Article(id=1190284222314156560, tenantId=1146029695717560320, journalId=1189873562199433220, issueId=1190291572731253087, articleNumber=null, orderNo=null, doi=10.19710/J.cnki.1003-8817.20250031, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=null, receivedDateStr=null, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1761715473010, onlineDateStr=2025-10-29, pubDate=1755619200000, pubDateStr=2025-08-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1761717226774, onlineIssueDateStr=2025-10-29, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=1761715473010, onlineFirstDateStr=2025-10-29, sourceXml=null, magXml=null, createTime=1761715473010, creator=13701087609, updateTime=1761715473010, updator=13701087609, issue=Issue{id=1190291572731253087, tenantId=1146029695717560320, journalId=1189873562199433220, year='2025', volume='', issue='8', pageStart='1', pageEnd='72', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=1, specialIssue=null, createTime=1761717225486, creator=13701087609, updateTime=1761717904141, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1190294419279545214, tenantId=1146029695717560320, journalId=1189873562199433220, issueId=1190291572731253087, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1190294419279545215, tenantId=1146029695717560320, journalId=1189873562199433220, issueId=1190291572731253087, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=51, endPage=55, ext={EN=ArticleExt(id=1190284222595174937, articleId=1190284222314156560, tenantId=1146029695717560320, journalId=1189873562199433220, language=EN, title=Determination of Impurity Elements in Primary Magnesium Ingots by ICP-AES and X-Ray Fluorescence Spectroscopy, columnId=1190284220686766583, journalTitle=Automobile Technology & Material, columnName=Original article, runingTitle=null, highlight=null, articleAbstract=
To ensure the purity during the aluminum alloy alloying process, it is necessary to control the impurity content in primary alloy ingots. The contents of silicon, iron, copper, aluminum, manganese, and nickel impurities in primary magnesium ingots are determined using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) and X-Ray Fluorescence spectrometry (XRF). For ICP-AES, samples are dissolved with hydrogen peroxide-hydrochloric acid, and the spectral lines are optimized along with the matrix-matching method, achieving a detection limit of 0.000 01%~0.000 27%, a spike recovery rate of 92%~102%, and a repeatability RSD of <2.3%. For XRF, the optimal analysis conditions are determined, with a detection range of 0.000 1%~0.100 0% and a repeatability RSD of ≤3.1%. The results indicate that both methods exhibit good accuracy and repeatability, with ICP-AES offering higher sensitivity, while XRF is more suitable for rapid and non-destructive testing.
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为保证铝合金合金化过程中的纯净度,需控制原生合金铸锭中的杂质含量。采用电感耦合等离子体原子发射光谱法(ICP-AES)与X射线荧光光谱法(XRF)测定原生镁锭中硅、铁、铜、铝、锰、镍杂质的含量。ICP-AES通过过氧化氢-盐酸溶解样品,优化谱线及基体匹配法,检出限达0.000 01%~0.000 27%,加标回收率为92%~102%,重复性RSD<2.3%。采用XRF确定最佳分析条件,检测范围为0.000 1%~0.100 0%,重复性RSD≤3.1%。结果表明,2种方法均具有良好的准确性与重复性,其中ICP-AES灵敏度更优,XRF适合快速无损检测。
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孟凡娇(1988—),女,工程师,学士学位,研究方向为金属材料化学分分析。
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孟凡娇(1988—),女,工程师,学士学位,研究方向为金属材料化学分分析。
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孟凡娇(1988—),女,工程师,学士学位,研究方向为金属材料化学分分析。
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2006(7): 68+70., articleTitle=ZL104铝合金熔炼过程中镁元素的质量控制, refAbstract=null), Reference(id=1190291584110399902, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1190284222314156560, doi=null, pmid=null, pmcid=null, year=2022, volume=51, issue=3, pageStart=25, pageEnd=27, url=null, language=null, rfNumber=[4], rfOrder=3, authorNames=张宇霆, 李洪亮, 马华, journalName=有色金属加工, refType=null, unstructuredReference=张宇霆, 李洪亮, 马华, 等. ICP-AES法测定铝铜中间合金中杂质元素硅和铁的含量[J].
有色金属加工,
2022,
51(3): 25-27., articleTitle=ICP-AES法测定铝铜中间合金中杂质元素硅和铁的含量, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1190291579286950240, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1190284222314156560, xref=null, ext=[AuthorCompanyExt(id=1190291579295338849, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1190284222314156560, companyId=1190291579286950240, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Liaoyang Xiangyu Aluminum Industry Co., Ltd., Liaoyang 111003), AuthorCompanyExt(id=1190291579307921762, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1190284222314156560, companyId=1190291579286950240, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=辽阳象屿铝业有限公司, 辽阳 111003)])], figs=[ArticleFig(id=1190291582579478921, tenantId=1146029695717560320, journalId=1189873562199433220, articleId=1190284222314156560, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
| 元素 | 测试范围/% | 脉冲高度调节(PHA)/(°) | 角度/(°) | 测试时间/s |
| Si | 0.006 3~0.062 0 | 28~72 | 108.90 | 10 |
| Fe | 0.002 2~0.027 0 | 28~82 | 57.52 | 10 |
| Cu | 0.000 63~0.025 00 | 30~80 | 45.00 | 10 |
| Al | 0.008 2~1.060 0 | 26~76 | 144.70 | 10 |
| Mn | 0.006 0~0.148 0 | 22~88 | 62.96 | 10 |
| Ni | 0.000 33~0.011 00 | 28~78 | 48.66 | 10 |
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分析条件及测试范围
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| 元素 | 测试范围/% | 脉冲高度调节(PHA)/(°) | 角度/(°) | 测试时间/s |
| Si | 0.006 3~0.062 0 | 28~72 | 108.90 | 10 |
| Fe | 0.002 2~0.027 0 | 28~82 | 57.52 | 10 |
| Cu | 0.000 63~0.025 00 | 30~80 | 45.00 | 10 |
| Al | 0.008 2~1.060 0 | 26~76 | 144.70 | 10 |
| Mn | 0.006 0~0.148 0 | 22~88 | 62.96 | 10 |
| Ni | 0.000 33~0.011 00 | 28~78 | 48.66 | 10 |
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镁元素加入量 /μg·mL-1 | Ii/I0 |
| Si | Fe | Cu | Al | Mn | Ni |
| 2 | 0.99 | 0.97 | 1.11 | 0.94 | 1.01 | 1.01 |
| 10 | 1.10 | 0.96 | 1.22 | 0.90 | 0.99 | 1.00 |
| 100 | 1.06 | 0.95 | 1.19 | 0.94 | 0.97 | 0.97 |
| 1 000 | 1.19 | 1.15 | 1.15 | 0.94 | 0.98 | 0.77 |
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基体元素的干扰试验
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镁元素加入量 /μg·mL-1 | Ii/I0 |
| Si | Fe | Cu | Al | Mn | Ni |
| 2 | 0.99 | 0.97 | 1.11 | 0.94 | 1.01 | 1.01 |
| 10 | 1.10 | 0.96 | 1.22 | 0.90 | 0.99 | 1.00 |
| 100 | 1.06 | 0.95 | 1.19 | 0.94 | 0.97 | 0.97 |
| 1 000 | 1.19 | 1.15 | 1.15 | 0.94 | 0.98 | 0.77 |
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干扰 元素 | 加入量 /μg·mL-1 | Ie/I0比值 |
| Si | Fe | Cu | Al | Mn | Ni |
| Si | 10 | | 1.01 | 1.03 | 1.02 | 1.02 | 1.01 |
| Fe | 10 | 1.00 | | 0.99 | 1.00 | 1.00 | 0.99 |
| Cu | 10 | 1.00 | 1.00 | | 1.00 | 0.96 | 0.99 |
| Al | 10 | 0.97 | 0.97 | 0.98 | | 0.99 | 0.98 |
| Mn | 10 | 0.99 | 0.99 | 0.99 | 0.99 | | 0.99 |
| Ni | 10 | 1.00 | 0.97 | 1.00 | 0.99 | 1.00 | |
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共存元素的干扰试验
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干扰 元素 | 加入量 /μg·mL-1 | Ie/I0比值 |
| Si | Fe | Cu | Al | Mn | Ni |
| Si | 10 | | 1.01 | 1.03 | 1.02 | 1.02 | 1.01 |
| Fe | 10 | 1.00 | | 0.99 | 1.00 | 1.00 | 0.99 |
| Cu | 10 | 1.00 | 1.00 | | 1.00 | 0.96 | 0.99 |
| Al | 10 | 0.97 | 0.97 | 0.98 | | 0.99 | 0.98 |
| Mn | 10 | 0.99 | 0.99 | 0.99 | 0.99 | | 0.99 |
| Ni | 10 | 1.00 | 0.97 | 1.00 | 0.99 | 1.00 | |
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| 元素 | 质量分数 参考值 | 质量分数实测值 |
| a方法 | b方法 | c方法 |
| Si | 0.030 0 | 0.030 8 | 0.021 0 | 0.230 0 |
| Fe | 0.005 5 | 0.004 8 | 0.004 8 | 0.005 0 |
| Cu | 0.003 9 | 0.003 5 | 0.003 2 | 0.003 3 |
| Al | 0.008 5 | 0.008 5 | 0.008 3 | 0.008 9 |
| Mn | 0.017 0 | 0.016 4 | 0.016 3 | 0.016 4 |
| Ni | 0.001 3 | 0.001 1 | 0.001 1 | 0.001 4 |
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前处理方式对样品的影响 %
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| 元素 | 质量分数 参考值 | 质量分数实测值 |
| a方法 | b方法 | c方法 |
| Si | 0.030 0 | 0.030 8 | 0.021 0 | 0.230 0 |
| Fe | 0.005 5 | 0.004 8 | 0.004 8 | 0.005 0 |
| Cu | 0.003 9 | 0.003 5 | 0.003 2 | 0.003 3 |
| Al | 0.008 5 | 0.008 5 | 0.008 3 | 0.008 9 |
| Mn | 0.017 0 | 0.016 4 | 0.016 3 | 0.016 4 |
| Ni | 0.001 3 | 0.001 1 | 0.001 1 | 0.001 4 |
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| 元素 | 检出限/% | 分析上限/% | R² |
| Si | 0.000 17 | 0.050 | 0.999 56 |
| Fe | 0.000 03 | 0.020 | 0.999 99 |
| Cu | 0.000 03 | 0.020 | 0.999 85 |
| Al | 0.000 27 | 0.040 | 0.999 76 |
| Mn | 0.000 01 | 0.040 | 0.999 99 |
| Ni | 0.000 07 | 0.014 | 0.999 98 |
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元素的分析范围及线性相关系数
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| 元素 | 检出限/% | 分析上限/% | R² |
| Si | 0.000 17 | 0.050 | 0.999 56 |
| Fe | 0.000 03 | 0.020 | 0.999 99 |
| Cu | 0.000 03 | 0.020 | 0.999 85 |
| Al | 0.000 27 | 0.040 | 0.999 76 |
| Mn | 0.000 01 | 0.040 | 0.999 99 |
| Ni | 0.000 07 | 0.014 | 0.999 98 |
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| 元素 | 质量分数 参考值 | 质量分数实测值 | RSD |
| 第1次 | 第2次 | 第3次 | 第4次 | 第5次 | 第6次 | 第7次 | 第8次 | 第9次 | 第10次 | 第11次 |
| Si | 0.01 | 0.010 1 | 0.010 4 | 0.009 9 | 0.010 0 | 0.010 0 | 0.010 2 | 0.010 1 | 0.010 1 | 0.010 0 | 0.010 2 | 0.010 0 | 1.2 |
| Fe | 0.02 | 0.019 9 | 0.019 9 | 0.019 9 | 0.019 8 | 0.019 9 | 0.019 9 | 0.019 8 | 0.019 9 | 0.019 9 | 0.019 9 | 0.019 9 | 0.3 |
| Cu | 0.01 | 0.010 0 | 0.010 0 | 0.010 0 | 0.010 0 | 0.010 0 | 0.010 0 | 0.010 1 | 0.010 0 | 0.010 0 | 0.010 0 | 0.010 0 | 0.2 |
| Al | 0.01 | 0.010 0 | 0.010 0 | 0.009 9 | 0.010 0 | 0.010 1 | 0.010 0 | 0.010 1 | 0.010 0 | 0.010 0 | 0.010 0 | 0.009 9 | 0.6 |
| Mn | 0.02 | 0.020 0 | 0.019 9 | 0.020 0 | 0.020 0 | 0.020 1 | 0.019 8 | 0.019 9 | 0.020 0 | 0.020 0 | 0.020 1 | 0.020 0 | 0.4 |
| Ni | 0.01 | 0.010 0 | 0.010 0 | 0.010 0 | 0.010 0 | 0.010 1 | 0.010 0 | 0.010 1 | 0.010 0 | 0.010 0 | 0.010 0 | 0.010 0 | 0.4 |
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重复性试验结果 %
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| 元素 | 质量分数 参考值 | 质量分数实测值 | RSD |
| 第1次 | 第2次 | 第3次 | 第4次 | 第5次 | 第6次 | 第7次 | 第8次 | 第9次 | 第10次 | 第11次 |
| Si | 0.01 | 0.010 1 | 0.010 4 | 0.009 9 | 0.010 0 | 0.010 0 | 0.010 2 | 0.010 1 | 0.010 1 | 0.010 0 | 0.010 2 | 0.010 0 | 1.2 |
| Fe | 0.02 | 0.019 9 | 0.019 9 | 0.019 9 | 0.019 8 | 0.019 9 | 0.019 9 | 0.019 8 | 0.019 9 | 0.019 9 | 0.019 9 | 0.019 9 | 0.3 |
| Cu | 0.01 | 0.010 0 | 0.010 0 | 0.010 0 | 0.010 0 | 0.010 0 | 0.010 0 | 0.010 1 | 0.010 0 | 0.010 0 | 0.010 0 | 0.010 0 | 0.2 |
| Al | 0.01 | 0.010 0 | 0.010 0 | 0.009 9 | 0.010 0 | 0.010 1 | 0.010 0 | 0.010 1 | 0.010 0 | 0.010 0 | 0.010 0 | 0.009 9 | 0.6 |
| Mn | 0.02 | 0.020 0 | 0.019 9 | 0.020 0 | 0.020 0 | 0.020 1 | 0.019 8 | 0.019 9 | 0.020 0 | 0.020 0 | 0.020 1 | 0.020 0 | 0.4 |
| Ni | 0.01 | 0.010 0 | 0.010 0 | 0.010 0 | 0.010 0 | 0.010 1 | 0.010 0 | 0.010 1 | 0.010 0 | 0.010 0 | 0.010 0 | 0.010 0 | 0.4 |
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| 元素 | 质量分数参考值 | 质量分数实测值 | 质量分数绝对差值 | 质量分数加标后分析值 | 加标回收率 |
| Si | 0.030 0 | 0.030 8 | 0.000 8 | 0.040 0 | 92 |
| Fe | 0.005 5 | 0.004 8 | 0.000 7 | 0.014 3 | 95 |
| Cu | 0.003 9 | 0.003 5 | 0.000 4 | 0.013 7 | 102 |
| Al | 0.008 5 | 0.008 5 | 0.000 0 | 0.017 9 | 94 |
| Mn | 0.017 0 | 0.016 4 | 0.000 6 | 0.026 3 | 99 |
| Ni | 0.001 3 | 0.001 1 | 0.000 2 | 0.010 3 | 92 |
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准确性和加标回收率 %
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| 元素 | 质量分数参考值 | 质量分数实测值 | 质量分数绝对差值 | 质量分数加标后分析值 | 加标回收率 |
| Si | 0.030 0 | 0.030 8 | 0.000 8 | 0.040 0 | 92 |
| Fe | 0.005 5 | 0.004 8 | 0.000 7 | 0.014 3 | 95 |
| Cu | 0.003 9 | 0.003 5 | 0.000 4 | 0.013 7 | 102 |
| Al | 0.008 5 | 0.008 5 | 0.000 0 | 0.017 9 | 94 |
| Mn | 0.017 0 | 0.016 4 | 0.000 6 | 0.026 3 | 99 |
| Ni | 0.001 3 | 0.001 1 | 0.000 2 | 0.010 3 | 92 |
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| 元素 | 质量分数实测值 | RSD |
| 第1次 | 第2次 | 第3次 | 第4次 | 第5次 | 第6次 | 第7次 | 第8次 | 第9次 | 第10次 | 第11次 |
| Si | 0.010 3 | 0.010 5 | 0.009 8 | 0.010 0 | 0.010 3 | 0.009 7 | 0.009 3 | 0.010 3 | 0.009 5 | 0.010 4 | 0.010 3 | 4.0 |
| Fe | 0.020 2 | 0.019 9 | 0.020 0 | 0.019 8 | 0.019 7 | 0.020 0 | 0.020 3 | 0.020 1 | 0.019 6 | 0.019 9 | 0.020 0 | 1.0 |
| Cu | 0.010 1 | 0.010 3 | 0.010 0 | 0.009 9 | 0.010 0 | 0.010 1 | 0.010 2 | 0.010 0 | 0.009 8 | 0.010 0 | 0.009 7 | 1.7 |
| Al | 0.009 8 | 0.010 0 | 0.009 9 | 0.010 0 | 0.010 1 | 0.010 0 | 0.010 1 | 0.010 0 | 0.010 2 | 0.010 0 | 0.009 9 | 1.1 |
| Mn | 0.020 0 | 0.019 9 | 0.020 1 | 0.019 9 | 0.020 1 | 0.019 8 | 0.019 9 | 0.020 2 | 0.019 6 | 0.020 1 | 0.020 3 | 1.0 |
| Ni | 0.009 9 | 0.010 0 | 0.010 0 | 0.010 1 | 0.010 0 | 0.010 0 | 0.010 1 | 0.010 0 | 0.010 2 | 0.010 0 | 0.010 0 | 0.8 |
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XRF重复性试验结果 %
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| 元素 | 质量分数实测值 | RSD |
| 第1次 | 第2次 | 第3次 | 第4次 | 第5次 | 第6次 | 第7次 | 第8次 | 第9次 | 第10次 | 第11次 |
| Si | 0.010 3 | 0.010 5 | 0.009 8 | 0.010 0 | 0.010 3 | 0.009 7 | 0.009 3 | 0.010 3 | 0.009 5 | 0.010 4 | 0.010 3 | 4.0 |
| Fe | 0.020 2 | 0.019 9 | 0.020 0 | 0.019 8 | 0.019 7 | 0.020 0 | 0.020 3 | 0.020 1 | 0.019 6 | 0.019 9 | 0.020 0 | 1.0 |
| Cu | 0.010 1 | 0.010 3 | 0.010 0 | 0.009 9 | 0.010 0 | 0.010 1 | 0.010 2 | 0.010 0 | 0.009 8 | 0.010 0 | 0.009 7 | 1.7 |
| Al | 0.009 8 | 0.010 0 | 0.009 9 | 0.010 0 | 0.010 1 | 0.010 0 | 0.010 1 | 0.010 0 | 0.010 2 | 0.010 0 | 0.009 9 | 1.1 |
| Mn | 0.020 0 | 0.019 9 | 0.020 1 | 0.019 9 | 0.020 1 | 0.019 8 | 0.019 9 | 0.020 2 | 0.019 6 | 0.020 1 | 0.020 3 | 1.0 |
| Ni | 0.009 9 | 0.010 0 | 0.010 0 | 0.010 1 | 0.010 0 | 0.010 0 | 0.010 1 | 0.010 0 | 0.010 2 | 0.010 0 | 0.010 0 | 0.8 |
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| 元素 | 质量分数 参考值 | 质量分数 实测值 | 质量分数 绝对差值 |
| Si | 0.030 0 | 0.031 0 | 0.001 0 |
| Fe | 0.005 5 | 0.006 3 | 0.000 8 |
| Cu | 0.003 9 | 0.003 4 | 0.000 5 |
| Al | 0.008 5 | 0.008 3 | 0.000 2 |
| Mn | 0.017 0 | 0.016 3 | 0.000 7 |
| Ni | 0.001 3 | 0.001 6 | 0.000 3 |
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XRF准确度试验结果 %
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| 元素 | 质量分数 参考值 | 质量分数 实测值 | 质量分数 绝对差值 |
| Si | 0.030 0 | 0.031 0 | 0.001 0 |
| Fe | 0.005 5 | 0.006 3 | 0.000 8 |
| Cu | 0.003 9 | 0.003 4 | 0.000 5 |
| Al | 0.008 5 | 0.008 3 | 0.000 2 |
| Mn | 0.017 0 | 0.016 3 | 0.000 7 |
| Ni | 0.001 3 | 0.001 6 | 0.000 3 |
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