高纯铋化学分析方法 痕量杂质元素含量的测定 辉光放电质谱法编制说明

请按照《国家标准管理办法》（2023.3.1实施）中的要求分10章撰写编制说明，或者按以前12章的结构。目前缺少内容。行业标准《高纯铋化学分析方法第2部分：痕量杂质元素含量的测定辉光放电质谱法》编制说明（预审稿）请按照《国家标准管理办法》（2023.3.1实施）中的要求分10章撰写编制说明，或者按以前12章的结构。目前缺少内容。工作简况任务来源根据《工业和信息化部办公厅关于印发2022年第一批行业标准制修订和外文版项目计划的通知》（工信厅科函【2021】94号）的要求，由国标（北京）检验认证有限公司负责行业标准《高纯铋化学分析方法第2部分：痕量杂质元素含量的测定辉光放电质谱法》的修订工作，计划编号为2022-0104T-YS。项目起止时间为2022年07月～2023年10月，由全国有色金属标准化技术委员会（SAC/TC243）提出并归口。立项目的和意义铋是一种稀有金属,由于具有优良的物理化学性能，被广泛应用于医药、电子、冶金、化工、半导体、超导体、电子陶瓷等领域，铋中的杂质元素的含量影响其纯度，进而影响纯铋的应用。随着技术的进步，下游应用市场的快速发展，对高纯金属铋的要求也越来越高。因此对铋材料中杂质元素含量快速、准确测定是高纯铋质量控制的重要环节。现行高纯铋标准分析方法是2013版的YS/T923-2014《高纯铋化学分析方法》，随着科技的发展，产品生产工艺水平和检测能力都有了大幅进步，现行的检测方法已不再满足分析的需求，GB/T1.1《标准化工作导则第1部分：标准化文件的结构和起草规则》已修订为2020版，其中编制规则、术语表达等都有了调整，因此，为适应技术发展和新版标准化工作导则的要求，需要对2013版《高纯铋化学分析方法第2部分：痕量杂质的测定辉光放电质谱法》进行修订。项目编制组单位情况和人员分工简要说明其他单位工作以及人员分工简要说明其他单位工作以及人员分工牵头单位国标（北京）检验认证有限公司隶属于有研科技集团有限公司，是国家新材料测试评价平台-主中心承建单位，为中国新材料测试评价联盟秘书处挂靠单位。公司自成立以来，积极整合完善现有测试评价、设计应用、大数据等平台资源，逐步形成立足北京、布点全国、服务全行业的国家新材料测试评价平台。国标（北京）检验认证有限公司作为国合通用测试评价认证股份公司的全资子公司，前身是北京有色金属研究总院分析测试技术研究所，是国家有色金属行业最知名的第三方检验机构。国标（北京）检验认证有限公司运营管理着国家有色金属及电子材料分析测试中心和国家有色金属质量监督检验中心，拥有一支基础理论扎实、实践经验丰富的研究和服务队伍，自2004年至今共承担了国家科技支撑计划、国家863计划、国家自然科学基金、军工配套等省部级科技项目40余项；曾获国家科技进步奖6项，国家发明奖3项，省部级科技进步一等奖10项，二、三等奖107项；近5年获得国家发明专利20余项；负责和参加起草制订分析方法国家标准、行业标准300余项；国家标准物质/标准样品120个，在国内外科技期刊上发表论文800余篇，撰写论著22部。表1主要起草人及工作职责起草人工作职责刘红负责标准的工作指导、行业调研，查阅相关标准、资料、确定标准制定方案标准的编写、试验方案确定组织协调负责试验方案的实施及实验数据的收集负责标准验证工作起草过程3.1起草阶段本项目在下达计划后，于2022年7月在河南省洛阳市召开了任务落实会和讨论会。会上决定由国标（北京）检验认证有限公司为标准起草牵头单位，由广东先导稀材股份有限公司、湖南柿竹园有色金属有限责任公司、江西金德铅业股份有限公司负责样品制备，由广东先导稀材股份有限公司、贵研铂业股份有限公司、深圳市中金岭南有色金属股份有限公司、负责一验、包头稀土研究院、山东恒邦、昆明冶金院等具体写清楚。负责二验验证工作。具体写清楚。根据任务要求，我公司组建了《高纯铋化学分析方法第2部分：痕量杂质元素含量的测定辉光放电质谱法》编制小组。编著编制小组技术人员查阅相关产品和分析方法的资料，拟定了试验方案，同时与国内生产厂家进行充分沟通，了解产品实际纯度水平以及对测试方法下限的要求，经过积累大量试验数据，论证方法的可行性。并采用江西金德铅业股份有限公司生产的高纯铋产品对方法进行开发和验证。按照行业标准的格式要求起草了本标准，形成了标准预审稿。标准编制原则、主要内容及其确定依据1、标准编制原则本标准起草单位自接受起草任务后，成立了标准编制组负责收集生产统计、检验数据、市场需求及客户要求等信息，初步确定了《高纯铋化学分析方法第2部分：痕量杂质元素含量的测定辉光放电质谱法》标准起草所遵循的基本原则和编制依据：（1）查阅相关标准和客户的相关技术要求；（2）根据国内生产企业的具体情况，力求做到标准的合理性和实用性；（3）根据技术发展水平及测试数据确定技术指标取值范围；（4）本文按照GB/T1.1-2020《标准化工作导则第1部分：标准化文件的结构和起草规则》、GB/T20001.4-2015《标准编写规则第4部分：试验方法标准》的原则进行起草。2、标准主要内容本标准为了能够真实反映当前国内高纯铋中杂质的含量水平，结合我国高纯铋的实际生产和使用情况而制定。标准主要内容：前言这一段一般就粘贴标准第一段即可、1.范围、2.规范性引用文件、3.方法提要、4.干扰因素、5.试剂和材料、6.仪器设备、7.试样准备、8.试验步骤、9.试验数据处理、10.精密度、11.试验报告。这一段一般就粘贴标准第一段即可2.11方法原理的确定高纯铋样品作为放电阴极进行辉光放电，其表面原子被等离子体中带电粒子轰击发生溅射，溅射产生的原子被离子化后，离子束通过电场加速进入质谱仪进行测定。在每一待测元素选择的同位素质量处以预设的扫描点数和积分时间对应谱峰积分，所得面积为谱峰强度。无标准样品时，计算机根据仪器软件中的“典型相对灵敏度因子”自动计算出各元素的质量分数；有标准样品时，需通过与被测试样相同的分析条件、离子源结构以及测试条件下对标准样品进行独立测定获得相对灵敏度因子，应用该相对灵敏度因子计算出各元素的质量分数。2.2测试范围的确定高纯铋中多数元素检测下限可以达到0.001ug/g，F、S、Cl、K、Br、Se、I等8种元素由于灵敏度稍差，因此检测下限设定为0.05ug/g，Na、Mg、Al、Si、P、Ca、Ga、Ge、As等9种元素属于易沾污以及质谱干扰严重的情况，因此下限设定为0.005ug/g。表2测定范围元素测定范围/μg/g元素测定范围/μg/g元素测定范围/μg/g元素测定范围/μg/g元素测定范围/μg/gLi0.001~50V0.001~50Y0.001~50Ba0.001~50Hf0.001~50Be0.001~50Cr0.001~50Zr0.001~50La0.001~50Ta0.001~50B0.001~50Mn0.001~50Nb0.001~50Ce0.001~50W0.001~50F0.05~50Fe0.001~50Mo0.001~50Pr0.001~50Re0.001~50Na0.005~50Co0.001~50Ru0.001~50Nd0.001~50Os0.001~50Mg0.005~50Ni0.001~50Rh0.001~50Sm0.001~50Ir0.001~50Al0.005~50Cu0.001~50Pd0.001~50Eu0.001~50Pt0.001~50Si0.005~50Zn0.001~50Ag0.001~50Gd0.001~50Au0.001~50P0.005~50Ga0.005~50Cd0.001~50Tb0.001~50Hg0.001~50S0.05~50Ge0.005~50In0.001~50Dy0.001~50Tl0.001~50K0.05~50As0.005~50Sn0.001~50Ho0.001~50Pb0.001~50Cl0.05~50Br0.05~50Sb0.001~50Er0.001~50Th0.001~50Ca0.005~50Se0.05~50I0.05~50Tm0.001~50U0.001~50Sc0.001~50Rb0.001~50Te0.001~50Yb0.001~50--Ti0.001~50Sr0.001~50Cs0.001~50Lu0.001~50--2.3样品制备样品尺寸应能放入辉光放电离子源内并且能够稳定地进行辉光放电。常规样品指棒状或片状的金属样品，棒状是指直径为2mm~3mm、长约20mm~25mm的棒状是否一定要具体到尺寸？，片状是指直径为12mm~60mm、厚度为1mm~20mm的片状，保持样品表面光洁和平整。在装样之前，试样的表面应通过腐蚀清洗：用无水乙醇（7.5）浸泡样品4min~5min，清洗掉表面上的油污，用盐酸（7.3）腐蚀8min~10min，用水超声清洗8min~10min，冲洗10次，再用高纯氮气（7.6）吹干，待测。是否一定要具体到尺寸？试验条件2.4试验工作条件选择2.4.1仪器工作参数选择调节辉光放电质谱仪工作参数中，放电气体氩气的流速GasFlow（mL/min）、放电电流I(mA)、放电电压U(V)是最重要的调节参数。以下分别考察三者对铋基体离子信号强度的影响情况。2.4.1.1放电气体流量调节设定放电电流为20mA，放电电压为1100V，调节放电气体流速，观察铋基体离子信号强度的变化见图1。从图中可以看出，在固定放电电流和放电电压情况下，铋基体信号随放电气体流量增加而变大，470mL/min后信号不再变化，实验选择氩气流速为470mL/min。图1Bi信号强度随放电气体变化曲线2.4.1.2放电电流的调节固定放电气体流速Gas值为470mL/min，放电电压为1100V，调节放电电流，观察放电电流变化和铋基体离子信号强度的变化见图2。从图中可以看出，放电电流增加，进入质谱仪的离子束强度增大，从而使离子信号强度增大。但电流太大，会使样品溅射速率增大，但长时间溅射产生的粒子会沉积在阳极帽、导流管、锥口，影响离子传输效率，降低仪器灵敏度，甚至导致短路，当铋基体信号中分辨模式达到1×109cps时已满足分析要求，此时电流强度为20mA。实验选择放电电流为20mA。图2Bi信号强度随放电电流变化曲线2.4.1.3放电电压的调节设定放电电流为20mA，放电气体流量为470mL，调节放电电压，观察铋基体信号强度随放电电压变化曲线。见图3，电压从600V增加到1400V，随放电电压变化，信号强度逐渐增大，1100V后信号强度增加不明显，因此选择放电电压为1100V。图3Bi信号强度随放电电压变化曲线2.4.2预溅射时间的选择在选定的仪器工作条件下，考察易污染元素钠、钙随溅射时间的变化，见图4、5，结果表明，随溅射时间的增加，各元素信号强度逐渐下降，溅射时间20min以后，信号达到稳定，因此选择预溅射时间为20min。图4Na信号强度随溅射时间变化曲线图5Ca信号强度随溅射时间变化曲线试验在18℃~24℃室温下进行，相对湿度：不大于65%。2.4试验数据分别对4个高纯铋样品进行检测，重复6次读数，考察方法测定精密度，结果表明，含量大于0.01ug/g元素的相对标准偏差均小于20%，精密度较好，见表3。表3.11#高纯铋精密度检测结果元素测定次数/ug/g平均值/ug/g/ug/g/ug/g标准偏差相对标准偏差123456AVGSTDEVRSD/%Li000000＜0.0010.000/Be000000＜0.0010.000/B0.0020.0040.0010.002000.0020.002101F12.4312.43312.89511.52313.50612.27612.50.6615Na0.0220.0220.0080.0160.0190.0160.0170.00530Mg0.0010.0010.0010.00100＜0.0050.001/Al0.0740.0580.0320.040.0260.0120.0400.02256Si0.4690.2470.2230.3070.2470.0090.250.14859P0.0050.0020.0010.0010.0020＜0.0050.002/S0.4580.310.290.430.290.1040.310.12640Cl3.7364.8485.127.3376.7895.2425.51.32524K0.7570.8130.5780.7890.7060.5550.700.10916Ca0.0530.0510.0460.030.0360.0430.0430.00920Sc000000＜0.0010.000/Ti0.0030.0040.0020.0030.0020.0010.0030.00142V0.0010.0010000＜0.0010.001/Cr0.0350.0280.0340.0320.0280.0250.0300.00413Mn0.0040.0030.0030.0030.0020.0020.0030.00127Fe0.0750.0850.0680.0770.0580.050.0690.01319Ni0.160.2240.10.1530.1320.1360.150.04127Co0.0070.0080.0090.0070.0080.0030.0070.00230Cu0.9170.480.3930.3280.5210.5160.530.20639Zn0.0180.0150.0130.010.020.0060.0140.00538Ga0.0090.0040.0010.00300.006＜0.0050.003/Ge0.1040.0580.0090.0240.0440.0350.0460.03373As0.0060.0040.0040.0050.0030.001＜0.0050.002/Br0.0410.0220.0140.0260.0170.019＜0.050.010/Se0.050.0180.0150.0330.0160.047＜0.050.016/Rb0.001000.00100＜0.0010.001/Sr0.0010.0010000＜0.0010.001/Y0000.00100＜0.0010.000/Zr0.0090.004000.0010.0010.0030.004140Nb0.0060.0020.0030.0040.0030.0010.0030.00254Mo0.0370.0510.0540.070.0620.0440.0530.01223Ru0.0040.0020.0040.0030.0030.0070.0040.00245Rh0.0120.0110.0040.0040.0050.0030.0070.00461Pd0.0070.0030.0030.0080.0060.0070.0060.00238Ag9.4548.0149.2149.88710.699.2759.420.8809Cd0.170.0840.0510.0940.080.0580.090.04348In0.0210.0070.0320.0230.030.0130.0210.01046Sn0.0030.00200.001000.0010.001126Sb0.0050.0050.0020.0040.0060.0070.0050.00236I0.001000.00100.001＜0.050.001/Te0.1370.1030.120.1460.0910.0940.120.02320Cs0.0010.0010.0010.001000.0010.00177Ba0.0020.00100000.0010.001167La0.0020.00100000.0010.001167Ce000000＜0.0010.000/Pr000000＜0.0010.000/Nd0.00600.0010.0040.00400.0030.003100Sm000000＜0.0010.000/Eu000000＜0.0010.000/Gd0.003000.001000.0010.001182Tb000.001000＜0.0010.000/Dy000000＜0.0010.000/Ho0000.00100＜0.0010.000/Er000000＜0.0010.000/Tm000000＜0.0010.000/Yb0.001000.0010.0010.0020.0010.00190Lu000000＜0.0010.000/Hf0.0020.00200.0020.0010.0030.0020.00162Ta0.070.1110.1470.3710.1120.0390.140.11884W0.0260.0030.0070.0170.0140.020.0150.00858Re0.0080.0010.0040.0020.00100.0030.003110Os0.0020.0040.0040.0020.0030.0040.0030.00131Ir0.0020.0050.0060.002000.0030.003100Pt0.0070.0050.0070.0240.0080.0020.0090.00888Au0.0250.0150.0870.0970.0550.0610.0570.03357Hg0.1820.0440.1460.1730.2710.1540.160.07345Tl0.110.0110.1080.1010.1240.0850.0900.04145Pb1.8371.8041.8021.7171.8481.5691.760.1066Bi10000001000000100000010000001000000100000010000000.0000Th00.0010000.001＜0.0010.001/U000000＜0.0010.000/表3.22#高纯铋精密度检测结果元素测定次数/ug/g平均值/ug/g/ug/g/ug/g标准偏差相对标准偏差123456AVGSTDEVRSD/%Li0.001000.00100＜0.0010.001/Be<=0.001<=0.0020.001<=0.002<=0.003<=0.0030.001#DIV/0!/B0.0210.040.0260.0130.0120.0140.0210.01151F16.57715.08411.12411.50411.49310.07412.62.56820Na0.0580.0270.0580.0650.040.0360.0470.01532Mg0.0130.0130.0090.0070.0030.0030.0080.00556Al0.4780.9140.6891.1160.7380.6280.760.22530Si0.040.3790.2120.1650.1080.1020.170.11971P0.0030.0180.0050.0110.0040.0040.0080.00679S0.0650.0440.0280.0230.0090.0080.0300.02274Cl0.6153.2882.541.9071.5581.3671.90.93750K2.2172.052.7012.1682.1021.712.20.32115Ca0.2290.2520.2180.1760.1310.0920.180.06234Sc0.0020.0010.0010.0010.00100.0010.00163Ti0.5260.2280.1650.1150.0930.0740.200.16984V0.0010.010.0080.0060.0030.0030.0050.00366Cr1.3552.9442.212.7312.8772.3062.40.59525Mn0.0070.0750.0510.0420.0330.020.0380.02463Fe1.7011.3931.8261.2691.2211.1511.40.27519Ni1.5391.2031.8181.7931.5581.2761.50.25517Co1.3481.7951.7972.1051.5961.4981.70.26716Cu2.8612.9682.1412.8152.5232.3872.60.31912Zn0.2530.2570.2540.2840.2160.2450.250.0229Ga0.0080.0090.010.003000.0050.00591Ge0.0280.0380.023000.0110.0170.01693As00.00100.00100.0010.0010.001110Br0.0290.070.0530.0450.0380.037＜0.050.015/Se0.0670.0510.04900.0380.059＜0.050.024/Rb0.0010.001000.0010.0010.0010.00177Sr0.00100.0010.001000.0010.001110Y0.0010.0010.00100.00100.0010.00177Zr0.4320.1960.1440.0990.0740.070.170.13781Nb0.0370.6010.4930.3450.230.2140.320.20464Mo1.3321.7081.5671.8251.3241.1551.50.25717Ru00.0160.0150.030.0110.0130.0140.01068Rh0.0040.0410.0340.0210.0210.0160.0230.01358Pd0.0160.0910.0620.0630.0260.0230.0470.03063Ag4.98513.31511.8399.868.6668.7349.62.89130Cd0.0580.7960.4290.2050.1940.2030.310.26484In0.1460.0770.0750.0440.0350.0340.0690.04362Sn000.001000＜0.0010.000/Sb00.0010.001000＜0.0010.001/I0.0020.0030.00300.0010＜0.050.001/Te0.0140.0790.0560.0530.0380.0340.0460.02249Cs00.0040.0010.0010.0020.0010.0020.00192Ba0.0170.0070.0090.0050.0060.0080.0090.00450La0.0010.0180.0160.0110.0050.0090.0100.00664Ce0.00100.0010.001000.0010.001110Pr000000＜0.0010.000/Nd0.0080.0140.0120.0030.0030.0070.0080.00558Sm000000＜0.0010.000/Eu0.00100.0010.001000.0010.001110Gd0.0120.0190.0140.0080.0060.0060.0110.00548Tb000000＜0.0010.000/Dy0.0040.0010.001<=0.0070.0030.0010.0020.00171Ho0.0020.0010.0010.0010.00100.0010.00163Er0.00100.001000＜0.0010.001/Tm000000＜0.0010.000/Yb00.0030.00400.0020.0020.0020.00287Lu000000＜0.0010.000/Hf0.2310.1090.0980.1010.0560.0660.110.06357Ta0.2170.360.2620.2530.2020.180.250.06426W1.0871.1081.091.0460.8870.7241.00.15416Re0.1640.0690.0590.0580.0420.0350.0710.04766Os0.0020.0010.0020.00700.0030.0030.00297Ir0.0240.010.0090.0070.0080.010.0110.00656Pt0.0640.0380.0380.0530.0230.0160.0390.01846Au0.750.1650.1440.1870.1620.1510.260.24193Hg0.3190.2150.2140.1830.1550.1450.210.06331Tl0.1010.0980.0920.0950.1220.1130.100.01211Pb2.5722.5352.5362.2762.032.2272.360.2199Bi10000001000000100000010000001000000100000010000000.0000Th0.0010.00100.001000.0010.001110U0.00100.001000＜0.0010.001/表3.33#高纯铋精密度检测结果元素测定次数/ug/g平均值/ug/g/ug/g/ug/g标准偏差相对标准偏差123456AVGSTDEVRSD/%Li0.00100000＜0.0010.0004/Be<=0.002<=0.003<=0.005<=0.007<=0.008<=0.011＜0.001//B00.0010.002000.0030.0010.0013126F2.3072.5762.5552.2291.8382.1372.30.276512Na0.1860.2480.2220.160.1410.1660.190.040622Mg0.00300.0030.00200＜0.0050.0015/Al0.3130.2750.2850.2290.1890.230.250.045418Si0.1730.1570.1720.1180.10.1160.140.031823P00.00200.00200＜0.0050.0010/S0.0080.0130.010.0040.0110.035＜0.050.0110/Cl13.92416.47217.7616.79517.92419.003171.744910K0.5570.570.6320.5990.5430.5220.570.03977Ca0.0790.0850.1350.1010.0850.110.100.021021Sc0.00100.0020.0010.00100.0010.000890Ti0.0250.0260.030.0220.0230.0220.0250.003112V0.00100.0010.0010.00100.0010.000577Cr1.5461.4261.3041.2231.2111.2331.30.135210Mn0.0180.0190.0260.0110.0250.0210.0200.005427Fe0.4830.5030.430.3660.3990.4460.440.051212Ni2.6042.5852.3292.0542.4912.412.40.20408Co1.181.070.9740.8550.7830.8360.950.153516Cu1.0121.0231.161.2251.21.0981.10.09018Zn1.2270.8740.6640.4830.5440.4520.710.297342Ga000000＜0.0050.0000/Ge000000＜0.0050.0000/As0.0030.003000.0050.006＜0.050.0025/Br0.0250.0170.0250.0270.0340.02＜0.050.0059/Se0.3550.470.3120.3850.2780.3580.360.066018Rb000000＜0.0010.0000/Sr000000＜0.0010.0000/Y0.0020.0030.0020.0040.0040.0020.0030.001035Zr0.0230.0170.0170.0150.0230.0280.0210.005024Nb0.1390.1320.1430.1140.1380.1250.130.01088Mo0.3450.3740.2820.2980.2440.3040.310.046115Ru0.0070.0110.0060.0110.0140.0060.0090.003336Rh0.0050.0130.0070.0070.0070.0080.0080.002735Pd0.0660.050.0470.0420.0110.0140.0380.021656Ag16.50717.10817.11816.68617.49718.221170.61484Cd0.0930.038000.1140.0460.0490.047197In0.1770.1590.1680.1970.1020.1310.160.034122Sn000000＜0.0010.0000/Sb000000＜0.0010.0000/I0.0010.00100.00200.002＜0.050.0009/Te0.150.1680.130.0990.1580.1630.140.026018Cs0.0010.0010.0020.00100.0020.0010.000865Ba0.0010.0030.0050.0020.00500.0030.002177La000.0010.00100.0010.0010.0005110Ce00000.0010.001＜0.0010.0005/Pr000000＜0.0010.0000/Nd0.0020.002000.00200.0010.0011110Sm000000＜0.0010.0000/Eu000000＜0.0010.0000/Gd0.00100.0030.0030.00200.0020.001492Tb000000＜0.0010.0000/Dy<=0.006<=0.003<=0.006<=0.008<=0.010<=0.012＜0.001#DIV/0!/Ho000000＜0.0010.0000/Er000000＜0.0010.0000/Tm000000＜0.0010.0000/Yb0.0030.0020000.0010.0010.0013126Lu000000＜0.0010.0000/Hf0.0210.0220.0280.0090.0160.0350.0220.009142Ta0.0850.10.0810.1240.1320.1090.110.020520W0.3870.3760.3010.3980.3870.3550.370.035610Re0.0140.0130.0040.010.0060.0040.0090.004552Os0.0020.0030.0020.003000.0020.001482Ir0.0040.0020.0040.005000.0030.002287Pt0.0120.0040.0070.009000.0050.004992Au0.1330.140.1590.2110.2110.2720.190.053428Hg0.1250.0670.2240.1990.1010.0650.130.067352Tl0.1320.1370.1170.060.0430.1120.100.039239Pb7.8588.2688.0418.2218.8668.4098.280.34614Bi1000000100000010000001000000100000010000001000000.000.00000Th0.0010.0010.0010.0010.0020.0010.0010.000435U000000＜0.0010.0000/表3.44#高纯铋精密度检测结果元素测定次数/ug/g平均值/ug/g/ug/g/ug/g标准偏差相对标准偏差123456AVGSTDEVRSD/%Li<=0.000<=0.000<=0.0000<=0.00000.0000.000/Be00<=0.000<=0.000000.0000.000/B0<=0.000<=0.000<=0.000<=0.00000.0000.000/F2.69100002.2430.8221.282156Na0.010.0120.0110.010.0110.010.0110.0018Mg0000000.0000.000/Al0.0880.0810.0890.0920.0970.1030.0920.0088Si0.0030.0010.0010.0010.0020.0010.0020.00156P0.0010.00100.001000.0010.001110S0.320.3270.2990.2780.2910.2850.3000.0207Cl3.5863.5973.6853.6783.7193.5653.6380.0632K0.0460.0430.0610.0630.0740.0760.0610.01423Ca0.0050.0030.0070.0020.0070.0040.0050.00244Sc0000000.0000.000/Ti0000000.0000.000/V0000<=0.00000.0000.000/Cr0.0010.0010.0010.0010.0010.0010.0010.0000Mn0000000.0000.000/Fe0.0250.0250.0240.0280.0260.0280.0260.0026Ni0.1210.1530.1170.1330.1530.1410.1360.01511Co0000000.0000.000/Cu0.2590.260.2750.2890.2860.2780.2750.0135Zn0.010.010.0080.010.0130.010.0100.00216Ga0000000.0000.000/Ge0<=0.005<=0.0150.002<=0.015<=0.0160.0010.001141As0.0070.0080.0070.0070.0070.0070.0070.0006Br0.0010.0020.0010.0010.0020.0010.0010.00139Se0.0060.0080.0120.0040.0110.0080.0080.00337Rb0000000.0000.000/Sr0000.001000.0000.000245Y00000.00300.0010.001245Zr0000000.0000.000/Nb0000000.0000.000/Mo0.0030.0030.0050.0030.0040.0040.0040.00122Ru0.00100.0010000.0000.001155Rh0.0010.0010.0020.0010.0010.0020.0010.00139Pd0.0010.0020.0020.0020.0030.0020.0020.00132Ag10.76810.04110.89410.51811.1110.23910.5950.4064Cd0.0050.0020.010.0070.0030.0080.0060.00352In0.0170.0150.0180.0170.0230.0150.0180.00317Sn000000.0010.0000.000245Sb0.0040.0020.0050.0040.0040.0040.0040.00126I0000000.0000.000/Te0.0640.0690.0610.0510.050.050.0580.00814Cs0000000.0000.000/Ba0000000.0000.000/La0000000.0000.000/Ce0000000.0000.000/Pr0000000.0000.000/Nd00.00100000.0000.000245Sm0000000.0000.000/Eu0000000.0000.000/Gd0000000.0000.000/Tb0000000.0000.000/Dy0000000.0000.000/Ho0000000.0000.000/Er0000000.0000.000/Tm0000000.0000.000/Yb0.001000000.0000.000245Lu00.00300000.0010.001245Hf0000000.0000.000/Ta0.0110.0090.010.0110.0110.0120.0110.00110W0000.003000.0010.001245Re0000000.0000.000/Os0000000.0000.000/Ir0000000.0000.000/Pt00.00100000.0000.000245Au0.0090.010.010.0090.010.0090.0100.0016Hg0.0220.0250.0260.0170.020.0290.0230.00419Tl0.0140.0130.0