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HG3-1107-1977化学试剂邻苯二甲酸酐.pdf

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'中华人民共和国石油化学工业部部标准HG3-1107-77代替HGB3377-60化学试剂邻苯二甲酸If本试剂为白色针状结晶,溶于热水,难溶于冷水,溶于乙醇、醚及苯。示性式:C,H,(O)iO分子量:148.12(按1975年国际原子量)一、技术条件1.C6H4(CO)20含量不少于:分析纯······················。‘··········································,⋯⋯99.7%;化学纯·····,·······························································⋯⋯99.Oyao2熔点范围〔C):分析纯························································⋯⋯129-1330,C);化学纯·.............................·.·····.....................129-133(2C).3.杂质最高含量(指标以%计):名称分析纯化学纯(1)灼烧残清(以硫酸盐计)0.0250.05(2)叙化物(CD0.0050.01(3)硫酸盐(SO)0.0010.005(4)重金属(以Pb计)0.0010.005二、检验规则按GB619--77之规定进行取样及验收。三、试验方法测定中所需标准溶液、杂质标准液、制剂及制品按GB601--77,GB602-77,GB603-77之规定制备。1.C6H4(CO)20含量测定:称取1克样品,称准至。.0002克。溶于100毫升热水中,加2滴1%酚酞指示液,用0.5N氢氧化钠标准溶液滴定至溶液呈粉红色C,H,(CO),O含量0/a(X)按下式计算:X=竺兰丝9卫7塑旦X100t了发布中华人民共和国石油化学工业部提出1978年10月1日实施夭津市化工局夭津市化学试剂一厂起草1269 HG3---1107一77式中:v氢氧化钠标准溶液之用量,毫升;C一氢氧化钠标准溶液之当量浓度,N;〔;样品重量,克;0.07406一每毫克当量C,H,(CO),O之克数。0熔点测定按(:B617--77之规定测定。3.杂质的测定:样品须称准至。.01克(”灼烧残渣:称取」克样品·置于恒重的柑祸中,加热炭化冷却,加1毫升硫酸,加热至硫酸蒸气逸尽.于800C灼烧至恒重,残渣重量不得大于:分析纯··················,,··············································⋯⋯1.。毫克;化学纯甲,·······························-,甲甲·甲甲,····‘·········一2.0毫克?(2)氯化物:称取0.5克样品,溶于15毫升乙醇及15毫升水中,加2毫升5N硝酸及1毫升。,1N硝酸银,摇匀,放置10分钟,所呈浊度不得大于标准标准是取下列数量的CI分析纯·······························································⋯⋯。.025毫克;化学纯······································,····,··············,·,·,··⋯。.050毫克。与样品同时同样处理(3)硫酸盐:称取1.5克样品,置于蒸发皿中,加10毫升水,3毫升1%碳酸钠溶液,在水浴上蒸千‘加热至样品逸尽,加3毫升饱和澳水,蒸干。加2毫升6N盐酸,再蒸干。残渣溶于10毫升水,过滤.用水洗涤残渣,稀释至25毫升。加1毫升3N盐酸于30-35C水浴中保温10分钟,加3毫升2500氯化钡溶液·摇匀放置30分钟。所呈浊度不得大于标准标准是取3毫升1%碳酸钠,2毫升6N盐酸及下列数量的SO,分析纯·························································,,····⋯⋯。.015毫克;化学纯。················································,········,,·⋯⋯。.075毫克。稀释土25毫升,与过滤后的样品溶液同时同样处理。(4)重金属:称取1克样品,温热溶于10毫升乙醇中,加30毫升水,用10yo氢氧化钠溶液(约2毫升)中和.并过量2毫升,加I毫升10%酒石酸钾钠溶液及2毫升2%硫代乙酞胺溶液,于60C水浴保温1。分钟所呈暗色不得深于标准。标准是取下列数量的Pb,分析纯···················,·········································⋯⋯。.01毫克;化学纯························································,······⋯⋯。.05毫克稀释至与中和后的试液相同体积,与样品溶液同时同样处理。四、包装及标志.包装:按HG3一119-64之规定内包装形式:G-2;外包装形式:工一1;包装单位;第4、5类。2.标志:按HG341964之规定1270'