《锑铍芯块化学分析方法 第4部分：铝、铅、铁、锰、镁含量的测定 电感耦合等离子体原子发射光谱法》编制说明(送审稿)

縁锻芯块化学分析方法第4部分：铝、铅、铁M孟、镁含量的测定

电感耦合等离子体原子发射光谱法编制说明（送审稿）西北稀有金属材料研究院宁夏有限公司2023.7锦皱芯块化学分析方法第4部分：铝、铅、铁、镒、镁含量的测定

电感耦合等离子体发射光谱法

编制说明一、工作简况（-）任务来源根据2022年4月29日工业和信息化部发布的《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[2022]94号）的要求，有色金属行业标准《锡钺芯块化学分析方法第4部分：铝、铅、铁、铭、镁含量的测定电感耦合等离子体原子发射光谱法》修订项目由全国有色金属标准化技术委员会负责归口，由西北稀有金属材料研究院宁夏有限公司负责起草，该项目计划编2O22-O23OT-YS,项目周期为18个月,完成年限为2023年10月。（二） 项目背景掃編芯块作为核工业用二次中子源部件及压水堆燃料元件，其用途不可替代。铝、铅、铁、铭、镁为锡繊芯块产品中需要重点检测的5种杂质元素，对产品性能影响至关重要，其含量要求铝不大于0.05%,铅和镐不大于0.04%,铁不大于0.10%,镁不大于0.02%,实现这—范围是保障锡編芯块产品性能的基本前提，因此精准检测锡編芯块中铝、铅、铁、钻、镁元素含量具有重要意义。目前，YS/T426.4-2000《锡編芯块化学分析方法原子吸收光谱法测定铅、铁、铭、镁量》及YS/T426.3-2000《锡钺芯块化学分析方法8劣基喳啡分光光度法测定铝量帥作业过程均需要化学分离除去锡基体，步骤较为复杂，容易带入试剂污染，造成分析方法不稳定,且方法步骤冗长，耗费较多人力及时间。随着产品工艺进步及检测设备更新，产品杂质含量变低，设备检测能力提高，运用电感耦合等离子体原子发射光谱法，采用标准加入法消除基体干扰，无需分离锡基体，可同时测定铝、铅、铁、铭、镁5种元素，一并替代流程复杂的YS/T426.3-2000（比色法）及YS/T426.4-2000（原子吸收光谱法），大幅度提高工作效率。相比于原标准的原子吸收光谱法及分光光度法，电感耦合原子发射光谱法测定，更能达到快速、准确的分析目的，适应生产及科技的发展需求。本次修订对锡編芯块产业发展在产品检测方面提供更有力的保障,有利于稳定锡編芯块产品质量，提高中国锡繊芯块的制造水平。同时，对我国核工业的发展也起到促进作用。（三） 主要参加单位和工作成员及其所做的工作1.本标准起草单位及其分工本标准起草单位为：西北稀有金属材料研究院宁夏有限公司、中核建中核燃料元件有限公司、中核北方核燃料元件有限公司。其中，西北稀有金属材料研究院宁夏有限公司主要负责试验方案制定，试验样品收集和分发，分析方法研究，试验结果处理，标准文本、试燈报告和编制说明撰写等工作；中核建中核燃料元件有限公司为一验单位，主要负责对试验方案中的条件实燈进行验证，提供精密度和准确度测试数据，以及对方法提出建议；中核北方核燃料元件有限公司为二燈单位，主要负责提供精密度试验数据，并对标准文本提出修改意见和建议。标准牵头单位西北稀有金属材料研究院宁夏有限公司是国内唯一的繊材研究和生产基地，国家高新技术企业，建有稀有金属特种材料国家重点实验室。公司通过多年的自主技术研发,研制生产出具备国外同类产品水平的锡編芯块，并制订相应产品及分析检测行业标准。公司分析检测所主持及参与多项編、編铝合金、铜編合金等国家军用标准和行业标准制修订工作。中核建中核燃料元件有限公司以核电燃料元件为主导产业，是我国唯一的压水堆核电燃料组件生产基地。同时以香料、锂钙、锂电池为主要民品产业，为集生产、科研和国内外贸易为一体的国有军民结合型大型骨干企业。在本次修订中，反馈产品使用情况及方法检测需求信息，同时作为第一燈证单位，提供实燈样本的准确度验证及精密度数据。中核北方核燃料元件有限公司是中国核工业集团有限公司的重要成员单位，是我国核工业最早建成的核材料和核燃料元件生产科研基地，为我国“两弾一艇”的研制以及和平利用原子能做出了重要贡献。在本次修订过程中，提供实燈样本的精密度数据，并对标准文本等提出了相应的修改意见。2.本标准起草人员及其工作职责本标准主要起草人：孙洪'涛、王巧、马肖、李晖、湛裁裁、袁翠宏、陈岚、纪秋宇、张健康、张新辉、刘军、殷艺丹。各起草人在本标准编制过程中的工作职责见表1。表1工作成员及所做工作起草人所做工作外洪涛、王巧、李峰、刘军、殷苴丹负责样品搜集、试验方案的确定、条件试验实施、样品删试、方法验证等。马肖标准技术内容审核、试验进度组织协调、标准文件和编制说明编写等。湛慧慧、袁翠宏、陈岚、纪秋宇、殷艺丹对标准文件和编制说明提出修改建议、方法试验验证等。张健康、张新辉标准修订工作的整体统筹及指导，技术性修改建议等。（四）主要工作过程西北稀有金属材料研究院宁夏有限公司在接到标准制订任务后，成立了标准编制组，召开了标准项目编制启动会议，对标准编写工作进行了部署和分工，主要工作过程经历了以下几个阶段。1.立项阶段2020年11月，西北稀有金属材料研究院宁夏有限公司向全国有色金属标准化技术委员会稀有金属分标委提交了YS/T426.4-2000《锡繊芯块化学分析方法原子吸收光谱法测定铅、铁、铭、镁量》标准修订的项目建议书、标准草案和立项报告等材料，经全体委员论证同意立项。随后由秘书处组织全体委员网络投票，投票通过后转报给工业和信息化部科技司,并挂网向社会公开征求意见。2022年4月290,工业和信息化部发布了《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[2022]94号），正式下达该标准的修订任务，标准名称为《锡钺芯块化学分析方法第4部分：铝、铅、铁、铭、镁含量的测定电感耦合等离子体原子发射光谱法为项目计划编号为2O22-O23OT-YS,项目周期为18个月，完成年限为2023年10月，技术归口单位为全国有色金属标准化技术委员会。2.起草阶段2.1任务落实2022年8月25日，全国有色金属标准化技术委员会稀有金属分标委在湖北省宜昌市组织召开了《锡編芯块化学分析方法》修订任务落实会。会上确定了由西北稀有金属材料研究院宁夏有限公司牵头负责《锡钺芯块化学分析方法第4部分：铝、铅、铁、铭、镁含量的测定电感耦合等离子体原子发射光谱法》的起草工作，由中核建中核燃料元件有限公司、中核北方核燃料元件有限公司两家单位协助起草；明确了所采用的分析方法及其测定范围；同时确定了样品制备单位、进度安排等事项。2.2样品收集及试验研究2022年9月~2022年11月编制组委托中核建中核燃料元件有限公司、中核北方核燃料元件有限公司根据市场上锡繊芯块产品的生产和应用情况,结合西北稀有金属材料研究院宁夏有限公司生产及研究情况，开展试验样品的成分设计、选材和制备，充分考虑到试验样品的代表性，共制备了SbBe-均、SbBe-2#、SbBe-3#三种牌号的锡編芯块样品为本标准统一的试验样品，相关信息见表2所示。表2本标准试验样品的基本仏息序号牌号样品状态铝、铅、铁、徭、镁的含里水平/%1SbBe-lff粉末状~0.0050%2SbBe-2fi粉末状-0.050%3SbEe-3#粉末状~0.20%2022年12月~2023年2月编制组开展大量试验研究工作，形成了方法研究报告及标准文本和编制说明的讨论稿。试验内容主要包含样样品预处理、分析谱线选择、基体效应的消除等方法影响因素讨论，以及方法相关精密度和准确度验证。3.征求意见阶段编制组通过发函，全国有色金属标准化技术委员会将《锡編芯块化学分析方法第4部分：铝、铅、铁、铭、镁含量的测定电感耦合等离子体原子发射光谱法》征求意见资料在中国有色金属标准质量信息网（）上挂网，向社会公开征求意见。征求意见的单位包括主要生产、经销、使用、科研、第三方检验机构等单位及大专院校，征求意见单位广泛且具有代表性。2023年2月22日〜23日由全国有色金属标准化技术委员会主持,在广东省佛山市召开标准讨论会，来自国标（北京）检燈认证有限公司、新疆湘润新材料科技有限公司、西北有色金属研究院、宝鸡钛业股份有限公司、金堆城铝业股份有限公司、广东省科学院工业分析检测中心、五矿編业股份有限公司等单位的四十多名专家代表参会，对本文件的讨论稿、编制说明、试燈报告进行了充分、细致的讨论，并提出修改意见。编制组根据汇总意见，采纳以上专家意见，对标准讨论稿进行修改和完善，形成预审稿。2023年5月29日〜31日由全国有色金属标准化技术委员会主持，在云南省大理市召开标准讨论会，来自国标（北京）检验认证有限公司、广东省科学院工业分析检测中心、宁夏东方担业股份有限公司、宝钛集团有限公司、金堆城铝业股份有限公司、五矿編业股份有限公司等单位的五十多名专家代表参会，对本文件的预审稿、编制说明、试燈报告进行了充分、细致的讨论，并提出修改意见。编制组根据汇总意见，采纳以上专家意见，对标准预审稿进行修改和完善，形成送审稿。二、标准的编制原则（-）符合性标准格式严格按照GE/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》等文件的要求编写。（-）适用性和先进性本标准是对YS/T426.4-2000《锡編芯块化学分析方法原子吸收光谱法测定铅、铁、铭、镁量》的修订起草。在充分调研国内外锡編芯块相关产品标准及行业内锡編芯块分析检测实际需求的基础上，对原标准的测定范围、测定方法、试验操作的技术细节、精密度数据进行修改或补充，进一步规范了锡編芯块中铝、铅、铁、铭、镁含量的分析方法，同时又体现了行业内对锡編芯块化学成分分析的技术水平，具有先进性、可操作性和广泛的适用性。主要修订内容如下：1） 更改了测定方法，由原子吸收光谱法修改为电感耦合等离子体原子发射光谱法，满足产品的准确、快速分析，提高了标准的适用性和先进性。2） 増加了测定元素，在电感耦合等离子体原子发射光谱法中増加铝元素的测定，拓展了标准的适用面。3） 补充精密度数据，提高了标准的可参照性。三、标准主要内容的确定依据及主要试验和验证情况分析（-）测定方法的修订YS/T426.4—2000《锡繊芯块化学分析方法第4部分：原子吸收光谱法测定铅、铁、镐、镁量》和YS/T426.3-2000《锡繊芯块化学分析方法第3部分：8为基喳啡分光光度法测定铝量》分别采用原子吸收光谱法测定锡繊芯块中的铅、铁、徳、镁含量以及分光光度法测定铝量，均需要分离去除锡基体，样品前处理操作繁琐，且为单元素测定，分析周期长。本标准采用电感耦合等离子体原子发射光谱法，线性范围贡、灵敏度高、检出限低、多元素同时测定、分析速度快。通过对本标准的修订，能够快速准确地测定锡編芯块中的铝、铅、铁、铭、镁含量，有利于产品质量控制和质量评定，促进锡钺产业的高质量发展。（-）测定范围的修订依据YS/T425-2013《锡繊芯块》以及产品客户的反馈要求，结合日常检测样品实际情况，确定本文件锡钺芯块中杂质元素铝、铅、铁、铭、镁含量的测定范围，见表3。表3产品要求各元素范围与本标准各元素的测定范围的比较元素产品要求范围，不大于/%本标准范围/%Fe0.100.0050~0,20Al0.050.0050~0,20Pb0.040.0050~0,20Mg0.020.0050~0,20Mn0.040.0050~0,20（三） 样品预处理样品预处理方法参照YS/T426.5—2021《锡繊芯块化学分析方法第5部分：硅含量的测定电感耦合等离子体原子发射光谱法》中试样前处理的方法，试样用5也盐酸和1也硝酸，在电热板上低温加热至完全溶解，加入10也酒石酸浴酒（10g/L）,冷却至室温后，用水稀释定容试样溶酒，可确保试样溶酒中锡不水解析出。（四） 分析谱线的确定按照实验方法，对标准系列溶海、各单元素标准溶酒（1.0吗/也）和样品试流进行谱

图扫描分析，分别选择待测元素铝、铅、铁、铭、镁的各2〜3条谱线。观察待测元素谱线益加时的谱图形状、峰强度及元素间的干扰，剔除元素之间有相互干扰的谱线，从中选择“灵敏度高，干扰小、信背比大〃的待测元素分析谱线，结果见图1,表4。图1元素分析谱图表4元素分析谱线元素波长海A1396.152Pb182.143

Fe240.489Mn257.610Mg279.553(五)基体效应的消除实燈对比了基体匹配和无基体时的不同含量的各元素的测定结果，结果见表5和图2。由表5结果及图2对比可以看出，铝、铅和铁元素在基体匹配前后强度有明显影响，铭和镁在该线性范围内有影响不显著。为保证各元素测定的准确性，需对各元素标准系列溶酒进行基体匹配，以消除干扰。由于高纯編(^>99.99%)难以获取，因此本实验采用标准加入法(MSA)配制标准溶流系列，使标准溶流系列的編基体、锡基体与锡編芯块样品溶酒的基体保持一致。表5基体影响实验元素样品编号无基体删定值，％加(岫基体删定值，％190.005420.00605Al2#0.04560.05183#0.1770.2011#0.008490.00595Pb2#0.05180.04473#0.2340.207190.04560.0277Fe2#0.1040.07583#0.2750.247190.006340.00495Mn2#0.05880.05493#0.1950.184190.004750.00487Mg2#0.04840.04893#0.1960.198離斓硬％鼾燭曜懒娜嫩9/1/u////JI //// r5 f//9////fIS /ff/IX// tt hZ/711刀e5ut k::-9 ■ %::■-一寧•顽噸尊■ahTimsi

图2不同含量的各兀素在有无縁被基体时的测定结果对比（六）元素检出限和定量下限的确定对实燈方法空白浴酒连续测定11次，计算标准偏差，以3倍的标准偏差作为元素的检出限（3s）,以10倍的标准偏差作为元素测定下限（10s）,结果见表6。表6元素检出限和定量下限元素删定值%平均值%标准偏差检出限%删定下限%A1D,0005,0.0006,0.0003,0.0002,0.0007,0.0008,D,0008,0.0007,0.0003,0.0005,0.00030.000520.000210.000620.0021Pb0.0005,0.0004,0.0004,0.0011,0.0006,0.0004,D,0006,0.0002,0.0004,0.0003,0.00040.000480.000220.000670.0022Fe0.0002,0.000b0.000b0.0002,0.000b0.0004,D,000b0.000b0.0003?0.0004,0.00030.000210.000120.00350.0012MnD,0006,0.0006,0.0006,0.0006,0.0007,0.0008,D,0007,0.0006,0.0005,0.0006,0.00070.000640.0000770.000230.0008Mg0.000b0.000b0.0002,0.000b0.000b0.000hD,0002,0.000b0.0002,0.000b0.00010.000130.0000450.000130.0005白表6可知，锡編芯块分析方法中铝、铅、钥、铭、镁量的定量下限均小于0.0050%,该方法满足测定范围要求。第一燈证单位（中核建中核燃料元件有限公司）的方法测定下限见表7。表7—验（中核建中核燃料元件有限公司）的方法测定下限元素删定值%平均值%标准偏差检出限%测定下限%A10.0007,0.0006,0.0006,0.0003,0.0002,0.0003,0.0008,0.0005,0.0003,0.0003,0.00050.000460.000190.000560.0019Pb0.0004,>0.00050.0004,0.0002,0.0004,0.0007,0.0004,0.0006,0.0004,0.0003,0.00080.000460.000170.000500.0017

Fe0.000b0.0003?0.000b0.000b0.0003?0.0002,0.000b0.000b0.0003,0.0002,0.00040.000310.000100.00310.0010Mn0.0005,0.0006,0.0005,0.0006,0.0007,0.0006,0.0007,0.0007,0.0008,0.0006,0.00050.000620.0000940.000280.0010Mg0.0002,0.000b0.000b0.000b0.000b0.000b0.0002,0.000b0.0002,0.0002,0.00010.000140.0000480.000140.0005由表7可知，锡編芯块分析方法中铝、铅、铁、铭、镁量的测定下艮均小于0.0050%,表明该方法满足测定范围要求，与起草单位结论一致。（七）准确度试验1.起草单位加标回收试验在3个不同铝、铅、铁、铭、镁含量的锡編芯块样品中各加入不同量的铝、铅、铁、铭、镁元素标准溶流，按实验方法进行加标回收试验，结果见表8。表8起草单位加标回收试验结果样品编号元素删定值/%加入里/%删得总里/%回收率％SbBe-1#Al0.006090.00500.0112102.10.0100.0165104.1Pb0.005640.00500.010495.20.0100.0161104.6Fe0.01790.00500.022898.00.0100.027899.0Mn0.006300.00500.011298.00.0100.016097.0Mg0.004760.00500.0099102.80.0100.014799.4SbBe-2#Al0.05190.0100.061596.30.0500.102100.3Pb0.04540.0100.0558104.40.0500.0976104.5Fe0.07300.0100.082797.20.0500.12298.0Mn0.05810.0100.068098.70.0500.10899.7Mg0.03130.0100.0414101.30.0500.0835104.5SbBe-38Al0.2000.0500.252103.30.100.304103.6Pb0.2120.0500.26197.60.100.30996.8Fe0.2430.0500.295104.10.100.346103.2Mn0.20?0.0500.25596.4

0.100.30598.2Mg0.1970.0500.249104.20.100.29598.1表8数据表明，锡繊芯块样品中铝、铅、铁、铭、镁元素测定加标回收率在95.2%〜104.6%之间，方法准确度满足要求。2.一验加标回收试验第一燈证单位（中核建中核燃料元件有限公司）的加标回收试验结果见表9。表9一验（中核建中核燃料元件有限公司）加标回收试验结果样品编号元素删定值/%加入里/%删得总里/%回收率％SbBe-1#Al0.006560.00500.0117103.60.0100.016498.8Pb0.005350.00500.010399.00.0100.0157103.5Fe0.01840.00500.0234100.90.0100.027995.5Mn0.005890.00500.010898.10.0100.0161102.1Mg0.004380.00500.0096104.40.0100.0146102.2SbBe-2#Al0.04910.0100.058997.90.0500.101103.8Pb0.04800.0100.0581101.20.0500.097799.4Fe0.07570.0100.0861103.50.0500.127102.5Mn0.05760.0100.0680104.30.0500.10798.9Mg0.03300.0100.0432101.90.0500.0833100.6SbBe-38Al0.1920.0500.243101.30.100.295102.6Pb0.2060.0500.25597.60.100.30295.8Fe0.2370.0500.288102.20.100.33497.1Mn0.2110.0500.25996.70.100.30695.4Mg0.2040.0500.255102.40.100.29995.2由表9可知，锡钺芯块样品中铝、铅、铁、铭、镁元素测定加标回收率均在95.2%〜104.4%之间，说明该方法准确可靠，与起草单位结论一致。（八）精密度试验

对3个不同铝、铅、铁、铭、镁含量的锡編芯块样品，采用本方法分别独立地进行11次测定，测定结果见表10。表10起草单位样品测定结果样品元素删定结果/%（n=ll）X/%sRSD/%SbBe-1#Al0.00600,0.00605,0.00603,0.00608,0.00615,0.00618,0.00638,0.00587,0.00606,0.00597,0.006250.006090.000142.31Pb0.00584,0.00546,0.0059b0.00575,0.00588,0.0061b0.00542,0.0052b0.00578,0.00516,0.005540.005640.000335.76FeD.0178?0.018b0.0178?0.0179,0.0178?0.018b0.0178?0.0117,0.0180?0.0180,0.01790.01790.000130.75Mn0.0062&0.00626,0.00630,0.00630,0.00629,0.00632,0.00630,0.0063b0.0063b0.00632,0.006290.006300.0000180.28Mg0.00473,0.00472,0.00473,0.00474,0.00477,0.00476,0.00477,0.00481,0.00476,0.00477,0.004780.004760.0000260.55SbBe-2#AlD.0517,0.0516,0.0516,0.0521,0.0524,0.0524,0.0519,0.0519,0.0517,0.0516,0.05170.05190.000310.59PbD.0469>0.0454,0.0434,0.0447,0.0473,0.0446,0.0465,0.Q464,0.0471,0.0435,0.04320.04540.0015?3.45Fe0.0714,0.0719,0.0717,0.0719,0.0746,0.0744,0.0746,0.0744,0.0740,0.0720,0.07190.07300.001381.88MnD.0571,0.0572,0.0572,0.0572,0.0594,0.0591,0.0592,0.0592,0.0590,0.0575,0.05730.05810.001021.75Mg0.0305,0.0306,0.0305,0.0307,0.0323,0.0319,0.0318,0.0317,0.0320,0.0311,0.03090.03130.000682.16SbBe-38AlD.200,0.200,0.200,0.200,0.200,0.200,0.200,0.201,0.201,0.201,0.2010.2000.000510.25Pb0.209,0.212,0.215,0.209,0.210,0.216,0.217,0.215,0.211,0.212,0.2080.2120.003131.47Fe0.244,0.239,0.239,0.239,0.239,0.240,0.247,0.247,0.247,0.247,0.2470.2430.004021.66Mn0.204,0.203,0.203,0.204,0.203,0.204,0.211,0.211,0.210,0.211,0.2110.20?0.003841.86MgD.195,0.193,0.194,0.193,0.194,0.194,0.201,0.201，0.200,0.201，0.2000.1970.003591.82由表10结果可知，样品中铝、铅、铁、铭、镁元素测定的RSD%在0.25%〜5.花％之间，精密度较好，能满足分析要求。第一燈证单位（中核建中核燃料元件有限公司）的精密度试验结果见表11。表11一验（中核建中核燃料兀件有限公司）精密度实验

样品元素删定结果/%<n=ll）X/%sRSD/%SbBe-1#A10.00659,0.00665,0.00630,0.00672,0.00635,0.00688,0.00633,0.00649,0.0065b0.00633,0.006590.006520.000192.86Pb0.00535,0.00542,0.00509,0.00555,0.00547,0.0059b0.00512,0.00535,0.00522,0.00543,0.004920.005350.000264.95Fe0.0183,0.0186,0.0185,0.0188,0.0179,0.0184,0.0179,0.0183,0.0179,0.0184,0.01890.01840.000351.89Mn0.0059b0.00593,0.00577,0.00602,0.00588,0.00572,0.00603,0.00589,0.00579,0.00582,0.006080.005890.000121.95Mg0.00449,0.00435,0.00439,0.00428,0.0044b0.00437,0.00442,0.00450,0.00439,0.00425?0.004310.004380.0000791.80SbBe-2#Al0.0488>0.0490,0.0497,0.0494,0.0491,0.0492，0.0489,0.0482,0.0500,0.0485,0.04940.04910.000521.05Pb0.0505,0.0472,0.0494,0.0484>0.0490,0.0477,0.0466,0.0464,0.0488,0.0458,0.04800.04800.001422.95Fe0.0782,0.0742,0.0736,0.0766,0.0747,0.0783,0.0744,0.0763,0.0777,0.0739,0.07530.07570.001762.32Mn0.0581,0.0569,0.0574,0.0579,0.0587,0.0566,0.0552,0.0595,0.0582,0.0565,0.05830.05760.001202.09Mg0.0335，0.0344，0.0322,0.0327,0.0336,0.0327,0.0328,0.0333,0.0340,0.0320,0.03190.03300.000822.49SbBe-38Al0.194,0.194,0.193,0.193,0.190,0.190,0.193，0.193,0.192,0.192,0.1920.1920.001360.71Pb0.206,0.202,0.206,0.207,0.208,0.203,0.203,0.208,0.211,0.203,0.2110.2060.003191.55Fe0.243,0.237,0.235,0.236,0.234,0.236,0.234,0.234,0.237,0.243,0.2370.2370.003241.37Mn0.207,0.215,0.215,0.214,0.206,0.212,0.212,0.206,0.210,0.207,0.2130.2110.003591.70Mg0.199,0.201,0.208,0.201,0.207,0.208,0.199,0.208,0.206,0.206,0.1990.2040.003971.95由表11结果可知，样品中铝、铅、铁、铭、镁元素测定的相对标准偏差在0.71%〜4.95%之间，说明该方法的精密度良好，与起草单位结论一致。第二燈证单位（中核北方核燃料元件有限公司）的精密度试验结果见表12。表12二验（中核北方核燃料兀件有限公司）精密度实验样品元素删定结果/%<n=ll）X/%sRSD/%SbBe-1#Al0.00589,0.00601,0.00590,0.00578,0.00580,0.00588,0.00607,0.00583,0.00612,0.00587,0.005930.0001161.96

0.00605Pb0.00501,0.00542,0.00514,0.00569,0.00536,0.00544,0.00599,0.00547,0.00584,0.00563,0.005970.005540.0003255.86Fe0.0176,0.0173,0.0177,0.0168,0.0174,0.0176,0.0176,0.0177,0.0169,0.0175,0.01730.01740.00030?1.76Mn0.00592,0.00618,0.00603,0.00602,0.00584,0.00597,0.00600,0.00601,0.00584,0.00594,0.005980.005980.00009471.58Mg0.00455,0.00452,0.00449,0.00453,0.00460,0.00430,0.00437,0.00446>0.00466,0.00433,0.004420.004480.0001132.51SbBe-2#Al0.0537,0.0544，0.0526，0.0540，0.0533，0.0529,0.0539,0.0527,0.0548,0.0536,0.05450.05370.0007401.38Pb0.0498,0.0515,0.0468>0.0502,0.0491,0.0479,0.0469,0.0490,0.0468,0.0472,0.04890.04860.0015?3.24Fe0.0780,0.0739,0.0755,0.0764,0.0737,0.0758,0.0779,0.0762,0.0773,0.0741,0.07690.07600.001552.03Mn0.0561,0.0545，0.0560，0.0542，0.0543，0.0562,0.0568,0.0570,0.0540,0.0553,0.05460.05540.001101.98Mg0.0341,0.0333，0.0350,0.0330,0.0355,0.0347,0.0335,0.0346,0.0339,0.0353,0.03520.03440.0008642.51SbBe-38Al0.194,0.194,0.195,0.196,0.196,0.196,0.198,0.198,0.195,0.195,0.1960.1960.001352.67Pb0.206,0.198,0.205,0.206,0.206,0.199,0.200,0.205,0.197,0.203,0.1970.2020.003821.89Fe0.232,0.239,0.233,0.235,0.237,0.235,0.238,0.240,0.238,0.234,0.2350.2360.002571.09Mn0.207,0.205,0.199,0.201,0.206,0.202,0.202,0.206,0.208,0.199,0.1990.2030.003421.68Mg0.194,0.192,0.196,0.195,0.200,0.200,0.194,0.198,0.0196,0.194,0.1920.1960.002811.43由表12结果可知，样品中铝、铅、铁、镐、镁元素测定的相对标准偏差在1.09%〜5.86%之间，说明该方法的精密度良好，与起草单位结论一致。（九）主要实验（或验证）的分析按照GB/T6379.2-2004《测量方法与结果的准确度》通过对西北稀有金属材料研究院宁夏有限公司、中核建中核燃料元件有限公司、中核北方核燃料元件有限公司三家单位的试好数据和验证数据分别按照重复性和允许差的公式进行计算，得到了不同含量的重复性限和允许差。1.样品数据对比起草单位与验证单位的试验结果统计对比见表13〜表17。表13铝的试验结果对比

试验单位水平1水平2水平3二%S*S*S西北稀有金属材料硏究院宁夏有限公司起草0.006090.000140.05190.000300.2000.00051中核建中核燃料元件有限公司0.006520.000190.04910.000520.1920.00136中核北方核燃料元件有限公司二歧0.005930.000120.05370.000740.1960.00135表14鉛的试验结果对比试验单位水平1水平2水平3S*S*S西北稀有金属材料硏究院宁夏有限公司起草0.005640.000330.04540.0015?0.2120.00313中核建中核燃料元件有限公司0.005350.000120.04800.001420.2060.00319中核北方核燃料元件有限公司二歧0.005540.000330.04860.0015?0.2020.00382表15铁的试验结果对比试验单位水£1水£F2水£F3S*S*§西北稀有金属材料硏究院宁夏有限公司起草0.01790.000130.07300.001380.243D.00402中核建中核燃料元件有限公司0.01840.000350.7570.001760.2370.00324中核北方核燃料元件有限公司二歧0.01740.000310.07600.001540.2360.00257表16缢的试验结果对比试验单位水平1水平2水平3二%S*S*S西北稀有金属材料硏究院宁夏有限公司起草0.006300.0000180.05810.001020.20?0.00384中核建中核燃料元件有限公司0.005890.000120.05760.001200.2110.00359中核北方核燃料元件有限公司二歧0.005980.0000950.05540.001100.2030.00342表17镁的试验结果对比试验单位水平1水£F2水£F3S*S*§西北稀有金属材料硏究院宁夏有限公司起草0.004760.0000260.03130.000680.197D.00359中核建中核燃料元件有限公司0.004380.0000790.03300.000820.2040.00397中核北方核燃料元件有限公司二歧0.004480.000110.03440.000860.1960.0280采用格拉布斯检验方法，分别值情况分析，结果见表18〜表32c&祥对三家单1立中铝、铅、铁、铭、镁含量测定数据1庄行异常表18不同铝含量水平样品分析结果异常值分析（西材院）样品X/%SD/9JG/%G/%舍弃界限值/n=ll,aM.05结论SbBe-1#0.006090.000141.5812.0392.234无异常值

SbBe-2#0.05190.000310.8981.7372.234无异常值SbBe-380.2000.000510.7211.2612.234无异常值表19不同鉛含量水平样品分斤结果异常值分析（西材院）样品X/%SD/95G/%G/%舍弃界限值/n=ll,aM.05结论SbBe-1#0.005640.000331.4821.4412.234无异常值SbBe-2#0.04540.0015?1.3821.2362.234无异常值SbBe-380.2120.00311.3381.5422.234无异常值表20不同铁含量水平样品分析结果异常值分析（西材院）样品X/%SD/«G/%G/%舍弃界限值/n=ll,aM.05结论SbBe-1#0.01790.000131.4911.4912.234无异常值SbBe-2#0.07300.001381.1501.1762.234无异常值SbBe-380.2430.004020.9501.0402.234无异常值表2不同钻含专水平样品分析结果异常值分析（西材院）样品X/%SD/«G/%G/%舍弃界限值/n=ll,aM.05结论SbBe-1#0.006300.0000182.1471.2272.234无异常值SbBe-2#0.05810.001021.0101.2522.234无异常值SbBe-380.20?0.003840.9941.0882.234无异常值表22不同镁含量水平样品分析结果异常值分析（西材院）样品X/%SD/«G/%G/%舍弃界限值/n=ll,a=0.05结论SbBe-1#0.004760.0000261.44?1.9642.234无异常值SbBe-2#0.03130.000681.1421.5182.234无异常值SbBe-380.1970.003591.0891.1392.234无异常值表23不同铝含量水平样品分析结果异常值分析（中核建中）样品X/%SD/«G/%G/%舍弃界限值/n=ll,aM.05结论SbBe-1#0.006520.000191.1911.9232.234无异常值SbBe-2#0.04910.000521.7601.7242.234无异常值SbBe-380.1920.0013?1.7361.2022.234无异常值表24不同鉛含量水平样品分析结果异常值分析（中核建中）样品X/%SD/«G/%G/%舍弃界限值/n=ll,a=0.05结论SbBe-1#0.005350.000261.6172.1212.234无异常值SbBe-2#0.04800.001421.5391.7762.234无异常值SbBe-380.2060.003191.3121.5112.234无异常值表25不同铁含量水平样品分析结果异常值分析（中核建中）

样品X/%SD/«G/%G/%舍弃界限值/n=ll,a=0.05结论SbBe-1#0.01840.000351.3081.5702.234无异常值SbBe-2#0.07570.001761.2201.4532.234无异常值SbBe-380.2370.003240.8981.8802.234无异常值表26不同钻含量水平样品分析结果异常值分析（中核建中）样品X/%SD/«G/%G/%舍弃界限值/n=ll,a=0.05结论SbBe-1#0.005890.000121.5151.6102.234无异常值SbBe-2#0.05760.001201.9701.6002.234无异常值SbBe-380.2110.003591.2931.2172.234无异常值表27不同镁含量水平样品分析结果异常值分析（中核建中）样品X/%SD/«G/%G/%舍弃界限值/n=ll,a=0.05结论SbBe-1#0.004380.0000791.6281.5482.234无异常值SbBe-2#0.03300.000821.3521.6962.234无异常值SbBe-380.2040.003971.2141.0532.234无异常值表28不同铝含量水平样品分析结果异常值分析（中核北方）样品X/%SD/«G/%G/%舍弃界限值/n=ll,aM.05结论SbBe-1#0.005930.000121.2701.6622.234无异常值SbBe-2#0.05370.000741.4491.5232.234无异常值SbBe-380.1960.001351.2811.6852.234无异常值表29不同铅含量水平样品分析结果异常值分析（中核北方）样品X/%SD/«G/%G/%舍弃界限值/n=ll,a=0.05结论SbBe-1#0.005540.000331.6361.3792.234无异常值SbBe-2#0.04860.0015?1.1161.8742.234无异常值SbBe-380.2020.003821.3091.0472.234无异常值表30不同铁含量水平样品分析结果异常值分析（中核北方）样品X/%SD/«G/%G/%舍弃界限值/n=ll,a=0.05结论SbBe-1#0.01740.000311.4302.1602.234无异常值SbBe-2#0.07600.001551.4701.3112.234无异常值SbBe-380.2360.002571.5571.5572.234无异常值表31不同钻含量水平样品分析结果异常值分析（中核北方）样品X/%SD/9JG/%G/%舍弃界限值/n=ll,aM.05结论

SbBe-1#0.005980.0000951.4302.1602.234无异常值SbBe-2#0.05540.001101.2411.4902.234无异常值SbBe-380.2030.003421.1961.4362.234无异常值表32不同镁含量水平样品分析结果异常值分析（中核北方）样品X/%SD/«G/%G/%舍弃界限值/n=ll,aM.05结论SbBe-1#0.004480.000121.5591.6402.234无异常值SbBe-2#0.03430.000861.5891.3052.234无异常值SbBe-380.1960.002811.2641.5882.234无异常值根据格拉布斯检验方法，查表得：n=ll,a=Q05时，舍弃界限值为2.234。表18〜表32数据结果表明不同铝、铅、铁、铭、镁含量的锡編芯块样品的11次测定数据无异常值。2.方法的重复性限和允许差在重复性条件下获得的两次独立测试结果的测定值，精密度原始数据参见附录A,在表33给出的平均值范围内，两个测试结果的绝对差值不超过重复性限（r）,超过重复性限（r）情况不超过5%。重复性限（工）按表33数据采用线性内插法或外延法求得。表33重复性限（r）铝的质里分数%0.00620.0520.20r/%0.00050.0020.01铅的质里分数%0.00550.04?0.21r/%0.00090.0050.01铁的质里分数%0.0180.0750.24r/%0.0010.0050.01德的质里分数%0.00610.05?0.21r/%0.00030.0040.01镁的质里分数%0.00450.0330.20r/%0.00030.0030.01实验室之间分析结果的差值应不大于表34所列允许差。表34允许差铝的质里分数%允许差%0.0050~0,0100.0010>0.010~0,100.007>0.10~0,200.02铅的质里分数允许差%%0.0050~0,0100.0010>0.010~0,100.007>0.10~0,200.02铁的质里分数允许差%%0.0050~0,0100.0010>0.010~0,100.007>0.10~0,200.02德的质里分数允许差%%0.0050~0,0100.0010>0.010~0,100.006>0.10~0,200.02镁的质里分数允许差%%0.0050~0,0100.0010>0.010~0,100.005>0.10~0,200.02四、标准中涉及专利的情况本文件不涉及专利问题。五、 预期达到的社会效益等情况本文件充分考虑了国内外锡繊芯块研制及生产企业和用户单位的生产工艺技术水平。本文件颁布执行后，将进一步规范锡編芯块中铝、铅、铁、铭、镁含量的分析检验工作，更好地指导相关行业锡繊芯块的分析检测和应用水平;有利于生产采用统一的分析方法开展产品质量检验工作，有利于市场公平交易环境的形成，具有较大的社会效益。六、 釆用国际标准和国外先进标准的情况无。七、 与现行法律、法规、强制性国家标准及相关标准协调配套情况本标准的技术内容与现行相关法律、法规和强制性国家标准没有冲突。在标准修订过程中充分考虑到了国内外锡編芯块相关产品标准的技术内容，修订后铝、铅、铁、