝支持施氮的提取和氯化钠滴定法SUMMARY概要Approximately50gramsofcatalystpelletsaredriedforonehourat150cthencooledinadesiccatortoroomtempertur

2、e.Thedriedsampleisweighedintoaflaskandrefluxedwithnitricacidsolutionwithstirring.Aftercooling,thesolutionisdilutedtoafinalweight.Analiquotistakenandanalyzedfortheextractedsliverusinganautomatictitratorequippedwithasilverindicatoreletrodeandadoubtjunctionreferenceelectrode.Standard0.1Nsodiumchlorides

3、olutionisthetitrant.大约50克的催化剂颗粒在150c干燥一个小时，然后放入干燥器内冷却至室温。干燥后的样品放入烧瓶中称重，然后在搅拌下用硝酸溶液溶解。冷却后，溶液稀释到恒重。取一等分试样，通过装有银指示电极，双盐桥参照电极的自动滴定仪进行分析。滴定剂为0.1N氯化钠标准溶液。SCOPEANDAPPLICATION范围和应用Thismethoddeterminestheamountofextractablesilverincatalystpellets.Non-extractablessuchassilverchloridearenotrecovered.Itisassume

4、dthatarepresentativesampleisinhandbeforetheanalysisisperformed.这种方法测定催化剂颗粒里可提取的银。像氯化银这种不可提取的是无法重新获得的。在进行分析之前，确保手上有具有代表性的样品。SAFETYNOTES安全注示Nitricacidanditssolutionsareverycorrosive.Alwayswearsafetyglasses,acid-proofglovesandlabcoatwhenhandling.Donotbreathesilverdust.Wearadustmaskorworkinahood.硝酸及其溶液腐

5、蚀性强。操作时戴上安全眼镜、耐酸手套和实验服。不要吸入银色尘埃，戴防尘面罩或在通风厨处操作。MODIFICATIONS修正1、 APPARATUSANDCHEMICALS仪器及试齐ij1.1 Erlenmeyerflasks,1liter,Pyrex,graduated,with24/40.锥型瓶，一L,耐热玻璃，合格的，24/40。1.28 alance,4000gcapacityreadableto0.01g,suchasANDElectronicBalanceModelFX-4000orequivalent.天平，称重4000克并精确至0.01克，如AND电子天平模型和FX-4000或相

6、似的。1.29 nalyticalbalance,weighingto0.1mg.分析天平，称重至0.1毫克。1.30 agneticstirrerbars.磁力搅拌子。1.31 raduatedcylinder,200ml.合格的圆筒，200毫升。1.32 olumetricpipet,25ml.移液管，25毫升。1.78 eaker,100ml,250ml.烧杯，100毫升，250毫升。1.79 utomatictitrator,suchasBrinkmannTitrinoModel702orequivalent,equippedwitha20mlburette.自动滴定仪，如702型滴定

7、仪或相似的，装有20毫升滴定管。1.9511 verelectrode.银电极。1.9512 ublejunctionreferenceelectrode.双盐桥参比电极。1.11Bottles,1litercapacity.容量并a,il。1.9513 ssicator.干燥器。1.9514 gneticstirrer/hotplate.磁力搅拌器/电热板。1.9515 ionizedwater.去离子水。1.9516 ncentratednitricacid,ACSgrade.浓硝酸，acs级。1.9517 diumchloride,ACSgrade.氯化钠，acs级。117Slivers

8、hot,99.99%,cat#12186,Alfa/JohnsonMatthey,P.O.Box8247,WardHill,MA1835-0747.银颗粒，99.99%1.9518 rs,withscrew-onlid,4orcap.广口瓶，带4旋帽。1.9519 yingoven.烘箱。1.9520 tercondenserwith24/40joint.水冷凝器，有24/40（关节）接合点。2、 REAGENTSANDSTANDARDS试剂J和标准2.11 1NitricAcidSolutioni：i硝酸溶液Cautiouslyadd,withstirring,avolumeofconcen

9、tratednitricacidtoanequalvolumeofdeionizedwater.Cool.Bottleandlabel.在搅拌下，小心地将一体积浓硝酸加入到等体积的去离子水中，冷却，移入容量瓶，贴上标签。2.11.1 NSodiumChlorideTitrant0.1n氯化钠滴定剂Drysodiumchloridereagentfor2hrsat110C.Storeindessicator.Dissolve5.84gofreagentin1literofdeionizedwaterinavolumetricflask.Mixthoroughly,bottleandlabel.在

10、110c下将氯化钠试剂干燥2小时，贮存在干燥器中。在容量并S中将5.84克的试剂溶解于一升去离子水，混匀，装瓶并贴上标签。3、 PROCEDURE步骤3.11 Addbetween50-51gramsofsamplepelletstoajar.将50-51g试样颗粒加入广口瓶中。3.12 Placetheopenjarintoadryingovenat150Cforonehour.将敞开的广口瓶至于150c烘箱中一个小时。3.13 Removefromoven,replacelid,andplaceinadesiccatoruntilcooledtoroomtemperature.从烘箱中移出

11、，盖上盖子，置于干燥器中冷却至室温。3.14 Tareaclean,dryPyrex1literErlenmeyerflask.Weightothenearest0.01g.Includthestopperandmagneticstirrerbar（6.1）.取一洁净干燥的1L锥形瓶，称重，精确至0.01g,包括塞子和磁力搅拌子（6.1）。3.51 ntotheflaskweight50gofdriedpelletstothenearest0.01g.称取50克（精确至0.01克）干燥试样颗粒于烧瓶中。3.52 dd200mlof1:1nitircacidfromagraduatedcylin

12、der.加入200毫升1:1硝酸。3.53 onnecttoacondenserandheattheflasktoobtainaslowboilandstiratmoderatespeeduntilnomoreyellowfumesareevolved.Continuetostirforanadditional10minutes.Cooltoroomtemperature.连接冷凝器，加热烧瓶，缓慢煮沸并以适当的速度搅拌至无黄色烟生成，继续搅拌10分钟，冷却至室温。3.54 ashdownthecondenserandtheneckoftheflaskwithsomedeionizedwate

13、r.用去离子水冲洗冷凝器和颈项。3.55 ooltoroomtemperatureanddiluteto1000g.withdeionizedwater.Dryofftheoutsideoftheflaskifnecessary.Weightothenearest0.01g.冷却到室温并用去离子水稀释到1000克。有必要则干燥烧瓶外壁。称重至0.01克。3.105 tirthisfor15minutes.搅拌15分钟。3.106 FilteraportionthroughaWhatman934-AH,12.5cmdia.glassmembranefilterintoan8oz.bottle.过

14、滤一部分（用934ah,12.5厘米直径的玻璃滤膜成一个8oz.瓶子）。3.107 singapipet,transfera25mlaliquottoatared100mlbeaker.Weightothenearest0.01g.用移液管移取25ml试样于已称重的、精确至0.01克白100ml烧杯中。3.108 ddapproximately25mlofdeionizedwatertothebeaker.力口大约25毫升去离子水于烧杯中。3.141 mmersetheelectrodesintothesamplesolution,andtitrateusingtheautomatictitr

15、ator,withstandardized0.1Nsodiumchloridesolution(4.1.6).Recordtheendpointvolume.将电极浸入到样品溶液中，采用全自动滴定仪滴定，用标准0.1N氯化钠溶液(4.1.6)。记录滴定终点的体积。3.142 nterthedataontheworksheet(T5.2-1)andcompletetheindicatedcalculations.将数据记在工作表上(T5.2-1),并完成指示的计算。4、 CALIBRATION校准4.141.1 andardizethesodiumchloridesolutionasfollow

16、s:配制标准氯化钠溶液：4.141.2 Weigh2gofsilvershot,tothenearest0.1mg,inatared1literErlenmeyerflask(See6.1).称取2克银颗粒，精确至0.1毫克，于一个已称重的1L锥型瓶(见6.1)。4.141.3 Add100ccof1:1nitric.力口入100cc的1:1硝酸。4.141.4 Followsteps3.7-3.9.(Instep3.9diluteto500g).Mixthoroughly.按照步骤3.7-3.9(在步骤3.9稀释到500克)，混合。4.141.5 Followsteps3.12and3.13

17、.参照步骤3.12和3.13。4.1.51 mmersethesilverelectrode,andthedoublejunctionreferenceelectrode.Makesurethestirrerdoesnotstriketheelectrode.浸没银电极和双盐桥参比电极，确保搅拌子不会打到电极。4.1.52 itratethesolutionwiththeautomatictitrator(seeautotitratormanualforsettings).Recordtheendpointvolume.用自动滴定仪滴定溶液(设置参考自动滴定仪手册)，记录终点的体积。4.1.5

18、3 epeatsteps4.1.1-4.1.6foratotaloftenstandardizations.重覆执行步骤4.1.1-4.1.6共计十规范化。4.1.54 alculatethenormalityofthesodiumchloridesolutionsasshownin5.1.Averagealltenresults.按图5.1计算氯化钠溶液的当量浓度，取十次结果的平均值。5、 CALCULATIONS计算5.1 Calculationoftitrantfactor:滴定剂因素的计算：N=A/BxC/(Dx0.10787)whereA=Wtgramsofsilvershot(4.

19、1.1)a=银颗粒的质量(4.1.1)B=Finalnetweightofsolution(4.1.3)b=溶液最终净重(4.1.3)C=Aliquotweighttakenfortitration(4.1.4)c=被滴定的等分试样的重量(4.1.4)D=End-pointvolume(4.1.6)d=滴定终点体积(4.1.6)5.2 Calculationofsilvercontentinaliquot:等分试样中银含量的计算：C=VxN/W=meq/gmwhereV=EndpointvolumeofNaClsolutionfrom(3.14)V=滴定终点氯化钠溶液的体积(3.14)N=NormalityofstandardizedNaClsolutionfrom(4.1.8)N=标准氯化钠溶液的浓度(4.1.8)W=Weightofsamplesolutionaliquotfrom(3.12)W=等分试样溶液的质量(3.12)5.3Calculatetheext