Article(id=1193534736632083265, tenantId=1146029695717560320, journalId=1190260162528112641, issueId=1193513023760466128, articleNumber=1672-0636(2025)01-0187-09, orderNo=null, doi=10.3969/j.issn.1672-0636.2025.01.016, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1735488000000, receivedDateStr=2024-12-30, revisedDate=1737043200000, revisedDateStr=2025-01-17, acceptedDate=null, acceptedDateStr=null, onlineDate=1762490456016, onlineDateStr=2025-11-07, pubDate=1738944000000, pubDateStr=2025-02-08, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1762490456016, onlineIssueDateStr=2025-11-07, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1762490456016, creator=13701087609, updateTime=1762490456016, updator=13701087609, issue=Issue{id=1193513023760466128, tenantId=1146029695717560320, journalId=1190260162528112641, year='2025', volume='42', issue='1', pageStart='1', pageEnd='217', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=0, articleOrder=1, issueType=-1, specialIssue=null, createTime=1762485279264, creator=13701087609, updateTime=1762498836216, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1193569885797184010, tenantId=1146029695717560320, journalId=1190260162528112641, issueId=1193513023760466128, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1193569885797184011, tenantId=1146029695717560320, journalId=1190260162528112641, issueId=1193513023760466128, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=187, endPage=195, ext={EN=ArticleExt(id=1193534736875352898, articleId=1193534736632083265, tenantId=1146029695717560320, journalId=1190260162528112641, language=EN, title=Determination of total carbon in nuclear grade boron carbide by high temperature infrared absorption method, columnId=1190343834849607834, journalTitle=World Nuclear Geoscience, columnName=RESEARCH ARTICALS, runingTitle=null, highlight=null, articleAbstract=
This paper established a high-temperature infrared method to determine the total carbon in nuclear grade boron carbide. The optimal experimental conditions were determined by studying the testing temperature,sample weight,selection of flux,and flux coverage method. At the same time, accuracy,precision,detection limit and quantification limit of the method were determined. The results show that the optimal testing temperature is 1 400 ℃,which not only ensures the release of total carbon but also extends the service life of the instrument. The optimal sample weight is 20-30 mg. Tin particles has the best melting effect,and boron carbide has the highest carbon release efficiency. The best coverage method was found to be 0.4 g tin particle + boron carbide + 0.6 g tin particle,and the carbon in boron carbide was totally released. The high-temperature infrared method for determining total carbon in nuclear grade boron carbide is good in accuracy and precision,the test results of boron carbide certified reference material are all within the uncertainty range of the certified value, while the RSD is<1.5 %, and the detection limit of the method is 0.001 9 %. This method is simple and fast,it can meet the requirements for measuring total carbon in nuclear grade boron carbide.
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LI Bowen,female,born in 1991,senior engineer,focusing on rock and soil chemical analysis. E-mail:libowen19910215@163.com
, authorsList=LI Bowen, LIU Gaohui, YUAN Jian, SUN Jin), CN=ArticleExt(id=1193534868253536266, articleId=1193534736632083265, tenantId=1146029695717560320, journalId=1190260162528112641, language=CN, title=高温红外吸收法测定核纯级碳化硼中总碳的方法研究, columnId=1190343834992214173, journalTitle=世界核地质科学, columnName=研究论文, runingTitle=null, highlight=null, articleAbstract=
建立高温红外吸收法测定核纯级碳化硼中总碳的方法,重点探讨测试温度、样品称样量、助熔剂的选择和助熔剂覆盖方式对测量结果的影响,确定实验的最佳条件;并对该方法的准确度、精密度、检出限和定量限等指标进行分析。结果表明: 最佳的测试温度为1 400 ℃,既保证总碳得到释放同时延长仪器使用寿命;最佳称样量介于20~30 mg之间;锡粒的助熔效果最好,碳化硼中碳释放效率最高;对助熔剂的覆盖方式进行探究,0.4 g锡粒+碳化硼+0.6 g锡粒的覆盖方式为最佳,碳化硼中碳得到全部释放。高温红外吸收法测定核纯级碳化硼中总碳的方法准确度高,碳化硼标准物质的测量结果均在标准值的不确定度范围内;该方法精密度良好,重复测定结果的RSD均<1.5 %;方法的检出限为0.001 9 %,该方法简单、快速,满足核纯级碳化硼中总碳测量的需求。
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, authorsList=李博文, 刘高辉, 袁建, 孙进)}, authors=[Author(id=1193593175307678408, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, orderNo=0, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=libowen19910215@163.com, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1193593175366398666, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, authorId=1193593175307678408, language=EN, stringName=LI Bowen, firstName=LI, middleName=null, lastName=Bowen, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=Beijing Research Institute of Uranium Geology, Beijing 100029, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1193593175425118923, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, authorId=1193593175307678408, language=CN, stringName=李博文, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=核工业北京地质研究院,北京 100029, bio={"content":"
李博文,女,1991年生,高级工程师,主要从事工作为岩石土壤化学分析测试。E-mail:libowen19910215@163.com
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李博文,女,1991年生,高级工程师,主要从事工作为岩石土壤化学分析测试。E-mail:libowen19910215@163.com
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2017 (in Chinese)., articleTitle=null, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1193593175232180932, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, xref=null, ext=[AuthorCompanyExt(id=1193593175240569541, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, companyId=1193593175232180932, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Beijing Research Institute of Uranium Geology, Beijing 100029, China), AuthorCompanyExt(id=1193593175248958150, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, companyId=1193593175232180932, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=核工业北京地质研究院,北京 100029)])], figs=[ArticleFig(id=1193593176914096867, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, language=EN, label=Fig. 1, caption=
Results of carbon content in nuclear grade boron carbide at different temperatures, figureFileSmall=RiA0c1LpyX3o2qmOeky/Kw==, figureFileBig=JxPWgNkbtnT0eVKmso3AyQ==, tableContent=null), ArticleFig(id=1193593177018954468, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, language=CN, label=图1, caption=
不同温度下核纯级碳化硼中碳含量结果, figureFileSmall=RiA0c1LpyX3o2qmOeky/Kw==, figureFileBig=JxPWgNkbtnT0eVKmso3AyQ==, tableContent=null), ArticleFig(id=1193593177111229157, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, language=EN, label=Fig. 2, caption=
The relationship between sample weight and carbon measured values, figureFileSmall=rKASNF/l8JnP6uMavomDHQ==, figureFileBig=GX/DHWu8v5c/JdLWwfWJBQ==, tableContent=null), ArticleFig(id=1193593177174143718, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, language=CN, label=图2, caption=
不同称样量与碳测定值关系, figureFileSmall=rKASNF/l8JnP6uMavomDHQ==, figureFileBig=GX/DHWu8v5c/JdLWwfWJBQ==, tableContent=null), ArticleFig(id=1193593177287389927, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, language=EN, label=Fig. 3, caption=
Release curve of carbon a-B4C;b-B4C+cupric oxide wire form;c-B4C+iron particles;d-B4C+tungsten particles;e-B4C+vanadium pentoxide powder;f-B4C+tin particles
, figureFileSmall=wJvlmrZr/LKtRneuzD0DnA==, figureFileBig=OvYJGbCnORWnVWYoy8LM+Q==, tableContent=null), ArticleFig(id=1193593177467745000, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, language=CN, label=图3, caption=
总碳释放曲线 a—B4C;b—B4C+线状氧化铜;c—B4C+铁粒;d—B4C+钨粒;e—B4C+五氧化二钒粉末;f—B4C+锡粒。
, figureFileSmall=wJvlmrZr/LKtRneuzD0DnA==, figureFileBig=OvYJGbCnORWnVWYoy8LM+Q==, tableContent=null), ArticleFig(id=1193593177564213993, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, language=EN, label=Table 1, caption=
Chemical parameters of three nuclear grade boron carbide types
, figureFileSmall=null, figureFileBig=null, tableContent=
| 组分 | 类型1 | 类型2 | 类型3 |
| 总硼/% | 76.5~81.0 | 73.0~81.0 | 70.0~81.0 |
| HNO3可溶性硼/% | ≤0.5 | ≤0.6 | 未确定 |
| 水溶性硼/% | ≤0.2 | ≤0.2 | ≤1.0 |
| 氟/10-6 | ≤25 | ≤25 | 未确定 |
| 氯/10-6 | ≤75 | ≤75 | 未确定 |
| 钙/% | ≤0.3 | ≤0.3 | 未确定 |
| 铁/% | ≤1.0 | ≤1.0 | ≤2.0 |
| 总硼+总碳/% | ≥98.0 | ≥97.0 | ≥94.0 |
), ArticleFig(id=1193593177648100074, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, language=CN, label=表1, caption=
核纯级碳化硼类型参数(ASTM C750-24)[9]
, figureFileSmall=null, figureFileBig=null, tableContent=
| 组分 | 类型1 | 类型2 | 类型3 |
| 总硼/% | 76.5~81.0 | 73.0~81.0 | 70.0~81.0 |
| HNO3可溶性硼/% | ≤0.5 | ≤0.6 | 未确定 |
| 水溶性硼/% | ≤0.2 | ≤0.2 | ≤1.0 |
| 氟/10-6 | ≤25 | ≤25 | 未确定 |
| 氯/10-6 | ≤75 | ≤75 | 未确定 |
| 钙/% | ≤0.3 | ≤0.3 | 未确定 |
| 铁/% | ≤1.0 | ≤1.0 | ≤2.0 |
| 总硼+总碳/% | ≥98.0 | ≥97.0 | ≥94.0 |
), ArticleFig(id=1193593177715208939, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, language=EN, label=Table 2, caption=
Test results of different fluxes
, figureFileSmall=null, figureFileBig=null, tableContent=
| 序号 | 助熔剂 | 用量/g | 熔出时间/s | 总碳测试结果/% |
| 1 | — | — | 150 | 7.23 |
| 2 | 线状氧化铜 | 0.6 | 280 | 13.53 |
| 3 | 铁粒 | 1.0 | 230 | 17.97 |
| 4 | 钨粒 | 1.0 | 200 | 18.94 |
| 5 | 五氧化二钒粉末 | 0.3 | 180 | 17.49 |
| 6 | 锡粒 | 1.0 | 130 | 20.25 |
), ArticleFig(id=1193593177786512108, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, language=CN, label=表2, caption=
不同助熔剂的测试结果
, figureFileSmall=null, figureFileBig=null, tableContent=
| 序号 | 助熔剂 | 用量/g | 熔出时间/s | 总碳测试结果/% |
| 1 | — | — | 150 | 7.23 |
| 2 | 线状氧化铜 | 0.6 | 280 | 13.53 |
| 3 | 铁粒 | 1.0 | 230 | 17.97 |
| 4 | 钨粒 | 1.0 | 200 | 18.94 |
| 5 | 五氧化二钒粉末 | 0.3 | 180 | 17.49 |
| 6 | 锡粒 | 1.0 | 130 | 20.25 |
), ArticleFig(id=1193593177866203885, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, language=EN, label=Table 3, caption=
Results of different coverage methods for tin particles
, figureFileSmall=null, figureFileBig=null, tableContent=
| 序号 | 助熔剂 | 总碳测定值/% | 总碳平均值/% | RSD/% |
| 1 | 锡囊包裹0.02 gB4C | 21.24 | 21.76 | 20.68 | 20.21 | 20.76 | 20.93 | 2.82 |
| 2 | 0.02 gB4C+0.6 g锡粒 | 19.28 | 20.12 | 19.99 | 20.54 | 19.65 | 19.92 | 2.39 |
| 3 | 0.4 g锡粒+0.02 gB4C+0.6 g锡粒 | 20.94 | 21.62 | 21.28 | 21.42 | 21.20 | 21.29 | 1.18 |
), ArticleFig(id=1193593177992033006, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, language=CN, label=表3, caption=
不同锡粒覆盖方式的结果
, figureFileSmall=null, figureFileBig=null, tableContent=
| 序号 | 助熔剂 | 总碳测定值/% | 总碳平均值/% | RSD/% |
| 1 | 锡囊包裹0.02 gB4C | 21.24 | 21.76 | 20.68 | 20.21 | 20.76 | 20.93 | 2.82 |
| 2 | 0.02 gB4C+0.6 g锡粒 | 19.28 | 20.12 | 19.99 | 20.54 | 19.65 | 19.92 | 2.39 |
| 3 | 0.4 g锡粒+0.02 gB4C+0.6 g锡粒 | 20.94 | 21.62 | 21.28 | 21.42 | 21.20 | 21.29 | 1.18 |
), ArticleFig(id=1193593178054947567, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, language=EN, label=Table 4, caption=
Test results of nuclear grade boron carbide certified reference material
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| 序号 | 标准物质编号 | 产地 | 总碳测试结果/% | 总碳标准值及不确定度/% |
| 1 | GBW06604 | 中国 | 21.25 | 21.20±0.06 |
| 2 | GBW06605 | 中国 | 20.35 | 20.41±0.06 |
| 3 | GBW06606 | 中国 | 20.23 | 20.19±0.06 |
| 4 | ERM-ED102 | 德国 | 20.99 | 21.01±0.28 |
), ArticleFig(id=1193593178117862128, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, language=CN, label=表4, caption=
核纯级碳化硼标准物质测试结果
, figureFileSmall=null, figureFileBig=null, tableContent=
| 序号 | 标准物质编号 | 产地 | 总碳测试结果/% | 总碳标准值及不确定度/% |
| 1 | GBW06604 | 中国 | 21.25 | 21.20±0.06 |
| 2 | GBW06605 | 中国 | 20.35 | 20.41±0.06 |
| 3 | GBW06606 | 中国 | 20.23 | 20.19±0.06 |
| 4 | ERM-ED102 | 德国 | 20.99 | 21.01±0.28 |
), ArticleFig(id=1193593178180776689, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, language=EN, label=Table 5, caption=
Precision test results of total carbon of nuclear grade boron carbide
, figureFileSmall=null, figureFileBig=null, tableContent=
| 序号 | 样品名称 | 总碳测试结果/% | 平均值/% | RSD/% |
| 1 | XEG-21 | 20.17 | 20.18 | 1.32 |
| 2 | 20.36 |
| 3 | 19.92 |
| 4 | 20.23 |
| 5 | 19.85 |
| 6 | 20.56 |
| 7 | SDQ-76 | 21.32 | 21.43 | 1.26 |
| 8 | 21.15 |
| 9 | 21.76 |
| 10 | 21.24 |
| 11 | 21.78 |
| 12 | 21.34 |
| 13 | ZZT-02 | 21.01 | 21.09 | 1.22 |
| 14 | 20.76 |
| 15 | 21.23 |
| 16 | 21.48 |
| 17 | 20.89 |
| 18 | 21.14 |
), ArticleFig(id=1193593178281439986, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, language=CN, label=表5, caption=
核纯级碳化硼总碳精密度测试结果
, figureFileSmall=null, figureFileBig=null, tableContent=
| 序号 | 样品名称 | 总碳测试结果/% | 平均值/% | RSD/% |
| 1 | XEG-21 | 20.17 | 20.18 | 1.32 |
| 2 | 20.36 |
| 3 | 19.92 |
| 4 | 20.23 |
| 5 | 19.85 |
| 6 | 20.56 |
| 7 | SDQ-76 | 21.32 | 21.43 | 1.26 |
| 8 | 21.15 |
| 9 | 21.76 |
| 10 | 21.24 |
| 11 | 21.78 |
| 12 | 21.34 |
| 13 | ZZT-02 | 21.01 | 21.09 | 1.22 |
| 14 | 20.76 |
| 15 | 21.23 |
| 16 | 21.48 |
| 17 | 20.89 |
| 18 | 21.14 |
), ArticleFig(id=1193593178340160243, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, language=EN, label=Table 6, caption=
The detection limit and quantification limit test results of the method
, figureFileSmall=null, figureFileBig=null, tableContent=
| 样品 | 总碳/% | 平均值/% | 标准偏差/% | 检出限/% | 定量限/% |
| 空白 | 0.001 1 | 0.000 8 | 0.001 1 | 0.000 3 | 0.001 9 | 0.019 0 |
| 0.001 3 | 0.001 4 |
| 0.000 8 | 0.001 4 |
| 0.001 4 | 0.000 7 |
| 0.000 8 | 0.000 9 |
| 0.001 2 |
), ArticleFig(id=1193593178398880500, tenantId=1146029695717560320, journalId=1190260162528112641, articleId=1193534736632083265, language=CN, label=表6, caption=
方法的检出限与定量限测试结果
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| 样品 | 总碳/% | 平均值/% | 标准偏差/% | 检出限/% | 定量限/% |
| 空白 | 0.001 1 | 0.000 8 | 0.001 1 | 0.000 3 | 0.001 9 | 0.019 0 |
| 0.001 3 | 0.001 4 |
| 0.000 8 | 0.001 4 |
| 0.001 4 | 0.000 7 |
| 0.000 8 | 0.000 9 |
| 0.001 2 |
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