HGT3696.3-2002无机化工产品化学分析用制剂及制品的制备.pdf 18页

'ICS71.060.01;71.060.99G10备案号:10941-10943-2002HG中华人民共和国化工行业标准HG/T3696.1一3696.3-2002无机化工产品化学分析用标准滴定溶液、杂质标准溶液和制剂及制品的制备2002一09一28发布2003一06一01实施中华少又民共和国国家经济贸易委员会It 备案号:10943-2002HG/T3696.3-2002目次前言·············，·······，·········································································，·················⋯⋯431范围···········，，·················，·····，，················，··················，·····································⋯⋯452引用标准·..............................................................................................................453一般规定·························································，···············································⋯⋯454制备方法·..............................................................................................................454.1制剂············································································································⋯⋯454.2制品··········································.......................................................................474.3试剂溶液·····································································································⋯⋯474.4缓冲溶液······································································································⋯⋯524.5指示剂及指示液····························································································⋯⋯53附录A(提示的附录)汉语拼音索引·····················，·，·········，，········，··················，·········⋯⋯56 备案号:10943-2002HG/T3696.3-2002前言本标准是非等效采用美国材料试验协会标准ASTME200-1997《化学分析用标准溶液和试剂溶液的配制、标定和贮存》中试剂溶液的配制的有关内容，并根据国内无机化工产品分析的需要而制定的。本标准与ASTME200-1997相比有如下差异。—制剂增设了九项;—增设了制品;—试剂溶液中增设了五十项;—缓冲溶液中增设了十项;—指示剂及指示液中增设了二十九项。—将所列制剂及制品分为5类:制剂、制品、试剂溶液、缓冲溶液、指示剂及指示液，并分别说明制备过程。本标准的附录A是提示的附录。本标准由原国家石油和化学工业局政策法规司提出。本标准由全国化学标准化技术委员会无机化工分会技术归口。本标准起草单位:天津化工研究设计院。本标准主要起草人:王彦。本标准为首次发布。本标准委托全国化学标准化技术委员会无机化工分技术委员会负责解释。 中华人民共和国化工行业标准无机化工产品HG/T3696.3-2002化学分析用制剂及制品的制备InorganicchemicalproductsPreparationsofreagentsolutionsforchemicalanalysis范围本标准规定了无机化工产品的试验方法中所用制剂、制品、试剂溶液、缓冲溶液、指示剂及指示液的制备方法。本标准适用于无机化工产品试验方法中所需制剂及制品的制备，也可供其他化工产品标准选用2引用标准下列标准所包含的条文，通过在本标准中引用而构成为本标准的条文。本标准出版时，所示版本均为有效。所有标准都会被修订，使用本标准的各方应探讨使用下列标准最新版本的可能性。(;B/T6682-1992分析实验室用水规格和实验方法(eqvISO3696:1987)G脚丁9733---1988化学试剂碳基化合物测定通用方法3一般规定3.1本标准中所用的水，在没有注明其他要求时，应符合GB/T6682中三级水规格。3.2本标准中所用试剂的纯度应在分析纯以上。3.3"V,+V”符号是指体积为V,的特定溶液被加人到体积为V:的溶剂中。3.4如果浓度以单位质量和体积表示，则浓度表示为克每升(9月一)。3.5当溶液出现混蚀、沉淀、颜色变化或超过规定限时应重新制备。3.6除另有说明外，本标准中的溶液均指水溶液，稀释是指用水冲稀。3.7本标准中所用未加说明的乙醇为体积分数为95%的乙醇(市售)4制备方法4.1制剂4.1.1无二氧化碳的水将水注人烧瓶中，煮沸10min，立即用装有钠石灰管的胶塞塞紧，放置冷却。使用期为一周4.1.2无氧的水将水注人烧瓶中，煮沸1h后立即用装有玻璃导管的胶塞塞紧，导管与盛有100g/I焦性没食子酸碱性溶液的洗瓶连接，冷却。使用期为两天。4.1.3无氨的水取2份强碱性阴离子交换树脂及1份强酸性阳离子交换树脂，依次填充于直径3cm、长50cm的交换柱中，将水以3^-5m工/min的流速通过交换柱。使用期为一周中华人民共和国国家经济贸易委员会2002-09-28批准2003-06-01实施 HG/T3696.3一20024.1.4无氨的氢氧化钠浴液将所需浓度的氢氧化钠溶液注人烧瓶中，煮沸30min，用装有体积分数为20%的硫酸溶液的安全漏斗(环颈双球)的胶塞塞紧(如图1)，冷却，用无氨的水稀释至原体积。1一氢氧化钠:z一安全漏=1-(环须双球)图14.1.5无碳酸盐的氨水取500ml氨水，注人1000m工圆底烧瓶中，加人预先消化10.0g生石灰所得的石灰浆，混匀，将烧瓶与冷凝器连接(如图2)，放置18-20h。将钠石灰管(2)摘下，再将氨气出口(3)用橡皮管与另一装有约200ml无二氧化碳的水的烧瓶进口(5)连接，外部用冰冷却。将氨水和石灰浆的混合液用水浴加热，将氨蒸出直至制得的氨水密度达。.9g/m工左右。1--氨水及石灰;2-钠石灰管;3-氨气出口;4钠石灰管;5-烧瓶进口;6一无二氧化碳水;7一冰浴图24.1.6饱和二氧化硫溶液将二氧化硫气体在常温15^-25℃下通人水中，至饱和为止。使用前制备4.1.7饱和硫化氢水将硫化氢气体通人无二氧化碳的水中，至饱和为止。使用前配制。4.1.8王水将1体积的硝酸缓缓注人3体积的盐酸中，混合均匀，使用时配制。4.1.9无拨基的甲醇量取2000m工_甲醇，注人2500ml蒸馏瓶中，加10.0g2,4一二硝基苯脐和0.5m工盐酸，在水浴卜回流2h，加热蒸馏，弃去最初的50ml蒸馏液，收集馏出液贮存于棕色具塞瓶中。 HG/T3696.3一2002按以上方法制备的无拨基的甲醇，按GB/T9733的规定测定，碳基含量不得大于。.001%,4.1.10无醛的乙醇量取2000ml乙醇，注人2500ml蒸馏瓶中，加10.0g2,4一二硝基苯麟和0.5m工盐酸，在水浴上回流2h，加热蒸馏，弃去最初的50ml蒸馏液，收集馏出液贮存于棕色具塞瓶中。取5m工按上述方法制备的无醛的乙醇，加5mL水，冷却至200C，加2mL品红一亚硫酸溶液，放置10min，应无明显红色。4.2制品4.2.1乙酸铅棉花取脱脂棉花，用50g/I乙酸铅[Pb(CH,COO)z"3H,O口溶液湿透后，除去过多的溶液，晾干，保存于密闭的瓶中。4.2.2无钙镁的氯化钠将一体积的优级纯氯化钠的饱和溶液与一体积的无水乙醇混合，不断搅拌至不再出结晶，抽滤，于105一110V烘干，备用4.2.3淀粉一碘化钾试纸于100ml新配制的10g/I淀粉溶液中，加。.20g碘化钾，将无灰滤纸放人该溶液中浸透，取出于暗处晾千。保存于密闭的棕色瓶中。4.2.4澳化汞试纸称取1.25g澳化汞，溶于25ml,乙醇中，将无灰滤纸放人该溶液中浸泡1h，取出于暗处晾干，保存于密闭的棕色瓶中。4.3试剂溶液4.3.1乙二胺四乙酸二钠一镁溶液[c(EDTA-Mg)二。.01mol/I习取25ml,乙二胺四乙酸二钠溶液[c(EDTA)}0.02mol/l」与25ml氯化镁[c(Mgclz)}0.02mot/I,]混合均匀后，加10ml氨一氯化钱缓冲溶液甲(pH=10)和少量铬黑丁指示剂，用乙二胺四乙酸二钠溶液仁c(EDTA)-^=0.02mol/I〕或氯化镁[c(MgCh)}0.02mol/l]调节至溶液恰呈纯蓝色或紫色。4.3.2乙酸溶液乙酸溶液(质量分数为5%):48m工，冰乙酸与961ml水混匀。乙酸溶液(质量分数为3000):量取298m工冰乙酸与731m工水混匀。4.3.3乙二醛缩双邻氨基酚乙醇溶液(2g/I-)称取0.20g乙二醛缩双邻氨基酚(钙试剂)，溶于乙醇，用乙醇稀释至100m工_。4.3.4乙酸铅(碱)溶液称取5.0g乙酸铅「Pb(CH,COO),"3H,O〕和15.0g氢氧化钠，溶于80ml水中，稀释至100m14.3.5二乙基二硫代氨基甲酸钠溶液(1g/L)称取0.10g二乙基二硫代氨基甲酸钠(铜试剂)，溶于水，稀释至100mL。使用期为一个月4.3.6二乙基二硫代氨基甲酸银一毗陡溶液称取。.5g二乙基二硫代氨基甲酸银，溶于100m工J毗吮。此溶液贮存于棕色瓶中，放在阴凉处，一周内有效4.3.7二乙基二硫代氨基甲酸银一三乙基胺三氯甲烷溶液称取0.25g二乙基二硫代氨基甲酸银，用少量三氯甲烷溶解，加人1.8g三乙基胺，用三氯甲烷稀释至100m工。静置过夜，过滤，贮存于密闭的棕色瓶中。放在阴凉处，一周内有效。4.3.8二甲基乙二醛厉氢氧化钠溶液(10g/1.)称取1.0g二甲基乙二醛肪(镍试剂)，溶于50g/工_氢氧化钠溶液中，用50g/1氢氧化钠溶液稀释至100m1。47 HG/T3696.3一20024.3.94,7一二苯基一1,10一菲罗琳溶液{c[(C,Hs),C,H,N,]=0.001mol/L}称取。.0332g4,7一二苯基一1,10一菲罗琳溶液，溶于乙醇，用乙醇稀释至100mLe4.3.10孔雀石绿溶液(2g/L)称取0.20g孔雀石绿，溶于水，稀释至100m工。4.3.”双硫赊三氯甲烷(或四氯化碳)溶液(0.01g/I.)称取。.0010g双硫踪，溶于三氯甲烷(或四氯化碳)中，用三氯甲烷(或四氯化碳)稀释至100m工贮存于棕色玻璃瓶中。使用期为两周4.3.12达旦黄溶液(0.5g/I)称取。.050g达旦黄，溶于水，稀释至100m工J。4.3.13纳氏试剂称取145.0g氢氧化钠，溶于700m工水中，冷却称取50.0g碘化汞和40.0g碘化钾，溶于200ml水中。将此溶液倾人上述氢氧化钠溶液中，稀释至1000m工，静置，取上层清液使用。按以上方法制备的纳氏试剂应符合下述要求:取0.005mg氨(N)杂质标准溶液，稀释至100mL,加2ml纳氏试剂，其颜色应深于空白颜色。4.3.14玫红三梭酸按溶液(0.5g/L)称取0.25g玫红三按酸钱(铝试剂)和5.0g阿拉伯胶，加250m工水，温热至溶解，加87.0g乙酸钱，溶解后，加质量分数为15%盐酸溶液145m工，稀释至500ml。必要时过滤，使用期为一个月。4.3.15苯基邻氨基苯甲酸一乙醇溶液(1g/l.)称取。.10g苯基邻氨基苯甲酸，溶于乙醇，用乙醇稀释至100ML.4.3.16苯甲酞苯基经胺溶液(20g/L)称取2.0g苯甲酸苯基经胺(担试剂)，溶于乙醇，用乙醇稀释至100ML.4.3.17苯基荧光酮溶液(0.1g/L)称取。.010g苯基荧光酮(苯荀酮)，溶于适量温热的乙醇中，加质量分数为20%盐酸溶液1ml，用乙醇稀释至100m工J4.3.18氢氧化钾一乙醇溶液称取30g氢氧化钾，溶于30m工水中，用无醛的乙醇稀释至1000ml-。放置24h，取清液使用。4.3.19氢氧化钾一甲醇溶液将330g/L氢氧化钾溶液15.0ml与50mI无拨基的甲醇溶液混合。使用期为两周4.3.20氨水溶液氨水溶液(质量分数为2.500):量取103m工一氨水与898m工水混匀。氨水溶液(质量分数为10%):量取400ml氨水与601ml_水混匀。4.3.21盐酸溶液盐酸溶液(质量分数为50o):量取117m工盐酸与895m工水混匀。盐酸溶液(质量分数为1000):量取240mI,盐酸与776mL水混匀。盐酸溶液(质量分数为15%):量取370mL盐酸与651m工水混匀。盐酸溶液(质量分数为20%):量取504mL盐酸与516m工水混匀。4.3.22盐酸苯阱溶液(10g/l)称取1g盐酸苯阱，溶于水，稀释至100ml。使用前制备。4.3.23铁一亚铁混合液称取10.0g硫酸亚铁钱[(NH,),Fe(S0))4)I·6H,0]和1.0g硫酸铁钱[NH4Fe(S04),·12H20],溶于水，加质量分数为20%硫酸溶液5mI，稀释至100ml。4.3.24淀粉一碘化锌溶液 HG/T3696.3一2002溶液工:称取2.0g可溶性淀粉与20m工J水混合，注人200ml沸水中，加10.0g氯化锌，溶解。溶液H:称取0.50g金属锌粉和1.0g碘，加10mL水，搅拌至黄色消失，过滤。将滤液煮沸，冷却。将溶液H注人冷却后的溶液I中，混匀，稀释至500mL.贮存于棕色瓶中，使用期为一周。量取1mL按以上方法制备的淀粉一碘化锌溶液，加50ml水、1+5硫酸溶液3m工，混匀，溶液应不得呈现蓝色。溶液中加1滴碘酸钾溶液仁c(1/6KIO,)一。.01mol/L],混匀，应立即产生蓝色。4.3.25混合碱将2体积的100g/工氢氧化钠溶液与1体积的100g/L无水碳酸钠溶液混合均匀。4.3.261,1o-菲罗琳(邻菲罗琳)溶液1,10一菲罗琳溶液(2g/L)称取。.20g1,10-菲v琳(C12H,N·H20)C或1,10一菲罗琳盐酸盐(C,2HeN2·HC1·H,O)]，加少量水振摇至溶解(必要时加热)，稀释至100mL1,10一菲罗琳溶液(5g/L):称取0.50g1,10一菲罗琳(C12H,N,·H2O)或[1110-菲罗琳盐酸盐(C12HeN2·HCl"H,0)],溶于pH-3的乙酸一乙酸钠缓冲溶液中，用pH}3的乙酸一乙酸钠缓冲溶液，稀释至100ML.4.3.27铬天青S混合液溶液工:称取。.50g十六烷基三甲基嗅化钱，溶于水，稀释至100ml-溶液I:称取。.040g铬天青S，加5m工乙醇溶解，稀释至100m工。量取10mL溶液工及50m工J溶液I,稀释至100m工。4.3.28铬酸溶液(100g/L)称取100.0g三氧化铬，溶于质量分数为35%硫酸溶液中，用质量分数为35%硫酸溶液稀释至1000mLo4.3.29偏钒酸钱溶液(2.5g/l)称取2.5g偏钒酸铰，溶于500mL沸水中，加20mL硝酸，冷却，稀释至1000mL贮存于聚乙烯瓶中4.3.30氯化亚锡溶液氯化亚锡盐酸溶液(4g/1,):称取。.4g氯化亚锡(SnC12"2H,0)，置于干燥的烧杯中，溶于50ML盐酸，稀释至100ml。使用期为2周。氯化亚锡盐酸溶液(20g/L):称取2.0氯化亚锡(SnC12"2H,0)，置于于燥的烧杯中，用少量盐酸溶解(必要时加热)，用盐酸稀释至100mL。使用期为两周氯化亚锡溶液(5g/lJ:称取。.50g氯化亚锡(SnClz"2H}0)，置于于燥的烧杯中，溶于1m工盐酸(必要时加热)，稀释至100mL。使用期为两周。氯化亚锡一抗坏血酸溶液称取。.50g氯化亚锡(SnC12"2H,0),置于干燥的烧杯中，溶于8m工盐酸，稀释至50m工，加。.7g抗坏血酸，摇匀。使用时配制。氯化亚锡溶液(400g/L):称取40.0g氯化亚锡(SnC12"2H,0)，置于干燥的烧杯中，溶于40mI,盐酸，稀释至100MI.。使用期为两周。4.3.31三氯化铁溶液(100g/I)称取10.0g三氯化铁(FeCl·6H20)，溶于1+9盐酸溶液中，用1+9盐酸溶液稀释至100m工J。4.3.32硝酸溶液硝酸溶液(质量分数为1300):量取150MI硝酸与863mL水混匀。硝酸溶液(质量分数为2000):量取240m工_硝酸与780mL水混匀。硝酸溶液(质量分数为25%);量取308mL硝酸与715ml水棍匀.4.3.33硝酸银溶液(17g/I)称取1.70g硝酸银，溶于水，稀释至100ml贮存于棕色试剂瓶中，避光保存49 HG/T3696.3一20024.3.34硫化馁溶液量取100m工无二氧化碳的氨水，通人硫化氢气体至溶液变为黄色。4.3.35硫酸溶液硫酸溶液(质量分数为。.5%):量取2.8mL硫酸，缓慢注人978mL水中，冷却，混匀硫酸溶液(质量分数为5%):量取29mL硫酸，缓慢注人966ml水中，冷却，混匀硫酸溶液(质量分数为20%):量取128mL硫酸，缓慢注人889mL水中，冷却，混匀。硫酸溶液(质量分数为40%):量取294ml硫酸，缓缓注入752m工，水中，冷却，棍匀。4.3.36硫酸铜溶液(20g/I)称取2g硫酸铜(CUS04·5H,O),溶于水，加两滴硫酸，稀释至100mL,4.3.37硫酸亚铁溶液(50g/L)称取5.0g硫铁亚铁(FeS04·7H,O),溶于适量水中，加10mL硫酸，稀释至100m工_。4.3.38硫酸亚铁按溶液(100g/I)称取10.0g硫酸亚铁钱[(NH,)2Fe(SO4)i"6H20],溶于适量水中，加10ml硫酸，稀释至100ml-4.3.39硫酸锰混合液称取67.0g硫酸锰(MnSO4"H,O),溶于500ml水中，加138mI.磷酸及130ml.硫酸，稀释至1000ml。4.3.40硫酸银溶液(10g/I)称取1.0g硫酸银，溶于质量分数为40%硫酸溶液50ml_中，稀释至100mL,4.3.41硫酸钾乙醇溶液取。.020g硫酸钾，溶于体积分数为30%乙醇溶液中，用体积分数为30%乙醇稀释至100ml。4.3.42紫脉酸铰溶液(0.5g/I)称取0.050g紫脉酸按，溶于水，稀释至100m工。此溶液使用前制备。4.3.43嗅溶液[c(1/2Br,)=0.1mol/L]4.3.43.1配制称取25.0g嗅化钾，溶于150mL水，加1.2一1.3ml,(4g)澳，稀释至500ml，贮存于塑料瓶中。4.3.43.2标定移取25.00ml上述溶液，注人250m工碘量瓶中，加2.0g碘经钾及30m工水，待碘化钾溶解后，于暗处放置5min，用硫代硫酸钠标准滴定溶液[c(Na,S,03)=0.1mol/L」滴定，近终点时，加10g/L淀粉指示液3ml，继续滴定至溶液蓝色消失澳溶液的浓度按式(I)计算:c(1/2Br,)=VV,c,(1)式中:c(1/2Br,)嗅溶液的浓度，mol/I;V—滴定到终点时消耗硫代硫酸钠标准滴定溶液的体积，ml;c—硫代硫酸钠标准滴定溶液的浓度，mol/L;V—标定所量取嗅溶液的体积，ml。4.3.44碱性品红一亚硫酸溶液称取。.20g碱性品红，溶于120mL热水中，冷却，加20ml亚硫酸钠溶液「或2.0g亚硫酸钠(Na2SO,"7H,(川，加20ml一水溶解，加2ml盐酸，稀释至200ml，放置1h按以上方法制备的碱性品红一亚硫酸溶液应符合下述要求:取。.005mg醛杂质标准溶液，稀释至20ml，加2m工碱性品红一亚硫酸溶液，摇匀，在1520℃放置10min,所呈红色应深于空白颜色。5O HG/T3696.3一20024.3.45碳酸钱溶液称取200.0g碳酸馁，溶于水，加80mL氨水，稀释至1000mL.4.3.46靛蓝二磺酸钠溶液[c(c,H8N2Na2OaS,)=0.001mol/I]4.3.46.1配制称取mg[由式(3)计算所得]靛蓝二磺酸钠(靛蓝胭脂红)，加1+5硫酸溶液2ml-溶解，稀释至1000mL。使用期为10天。4.3.46.2标定称取0.20g预先在105℃干燥至恒重的靛蓝二磺酸钠(精确至。.0002g),溶于30m工水，加1mL硫酸，稀释至600mL，用高锰酸钾标准滴定溶液〔c(1/5KMnO,)=0.1mol/L」滴定至溶液由绿色变为淡黄色。靛蓝二磺酸钠含量按式(2)计算:VcX0.1166.，__u=—入IUU(2)刀I式中:W-靛蓝二磺酸钠的质量分数，%;v—滴定到终点时消耗高锰酸钾标准滴定溶液的体积，m工;c—高锰酸钾标准滴定溶液的浓度，mol/L;M-靛蓝二磺酸钠质量，9;0.1166—与1.00mL高锰酸钾标准溶液[c(1/5KMnO,)=1.000mol/L]相当的以克表示的靛蓝二磺酸钠的质量。制备靛蓝二磺酸钠溶液[(C,HaN,NazO.S)=0.001mol/L]所需靛蓝二磺酸钠质量按式(3)计算:m_0.46旦4.⋯，，.，..⋯⋯，...........⋯⋯，.，....⋯⋯(3)式中:M-靛蓝二磺酸钠质量，9;二—靛蓝二磺酸钠质量分数，%;0.4664—配制1000mL靛蓝二磺酸钠溶液[c(CsHsN2Na,OgS)=0.001mol/L]所需靛蓝二磺酸钠的质量，9。4.3.47磷试剂甲称取5.0g钥酸馁[(NH,)6M0,02,·4H20],溶于水，稀释至100mL.4.3.48磷试剂乙称取。.20g对甲氨基苯酚硫酸盐，溶于100mL水中，加20.0g偏重亚硫酸钠，溶解，贮存于棕色具塞瓶中，使用期为两周。4.3.49磷酸二氢钠溶液(200g/L)称取20.0g磷酸二氢钠(NaH2PO,·2H}0)，溶于水，加200o硫酸溶液1ml，稀释至100mL.4.3.50哇锢柠酮溶液溶液1:称取70g钥酸钠，溶于150ml_水中。溶液2:称取60g柠檬酸，溶于150ml水和85ml硝酸的混合液中。溶液3:边搅拌边将溶液1缓慢加人溶液2中。溶液4:在35ml硝酸和100ml水的棍合液中加人5ml喳琳。溶液5:将溶液4加人溶液3中，搅拌均匀，放置24h，过滤，滤液中加人280mL丙酮，用水稀释至1000ml，混匀安全提示:此溶液要保存于聚乙烯瓶中。此溶液中含丙酮，不得靠近火焰使用。操作中如要加热或煮沸必须在通风橱中操作。 HG/T3696.3一20024.3.51四苯硼钠溶液四苯硼钠溶液(15g/L):称取15g四苯硼钠仁NaB(C6Hs),]溶于960ml一水中，加400g/l,氢氧化钠溶液4ml和100g/l氯化镁(MgCh·6H,O)溶液20ml-，搅拌15min，放置24h后用滤纸过滤，溶液贮存在棕色瓶或聚乙烯瓶中，在一个月内如发现浑浊，使用前应过滤。四苯硼钠溶液(10g/L):称取10g四苯硼钠[NaB(C6H;),]于500ml烧杯中，加水约300ml使之溶解，加人2g氢氧化铝或三氯化铝(溶液如有色需加2g活性炭脱色)搅拌10min，用慢速滤纸过滤。滤液在开始时如呈浑浊，再过滤，直至清亮为止。全部滤液收集于1000mI.容量瓶中，加人200g八_氢氧化钠溶液2mL，稀释至刻度，棍匀，静置48h，备用。四苯硼钠洗涤液(1.5g/l):用10份体积水稀释1份体积15g/L四苯硼钠溶液。四苯硼钠洗涤液(1g/l):用10份体积水稀释1份体积10g/I四苯硼钠溶液4.3.52四苯硼钠乙醇溶液(34g八一)称取3.4g四苯硼钠，溶于100ml无水乙醇中，过滤。4.3.53四苯硼钾乙醇饱和溶液4.3.53.1四苯硼钾的制备称取。.2g碳酸钾(精确至。.001g).溶于300ml水中，加人5滴甲基红指示液，用1+9乙酸溶液调至红色，于水浴上加热至400C，在搅拌下加人45ml四苯硼钠乙醇溶液，放置10min，取下，冷至室温用清洁的滤板孔径为5-15I"m的柑涡式过滤器抽滤，用5%的乙醇溶液洗涤，转移沉淀，抽干、取下琳涡式过滤器，用10m工无水乙醇分三次沿柑祸式过滤器壁洗涤，抽干。4.3.53.2四苯硼钾乙醇饱和溶液将制得的四苯硼钾，加人50m工乙醇,950m工，水，充分振荡使之饱和。使用前干过滤。4.3.54硫化钠溶液方法一:称取硫化钠5g，在10m1水及30ml，丙三醇的棍合溶液中溶解。方法二:称取氢氧化钠5g，在30m工J水和90ml甘油的混合溶液中溶解。将一半体积的溶液边冷却边通入硫化氢气体使之饱和，然后将剩下的一半加人混合。此溶液应遮光、加盖密闭保存于棕色瓶。配制后三个月内有效。4.3.55马钱子碱溶液(50g/L)称取5.0g马钱子碱，溶于冰乙酸中，用冰乙酸稀释至100mL4.4缓冲溶液4.4.1乙酸一乙酸钠缓冲溶液(PH}3)称取。.8g乙酸钠(CH,000Na"3H,0)，溶于水，加5.4ml一冰乙酸，稀释至1000mL,4.4.2乙酸一乙酸钠缓冲溶液(pH-^=4)称取54.4g乙酸钠(CH,000Na"3H,0)，溶于水，加92ml)冰乙酸，稀释至1000ml4.4.3乙酸一乙酸钠缓冲溶液(pH}4.5)称取164g乙酸钠(CH,000Na"3H,O),溶于水，加84mL冰乙酸，稀释至1000ml。4.4.4乙酸一乙酸钠缓冲溶液(pH4-5)称取68.0g乙酸钠(CH,COONa"3H20),溶于水，加28.6mL冰乙酸，稀释至1000ml,.4.4.5乙酸一乙酸钠缓冲溶液(pH-6)称取100g乙酸钠(CH,COONa"3H,0),溶于水，加5.7ml冰乙酸，稀释至1000ml4.4.6乙酸一乙酸钱缓冲溶液(pH4-5)称取38.5g乙酸按，溶于水，加28.6m工一冰乙酸，稀释至1000ML.4.4.7乙酸一乙酸钱缓冲溶液(pH}6.5)称取59.8g乙酸按，溶于水，加1.4m1,冰乙酸，稀释至200m工。4.4.8氨一氯化按缓冲溶液甲(pH-x.10)52 HG/T3696.3-2002称取54.0g氯化馁，溶于水，加350ml氨水，稀释至1000MI_4.4.9氨一氯化馁缓冲溶液乙(PHN10)称取26.7g氯化钱，溶于水，加36m丁氨水，稀释至1000mL,4.4.10柠檬酸一柠檬酸钠缓冲溶液(pH5.5^-6.0)称取270g二水柠檬酸钠与24g一水柠檬酸，溶于水中，并稀释至1000mL,混匀。4.4.11调节总离子浓度的缓冲溶液(TISAB)量取约500ml_水置于1000ml烧杯中，加入57ml冰乙酸、58g氯化钠和12g二水柠檬酸钠(Na,C,H;07·2H}O)，搅拌、溶解。将烧杯放人冰水浴中，用pH计测定溶液的pH值，边搅拌边缓慢注人约6mol/I的氢氧化钠溶液(需加约125mL)，使溶液pH值为5.0-5.5冷却，移人1000ml_容量瓶中，稀释至刻度4.5指示剂及指示液4.5.1二甲酚橙指示液(2g/L)称取。.20g二甲酚橙，溶于水，稀释至100ml。使用期为10天4.5.2二苯胺磺酸钠指示液(5g/L)称取。.50g二苯胺磺酸钠，溶于水，稀释至100mL,4.5.3二苯基偶氮碳酞麟指示液(0.25g/L)称取。.025g二苯基偶氮碳酞脱，溶于乙醇，用乙醇稀释至100ML.4.5.44-(2-毗陡偶氮)一间苯二酚指示液(1g/L)称取。10g442-毗吮偶氮卜间苯二酚(PAR),溶于乙醇，用乙醇稀释至100MI。4.5.5甲基百里香酚蓝指示剂将l.0g甲基百里香酚蓝与100.0g硝酸钾，混匀，研细。4.5.6甲基红指示液(1g/L)称取。.10g甲基红，溶于乙醇，用乙醇稀释至100mL,4.5.7甲基红一次甲基蓝混合指示液将一体积的1g月_次甲基蓝乙醇溶液与两体积1g/L甲基红乙醇溶液混合4.5.8甲基橙指示液(1g/1,)称取。.10g甲基橙，溶于70℃的水中，冷却，稀释至100mL.4.5.9甲基紫指示液(0.5g/L)称取。.050g甲基紫，溶于水，稀释至100m工。4.5.10对硝基酚指示液(1g/L)称取。.10g对硝基酚，溶于乙醇，用乙醇稀释至100ML,4.5.11百里香酚酞指示液(1g/1,)称取。.10g百里香酚酞，溶于乙醇，用乙醇稀释至100mLo4.5.12百里香酚蓝指示液(1g/l)称取0.10g百里香酚蓝，溶于乙醇，用乙醇稀释至100m工。4.5.13邻甲苯酚酞指示液(4g/L)称取。.40g邻甲苯酚酞，溶于乙醇，用乙醇稀释至100ML,4.5.14邻甲苯酚酞络合指示剂一蔡酚绿B混合指示剂称取。.10g邻甲苯酚酞络合指示剂,0.16g蔡酚绿B及30.0g氯化钠，混匀，研细。4.5.15邻联甲苯胺指示液(1g/L)称取。.10g邻联甲苯胺，加10mL盐酸及少量水溶解，稀释至100ML.4.5.16饱和2,4一二硝基酚指示液2,4一二硝基酚的饱和水溶液。 HG/T3696.3一20024.5.17荧光素指示液(5g/I)称取。.50g荧光素(荧光黄或荧光红)，溶于乙醇，用乙醇稀释至100mL4.5.18结晶紫指示液(5g/I,)称取。.50g结晶紫，溶于冰乙酸中，用冰乙酸稀释至100m工_4.5.19淀粉指示液(10g/L)称取1.0g淀粉，加5m工水使成糊状，在搅拌下将糊状物加到90mL沸腾的水中，煮沸1--2min,冷却，稀释至100m工。使用期为两周。4.5.201,10-菲罗琳一亚铁指示液称取。.70g硫酸亚铁(FeS04.7H,O),溶于70m工一水中，加2滴硫酸，加1.5g1,10-菲罗琳W12H8N·Hi0)[或1.76g1,10一菲罗琳盐酸盐(C,,HaN·HCl·H"O)],溶解后，稀释至100MI。使用前制备。4.5.21酚酞指示液(10g/L)称取1.0g酚酞，溶于乙醇，用乙醇稀释至100mLe4.5.22铬黑T指示剂称取10g于(105士5)℃下烘干2h的氯化钠，置于研钵内，加人。.1g铬黑T研细、混匀置于称量瓶中，于干燥器中保存使用期为三个月4.5.23铬黑T指示液(5g/L)称取。.50g铬黑丁和2.0g盐酸轻胺，溶于乙醇，用乙醇稀释至100mL。此溶液使用前制备。4.5.24硫酸铁按指示液(80g/I)称取8.0g硫酸铁按LNH4Fe(SO4)2·12H20],溶于水中(加几滴硫酸)，稀释至100ML.4.5.25紫脉酸钱指示剂称取10g于(105士5)℃下烘干2h的氯化钠，置于研钵内，加人。.5g紫脉酸钱研细、混匀。置于称量瓶中，于干燥器中保存。4.5.26溟百里香酚蓝指示液(1g/L)称取。.10g澳百里香酚蓝，溶于乙醇(体积分数为50%)，用乙醇(体积分数为so%)稀释至100mL4.5.27澳甲酚绿指示液(1g/L)称取。.10g澳甲酚绿，溶于乙醇，用乙醇稀释至100ml-4.5.28澳甲酚绿一甲基红指示液将1g/L嗅甲酚绿乙醇溶液与2g/L甲基红乙醇溶液按3+1体积比混合，摇匀。4.5.29澳酚蓝指示液(0.4g/l)称取。.040g澳酚蓝，溶于乙醇，用乙醇稀释至100ML.4.5.30曙红钠盐指示液(5g/l_)称取0.50g曙红钠盐，溶于水，稀释至100ml。4.5.31二氯荧光黄指示液(1g/l)将。.1g的二氯荧光黄溶于6070ml的乙醇中，再用水稀释至100mLo4.5.32钙试剂竣酸钠盐指示剂称取10g于(105士5)℃下烘干2h的氯化钠，置于研钵内，加人o.1g钙试剂梭酸钠盐研细、混匀。置于称量瓶中，于干燥器中保存。使用期为两个月。4.5.33酸性铬蓝K-蔡酚绿B混合指示液(KB指示液)称取。.3g酸性铬蓝K和。.Ig蔡酚绿B，溶解于水中，稀释至100mL,4.5.34邻苯氨基苯甲酸溶液(0g/工一)#a170.2917k(kiM溶于100mL水中，再加人。.1g邻苯氨基苯甲酸，溶解。 HG/T3696.3一20024.5.35亚铁一邻菲罗琳指示液称取。.7g硫酸亚铁(FeSO,"7H,0)置于烧杯中，加人6mI硫酸溶液[c(1/2)H2S0,=0.1mot/I习，再加入1.5g邻菲罗琳振摇溶解后，再加人硫酸溶液稀释至100ml。4.5.36红紫酸铰指示剂称取20g于(105士5)℃下烘干2h的氯化钠，置于研钵内，加人。.1g红紫酸钱研细、混匀。置于称量瓶中，于干燥器中保存。使用期为三个月。 HG/T3696.3一2002附录A(提示的附录)汉语拼音索引氨水溶液·······················································································⋯⋯4.3.20氨一氯化钱缓冲溶液甲(pH-10).................................................................4.4.8氨一氯化铁缓冲溶液乙(pH-10)····························································⋯⋯4.4.9LUaI百里香酚蓝指示液(1g/L)···························，······································⋯⋯4.5.12百里香酚酞指示液(1g门)··································，，···，··························⋯⋯4.5.11卜aO饱和2,4一二硝基酚指示液··············，·················，···············，，················⋯⋯4.5.16饱和二氧化硫溶液··············································································⋯⋯4.1.6饱和硫化氢水······························，·····················································⋯⋯4.1.7L曰en苯基邻氨基苯甲酸一乙醇溶液(1g/工.)····································.·············⋯⋯4.3.15苯基荧光酮溶液(0.1g/L)··················································，···········⋯⋯4.3.17苯甲酞苯基轻胺溶液(20g/IJ······································，··············，···⋯⋯“‘4.3.16达旦黄溶液(0.5g/L).............··························································⋯⋯4.3.12dtahan淀粉一碘化钾试纸···················································，····················⋯⋯“““4.2.3淀粉一碘化锌溶液·······················································，······················⋯⋯4.3.24淀粉指示液(10g/L)·······································································⋯⋯4.5.19靛蓝二磺酸钠溶液[c(C,,H,N2Na,OeS,)=0.001mol/I〕··，························⋯⋯4.3.46dui对硝基酚指示液(1g/L)··········································，····························一4.5.10二苯胺磺酸钠指示液(5g/L)·······························································⋯⋯4.5.24,7一二苯基一1,10一菲罗琳溶液{c[(CH,)IC,zHsNzC,HsN2]=0.001mol/L}·‘·⋯⋯4.3.9二苯基偶氮碳酞脐指示液(0.25g/I》·····················································⋯⋯4.5.3二甲酚橙指示液(2g/I,)·······························································⋯⋯，，，⋯4.5.1二甲基乙二醛厉氢氧化钠溶液(10g/L)..............................................····⋯⋯4.3.8二氯荧光黄指示液(1g/L)································································⋯⋯4.5.31二乙基二硫代氨基甲酸钠溶液(0g/L)··················································⋯⋯4.3.5二乙基二硫化氨基甲酸银一毗陡溶液··，···················································⋯⋯4.3.6二乙基二硫代氨基甲酸银一三乙基胺三氯甲烷溶液····································⋯⋯4.3.7飞>10-菲罗琳(邻菲罗琳)溶液4.3.261,10一菲罗琳一亚铁指示液·，·························⋯⋯4.5.20 HG/T3696.3一2002fen酚酞指示液(10g/1)4.5.21钙试剂梭酸钠指示剂4.5.32::’铬黑T指示剂······⋯⋯4.5.22铬黑T指示液(5g/L)4.5.23铬酸溶液(100g/L)......4.3.28铬天青S混合液···⋯⋯4.3.27红紫酸钱指示剂4.5.36houng混合碱······⋯⋯4.3.25甲基百里香酚蓝指示剂·····································，··································⋯⋯东5.5甲基橙指示液(1g/L).................................................................................4.5.8甲基红一次甲基蓝混合指示液································································⋯⋯4.5.7甲基红指示液(1g/L).................................................................................4.5.6甲基紫指示液(0.5g/L)..............................................................................4.5.9碱性品红一亚硫酸溶液········，·······························································⋯⋯4.3.44:一:n结晶紫指示液(5g/1)·········································，······························⋯⋯4.5.18孔雀石绿溶液(2g/L)4.3.10kounig喳钥柠酮溶液···⋯⋯4.3.50邻甲苯酚酞络合指示剂一蔡酚绿B混合指示剂····················，········，············⋯⋯4.5.14邻甲苯酚酞指示液(4g八)··································································⋯⋯4.5.13邻联甲苯胺指示液(1g八一)··································································⋯⋯4.5.15邻苯氨基苯甲酸溶液(1g/L)·······。··································，····················⋯⋯4.5.34磷试剂甲·····················································································⋯⋯4.3.47磷试剂乙·······················································································⋯⋯4.3.48磷酸二氢钠溶液(200g/L)························，··········，······························⋯⋯4.3.34硫化馁溶液···············，········，········，·················································⋯⋯4.3.54硫化钠溶液·························································，··························⋯⋯4.3.41硫酸钾乙醇溶液··············································································⋯⋯4.3.41硫酸锰混合液·········································，········································一4.3.39硫酸溶液·······················································，·······························⋯⋯4.3.35硫酸铁钱指示液(80g/L)···································，·····························⋯⋯4.5.24硫酸铜溶液(20g/L)···········································‘··························，·⋯⋯4.3.36硫酸亚铁按溶液(100g/L)·································································⋯⋯4.3.38硫酸亚铁溶液(50g八_)············································，·······················⋯⋯4.3.3757 HG/T3696.3一2002硫酸银溶液(10g/1)········································································⋯⋯4.3.40三氯化铁溶液(100g/L)...........................................................................4.3.31氯化亚锡溶液·································································，··············⋯⋯4.3.30邪马钱子碱溶液(50g/L).................maei:.:.议玫红三梭酸铁溶液(0.5g/L)一纳氏试剂二!4-(2-毗陡偶氮)-间苯二酚指示液(1g/L)4.5.4ian偏钒酸按溶液(2.5即L).......................................................4.3.29ing19氢氧化钾一甲醇溶液··⋯;.:.玲氢氧化钾一乙醇溶液··⋯hu曙红钠盐指示液(5g/L)4.5.30shuang双硫粽三氯甲烷(或四氯化碳)溶液(0.01g/工.)4.3.1151四苯硼钾乙醇饱和溶液4.3.53四苯硼钠溶液4.3.51四苯硼钠乙醇溶液4.3.52IIIan酸性铬蓝K-蔡酚绿B混合指示液(KB指示液)4.5.33碳酸钱溶液4.3.45调节总离子浓度的缓冲溶液(TISAB)4.4.11铁一亚铁混合液························⋯⋯4.3.23wan只王水4.1.无氨的氢氧化钠溶液4.1.无氨的水4.1.无二氧化碳的水4.1.无钙及镁的氯化钠4.2.无醛的乙醇································⋯⋯4.1.10无碳酸盐的氨水4.1.5无碳基的甲醇无氧的水:. HG/T3696.3一2002xiao硝酸溶液······················································································⋯⋯4.3.32硝酸银溶液(17g/L)··········，····························································⋯⋯4.3.33XIU澳百里香酚蓝指示液(1g/L).............................................................⋯⋯，4.5.26嗅酚蓝指示液(0.4g/L)...................................................................⋯⋯4.5.29澳化汞试纸············，，··········，，·····························································⋯⋯4.2.4澳甲酚绿一甲基红指示液·································································，·..⋯⋯4.5.28滇甲酚绿指示液(1g/I)··································································...⋯⋯4.5.27澳溶液[c(Br)=0.1mol/L]·······································，，······················⋯⋯4.3.43亚铁一邻菲罗琳指示液·································································，······⋯⋯4.5.35yan盐酸苯腆溶液(10g/L)·····，·····································⋯⋯，...................⋯⋯4.3.22盐酸溶液······························，·······················································⋯⋯4.3.21乙二胺四乙酸二钠镁溶液[c(EDTA-Mg)=0.01mol/L]................·············⋯⋯4.3.1乙二醛缩双邻氨基酚乙醇溶液(2g/L)···················································⋯⋯4.3.3乙酸铅(碱)溶液······························，·············································，··⋯⋯4.3.4乙酸铅棉花································································，·······，，·············⋯⋯4.2.1乙酸溶液·························································································⋯⋯4.3.2乙酸一乙酸钱缓冲溶液(pH4-5)································⋯⋯，，.，.................⋯⋯4.4.6乙酸一乙酸按缓冲溶液(pH}6).....................................................................4.4.7乙酸一乙酸钠缓冲溶液(pH}3).....................................················，········⋯⋯4.4.1乙酸一乙酸钠缓冲溶液(pH-4).....................................................................4.4.2乙酸一乙酸钠缓冲溶液(PH}4.5)..................................................................4.4.3乙酸一乙酸钠缓冲溶液(pH4-5)······，·······································，，··········⋯⋯4.4.4乙酸一乙酸钠缓冲溶液(pH-6).....................................................................4.4.5ying荧光素指示液(5郊L)....................··········································.⋯⋯，，.4.5.17紫脉酸钱溶液(0.5g/L)⋯⋯4.3.42紫脉酸按指示液4.5.25'