GB-T 43901-2024 镍铁 砷、锡、锑、铅和铋含量 电感耦合等离子体质谱法（ICP-MS）

ICS77.100CCSH11中华人民共和国国家标准GB/T43901—2024电感耦合等离子体质谱法(ICP-MS)国家市场监督管理总局国家标准化管理委员会ⅠGB/T43901—2024本文件按照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》的规定起草。请注意本文件的某些内容可能涉及专利。本文件的发布机构不承担识别专利的责任。本文件由中国钢铁工业协会提出。本文件由全国生铁及铁合金标准化技术委员会(SAC/TC318)归口。本文件起草单位:山西太钢不锈钢股份有限公司、广东邦普循环科技有限公司、青岛博正检验技术有限公司、广东中南钢铁股份有限公司、内蒙古新太实业集团有限公司、石家庄创谱科技有限公司、青岛德泓谨信科技有限公司、吉铁铁合金有限责任公司、河北津西国际贸易有限公司、冶金工业信息标准研究院。1GB/T43901—2024电感耦合等离子体质谱法(ICP-MS)警告—使用本文件的人员应有正规实验室工作的实践经验。本文件并未指出所有可能的安全问题。使用者有责任采取适当的安全和健康措施,并保证符合国家有关法规规定的条件。1范围本文件描述了镍铁中砷、锡、锑、铅和铋含量的电感耦合等离子体质谱法分析方法。本文件适用于镍铁中砷、锡、锑、铅和铋含量的测定。各元素的测定范围见表1。表1元素及测定范围元素测定范围(质量分数)/%As0.0005~0.01Sn0.0002~0.009Sb0.0002~0.01Pb0.0001~0.008Bi0.00004~0.00352规范性引用文件下列文件中的内容通过文中的规范性引用而构成本文件必不可少的条款。其中,注日期的引用文件,仅该日期对应的版本适用于本文件;不注日期的引用文件,其最新版本(包括所有的修改单)适用于本文件。GB/T6379.1测量方法与结果的准确度(正确度与精密度)第1部分:总则与定义GB/T6379.2测量方法与结果的准确度(正确度与精密度)第2部分:确定标准测量方法重复性与再现性的基本方法GB/T6682分析实验室用水规格和试验方法GB/T8170数值修约规则与极限数值的表示和判定GB/T12806实验室玻璃仪器单标线容量瓶GB/T12808实验室玻璃仪器单标线吸量管GB/T25050镍铁锭或块成分分析用样品的采取GB/T25051镍铁颗粒成分分析用样品的采取3术语和定义本文件没有需要界定的术语和定义。2GB/T43901—20244原理试料用稀硝酸分解,以氩等离子体为离子化源,使用电感耦合等离子体质谱仪测定砷、锡、锑、铅和铋,测定时以钇作为内标元素(亦可采用其他合适的内标元素或混合内标)进行校正。5试剂除非另有说明,在分析中仅使用各待测元素质量分数均低于0.0001%的高纯试剂和高纯水(符合GB/T6682中实验室用水一级水规格,同时电阻率不小于18MΩ/cm)。在分析中使用的标准溶液可以按本文件规定的方法配制,也可采用市售的有证溶液标准物质/标准样品。5.1高纯镍。砷、锡、锑和铅元素质量分数均小于0.0001%,铋元素质量分数小于0.00004%。5.2高纯铁。砷、锡、锑和铅元素质量分数均小于0.0001%,铋元素质量分数小于0.00004%。5.3盐酸,ρ≈1.19g/mL。5.4硝酸,ρ≈1.42g/mL。5.5氢氟酸,ρ≈1.15g/mL。5.6盐酸溶液(1+1)。5.7硝酸溶液(1+1)。5.8硝酸溶液(1+3)。5.9盐酸溶液(1+9)。5.10硝酸溶液(1+9)。5.11砷标准储备溶液,1mg/mL。称取1.0000g单质砷(质量分数不小于99.99%),置于300mL烧杯中,慢慢加入50mL硝酸溶液(5.7),低温加热溶解后,转至1000mL容量瓶中,以水稀至刻度,混匀。此溶液1mL含1mg砷。5.12锡标准储备溶液,1mg/mL。称1.0000g金属锡(质量分数不小于99.99%),移入一个300mL烧杯中,加入50mL盐酸溶液(5.6),加热溶解,冷至室温,转移入1000mL容量瓶中,用盐酸溶液(5.9)稀释至刻度,混匀。用水稀释至刻度,混匀。此溶液1mL含1mg锡。5.13锑标准储备溶液,1mg/mL。称取1.0000g金属锑(质量分数不小于99.99%),加50mL盐酸(5.3)微热溶解后,转至1000mL容量瓶中,以水稀至刻度,混匀。此溶液1mL含1mg锑。5.14铅标准储备溶液,1mg/mL。称取1.0000g金属铅(质量分数不小于99.99%),置于300mL烧杯中,慢慢加入50mL硝酸溶液(5.7),煮沸,赶尽氮氧化物,冷却后移入1000mL容量瓶中,用水稀释至刻度,混匀。此溶液1mL含1mg铅。5.15铋标准储备溶液,1mg/mL。称取1.0000g金属铋(质量分数不小于99.99%),置于300mL烧杯中,慢慢加入50mL硝酸溶液(5.7),加热溶解,取下稍冷,移入1000mL容量瓶中,用硝酸溶液(5.10)稀释至刻度,混匀。此溶液1mL含1mg铋。5.16混合标准溶液A,砷、锡、锑和铅元素各10μg/mL,铋元素5μg/mL。分别移取10.00mL砷标准储备溶液(5.11)、锡标准储备溶液(5.12)、锑标准储备溶液(5.13)、铅标准储备溶液(5.14);移取5.00mL铋标准储备溶液(5.15)于一个1000mL容量瓶中。加入20mL硝酸(5.4),用水稀释至刻度,混匀。此溶液1mL含砷、锡、锑、铅元素各10μg,含铋元素为5μg。3GB/T43901—20245.17混合标准溶液B,砷、锡、锑、铅元素各1μg/mL,铋元素0.5μg/mL。分别移取10.00mL混合标准溶液A(5.16)于一个100mL容量瓶中,加入2mL硝酸(5.4),用水稀释至刻度,混匀。此溶液1mL含砷、锡、锑和铅元素各1μg,含铋元素为0.5μg。5.18钇标准溶液。a)钇标准储备溶液,1mg/mL。称取0.1270g纯氧化钇(Y2O3质量分数不小于99.99%),置于300mL烧杯中,加入20mL硝酸溶液(5.7),待完全溶解后,冷却,移入100mL容量瓶中,用水稀释至刻度,混匀。此溶液1mL含1mg钇。b)钇标准溶液,100μg/mL。移取10.00mL钇标准储备溶液[5.18a)]于一个100mL容量瓶中,加入2mL硝酸(5.4),用水稀释至刻度,混匀。此溶液1mL含钇100μg。c)钇标准溶液,1μg/mL。移取10.00mL钇标准溶液[5.18b)]于一个1000mL容量瓶中,加入20mL硝酸(5.4),用水稀释至刻度,混匀。此溶液1mL含钇1μg。5.19钇内标溶液,50ng/mL。移取50.00mL钇标准溶液[5.18c)]于一个1000mL容量瓶中,用水稀释至刻度,加入20mL硝酸(5.4),混匀。此溶液1mL含钇50ng。5.20镍基体溶液,10mg/mL。称取1.0g高纯镍(5.1),精确至0.001g,置于300mL烧杯中,加入50mL硝酸溶液(5.7),待完全溶解后,冷却,移入100mL容量瓶中,用水稀释至刻度,混匀。此溶液1mL含10mg镍。5.21铁基体溶液,10mg/mL。称取1.0g高纯铁粉(5.2),精确至0.001g,置于300mL烧杯中,加入50mL硝酸溶液(5.7),待完全溶解后,冷却,移入100mL容量瓶中,用水稀释至刻度,混匀。此溶液1mL含10mg铁。5.22氩气,纯度大于99.99%。6仪器和设备6.1实验室玻璃仪器GB/T12808规定的A级。所有玻璃器皿应用盐酸溶液(5.9)清洗,然后再用水洗净。6.2电感耦合等离子体质谱仪6.2.1测定同位素的推荐参数配备有磁扇式电感耦合等离子质谱仪(高分辨电感耦合等离子质谱仪)或四极杆电感耦合等离子质谱仪(低分辨电感耦合等离子质谱仪)或飞行时间电感耦合等离子质谱仪。依据仪器使用说明书建立分析程序,按照表2选择待测元素和内标元素的测定同位素。砷、锡、锑、铅和铋的同位素丰度及干扰见附录C。4GB/T43901—2024表2各元素测定同位素的推荐质量数、内标元素的同位素质量数、丰度元素测定同位素及质量数丰度%As75As100Sn118Sn24.3120Sn32.4Sb121SbPb208PbBi209Bi100Y(内标)89Y100在仪器最佳工作条件下,凡能达到6.2.2和6.2.3指标者均可使用。6.2.2最小精度(RSD)测量浓度为10ng/mL或5ng/mL的待测元素的基体匹配标准溶液,计算连续10次测量结果的相对标准偏差,最小精度(RSD)应不超过5%。6.2.3检出限(LOD)和定量限(LOQ)检出限(LOD)和定量限(LOQ)定义分别如式(1)和式(2)。LOD=4.65×σ×…………(1)LOQ=14.1×σ×…………(2)式中:σ—测量10次空白溶液强度的标准偏差;Cs—标准溶液的浓度,单位纳克每毫升(ng/mL);Xs—测量10次标准溶液的平均强度;Xb—测量10次空白溶液的平均强度。测量基体和酸度与试液一致的空白溶液10次,计算各元素检出限和定量限。砷元素的检出限应小于0.8ng/mL,定量限应小于2.4ng/mL。锡、锑、铅元素的检出限应小于0.3ng/mL,定量限应小于0.9ng/mL。铋元素的检出限应小于0.1ng/mL,定量限应小于0.3ng/mL。7取样和样品制备7.1按照GB/T25050或GB/T25051的规定取样。7.2实验室样品通常以钻、铣或磨加工而成,屑、粉或颗粒状样品不需再加工。注1:如怀疑在钻、铣或磨过程中样品沾上油或油脂,用高纯度丙酮清洗后晾干。注2:如实验室样品粒度不均匀,测试样品采用分样器缩分出来。5GB/T43901—20248分析步骤8.1试料称取0.10g试样(7.2),精确至0.0001g,置于150mL锥形瓶中。8.2测定次数对同一个试样至少进行两次独立分析。8.3空白试验随同试料做空白试验。空白试验应使用相当于试料中的镍和铁量的高纯镍(5.1)和高纯铁(5.2)的代替试料。8.4试液的制备将称有试料(8.1)的锥形瓶中加入10mL硝酸溶液(5.8),低温加热至完全溶解,冷却至室温,转移至100mL的容量瓶中,用水稀释至刻度,混匀。此溶液为待测试液。注1:高硅试样可加3滴~5滴氢氟酸(5.5)助溶。有些高碳样品可能会有残余碳不溶,定容100mL后用快速滤纸干过滤。注2:如使用离线内标校正法,则在空白和试样溶液稀释至刻度前加入5.00mL的钇标准溶液[5.18c)]。8.5校准系列溶液的配制按照样品含镍量的高低分别配置不同镍和铁比例的三组标准系列,每组制备1份校准空白溶液和5份校准标准溶液。每组分别将约50mL水加入6个100mL容量瓶中,按表3加入镍基体溶液、铁基体溶液、多元素混合标准溶液,加入硝酸(5.4)2.0mL,用水稀释至刻度,混匀。表3多元素混合校准空白溶液和校准溶液镍铁牌号(含镍量)加入镍基体溶液量(5.20)mL加入铁基体溶液量(5.21)mL加入多元素混合标准溶液B(5.17)mL校准系列溶液中元素浓度ng/mL校准系列溶液中铋元素浓度ng/mLFeNi20、FeNi30(含镍量15%~35%)2.57.50002.57.50.5052.52.57.51.001052.57.52.50252.57.55.0050252.57.510.00100506GB/T43901—2024表3多元素混合校准空白溶液和校准溶液(续)镍铁牌号(含镍量)加入镍基体溶液量(5.20)mL加入铁基体溶液量(5.21)mL加入多元素混合标准溶液B(5.17)mL校准系列溶液中元素浓度ng/mL校准系列溶液中铋元素浓度ng/mLFeNi40、FeNi50(含镍量35%~60%)5.05.00005.05.00.5052.55.05.01.001055.05.02.50255.05.05.0050255.05.010.0010050FeNi70(含镍量60%~80%)7.03.00007.03.00.5052.57.03.01.001057.03.02.50257.03.05.0050257.03.010.00100508.6测定根据待测镍铁样品的含镍量,选择合适镍和铁比例的校准系列溶液(见表3)。待电感耦合等离子体质谱仪运行稳定后,于待测元素和内标元素质量数处(见表2),依次测定标准系列溶液(按8.5配制)、空白试液(按8.3制备)、分析试液(按8.4制备)中待测元素和内标元素的离子流信号强度。以标准溶液中待测元素的质量浓度为横坐标,待测元素与内标元素的离子流信号强度比值为纵坐标,绘制校准曲线。各元素校准曲线相关系数应在0.9990以上,否则需重新进行校准或重新配制标准溶液进行标准化。测量试液中的待测元素的信号强度,减去空白试验溶液的强度即为净强度,由工作曲线查得待测元素的浓度,以ng/mL计。9分析结果计算及表示9.1分析结果的计算按式(3)计算待测元素含量(ωM),以质量分数(%)表示。ωM=×100…………(3)式中:ρ—由校准曲线得到的元素质量浓度,单位为纳克每毫升(ng/mL);V—试液体积,单位为毫升(mL);m—试料质量,单位为克(g)。7GB/T43901—20249.2分析结果的确定与表示同一试样两次独立分析结果差值的绝对值不大于重复性限,则取算术平均值作为分析结果。如果两次独立分析结果差值的绝对值大于重复性限,则按照附录A的规定追加测量次数并确定分析结果。分析结果按GB/T8170修约,保留两位有效数字。10精密度精密度试验是2022年由10个实验室对11个镍铁样品中的砷、锡、锑、铅和铋5个元素进行测定。样品信息参见附录B中的表B.1。精密度试验原始数据见附录B的表B.2~表B.6。各实验室对每个样品测试3次。在GB/T6379.1定义的可重复性条件下进行两次测定,第3次测定是使用同一台仪器在不同时间,在新的校准之后进行的。按照GB/T6379.2的规则对共同精密度试验得到的结果数据进行统计处理。各元素含量与试验结果的重复性限、室内再现性和再现性限的函数关系式见表4。表4精密度函数关系式元素水平范围/%重复性/%室内再现性/%再现性/%As0.0005~0.01lgr=0.7373lgm-1.8188lgRw=0.6250lgm-1.9201lgR=0.7764lgm-1.1591Sn0.0002~0.009lgr=0.7114lgm-2.1515lgRw=0.7500lgm-1.8152lgR=0.7366lgm-1.3063Sb0.0002~0.01lgr=0.6713lgm-2.0387lgRw=0.7960lgm-1.4395lgR=0.5474lgm-1.7219Pb0.0001~0.008lgr=0.7461lgm-1.9415lgRw=0.8185lgm-1.5183lgR=0.7215lgm-1.2785Bi0.00004~0.0035lgr=0.6947lgm-1.9802R=0.1029m+0.000015lgR=0.7360lgm-1.3256由精密度函数关系式计算得出的各元素均匀分布含量的重复性限、再现性限值见表5。表5均匀分布含量的重复性限(r)和再现性限(Rw和R)元素m/%r/%Rw/%R/%As0.00050.0000560.000100.000190.00100.0000930.000160.000320.00300.000210.000320.000760.00500.000310.000440.00110.00700.000390.000540.00150.00900.000470.000630.00180.0100.000510.000680.0019Sn0.00020.0000160.0000260.0000930.00050.0000320.0000510.0001830.00100.0000520.0000860.0003050.00300.000110.000200.000680.00500.000160.000290.00100.00700.000210.000370.00130.00900.000250.000450.00158GB/T43901—2024表5均匀分布含量的重复性限(r)和再现性限(Rw和R)(续)元素m/%r/%Rw/%R/%Sb0.00020.000030.000040.000180.00050.000060.000090.000300.00100.000090.000150.000430.00300.000190.000360.000790.00500.000260.000540.001040.00700.000330.000700.001250.00900.000390.000860.001440.0100.000420.000930.00153Pb0.00010.0000120.0000120.000070.00050.0000390.0000480.000220.00100.0000660.0000860.000360.00200.000110.000160.000590.00400.000190.000280.000980.00600.000250.000390.00130.00800.000310.000500.0016Bi0.000040.0000090.0000190.0000270.000100.0000170.0000250.0000540.000500.0000530.0000660.000180.00100.0000860.000120.000290.00200.000140.000220.000490.00300.000180.000320.000660.00350.000210.000380.00074在重复性限(r)条件下,获得的两次独立测试结果的绝对差值不大于重复性限(r),以大于重复性限(r)的情况不超过5%为前提。在室内再现性限(Rw)条件下,获得的两次独立测试结果的绝对差值不大于室内再现性(Rw),以大于室内再现性(Rw)的情况不超过5%为前提。在再现性限(R)条件下,获得的两次独立测试结果的绝对差值不大于再现性限(R),以大于再现性限(R)的情况不超过5%为前提。11试验报告试验报告应包括下列内容:a)实验室的名称和地址;b)试验报告的签发日期;c)本文件编号;d)识别试样必要的细节;9GB/T43901—2024e)分析结果;f)结果的编号;g)在测定过程中观察到的异常现象和本文件中没有规定的可能对试样和认证标准物质的结果产生影响的任何操作。10GB/T43901—2024附录A(规范性)试验结果接受程序流程图试验结果接受程序流程图如图A.1所示。标引符号说明:r—重复性限;X—分析值。图A.1试验结果接受程序流程图2424附录B(资料性)精密度试验原始数据共同精密度样品信息如表B.1所示。精密度试验原始数据见表B.2~表B.6。表B.1共同精密度试验样品信息%(质量分数)试样编号牌号NiAssnsbPbBiCsiPsCrCoCuNiFe-1FeNi2014.350.00240.00120.00030.00400.00351.731.390.0230.0732.291.940.094NiFe-216.810.00200.000730.00970.000140.000440.02060.01460.00490.02090.04690.3790.040NiFe-320.00.000560.000120.000220.000190.000220.00150.00170.00070.00090.00020.00020.0005NiFe-423.570.000930.00250.00340.00330.00301.4561.9030.00660.05050.750.7150.003NiFe-5FeNi3025.680.00290.00090.00090.000420.000221.162.900.0240.2651.171.560.094NiFe-634.090.00960.00610.00970.00610.00230.1680.4810.01620.00650.300.6250.04NiFe-735.80.00600.00510.00560.00220.00240.02080.02250.00490.1090.0320.800.088NiFe-8FeNi4041.60.01070.00650.000750.00540.00140.01110.01850.01480.06850.02510.8060.112NiFe-942.980.00250.00060.00170.00060.000040.0530.740.00940.0180.520.530.019NiFe-10FeNi5061.340.01040.00870.001480.00790.00110.0050.0030.0070.100.010.900.19NiFe-11FeNi7079.970.002240.000490.000880.000740.000850.0020.00250.00270.00050.00010.00070.001411GB11GB/T43901—20GBGB/T43901—202412表B.2砷(As)元素精密度试验原始数据12%(质量分数)水平j测定次数n实验室i1234567891011230.001720.001710.001730.003590.003730.003890.003110.003110.003050.002320.002280.000530.003790.003860.003930.003370.003430.003540.002760.002700.002680.002340.002350.002460.002170.002210.0021121230.002050.002070.001950.002110.002090.002470.001910.001970.001760.001770.001830.001350.002220.002270.002200.001920.001860.001750.002050.002100.002210.001770.001980.001980.001820.001850.001760.001860.001790.0018231230.0004880.0004550.0005180.000878b0.000920b0.000797b0.0005310.0004950.0005440.0005700.0005460.0005720.0005980.0006060.0006000.0005750.0005820.0005930.000895b0.000909b0.000888b0.0006010.0005770.0006780.0005300.0005450.0005000.0005430.0005900.00054541230.0005020.0004890.0004930.001480.001340.001510.0009150.0009140.0009840.001260.001240.001110.0004350.0004300.0004260.001120.001000.001060.001440.001380.001310.0007890.0007630.0008360.0008660.0009120.0009810.0006670.0006490.00068451230.002900.002840.002860.003940.003870.003860.003280.003260.003280.004080.004050.003610.002480.002420.002430.003220.003380.003310.003950.003900.003810.003050.003140.002910.00281a0.002560.002610.0025961230.009210.009270.009030.009220.009390.009820.009770.009470.009640.009890.009770.00990.01010.01040.01030.009220.009190.008920.009570.009490.009720.009980.009730.01000.008640.008510.008850.009840.009960.0098871230.005940.005930.005820.006240.006500.006560.005590.005930.005740.005880.005820.006010.005880.005790.005700.006350.006450.006390.006380.006460.006550.006090.005730.005880.005670.005680.005370.005730.005680.005762424表B.2砷(As)元素精密度试验原始数据(续)%(质量分数)水平j测定次数n实验室i1234567891081230.008470.008370.008260.01190.01210.01250.01130.01120.01100.01120.01040.01070.01170.01150.01150.01150.01090.01160.01080.01100.01160.01160.01160.01080.01000.01010.01040.009030.009120.0090591230.002840.002890.002710.003630.003560.003480.002630.002590.002590.00221b0.00184b0.00268b0.002430.002300.002250.003110.002930.003090.003490.003560.003610.003160.002880.002940.002620.002710.002570.003020.003170.00321101230.01050.01040.01030.01110.01120.01090.01010.01050.01020.01010.01020.01010.01040.01020.01020.01080.01090.01010.01060.01080.01010.01020.01070.01020.009640.009650.009890.01030.01040.0107111230.001930.001920.002150.002460.002440.002680.002070.002140.002260.002190.002160.002240.002130.002250.002070.001930.002070.002040.002430.002390.002510.002380.002410.002210.002340.002450.002560.002410.002370.00244a数据为歧离值。b数据为离群值。13GB13GB/T43901—20GBGB/T43901—202414表B.3锡(sn)元素精密度试验原始数据14%(质量分数)水平j测定次数n实验室i1234567891011230.001060.001120.001080.001280.001260.001250.001180.001170.001130.001290.001340.001480.0009860.0009970.0009910.001050.001150.001010.001130.001080.001160.001290.001280.001240.001360.001330.001220.001450.001460.0013421230.001010.0009930.001050.0006890.0006920.0007040.0007400.0007540.0007070.0008040.0007900.0008190.0007280.0007270.0007270.0002650.0002860.0002760.0007070.0006980.0006890.0007390.0007410.0007430.0008770.0008930.0008460.00101b31230.0001420.0001310.0001520.0001540.0001560.0001510.0001300.0001250.0001300.0001920.0001970.0001920.0001100.0001190.0001090.0001470.0001580.0001620.0001600.0001560.0001450.0001350.0001250.0001050.0002050.0002100.0001780.0001850.0001600.00016641230.002230.002180.002210.002520.002510.002580.002490.002460.002340.002670.002750.002670.002960.002910.002870.002060.002080.001970.002570.002510.002400.002370.002470.002460.002760.002890.003020.002480.002450.0024451230.0009240.0009210.0009590.0009410.0009430.0009630.0009190.0009120.0008580.001110.001080.001090.000289b0.000277b0.000273b0.0008770.0008960.0009020.0009620.0009490.0009650.0009830.0009710.0009180.00102b0.00109b0.0008630.0008500.00084361230.005980.006130.006210.005970.006010.005900.006230.006270.006080.006250.006230.006390.006090.006150.006130.006110.006240.006160.005790.005880.005970.005620.005660.006050.006330.006420.006590.006370.006410.0063871230.004890.004990.005070.005310.005330.005540.005170.005330.004840.005020.005120.005190.005230.005110.005050.004860.005010.004960.005230.005180.005350.004600.004630.004780.005660.005690.005370.004990.004950.005012424表B.3锡(sn)元素精密度试验原始数据(续)%(质量分数)水平j测定次数n实验室i1234567891081230.006880.006870.006730.006070.005990.006160.006960.006940.006980.006680.006470.006430.007100.007010.006980.00444a0.00620b0.00624b0.00531b0.006800.006700.006950.007140.007210.007000.006220.006310.0063791230.0006810.0006810.0006450.0006790.0007010.0007270.0005830.0006020.0006160.0006640.0006390.0006400.0005170.0005020.0004950.0005710.0005810.0005950.0007110.0007060.0006920.0007080.0006560.0006760.0006440.0006510.0006870.0005920.0005800.000579101230.009080.009100.009260.008690.008620.008590.008550.008510.008820.008270.008290.008480.008950.009050.008870.009190.008990.009060.008980.008860.008840.008670.008720.008790.009470.009230.009690.007580.007500.00747111230.0005110.0005080.0005140.0005800.0005880.0005690.0004960.0004900.0005010.0005420.0005360.0005520.0004840.0005030.0004900.0005010.0005230.0004990.0005720.0005610.0005890.0005210.0005110.0004940.000586b0.000623b0.000692b0.0004730.0004780.000487a数据为歧离值。b数据为离群值。15GB15GB/T43901—20GBGB/T43901—202416表B.4锑(sb)元素精密度试验原始数据16%(质量分数)水平j测定次数n实验室i1234567891011230.0004230.0003960.0004090.000733b0.000728b0.000570b0.0004240.0004070.0003750.0004090.0004270.0004800.0002200.0002310.0002260.0004650.0004540.0004460.0006330.0006410.0006530.0006010.0006140.0006030.0003920.0003880.0003530.0003530.0003460.00034921230.01030.01020.01000.009910.009910.009900.009580.009690.009080.01000.009880.009860.0122b0.0124b0.01000.009860.009890.009800.009720.009870.009070.009330.009630.009350.009210.009140.009510.009690.0097231230.0002560.0002430.0002240.000303b0.000355b0.000493b0.0002490.0002320.0002610.0002450.0002180.0002340.0001380.0001450.0001330.0001790.0001960.0001930.0003330.0003450.0003630.0002550.0002640.0002840.0001910.0002210.0002410.0002290.0002380.00022941230.003020.002910.003180.003710.003620.003310.003550.003560.003410.003750.003930.003750.004100.004020.003960.003170.003270.003380.003380.003490.003550.002690.003090.002780.003050.003220.003450.003130.003060.0030551230.0009870.0009710.0009930.001090.001160.001210.0009670.0009470.0008580.001020.0009710.001030.000273b0.000282b0.000277b0.0008280.0008250.0007990.001050.001120.001180.001230.001100.001140.0008570.0008470.0008960.0008610.0008710.00084661230.009830.01000.01010.009130.009060.009570.01090.01080.01010.00586b0.0114b0.01050.01080.01060.008770.008670.008560.009230.009360.009410.008490.008630.009560.009730.009780.009460.01020.01030.010271230.005090.004920.005070.005660.005690.005530.00453b0.00557b0.005750.005860.005690.005790.005860.005910.005420.005540.005690.005760.005770.006580.005260.005410.005630.005280.005240.005362424表B.4锑(sb)元素精密度试验原始数据(续)%(质量分数)水平j测定次数n实验室i1234567891081230.0007210.0007040.0007310.001000.001020.0009430.0007920.0007870.0008000.0006940.0006050.0007350.0007050.0006920.0006890.001000.001090.0009890.0007690.0007430.0009670.0007710.0007590.0007890.0007180.0007030.00070791230.002010.002080.002110.002290.002210.002090.001710.001850.001860.001430.001210.001800.001450.001510.001360.001790.001860.001710.002240.002170.002250.001580.001630.002090.001770.001730.001680.001830.001820.00178101230.001770.001740.001810.001550.001530.001320.001580.001620.001660.001550.001570.001550.001080.001140.001010.001510.001670.001640.001280.001370.001450.001260.001390.001680.001560.001540.001620.001300.001390.00132111230.0009750.0009430.0009240.001100.001070.001030.0008920.0009040.0009300.0008960.0008460.0008800.000332b0.000344b0.000327b0.0009050.0008970.0009140.001040.001010.001080.0009290.0009360.0009270.0009040.0009130.0009740.0009530.0009380.000949a数据为歧离值。b数据为离群值。17GB17GB/T43901—20GBGB/T43901—202418表B.5铅(pb)元素精密度试验原始数据18%(质量分数)水平j测定次数n实验室i1234567891011230.004120.004240.004130.003890.003840.004120.003930.003890.004000.00487b0.00529b0.00559b0.004480.004410.004450.003950.004210.004160.003750.003680.003890.004130.003990.004390.004020.003970.003840.003890.003900.0038621230.0001780.0001840.0001560.0001660.0001680.0001750.0001130.0000970.0001110.0001410.0001430.0001470.0000820.0000850.0000830.0000960.0000980.0001020.0001780.0001690.0001800.0001300.0001080.0001000.0000950.0001130.0001340.0002310.0002600.00024131230.0002720.0003100.0002860.0003540.0003440.0003660.0002000.0001880.0001970.0003150.0003100.0003140.0002410.0002470.0002370.0001900.0001760.0001810.0003650.0003620.0003560.0001960.0002210.0001970.0002470.0022500.0002350.0002620.0002780.00026941230.003310.003380.003270.002910.002920.002850.003380.003230.003160.003130.003190.003250.002880.002890.002920.002980.003170.003400.003110.003110.003340.003330.003410.0032951230.0004470.0004540.0004320.0004730.0004790.0005110.0004000.0003980.0003700.000698b0.000615b0.000652b0.0002650.0002750.0002710.0004320.0004250.0004190.0004790.0004720.0004880.0003260.0003190.0003280.000532b0.000497b0.000424b0.0004580.0004440.00043561230.006090.006280.006150.005500.005460.005190.006160.006490.006610.007190.007170.007470.006050.005940.006010.006390.006150.006260.005470.005530.005390.005290.005270.006140.005470.005670.005990.006460.006510.0064971230.001980.002070.002160.002040.002040.001980.002260.002380.002170.002630.002500.002610.001880.001980.001910.002260.002160.002310.002140.002110.002250.001780.001920.002130.002170.002060.001860.002270.002320.002202424表B.5铅(pb)元素精密度试验原始数据(续)%(质量分数)水平j测定次数n实验室i1234567891081230.005260.004980.005110.005080.005130.005340.006130.006120.006030.005580.005490.005300.005930.006010.005890.005420.005210.005340.005080.005010.005150.00623b0.00606b0.00721b0.004930.004960.005120.005550.005470.0055791230.0007150.0007250.0006910.0006050.0006110.0005880.0005610.0005510.0005630.0006570.0006490.0006450.0005870.0005990.0005820.0005960.0006050.0005830.0006010.0005960.0006110.0006470.0006270.0006760.000711b0.000678b0.000614b0.001490.001380.00135101230.00807b0.008770.008770.009160.007850.007730.008090.007310.007430.007450.008050.008160.008000.008860.008690.008790.008650.008710.008770.007970.008110.008170.006350.006450.006540.006430.006500.00658111230.0007000.0006930.0007570.0007010.0007140.0006770.0007330.0007340.0007430.0007320.0007060.0007240.0006240.0006330.0006240.0007370.0007470.0007360.0007010.0006920.0007090.0008680.0008380.0007520.0006640.0006680.0007150.0007630.0007520.000764a数据为歧离值。b数据为离群值。19GB19GB/T43901—20GBGB/T43901—202420表B.6铋(Bi)元素精密度试验原始数据20%(质量分数)水平j测定次数n实验室i1234567891011230.003210.003330.003180.003480.003440.003660.003340.003310.003440.00400b0.00441b0.00450b0.003830.003760.003710.00406a0.003530.003600.003720.003430.003320.003620.003260.003340.003490.003420.003400.0033921230.0004730.0005280.0004560.0004630.0004640.0005010.0004220.0004390.0004150.0004850.0004840.0005140.0003870.0003750.0003700.0004090.0004080.0003920.0005100.0005020.0004970.0005010.0004640.0004610.0003640.0003620.0003700.0004550.0004410.00044031230.0002000.0001780.0002200.0002440.0002410.0002570.0002280.0002160.0002250.0002400.0002360.0002420.0001840.0001960.0001810.0002580.0002450.0002350.0002650.0002540.0002430.0002300.0002470.0002300.0001920.0001830.0001680.0002330.0002230.00022341230.003060.003020.003160.002950.002960.003030.002940.0