HGT3467-1977化学试剂50％硝酸锰溶液(原HGT3-1065-77).pdf 3页

'中华人民共和国石油化学工业部部标准HG3-1065-77化学试剂代替HGB3256-60500o石肖酸锰溶液本试剂为淡粉红色的液体，溶于醇。分子式:Mn(NO,),:分子量:178.95按1975年国际原子量)一、技术条件1.Mn(N03):含量:分析纯、化学纯···············，··························，·······一49.0-51.0%。2.杂质最高含量(指标以%计):名称分析纯化学纯(1)水不溶物0.0050.01(2)抓化物(CU0.0010.002(3)硫酸盐(SO)0.010.04(4)铁(Fe)0.00050.002(5)锌(Zn)0.020.05(6)重金属(以Pb计)0.0010.002‘(7)碱金属及碱土金属(硫酸盐)0.100.25二、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.Mn(N03)。含量测定:称取。.5克(0.4毫升)样品，称准至。.0002克。加10。毫升水及2毫升1000盐酸羚胺溶液，用。.05M乙二胺四乙酸二钠标准溶液滴定，近终点时加10毫升氨一氮化按缓冲溶液甲(pH10)及5滴。.5%铬黑T指示液，继续滴定至溶液由紫红色变为纯蓝色。Mn(N03)i含量%(X)按下式计算:V·CX0.1790.，__人今—入iuu行中华人民共和国石油化学工业部发布1978年10月1日实施辽宁省石油化工局提出沈阳市新城化工厂起草 HG3-1065-77式中:v一一乙二胺四乙酸二钠标准溶液之用量，毫升;G-一乙二胺四乙酸二钠标准溶液之克分子浓度，M;G样品重量，克;0.1790每毫克分子Mn(NO,)。之克数。2.杂质测定:样品须量准至0.1毫升。(1)水不溶物:量取40毫升(50克)样品，注人10。毫升水中，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硝酸盐反应。于105-110C烘至恒重，残渣重量不得大于:分析纯··············.················································⋯⋯2.5毫克;化学纯······································。···························⋯⋯5.。毫克(2)氯化物:量取。.8毫升(L<克)样品，加25毫升水(必要时过滤),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:分析纯0.01毫克;化学纯0.02毫克。稀释至25毫升，与同体积样品溶液同时同样处理。(3)硫酸盐:量取。.4毫升(0-5克)样品，加20毫升水、2毫升甲醛溶液及2毫升盐酸，摇匀，温热至反应停止，在水浴上蒸干，溶于水，稀释至50毫升。取10毫升‘，加5毫升95%乙醇,1毫升3N盐酸，在不断振摇下滴加3毫升2500氯化钡溶液，稀释至25毫升，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分析纯·····························································⋯⋯0.01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。(4)铁:量取。.8毫升(1克)样品，稀释至25毫升，加1毫升盐酸，3Q毫克过硫酸按及2毫升250硫氰酸铁溶液，用10毫升正丁醇萃取，有机层所呈红色不得深于标准标准是取下列数量的Fe:分析纯······························································⋯⋯。.005毫克;化学纯·······························································⋯⋯。.020毫克。与样品同时同样处理(5)锌:a.原子吸收分光光度法仪器条件:光源:锌空心阴极灯;波长:213.9毫微米;火焰乙1块空气测定方法:量取。.8毫升(1克)样.钻·稀释至10。毫升。取10毫升，共四份。按HG3---1013--76第二章第2条第(2)款之规定制定。b.化学分析法量取。.4毫升(0.5克)样品，注人250毫升容量瓶中，稀释至刻度。取5毫升，稀释至20毫升，加5毫升乙酸一乙酸钠缓冲溶液(PH4^-5),1毫升一250o硫代硫酸钠溶液，摇匀，用5毫升。001%苯基硫脉四氯化碳溶液萃取，有机层所呈紫红色不得深于标准标准是取下列数量的Zn:分析纯······························································⋯⋯。.002毫克;化学纯·······························································⋯⋯。.005毫克 HG3-1065-77稀释至.5毫升，与同体积样品溶液同时同样处理。(6)重金属量取。.8毫升(1克)样品，加1毫升1N乙酸，稀释至30毫升，加10毫升95%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30毫升不含重金属的硝酸锰溶液及下列数量的Pb:分析纯···，···························································⋯⋯0.01毫克;化学纯·····················。·········································⋯⋯。.02毫克。与同体积样品溶液同时同样处理。注:不含重金属的硝酸锰溶液的制备—量取4毫升(5克)样品，稀释至100毫升，加热至80"C，加5毫升1N乙酸及20毫升新制备的饱和硫化氢水，摇匀，放置12-18小时，过滤，煮沸，冷却，稀释至150毫升。(7)碱金属及碱土金属:量取1.6毫升(2克)样品，溶于90毫升不含二氧化碳的水中，煮沸，加10毫升不含三氧化碳的氨水，于60^-70C通人硫化氢，使锰沉淀完全，在水浴上加热至沉淀完全变为绿色。冷却，稀释至100毫升，过滤，取50毫升，置于恒重的蒸发皿中，加2毫升4N硫酸，在水浴上蒸发近干，加热至硫酸蒸气逸尽，于800℃灼烧至恒重。残渣重量不得大于:分析纯··································································⋯⋯1.。毫克;化学纯·································································⋯⋯2.5毫克。四、包装及标志1.包装:按HG3-119-64之规定。内包装形式:Xz--1;外包装形式:1-1,1--2,1-3;包装单位:第4类。2.标志:按HG3-119---64之规定'