GBT 24194-2024 硅铁 多元素含量的测定 电感耦合等离子体原子发射光谱法

CCSH11硅铁多元素含量的测定电感耦合等离子体原子发射光谱法国家标准化管理委员会国家市场监督管理总局发布国家标准化管理委员会IGB/T24194—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。本文件代替GB/T24194—2009《硅铁铝、钙、锰、铬、钛、铜、磷和镍含量的测定电感耦合等离子体原子发射光谱法》,与GB/T24194—2009相比，除结构调整和编辑性改动外，主要技术变化如下：b)增加了甘露醇试剂(见5.7);c)更改了试料量(见8.2,2009年版的7.2);d)更改了试样溶液的制备(见8.4.1,2009年版的7.4.1);e)更改了校准曲线溶液的制备(见8.4.2,2009年版的7.4.2);f)增加了结果的表示(见9.2);g)用重复性限和再现性限替代了允许差(见第10章，2009年版的第9章)。请注意本文件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：鄂尔多斯市西金矿冶有限责任公司、武汉钢铁有限公司、青岛远诚创智科技有限公司、内蒙古鄂尔多斯电力冶金集团股份有限公司、乌兰察布市产品质量计量检验检测中心、内蒙古工业大学、广东中色研达新材料科技股份有限公司、宁夏科通新材料科技有限公司、青海百通高纯材料开发有限公司、天津精一仪器仪表有限公司、青海华晟铁合金冶炼有限责任公司、冶金工业信息标准研究院。本文件于2009年首次发布，本次为第一次修订。1GB/T24194—2024硅铁多元素含量的测定电感耦合等离子体原子发射光谱法警告——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。的测定。各元素测定范围见表1。分析元素测定范围(质量分数)/%FeAlMnPNiMgVNbPbB2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。2GB/T24194—2024GB/T4010铁合金化学分析用试样的采取和制备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数字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/T12807实验室玻璃仪器分度吸量管GB/T12808实验室玻璃仪器单标线吸量管GB/T36244电感耦合等离子体原子发射光谱仪JJG768发射光谱仪本文件没有需要界定的术语和定义。4原理准溶液制作的校准曲线计算出分析元素质量分数。5试剂分析中除另有说明外，仅使用认可的分析纯试剂和符合GB/T6682规定的二级及以上蒸馏水或与其纯度相当的水。5.6盐酸，1+3。5.8标准溶液5.8.1铁标准溶液称取1.0000g金属铁(质量分数大于99.95%)于250mL烧杯中，加入40mL盐酸(1+1),低温加丙烯或聚乙烯的专用试剂瓶中。此溶液1mL含1000.0μg铁。分取10.00mL铁标准贮备溶液(5.8.1.1)于200mL容量瓶中，加入10mL盐酸(1+1),用水稀释3GB/T24194—20245.8.2铝标准溶液a)称取1.0000g金属铝(质量分数大于99.95%)于250mL聚四氟乙烯烧杯中，加入30mL盐聚丙烯或聚乙烯的专用试剂瓶中。b)称取1.0000g金属铝(质量分数大于99.95%)于250mL聚四氟乙烯烧杯中，加入30mL氢分取10.00mL铝标准贮备溶液(5.8.2.1)于200mL容量瓶中，加入10mL盐酸(1+1),用水稀释此溶液1mL含50.0μg铝。5.8.3钙标准溶液称取2.4973g先于105℃±5℃干燥并于干燥器中冷却至室温的碳酸钙(质量分数大于99.99%)于250mL烧杯中，加20mL水，混匀。盖上表皿，小心滴加盐酸(1+1)至碳酸钙溶解，再加入20mL丙烯或聚乙烯的专用试剂瓶中。分取10.00mL钙标准贮备溶液(5.8.3.1)于200mL容量瓶中，加入10mL盐酸(1+1),用水稀释5.8.4锰标准溶液称取1.0000g电解锰[质量分数大于99.95%,预先用硝酸(1+3)洗净表面氧化膜，再放入无水乙醇中洗4次～5次，取出，自然干燥后放在干燥器中12h以上]置于250mL烧杯中，加入30mL硝酸于聚丙烯或聚乙烯的专用试剂瓶中。此溶液1mL含1000.0μg锰。或聚乙烯的专用试剂瓶中。4GB/T24194—20245.8.5铬标准溶液5.8.5.1铬标准贮备溶液，1000.0pg/mL称取1.0000g金属铬(质量分数大于99.95%)于250mL烧杯中，加入50mL盐酸(1+1),滴加过分取10.00mL铬标准贮备溶液(5.8.5.1)于100mL容量瓶中，加入10mL盐酸(1+1)用水稀释至刻度，混匀，贮于聚丙烯或聚乙烯的专用试剂瓶中。分取5.00mL铬标准贮备溶液(5.8.5.1)于100mL容量瓶中，加入10mL盐酸(1+1)用水稀释至刻度，混匀，贮于聚丙烯或聚乙烯的专用试剂瓶中。5.8.6钛标准溶液称取0.5000g金属钛(或海绵钛，质量分数大于99.9%)于100mL铂皿或聚四氟乙烯烧杯中，加入10mL氢氟酸和20mL硫酸(1+1)溶解，加热蒸发至冒硫酸烟，用水冲洗铂皿或聚四氟乙烯烧杯，继续加热至冒硫酸烟使氟驱尽。冷却至室温，加约50mL水溶解盐类，移入1000mL容量瓶中，用硫酸(1+9)洗净铂皿或聚四氟乙烯烧杯，洗液合并于容量瓶中，并用硫酸(1+9)稀释至刻度，混匀，贮于聚丙烯或聚乙烯的专用试剂瓶中。此溶液1mL含500.0μg钛。分取20.00mL钛标准贮备溶液(5.8.6.1)于100mL容量瓶中，用硫酸(5+95)稀释至刻度，混匀，贮于聚丙烯或聚乙烯的专用试剂瓶中。分取10.00mL钛标准贮备溶液(5.8.6.1)于100mL容量瓶中，用硫酸(5+95)稀释至刻度，混匀，贮于聚丙烯或聚乙烯的专用试剂瓶中。5.8.7磷标准溶液称取2.1968g预先经105℃±5℃干燥至恒量并冷却至室温的基准磷酸二氢钾(KH₂PO₄),置于300mL烧杯中，用适量水溶解，煮沸，冷却，移入1000mL容量瓶中，用水稀释至刻度，混匀，贮于聚丙烯或聚乙烯的专用试剂瓶中。分取20.00mL磷标准贮备溶液(5.8.7.1)于100mL容量瓶中，用水稀释至刻度，混匀，贮于聚丙烯或聚乙烯的专用试剂瓶中。5GB/T24194—2024乙烯的专用试剂瓶中。此溶液1mL含20.0μg磷。5.8.8铜标准溶液称取0.5000g金属铜(质量分数大于99.95%)于250mL烧杯中，加20mL硝酸(1+1),低温加热丙烯或聚乙烯的专用试剂瓶中。硝酸(1+1),用水稀释至5.8.9镍标准溶液称取0.5000g金属镍(质量分数大于99.95%)于250mL烧杯中，加20mL硝酸(1+1),低温加热聚乙烯的专用试剂瓶中。分取10.00mL镍标准贮备溶液(5.8.9.1)于100mL容量瓶中，加硝酸(1+1),用水稀释至此溶液1mL含50.0pg镍。5.8.10镁标准溶液称取0.5000g金属镁(质量分数大于99.95%)于500mL烧杯中，加20mL盐酸(1+1),加热溶解，冷却至室温，移入1000mL容量瓶中，用水稀释至刻度，混匀，贮于聚丙烯或聚乙烯的专用试剂瓶中。分取10.00mL镁标准贮备溶液(5.8.10.1)于100mL容量瓶中，加10mL盐酸(1+1),用水稀释至5.8.11钒标准溶液称取0.8926g预先在105℃±5℃烘干4h置于干燥器中的光谱纯五氧化二钒于250mL烧杯中，加20mL盐酸(1+1),滴加过氧化氢(p,1.10g/mL)加热溶解，煮沸，冷却至室温，移入1000mL容6GB/T24194—2024分取10.00mL钒标准贮备溶液(5.8.11.1)于100mL容量瓶中，加10mL盐酸(1+1),用水稀释至此溶液1mL含50.0μg钒。5.8.12铌标准溶液称取0.1431g经研钵研细并在105℃±5℃烘干2h的光谱纯五氧化二铌(Nb₂O₅)于150mL石英坩埚中，加入3g焦硫酸钾，搅拌均匀后再覆盖1g焦硫酸钾，于600℃加热熔融，冷却，加入20mL聚乙烯的专用试剂瓶中。此溶液1mL含10.0μg铌。5.8.13铅标准溶液称取0.1600g硝酸铅于250mL烧杯中，加20mL水，5mL硝酸(1+1)溶解，移入1000mL容量分取10.00mL铅标准贮备溶液(5.8.13.1)于100mL容量瓶中，用水稀释至刻度，混匀，贮于聚丙烯或聚乙烯的专用试剂瓶中。5.8.14锑标准溶液称取0.2740g酒石酸锑钾(C₄H₄KO₇Sb·1/2H₂O)于250mL烧杯中，加20mL盐酸(1+4)溶解，移入1000mL容量瓶中，用盐酸(1+9)稀释至刻度，混匀，贮于聚丙烯或聚乙烯的专用试剂瓶中。分取10.00mL锑标准贮备溶液(5.8.14.1)于100mL容量瓶中，用盐酸(1+9)稀释至刻度，混匀，贮于聚丙烯或聚乙烯的专用试剂瓶中。5.8.15锆标准溶液称取0.353g氧氯化锆(ZrOCl₂·8H₂O)于250mL烧杯中，加40mL盐酸(1+4)溶解，移入1000mL容量瓶中，用盐酸(1+9)稀释至刻度，混匀，贮于聚丙烯或聚乙烯的专用试剂瓶中。分取20.00mL锆标准贮备溶液(5.8.15.1)于100mL容量瓶中，用盐酸(1+9)稀释至刻度，混匀，贮于聚丙烯或聚乙烯的专用试剂瓶中。7GB/T24194—20245.8.16硼标准溶液称取2.8611g预先经105℃±5℃干燥至恒量并冷却至室温的基准试剂硼酸于250mL烧杯乙烯的专用试剂瓶中。烯或聚乙烯的专用试剂瓶中。聚乙烯的专用试剂瓶中。5.8.17钇标准溶液称取1.2699g三氧化二钇(质量分数大于99.9%,预先经1000℃灼烧1h),置于500mL烧杯中，加入50mL盐酸(1+1),加热溶解，冷却至室温，移入1000mL容量瓶中，用水稀释至刻度，混分取10.00mL钇标准溶液(5.8.17.2)于100mL容量瓶中，加入5mL盐酸(1+1),用水稀释至刻此溶液1mL含10.0μg钇。5.9可使用有证系列元素标准溶液及由有证元素系列标准溶液稀释而成的元素系列标准溶液。5.10纯铁(质量分数大于99.98%或分析元素含量已知)。规定。6.2电感耦合等离子体(ICP-AES)原子发射光谱仪。可以使用任何型号的电感耦合等离子体原子发射光谱仪，仪器应符合GB/T36244和JJG768的要求。电感耦合等离子体原子发射光谱仪的性能试本文件不指定特殊的分析谱线，推荐使用表2的分析谱线。使用时，应根据仪器特点仔细检查谱线的背景校正位置以及光谱干扰情况。GB/T24194—2024元素波长/nm可能干扰元素元素波长/nm可能干扰元素Fe248.327252.285Ni231.604221.647Al396.152394.401Mg279.553280.27Mn279.482V280.280393.366317.933V309.311310.23Mg309.299Ca310.236Mn257.610279.827Nb309.418313.079V309.420Ti313.081357.869283.563—Pb216.999220.353Cu216.953Nb220.317334.941336.121Cr334.932Ni336.156217.581206.833P213.618Cu213.598339.198343.823Cr339.143324.754223.008Ti223.022B208.955208.893Mo208.952Y224.306324.228371.0307取样和制样8分析步骤对同一试样，至少独立测定2次。8.2试样量按表3称取试样，精确至0.0001g。试样量/g检测范围0.2000I组，适用于高硅硅铁、普通硅铁和低铝硅铁的常规元素0.5000Ⅱ、Ⅲ组，适用于高纯硅铁、硼元素的测定89GB/T24194—2024称取相当于试样量中铁含量的纯铁(5.10),精准至0.001g,纯铁的称样量见表4,随同试样做空白试验。表4试样量及纯铁量试样量/g称取纯铁的量/g注1:检测高硅硅铁中杂质时不加纯铁。注2:对于PGFeSi65、PGFeSi40牌号的硅铁，根据待测样品中相当的铁含量计算称量纯铁的量。慢滴加约5mL氢氟酸(5.2),至激烈反应停止，加入5mL盐酸(5.6),轻轻小幅度摇动，低温加热至试样溶解完全。加入5mL高氯酸(5.3),低温加热至冒高约2mL～3mL溶液，取下，稍冷，加入20mL盐酸(5.6),加热溶解盐类，冷却至室温。将试液移入100mL聚四氟乙烯或石英容量瓶中，用水稀释至刻度，混匀。如果用内标法测量，在稀释之前，加入将试样(见表3)置于200mL聚四氟乙烯烧杯中，用聚乙烯吸量管或刻度聚乙烯滴管准确加入5mL氢氟酸(5.2),加入5mL甘露醇(5.7),缓慢滴加10mL硝酸(5.1),反应比较剧烈，每次滴加硝酸反应缓慢后再小幅度转动聚四氟乙烯烧杯，直至试样完全溶解至溶液清亮，室温放置30min。将溶液移入100mL聚四氟乙烯容量瓶中，用水稀释至刻度，混匀。如用内标法测量，在稀释之前，加入用相当于试样中铁含量(见表4)的纯铁7份(5.10)代替试样，分别置于200mL聚四氟乙烯烧杯中，按8.4.1步骤将其溶解，冷却至室温，将溶液转移至100mL聚四氟乙烯容量瓶中，按表5、表6和GB/T24194—2024表7加入被测元素的校准溶液。校准溶液的浓度范围要覆盖所分析元素的浓度范围，某一校准溶液中各分析元素不应都是最高或最低，每一校准曲线需要由5点(含5点)以上校准溶液组成，并成合适梯次灵敏线或者适当稀释试样溶液和校准溶液。如果用内标法，用移液管加5.00mL钇标准溶液(5.8.17.3),用水稀释至刻度，混匀。在校准曲线系列溶液中，应使共存元素的量与样品溶液中此共存元素的量相当，包括被测元素以外的共存元素。表5制作校准曲线的标准溶液I组元素标准溶液V——100mL容量瓶中加入标准溶液的体积/mLc——标准溶液稀释后的浓度/(μg/mL)序号浓度/(μg/mL)体积或浓度012345铁5.8.1.1V00.602.006.00C06.0020.0030.0050.0060.00铝5.8.2.1V00.602.006.00C06.0020.0030.0050.0060.00钙5.8.3.1V00.602.006.00C06.0020.0030.0050.0060.00锰5.8.4.2V02.004.006.00C02.004.006.00铬5.8.5.2V02.004.006.00C02.004.006.00钛5.8.6.2V02.004.006.00C02.004.006.00磷5.8.7.320.0V02.006.00C00.200.400.60注1:铁元素仅适用于高硅硅铁中铁含量的检测。注2:本表中校准曲线对应的浓度范围是待测试样量为0.2000g的待测元素的含量范围。表6制作校准曲线的标准溶液Ⅱ组元素标准溶液V-——100mL容量瓶中加入标准溶液的体积/mLc——标准溶液稀释后的浓度/(μg/mL)序号浓度/(μg/mL)体积或浓度012345铝V0C0元素标准溶液V—--100mL容量瓶中加入标准溶液的体积/mLc——标准溶液稀释后的浓度/(μg/mL)序号浓度/(μg/mL)体积或浓度012345钙5.8.3.2V00.502.0025.00C00.252.50锰5.8.4.3V00.502.0020.00C00.252.50铬5.8.5.3V00.502.00C00.250.502.50钛5.8.6.3V00.502.00C00.250.502.50磷5.8.7.2V00.502.004.00C00.252.002.505.8.8.2V00.200.502.00C00.100.252.50镍5.8.9.2V00.200.502.00C00.100.252.50镁5.8.10.2V00.2020.00C00.100.502.50钒5.8.11.2V00.1020.00C00.050.502.50铌5.8.12.2V00.5020.00C00.050.100.502.00铅5.8.13.2V00.502.00C00.050.100.200.300.50锑5.8.14.2V00.502.00C00.050.100.200.300.50锆5.8.15.220.0V02.00C00.200.402.00注：本表中校准曲线对应的浓度范围是待测试样量为0.5000g的待测元素的含量范围。GB/T24194—2024表7制作校准曲线的标准溶液Ⅲ组元素标准溶液V———100mL容量瓶中加入标准溶液的体积/mLc——标准溶液稀释后的浓度/(μg/mL)序号浓度/(μg/mL)体积或浓度012345硼5.8.16.3V020.00C00.100.300.502.00注：本表中校准曲线对应的浓度范围是待测试样量为0.5000g的待测元素的含量范围。开启ICP光谱仪，检查仪器状态，点火后确认仪器运行参数在确定范围内，雾化系统及等离子火焰测量最浓的校准溶液，按照仪器操作说明对仪器工作条件进行优化，调节仪器参数，选择合适的分如果使用内标，准备用Y(371.03nm)作内标并计算每个元素与钇的强度比的软件，内标强度应与分析物强度同时测量。如测量Ⅲ组溶液，需使用耐氢氟酸的雾化器。准备工作曲线绘制、测量及统计计算等软件。开启点火键，点火后确认仪器运行参数在确认范围内，雾化系统及等离子火焰工作正常，稳定数分钟。开始用最低浓度校准溶液(零号相当于空白试验),再按顺序吸入校准溶液，在每次吸入溶液之间吸入去离子水或稀硝酸溶液。至少重复测量2次，取两个读数的平均值。以被测元素浓度为横坐标，光谱强度为纵坐标作图，以最小二乘法作线性回归，得到校准曲线。计算相关系数，相关系数应大于0.999。在与8.4.4.1相同条件下测量空白试液和试样溶液的光谱强度，每次测量之间吸入去离子水冲洗，至少重复测量2次。取两个读数的平均值，计算机采集所测定的试样溶液中待测元素的净强度，由校准曲线计算出各元素的含量结果。9结果的计算及表示9.1结果的计算 (1)GB/T24194—2024V——校正和试验溶液的最终体积，单位为毫升(mL);9.2结果的表示同一试样两次独立测定的分析结果差值的绝对值不大于重复性限r,则取算数平均值作为分析结果。如果两次独立测定的分析结果差值的绝对值大于重复性限r,则按照附录B的规定追加测定次数数值修约按GB/T8170的规定进行。元素测定范围(质量分数)/%重复性限r/%再现性限R/%R=0.0618m+0.0233r=0.0261m+0.0009r=0.0309m+0.0109R=0.0937m+0.0061r=0.0456m+0.0013r=0.0448m+0.0008Pr=0.0461m+0.0008R=0.0883m+0.0016R=0.2156m+0.0001r=0.0456m+0.0008VB注：式中m是分析元素的含量(质量分数),%。在重复性条件下，获得的两次独立测试结果的绝对差值不大于重复性限(r),大于重复性限(r)的情况不超过5%。GB/T24194—2024在再现性条件下，获得的两次独立测试结果的绝对差值不大于再现性限(R),大于再现性限(R)的情况不超过5%。试验报告应包括以下内容：a)实验室名称和地址；b)试验报告的签发日期；g)在测定过程中注意到的任何特性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GB/T24194—2024(规范性)电感耦合等离子体光谱仪的性能试验A.1目的本附录中给出的性能试验目的在于使用不同类型的仪器对等离子体光谱仪的性能进行适当的测定，允许不同的仪器使用不同的操作条件，但等离子体光谱仪最终能产生一致的结果。制定利用电感耦合等离子体原子发射光谱(ICP-AES)分析标准方法。A.2校准溶液制备3份溶液，含待测物浓度水平分别为0浓度水平(0×DL)、10倍检测限(10×DL)、1000倍检测限(1000×DL)的校准溶液，这些溶液中要含有与待测样品相似溶度的酸、溶剂和基体元素(铁元素)。制备校准的检出限(DL)值可以参考实验室值或表3中的值。A.3程序和操作按仪器说明书和实验室的定量分析的实践经验对等离子体原子发射光谱仪进行最初的调节。吸入1000倍检测限的校准溶液，在溶液进入等离子体后等待10s,以保证稳定雾化。对待测元素设定操作和仪器条件，将选择的波长定位在最高峰处，选择适当的光电倍增管(对于非自动选择的设备),保证测到的光强度为4位有效数字，设定积分时间为3s。吸入空白试液约10s,以预设积分时间测定10次。吸入10倍检测限试液约10s,以预设积分时间测定10次。吸入1000倍检测限试液约10s,以预设积分时间测定10次。A.4背景等效浓度(BEC)和检测限的确定由空白试液和10倍检测限溶液的平均强度、10倍检测限溶液的浓度和10次空白强度的标准偏M=c₂/(I₂—Ib)…………………(A.1)式中：M——分析曲线的斜率；I₂——10倍检测限溶液10次原始强度的平均值；Ib——空白溶液10次原始强度的平均值。式中：DL=3S,M…………………(A.3)式中：Sb——10次空白强度读数的标准偏差。注：由于重复测量次数有限，按此方法计算出的检测限的范围较宽。GB/T24194—2024A.5短期精度(RSD)由1000倍检测限溶液10次原始平均强度(I₃)与空白溶液10次原始平均强度(I₆)按式(A.4)计算1000倍检测限溶液的净平均强度(IN₃)。IN₃=I₃Ib…………(A.4)式中：IN₃——1000倍检测限溶液(1000×DL)的净平均强度；I₃———1000倍检测限溶液10次原始强度的平均值。RSD是元素浓度为1000倍检测限溶液的估计值。按式(A.5)计算1000倍检测限溶液(1000×DL)的净强度相对标准偏差。………………(A.5)式中：S₃——1000倍检测限溶液10次强度读数的标准偏差。GB/T24194—2024(规范性)试样分析结果接受程序流程见图B.1。分析结果分析结果X,X₂否再次测定是X否Xra-xrl≤1,3否μ=中位值(X₁,X,X₃,X4)u=X+₂+X₃+X是是图B.1试样分析结果接受程序流程图(资料性)精密度试验原始数据各元素的精密度试验原始数据见表C.1～表C.16。表C.1Fe精密度试验原始数据水平j实验室i12345678912.8812.7002.6892.6982.6962.8052.7312.7302.7242.9572.7302.7042.7152.6962.8722.7352.6802.6982.8162.7112.7012.7062.6962.8382.7212.7602.715232.1872.1502.0902.1352.0642.2092.1452.1302.1422.1852.1702.1252.1322.0642.2922.1462.1002.1342.1792.1552.1352.1432.0642.1632.1312.1602.14040.9550.9600.9540.9670.9420.9510.9490.9670.9670.9590.9610.9530.9600.9460.9450.9460.9660.9680.9470.9600.9590.9610.9510.9420.9550.9640.96850.6620.6610.6590.65806560.6670.6580.6660.6580.6710.6610.6610.6590.6680.6660.6590.6630.6620.6700.6580.6630.6560.6630.6690.6640.6620.662表C.2AI精密度试验原始数据水平j实验室123456789123表C.2Al精密度试验原始数据(续)水平j实验室i12345678940.6180.6210.6000.6150.6110.6010.6110.6200.5990.6170.6260.6100.6220.6110.5980.6140.5800.6110.6140.6230.6000.6180.6110.5900.6120.6000.6105672.1582.1912.1132.1322.1002.0792.1822.1702.1212.1712.2022.1282.1422.1002.0962.1602.1802.1232.1772.1802.1392.1362.1002.0992.1762.2402.12582.4822.5112.4082.4432.4202.4132.4692.5002.4232.4272.5092.4282.4522.4202.4012.4982.3802.4252.4602.5002.4252.4362.4202.4002.4682.5002.42992.7772.8162.7182.7392.7402.6902.7592.7602.7152.8012.8072.7292.7422.7402.6912.7802.7202.7162.7992.8302.7342.7312.7402.6482.7612.6702.7210.00990.01000.01010.00950.00950.01090.00890.00970.00980.00980.01000.00990.00940.00940.01060.00940.00950.00920.00950.01000.01060.00930.00940.00980.00930.01000.00960.02320.02300.02480.02230.02600.02290.02170.02300.02430.02380.02400.02390.02310.02600.02360.02190.02370.02250.02270.02300.02330.02360.02600.02210.02180.02390.02290.05350.05600.05440.05260.05800.05070.05130.05200.05300.05320.05500.05400.05210.05800.05200.05050.05250.05150.05260.05200.05350.05120.05800.04980.05090.05300.05230.07310.07700.07440.07240.07400.07200.06930.07200.07230.07180.08000.07480.07200.07400.07120.06920.07300.07220.07250.08100.07550.07160.07400.06930.06930.07250.07150.04540.04700.04610.04480.04600.04430.04210.04510.04500.04510.04900.04500.04560.04600.04440.04230.04600.04430.04440.04500.04550.04420.04600.04550.04190.04580.0447GB/T24194—2024表C.2Al精密度试验原始数据(续)水平j实验室i1234567890.01100.01000.01290.01080.01210.01130.01070.01220.01070.01080.01000.01240.01140.01150.01030.00960.01100.01090.01100.01100.01230.01020.01110.01040.01050.01180.01l1表C.3Ca精密度试验原始数据水平j实验室i12345678910.55500.58200.61100.61500.56800.59300.58000.63000.60800.57200.58200.59800.61100.56800.59200.58900.610-00.59600.55000.57700.60200.60600.56800.57800.59000.59000.595020.32900.320.00.31800.33600.32600.33500.32900.32000.33800.32700.32400.31500.33300.32600.33700.33300.35500.34600.33900.32200.31200.33100.32600.33100.33100.33000.327030.32500.30500.30100.31100.35000.31800.32200.31000.32300.32600.30900.30200.32100.35000.31500.31600.31000.31500.32800.30500.33200.31800.35000.30800.32200.32000.320040.22500.22000.20000.20500.22600.21800.21400.22700.20100.22700.21800.22000.20800.22600.22000.21600.21000.19800.22800.21800.20000.21200.22600.20200.21500.24000.1970560.52600.52200.51000.48400.50800.49600.51100.53000.47100.52500.52100.50000.49200.50800.49500.51100.50000.47800.52600.51800.51000.48700.50800.44400.51000.55000.476072.15802.02802.00002.04602.02202.00402.10002.02102.14902.03602.01002.05202.05602.060.02.02502.17102.03302.13002.03802.06002.00202.10002.019082.48502.64802.46002.46602.37902.48802.49902.51002.39902.47802.66502.45002.47302.37902.48502.52902.40002.41702.53902.66002.44002.46102.37902.43502.49802.53002.4230GB/T24194—2024表C.3Ca精密度试验原始数据(续)水平j实验室i12345678990.64400.61600.60000.61900.62300.61800.61100.61400.59800.64000.61400.60000.61200.62200.59700.62100.61000.59700.63600.61400.60000.60900.62200.54700.61700.63000.59900.00860.01100.00980.01130.01090.01120.00950.01100.01120.00860.01000.00990.01100.01120.01270.00860.01120.01100.00890.01100.01050.01080.01120.01060.00920.01150.01130.01360.01300.01700.01380.01390.01500.01350.01400.01350.01200.01300.01560.01400.01440.01660.01180.01450.01370.01280.01400.01510.01320.01360.01460.01240.01430.01340.08850.08600.07900.08290.08350.08120.07800.08300.07920.09070.08600.08540.08260.08360.08120.07780.08350.07950.09070.08300.08250.08140.08380.08460.07800.08410.07960.03390.03300.03200.03410.03500.03260.03090.03400.03470.03390.03500.03600.03360.03500.03370.03050.03550.03420.03370.03400.03700.03280.03500.03160.03070.03450.03410.03830.03700.03480.03490.03370.03770.03450.03510.03350.04040.03600.03590.03510.03420.03690.03220.03600.03370.03770.03500.03550.03420.03350.03130.03320.03700.03390.00150.00100.00100.00120.00110.00140.00080.00110.00120.00120.00100.00110.00130.00120.00140.00150.00160.00120.00160.00100.00110.00120.00110.00120.00160.00130.0012表C.4Mn精密度试验原始数据水平j实验室i12345678910.03850.03900.03990.03820.04200.03700.03440.03900.03670.037.80.03870.03980.03870.04200.03850.03510.04010.03740.03840.03880.03580.03790.04200.03350.03470.03710.037320.01730.01880.01480.01520.01640.01590.01510.01530.01540.01700.01850.01440.01550.01640.01590.01460.01690.01530.01690.01860.01500.01620.01650.01340.01520.01510.0156表C.4Mn精密度试验原始数据(续)水平j实验室i12345678930.02140.02260.020.50.02220.02260.02210.02080.02180.02180.02200.02310.02180.02240.02250.02160.02020.02350.02150.02250.02310.02090.02210.02250.02550.02060.02170.021640.04520.05080.05000.04650.04660.04780.04770.04770.04680.04450.05100.05000.04720.04680.04800.04770.04450.04690.04400.05090.05000.04760.04670.04300.04780.04550.047450.20760.22070.22580.21400.19700.21300.21100.20600.21500.20730.22120.22140.21800.19500.20700.21200.20000.21600.20750.22020.20150.21200.19800.18800.21100.19000.205060.29600.32860.30000.30200.30200.29900.30500.29800.30100.29720.32880.30000.30400.30100.29900.30600.280-00.30500.29760.32870.30000.30100.30200.27200.30600.280-00.304070.21640.24850.20000.23800.20100.22200.22400.23000.22400.21940.23730.20000.23600.20300.22000.22200.23000.21900.21880.24230.22000.23200.20200.20900.22300.230-00.225080.29310.32540.30000.30900.29900.29700.29600.290-00.29700.29030.328.20.29000.30700.30000.29700.29600.28000.30500.28980.32550.30000.30200.29900.29400.29800.29400.301090.13110.14080.13000.13400.13000.13100.13100.13000.13500.13200.14130.13000.14200.13100.13200.13600.13000.13600.13050.14120.12800.13800.13100.12700.13200.12000.13100.08710.08720.08500.08360.08100.08340.08280.08400.08430.08580.08740.08610.08290.08100.08210.08300.08600.08410.08770.08770.08590.08390.08100.09020.08290.08400.08400.05670.05940.04890.05380.05350.05330.05280.05500.05560.05640.05820.04990.05290.05340.05330.05370.05800.05570.05740.05850.05120.05340.05380.05100.05340.05700.05580.05520.05610.04910.05390.05200.05140.05060.05200.05210.05500.05710.05240.05440.05210.05190.05060.05360.05240.05480.05660.05540.05480.05210.04980.05070.05350.05230.04890.04820.04200.04520.04560.04490.04440.04700.04620.04660.04780.04800.04560.04570.04430.04450.04500.04590.04750.04810.04800.04480.04560.04310.04440.04640.0458表C.4Mn精密度试验原始数据(续)水平j实验室i1234567890.07830.07530.07780.07410.07080.07320.07220.07510.07450.07780.07710.07640.07520.07060.07410.07110.07700.07470.07880.07700.07610.07460.07090.07170.07160.07800.07490.14890.15780.14500.14300.14300.15100.14400.14900.15100.14930.15870.14800.14800.14300.14900.14400.14000.15000.14810.15840.14500.14000.14300.14500.14600.14500.1500表C.5Cr精密度试验原始数据水平j实验室i12345678910.01370.01310.00730.00930.00900.014.50.01320.00880.01340.01390.01310.00750.00950.00900.01440.01320.00830.01280.01380.01300.00760.00960.00900.01410.01280.00760.012920.00510.00490.00300.00550.00510.00700.00510.00280.00400.00510.00520.00270.00510.00470.00640.00430.00310.00370.00480.00510.00300.00530.00490.00620.00460.00270.003930.00960.00890.00390.01020.00650.01020.00990.00530.00820.00960.00930.00400.00980.00660.01010.00970.00580.00880.00960.00940.00380.00960.00620.00990.00990.00600.008740.00370.00280.00350.00310.00260.00340.00300.00340.00250.00410.00270.00370.00330.00260.00350.00310.00390.00230.00390.00260.00310.00330.00260.00280.00320.00370.002450.07340.06770.08150.08380.06780.07220.07200.06820.06590.07260.06760.08510.08340.07060.07070.07250.07210.06420.07230.06740.08410.08260.06880.07190.07250.06880.065360.29770.29960.29800.29800.27700.26700.29500.27900.29500.29140.29960.29100.30100.27700.26500.29800.27100.29600.30140.29970.29540.29400.27800.24800.29600.28200.298070.02690.02100.02080.02240.02240.02150.02360.02290.02070.02560.02180.02030.02190.02250.02180.02360.02330.02100.02400.02160.02180.021]0.02260.021.50.02360.02240.0208表C.5Cr精密度试验原始数据(续)水平j实验室i12345678980.08110.08060.07020.07680.07200.07430.08110.07870.07600.08090.07850.07890.07720.07200.07510.08160.07800.07650.07930.07800.07580.07610.07200.07240.08090.07750.074990.04580.04670.04490.04350.04210.04520.04400.04570.03850.04540.04490.04400.04420.04230.04460.04420.04400.03860.04030.04610.04510.04460.04230.03900.04430.04540.03820.00860.00870.00910.00900.00830.00900.00910.00920.00930.00820.00860.01010.00910.00810.00870.00940.00980.00920.00880.00870.01020.00890.00820.00760.00920.00850.00930.00620.00680.00690.00730.00740.00840.00790.00740.00770.00660.00680.00680.00720.00740.00730.00770.00750.00750.00620.00670.00650.00710.00750.00670.00780.00800.00730.00650.00670.00810.00690.00730.00720.00760.00710.00720.00620.00680.00750.00700.00730.00730.00750.00800.00710.00700.00660.00720.00690.00740.00640.00760.00810.00720.00710.00710.00780.00800.00690.00790.00740.00780.00760.00710.006.80.00790.00780.00690.00800.00730.00850.00770.00650.00740.00840.00790.00690.00620.00720.00750.00750.00780.00770.01020.00890.00810.00880.00840.00910.00930.00860.00770.00950.00870.00820.00850.00850.00950.00920.00830.00780.00910.00880.00820.00670.00840.00980.00920.07510.07700.07200.07780.07800.07700.08080.07810.07560.07520.07930.07560.07720.07760.07890.07930.07620.07570.07260.078.80.07980.07680.07840.06910.07940.07330.0755表C.6Ti精密度试验原始数据水平j实验室i1234567891表C.6Ti精密度试验原始数据(续)水平j实验室i12345678920.09140.08650.08240.08740.08510.08780.08530.08330.085.60.09010.09000.08380.08820.08510.08540.08580.08800.08430.09150.08880.08400.08690.08510.08060.08550.08520.086330.11870.11520.12090.11700.11400.11400.11000.11000.11400.11940.11600.12160.11400.11400.11300.11100.11800.11500.11720.11550.12040.11200.11400.10100.11100.11200.113040.03950.03890.03870.03920.04090.03800.03900.03910.03970.03870.03920.03800.040.60.04090.03860.03920.03650.03940.03980.03910.03560.03980.04090.03530.03910.03720.039550.13480.12660.13010.13200.13300.12500.13400.12700.13000.13390.12740.12980.13400.13300.12600.13300.12000.13500.13360.12740.13240.13100.13300.11300.13400.12000.133060.11210.10940.11320.10200.11200.10300.10900.10800.10900.11130.11030.11280.10400.1l100.10300.10900.10000.10800.11160.11120.11270.10300.11100.09030.11000.11000.110070.12020.12330.11790.11400.11800.11600.12100.12000.11900.12110.120.70.11850.11600.11900.11500.12100.12000.11700.12250.12200.11840.11500.11900.10700.12000.12000.118080.08110.20140.18650.18800.19600.19400.20000.19500.20100.08090.20320.18770.18700.19700.18900.19700.19000.19700.07930.20370.18710.18900.19500.17700.19800.19600.201090.25420.25220.24890.24200.24900.24300.24200.25000.25600.25950.25230.24920.23900.24800.24300.24800.24000.25700.25840.25190.24950.24400.24800.21600.24600.24000.24900.00770.00830.00790.00760.00760.00730.00730.00810.00780.00770.00780.00850.00740.00760.00740.00740.00850.00790.00760.00810.00800.00750.00760.00580.00740.00890.00760.01900.01890.01920.01870.02010.01770.01810.01900.01870.01920.01840.01980.01910.02010.01810.01810.01800.01890.01930.01870.01910.01810.02010.01540.01810.02100.01860.02410.02310.02540.02360.02390.02230.02260.02400.02270.02380.02380.02490.02410.02390.02210.02250.02500.02290.02390.02330.02430.02330.02390.01980.02270.02400.0227表C.6Ti精密度试验原始数据(续)水平j实验室i1234567890.02910.02770.02890.02810.02850.02610.02710.02900.02810.02900.02760.02810.02870.02850.02720.02720.03000.02830.02900.02770.02880.02730.02850.02370.02750.03100.02790.05010.04620.04790.04590.04770.04670.04600.04900.04790.05040.04680.04910.04650.04770.04580.04650.05200.04830.05050.04660.04990.04690.04770.04420.04620.04850.04820.02670.02680.02500.02640.02840.02600.02590.02720.02730.02670.02680.02690.02740.02840.02590.02580.02680.02710.02680.02660.02670.02720.02840.02350.02590.02670.0270表C.7P精密度试验原始数据水平j实验室i12345678910.02670.02680.02500.02640.02840.02600.02590.02720.02730.026.70.02680.02690.02740.02840.02590.02580.02680.02710.02680.02660.02670.02720.02840.02350.02590.02670.027020.00740.00730.00680.00770.00730.00810.00580.00700.00730.00710.00790.00690.00760.00730.00880.00640.00760.00720.00750.00770.00690.00780.00730.00730.00630.00740.007030.01020.00810.00960.01010.00820.01060.00810.00990.00860.01040.00800.00960.01020.00820.00960.00740.01030.00890.01080.00800.00980.00990.00820.00990.00800.00950.009340.02150.01920.01850.01840.01990.01920.01850.01910.01910.02280.01970.01800.01810.01970.01850.01810.01880.01940.01880.01940.01890.01920.01900.01770.01870.01990.019050.03090.03230.02980.03180.03010.03020.02950.03220.03050.03270.03100.03250.03220.03100.02970.02950.03100.02960.03130.03110.03080.03120.03030.02900.02950.03180.030460.02730.02370.02510.02290.02140.02250.02180.02500.02090.02540.02300.02410.02300.02170.02170.02190.02250.02130.02530.02290.02400.02240.02190.02160.02190.02440.0221表C.7P精密度试验原始数据(续)水平j实验室i12345678970.02390.02480.02180.02280.02310.02300.02240.02400.02180.02510.02440.02090.02300.02300.02310.02280.02300.02220.02560.02470.02110.02230.02270.02330.02260.02440.022880.02410.02950.02580.02610.02740.02720.02670.02940.02630.02470.02810.02680.02700.02650.02760.02660.02670.02670.02290.02850.02660.02660.02630.02540.02670.02770.026590.02080.02370.02010.02000.02100.02080.02080.02170.02040.02010.02200.02080.02100.02140.02190.02000.02110.02050.02020.02330.02100.02140.02070.02070.02050.02200.02110.01170.01030.00950.00980.00940.00930.00940.00970.00960.01120.00990.01010.01000.00930.00870.00940.00920.00950.01160.01010.00990.00990.00940.00850.00940.01000.00970.00890.00850.00800.00910.00810.00790.00750.00850.00850.00830.00900.00820.00920.00800.00740.00730.00890.00800.00910.00880.00840.00910.00810.00850.00740.00920.00830.00950.00870.00910.00850.00780.00910.00670.00830.00810.01000.00850.00840.00840.00790.00720.00710.00850.00820.01020.00890.00810.00860.00790.00710.00710.00890.00810.00740.00820.00740.00820.00760.00730.00700.00810.00780.00930.00890.00790.00810.00760.00770.00680.00850.00790.00890.00820.00750.00790.00760.00810.00590.00900.00760.02770.02880.02450.02640.02440.02560.02480.02500.02500.02690.02850.02560.02520.02420.02840.02540.02600.02520.02810.02840.02490.02730.02440.02710.02520.02700.02530.01490.01410.01570.01380.01260.01450.01260.01400.01360.01340.01430.01510.01400.01240.01390.01240.01490.01370.01460.01410.01520.01270.01260.01290.01280.01430.0136GB/T24194—2024表C.8Cu精密度试验原始数据水平j实验室i12345678910.00630.00800.00790.00790.00810.00700.00700.00780.00800.00630.00740.00780.00810.00810.00730.00710.00830.00810.00610.00780.00780.00810.00690.00740.00800.008020.00200.00250.00320.00280.00230.00240.00240.00280.00300.00200.00250.00350.00290.00230.00240.00230.00320.00310.00190.00250.00310.00280.00230.00200.00250.00300.003230.00190.00230.00280.00250.00220.00220.00220.00240.00240.00140.00240.00290.00260.00220.00210.00210.00270.00230.00170.00240.00280.00240.00220.00190.00220.00240.002340.02300.02770.02810.02950.02990.02630.02720.02590.02810.02320.03120.02850.02910.02990.02700.02740.02700.02840.02350.02890.02780.03020.02990.02500.02730.02640.028250.02410.02920.02950.03210.03110.02800.02830.02730.03010.02390.02880.02990.03180.03110.02820.02830.02740.03050.02450.02910.03010.03140.03110.02700.02830.02810.030660.06890.07830.07190.06220.08200.07490.07350.07140.07200.06870.07970.07250.06180.08200.07330.07290.07370.07210.06860.07920.07280.06200.08210.07350.07340.07290.072570.01860.01900.01810.01840.01830.01830.01840.01810.01990.01880.01990.01870.01850.01830.01830.01830.01660.02010.01880.01970.01890.01830.01810.01610.01840.01770.020580.07990.09230.08110.07180.09590.08790.08670.08430.08270.08020.09000.08160.07200.09600.08680.08720.08940.08310.08080.09110.08140.07230.09590.08170.08710.08620.083290.03540.04390.04100.03100.04430.04010.03980.03980.04000.03570.04200.04080.03100.04420.04040.03980.04010.04030