HGT3485-1979化学试剂五氧化二钒(原HGT3-1218-79).pdf 3页

'中华人民共和国化学工业部部标准HG3一1218一79化学试剂五氧化二钒本试剂为黄棕色或砖红色粉末，微溶于水，易溶于碱，溶于热浓酸中。分子式:V205分子量:181.88(按1975年国际原子量)一、技术条件1.VSO:含量不少于:优级纯·····························································⋯⋯99.5%;分析纯、化学纯·····························..·..·................⋯⋯99.0%,2.杂质最高含量(指标以00计):名称优级纯分析纯化学纯1.盐酸不溶物及硅酸盐0.10.20.32.灼烧失重0.10.150.253.抓化物(CD0.0050.010.024.硫酸盐(S(),)0.010.020.045.钱盐(NH4)0.020.050.106.钠(Na)0.020.040.107.铁(Fe)0.010.020.038.重金属(以Pb计)0.0020.0050.010二、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.V205含量测定:称取。.25克样品，称准至0.0002克，加50毫升水，缓缓注人10毫升硫酸，加热溶解、冷却，加4滴0.1写苯基邻氨基苯甲酸乙醉溶液，用。.1N硫酸亚铁按标准溶液滴定至溶液由紫红色变为亮绿色。V20,含量%(X)按下式计算:X=竺丝逐全丝卫旦盛X100几J中华人民共和国化学工业部1979年10月1日实施四川省化工局成都化学试剂厂起草 He3一1218一79式中:v硫酸亚铁按标准溶液之用量，毫升;C一硫酸亚铁钱标准溶液之当量浓度，N;G一样品f(量，克;。.09099每毫克当量VP。之克数。2·杂质测定:样品须称准至。.01克。(1)盐酸不溶物及硅酸盐:称取3克样品，加20毫升盐酸及1克盐酸经胺，加热溶解，在水浴上蒸干冷却，加10毫升盐酸、1克盐酸经胺及100毫升水，加热至沸，用无灰滤纸过滤，以含有10yo盐酸的热水洗涤滤渣至洗液无色。将滤渣置于已恒重的增涡中，缓缓加热炭化，于800"C,灼烧至恒重，残渣重量不得大于:优级纯···············-·，·····································甲，···一3毫克;分析纯·····················，·············44，，·········。········，······⋯⋯6毫克;化学纯·.......................................................................9毫克。(2)灼烧失重:称取2克样品，置于恒重的增竭中，称准至。.0002克，于400℃灼烧至恒重。由减轻之重量计算灼烧失重百分数(3)氯化物:量取20毫升“溶液1",稀释至25毫升，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C1;优级纯·。，·，············‘···，，，················，············，·····，··，·。⋯0.01毫克;分析纯···，································，····.....................。.02毫克;化学纯··········.........................................................。.04毫克。稀释至25毫升，与同体积样品溶液同时同样处理。注:‘溶液1”的制备—称取1克样品，加15毫升10y,氢氧化钠溶液.加热溶解，加25毫升水，10毫升冰乙酸，水浴加热至溶液无色(1^2小时)，搅拌〔必要时补充水)，冷却，过撼，洗涤.稀释至100毫升(4)硫酸盐:量取10毫升“溶液1=，加5毫升95%乙醇，1毫升3N盐酸，在不断振播下滴加3毫升25写氯化钡溶液，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S04优级纯················。····，，，····································⋯⋯。.01毫克;分析纯-甲······，···········-·，········，·，.·········甲·····⋯。.02毫克;化学纯···················，········································⋯’⋯。04毫克。稀释至10毫升，与同体积样品溶液同时同样处理。(5)钱盐:称取。.5克样品，置于支管蒸馏瓶中，加80毫升不含氨的水，沿壁加人20毫升10环不含氨的氢氧化钠溶液，加热蒸馏出50毫升液体，用装有50毫升水的100毫升比色管收集。取20毫升，加2毫升纳氏试剂，摇匀。所呈黄色不得深于标准。标准是取下列数量的NH4,优级纯·····················，·················，····················。··⋯。.02毫克;分析纯·····················，，···················。····················⋯⋯0.05毫克;化学纯··········‘··‘···································⋯⋯。.10毫克。与样品同时同样处理。(6)钠:原子吸收分光光度法:仪器条件:光源:钠空心阴极灼一;波长:589皇微来 HG3一1218一79火焰:乙炔一空气。测定方法:称取1克样品，加5毫升盐酸及。.5克盐酸经胺，加热溶解，冷却，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。(7)铁:a.原子吸收分光光度法仪器条件;光源:铁空心阴极灯;波长:248.3毫微米;火焰:乙炔一空气。测定方法:称取5克样品，加25毫升盐酸及3克盐酸经胺，加热溶解，冷却，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.化学方法:称取1克样品，加20毫升IN氢氧化钠加热溶解、冷却，稀释至100毫升。取10毫升，稀释至20毫升，加2毫升用氨水中和至微碱性的10%磺基水杨酸溶液，于水浴中保温5分钟，加5毫升10写氨水，摇匀。所呈黄色不得深于标准。标准是取2毫升INNaOH及下列数量的Fe:优级纯·······························································⋯⋯0.01毫克;分析纯.....................................................................0.02毫克;化学纯·....................................................................。.03毫克。稀释至20毫升，与同体积样品溶液同时同样处理。(8)重金属:称取。.7克样品，加25毫升10%氢氧化钠溶液，加热溶解，冷却，加4毫升300o酒石酸溶液，冷却，加2毫升新配制的5%硫化钠溶液，放置10分钟。所呈暗色不得深于标准。标准是取0.2克样品及下列数量的Pb:优级纯···························································⋯⋯。.010毫克;分析纯”················································，········⋯⋯。.025毫克;化学纯··························································⋯⋯。.050毫克。与样品同时同样处理四、包装及标志1.包装按HG3-119-64之规定。内包装形式:G-3,GZ3;外包装形式:1-1;包装单位:第3类。2.标志按HG3-119-64之规定。'