HG3-1160-1978化学试剂氯化锂.pdf 4页

'中华人民共和国石油化学工业部部标准化学试剂HG3-1160-78氯化锉本试剂为无色结晶，易溶于水，在空气中潮解。分子式:Lici·Hz0分子量:60.41(按1975年国际原子量)一、技术条件l.LiCl.HBO含量不少于97.。%。2·水溶液反应:合格3.杂质最高含量(指标以%计):名称分析纯化学纯(1)澄清度试验合格合格(2)水不溶物0.0050.02(3)硫酸盐(SO)0.010.02(4)硝酸盐(NO,)0.0020.005(5)钱盐(NH)0.0020.005(6)磷酸盐(PO.)0.0010.003(7)钠(Na)0.030.1(8)镁(Mg)0.0020.005(9)钾(K)0.030.05(10)钙(Ca)0.0050.02(11)铁(Fe)0.0010.003(12)钡(13a)0.0050.01(13)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之规定制务年中华人民共和国石油化学工业部化10月1日实施陕西省石油化工局学试剂厂起草 HG3--1160-781.Lift·H必含量测定:称取。2克样品，称准至。.0002克。溶于70毫升水中，加10毫升7X淀粉济液在摇动「用。.]N硝酸银标准溶液避光滴定，近终点时，加3滴。.5%荧光素指示液，继续滴定至乳液呈粉红色。LIC卜FLO含量0n(X)按下式计算:V·CX0.06041X100之.一一乙犷一一，式中:V一硝酸银标准溶液之用量，毫升;C一硝酸银标准溶液之当量浓度，N;‘一样品重量，克;0.06041一每毫克当量LiC卜H2O之克数。2.水溶液反应:称取5克样品，称准至。.01克。溶于100毫升不含二氧化碳的水中，用酸度计测定,pH值应在4.5-7.5之间。3.杂质测定:样品须称准至。01克(L)澄清度试验:称取25克样品，溶于100毫升水中，其浊度不得大于澄清度标准;分析纯·价·····，-·，····1价···，·····，·~··，-，价二4号;化学纯································································，······⋯⋯6号。(2)水不溶物将测定澄清度试验的溶液，在水浴上保温1小时，用恒重的4号玻璃滤祸过滤，以热水洗涤滤渣至洗液无氯离子反应，于105^-110C烘至恒重。滤渣重量不得大于:分析纯····】····‘·，··，，··········。‘，·‘·······················二·.........1.25毫克;化学纯·....................................................................5.00毫克。(3)硫酸盐:称取。.5克样品，溶于25毫升水中，加1毫升3N盐酸，于3。一35C水浴中保温10分钟加3毫升2500抓化钡溶液，摇匀，放置30分钟。所呈浊度不得大于标准。标准是取下列数量的SO,e分析纯·..................................··················，·······⋯⋯0.05毫克;化学纯····。·········。······································，，·······⋯⋯。.10毫克。与样品同时同样处理。(4)硝酸盐:称取1克样品，溶于10毫升水中，加1毫升10yo抓化钠溶液，1毫升。.001M靛蓝二磺酸钠·在摇动下于1015秒钟内加i0毫升硫酸，放置10分钟。所呈蓝色不得浅于标准。标准是取下列数量的NO,分析纯··············。·，········，，，，······，，，············，··⋯⋯，..，一。.02毫克;化学纯····，·······，.····，···，.··，······，甲·，.······一0.05毫克.与样品同时同样处理(5>馁盐:称取1克样品，溶于25毫升不含氨的水中，加2毫升100o氢氧化钠溶液及2毫升纳氏试齐」‘摇匀。所呈黄色不得深于标准。标准是取下列数量的NH4:分析纯·······，···························.................................0.02毫克;化学纯·‘···，··‘··甲···，··‘··，······‘·······，··················一。.05毫克。与样品同时同样处理。(6)磷酸盐:称取1克样品.溶于20毫升水中，加4毫升4N硫酸及磷试剂甲、乙各I毫升，摇匀，于。℃水浴中保温10分钟。所呈蓝色不得深于标准。标准是取下列数量的PO,分析纯····，-············‘······························，········，⋯。.01毫克; HG3-1160-78化学纯·····························································，.⋯⋯0.03毫克。J样品同时同样处理。(7)钠:称取。.5克样品，溶于水，稀释至10。毫升，摇匀。用火焰光度计在589毫微米测定。检流计听示电流值不得大于标准。标准是取下列数量的Na:分析纯·······························································⋯⋯。.15毫克;化学纯·····。。·······················································⋯⋯。.50毫克。与样品同时同样处理(8)镁:a.原子吸收分光光度法仪器条件:光源:镁空心阴极灯;波长:285.2毫微米;火焰:乙炔一空气。测定方法:称取5克样品，溶于水，稀释至100毫升，取10毫升，共四份。按HG3-1013-76第二章第2条第(2)款之规定测定。b.化学分析法称取0.5克样品，溶于20毫升水中，加1毫升0.05%达旦黄溶液，摇匀，加2.5毫升1N氢氧化钠，摇匀口所呈红色不得深于标准。标准是取下列数量的Mg:分析纯···························································⋯⋯。.010毫克;化学纯···································”···················⋯⋯0.025毫克。与样品同时同样处理。(9)钾:称取1克样品，溶于水，稀释至100毫升，摇匀。用火焰光度计在766.5毫微米测定。检流计听不电流值不得大于标准。标准是取下列数量的K:分析纯·.......................................................................。.3毫克;化学纯··································································⋯⋯。5毫克。与样品同时同样处理。(10)钙:a.原子吸收分光光度法仪器条件:光源:钙空心阴极灯;波长:422.7毫微米;火焰:乙炔一空气。测定方法:称取10克样品，溶于水，稀释至100毫升，取20毫升，共四份。按HG3-1013-76第二章第2条第(2)款之规定测定。b·化学分析法称取0.5克样品，溶于水，稀释至50毫升。取4毫升，稀释至15毫升，加10毫升95%乙醇，。.5毫t卜混合碱及1毫升。·2%乙二醛缩双(邻氨基酚)乙醇溶液，摇匀，放置5分钟。用5毫升三抓甲烷萃取温度不超过30C)立即比色，有机层所呈红色不得深于标准。标准是取4毫升不含钙的氯化铿溶液及下列数量的Ca: He3-1160-78分析纯002毫克化学纯008毫克稀释至15毫升，与同体积样品溶液同时同样处理。注:不含钙的抓化锉溶液的制备—称取0.5克分析纯的样品，溶于10毫升水，加10毫升95%乙醉，0.5毫升混合碱及1毫升。.2%乙二醛缩双(邻氨基酚)乙醇溶液，摇匀，放置5分钟。用5毫升三抓甲烷萃取，分离有机层，继续用三氛甲烷萃取，直至有机层无色。水层用3N盐酸中和，稀释至50毫升(11)铁:称取1克样品，溶于20毫升水中，加2毫升1000磺基水杨酸溶液，摇匀。加5毫升10%氯水，摇匀。所呈黄色不得深于标准。标准是取下列数量的Fe:分析纯·····································································⋯⋯0.01毫克;化学纯·························。··········································⋯⋯。.03毫克。与样品同时同样处理。(12)钡:称取2克样品，溶于10毫升水中，加5毫升95肠乙醇，加1毫升4N硫酸，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Ba:分析纯·····································.························⋯⋯。.1毫克;化学纯··································································⋯⋯0.2毫克。与样品同时同样处理。(13)重金属:称取2克样品，溶于水，稀释至40毫升。取30毫升，稀释至40毫升，加1毫升1N乙酸及10毫升新制备的饱和硫化氢水，摇匀，放置10分钟。所呈暗色不得深于标准。标准是取剩余的10毫升样品溶液及下列数量的Pb:分析纯···························-·，···································⋯⋯。。01毫克;化学纯····································································⋯⋯0.05毫克。释释至40毫升，与同体积样品溶液同时同样处理。四、包装及标志1.包装:按HG3-119-64之规定。内包装形式:G-2,Gz-2;G-3,Gz-3;外包装形式;I-1,I、.;包装单位:第4类。2.标志:按HG3-119-64之规定。'