样品化验与质量评述

页脚内容页脚内容21商州区潘河钼矿区化学样品

钼元素分析质量总结受综合地质大队地调所的委托我室于2010年5月至2011年3月期间承担了商州区潘河钼矿区化学样品的分析测试工作，分析项目M。共1种元素。依据DZ/T0130.4-2006及GB/T14352.2-1993标准要求，我室采用了721-100分光光度计等仪器进行分析测试。本次工作共采钻孔基本分析样5394件。按照中华人民共和国地质矿产行业标准DZ/T0130.4-2006《地质矿产实验室测试质量管理规范第2部分：岩石矿物分析试样制备和第2部分：岩石矿物样品化学成分分析》的要求，分别对样品进行加工和分析测试，具体步骤如下：1、试样制备我室对钼矿石的分析，样品加工遵循切乔特（Henomm）经验公式，即：Q=Kd2。样品的K值采用0.5.分析试样的制备分为三个阶段：即粗碎、中碎和细碎。每个阶段又包括破碎、过筛、混匀和缩分四道工序。分析试样的制备流程见下图粗碎阶段损耗率低于3%、中碎阶段低于5%和细碎阶段低于7%，且过筛率大于95%。样品经过加工后，分析样置于60~80°C的烘箱中烘干，分析。2、样品化验选用中华人民共和国国家标准GB/T14352.1-1993和GB/T14352.2-1993作为分析钨钼的主要方法。称0.1000－0.5000克样品至镍坩锅中，经过氧化钠熔融，水浸取，钼呈钼酸盐进入溶液中，钼酸盐在9%~10%的硫酸介质中以铜盐催化，用硫脲将钼还原至五价状态，与硫氰酸盐结合成可溶性橘红色硫氰酸钼络合物，在分光光度计上于波长460nm处测定吸光度，计算钼量。每一批样品，插入2个或2个以上标准物质或监控样与样品平行测定。标准物质插入分布在该批样品的前、中和后部位。每一批样品随机抽取25％样品作为检查样，并编成密码交由不同人员分别进行基本分析和检查分析。每一批样品插入2份空白试验，与样品平行测定，插入位置为前部和后部。统计基本分析与内检分析成果的相对偏差，再用《DZ0130-2006地质矿产实验室测试质量管理规范中规定的数学模型计算（也可查表求得）相对偏差允许限，相对偏差小于等于允许限时为合格，大于允许限时为不合格。在准确度判定后按批次统计试样的合格率，内检合格率大于95%。基本分析成果从正样中抽取样品总数的5%送外检。统计外检分析成果与基本分析成果的相对偏差，确定相对偏差允许限，在准确度判定后计算合格率，外检合格率大于90%。达到了《DZ0130-2006地质矿产实验室测试质量管理规范》要求。3、内、外检质量本次工作共采钻孔基本分析样5394件，内检由陕西省地矿局综合地质大队地调所项目组抽取粗副样交由我室进行自检代替，自检合格后出具化验报告和对应的自检报告（见附表1），共抽取自检样540个，自检率10.01%，大于内检要求的总样品数的10%，内检合格率97.04%，达到《DZ0130-2006地质矿产实验室测试质量管理规范》要求的内检合格率大于95%.计算公式如下：相对双差值RD=（基分结果一内验结果）/（基分结果+内验结果）X100；相对偏差允许限Yc=C・（14.37・7-0.1263—7.659）Yc—重复分析试样中Mo的相对偏差允许限，%1—重复分析试样中M。的平均质量分数，%C-某矿种某组分重复分析相对偏差允许限系数,Mo=1当RD〉Yc时，检验结果为超差。当RD<Yc时，检验结果为合格。外检样从内验合格且高于矿体边界的副样中提取，重新编号后送西安矿产地质研究所实验测试中心分析。共抽取外检样270个，占样品总数的5%。外检合格率94.07%，其中超差16件，达到《DZ0130-2006地质矿产实验室测试质量管理规范》要求的90%以上。内外检质量统计表见附表2。附表1内检送样号原检测结果内检检测结果相对偏差（RD）允许偏差合格丁3（Mo）/10-23（Mo）/10-2（Yc）超差X内11.5511.5151.1745.956V内20.0640.076-8.57112.447V内30.1480.152-1.33310.602V内40.1470.164-5.46610.519V内50.0910.097-3.19111.712V内60.1040.112-3.70411.375V内70.0950.098-1.55411.648V内80.1190.1161.27711.174V内90.1010.112-5.16411.409V内100.3370.341-0.5908.815V内110.0750.0712.74012.340V内120.0950.106-5.47311.549V内130.0790.083-2.46912.080V内140.1070.115-3.60411.309V内150.0480.051-3.03013.346V版版-本-变-更-履-历:页脚内容页脚内容21内170.1480.158-3.26810.556V内180.0840.088-2.32611.931V内190.0480.053-4.95013.293V内200.0780.083-3.10612.095V内210.0150.01020.00017.334X内220.0810.086-2.99412.004V内230.0890.092-1.65711.805V内240.0960.103-3.51811.573V内250.0510.057-5.55613.117V内260.1690.1486.62510.475V内270.1630.172-2.68710.349V内280.3090.2981.8129.047V内290.0340.035-1.44914.326V内300.5640.629-5.4487.680V内310.1100.117-3.08411.256V内320.0610.0582.52112.864V内330.2390.256-3.4349.482V内340.1170.1150.86211.204V内350.0430.044-1.14913.692V内360.0740.0656.47512.465V内370.0930.0882.76211.805V内381.2201.0955.4006.448V内390.0670.05212.60512.864V内400.1220.1124.27411.184V内410.0770.080-1.91112.158V内420.0750.0684.89512.393V内430.0730.0683.54612.429V内440.1010.0962.53811.598V内450.0790.0659.72212.375V内460.0430.03411.68814.024V内470.0620.0601.63912.799V内480.0660.0595.60012.737V内490.0160.01118.51917.092X内500.2940.2615.9469.237V内510.9080.938-1.6256.857V内520.1630.1426.88510.564V内530.1030.08211.35111.751V内540.1120.08911.44311.549V内550.0720.05711.62812.656V内560.0590.04513.46213.216X内570.6260.5873.2157.648V内580.0760.0657.80112.429V内16V—2.8999.8740.2010.213

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