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目的 建立超声浸提电感耦合等离子体原子发射光谱法直接测定煤中各种形态硫的方法。方法 采用煤试样在盐酸介质、硝酸介质中使用超声连续浸提,离心分离,残渣用艾士卡试剂熔融,电感耦合等离子体原子发射光谱法直接测定煤中硫酸盐硫、硫化铁硫和有机硫含量。结果 硫质量浓度在 1.00~100.0 µg/mL 范围内时浓度与响应强度线性关系良好,相关系数0.9997,检出限为0.20µg/mL。本方法用于多种不同煤质样品中各种形态硫检测,测定值的相对标准偏差(n=7)为0.63%~4.55%,加标回收率为85.5%~109.8%,测定结果与标准方法对比无显著性差异。本方法实现一种同时直接测定煤中各种形态硫的分析方式,减少了间接法中其他组分对待测物质测定的影响,避免因采用不同方法对煤中形态硫的测定带来的系统误差,具有检出限低、准确度高、操作简便的优点。结论 本方法缩短了检测时间,提高了检测效率,能够满足批量煤样品中各种形态硫含量的快速准确测定,值得推广。
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*双龙,硕士,地质实验测试正高级工程师,研究方向为岩石矿物、土壤、水系沉积物、煤质、环境、食品、生物等样品分析方法。E-mail:
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2013,(6): 73-75., articleTitle=煤中各种形态硫测定应注意的问题, refAbstract=null)], funds=[Fund(id=1154353360686800984, tenantId=1146029695717560320, journalId=1146119944283992078, articleId=1149789897323671600, awardId=2024FX13, language=CN, fundingSource=内蒙古自治区自然科学基金项目(2024FX13), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1154353352503714756, tenantId=1146029695717560320, journalId=1146119944283992078, articleId=1149789897323671600, xref=null, ext=[AuthorCompanyExt(id=1154353352524686277, tenantId=1146029695717560320, journalId=1146119944283992078, articleId=1149789897323671600, companyId=1154353352503714756, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=内蒙古地矿科技有限责任公司 自然资源部呼和浩特矿产资源检测中心 呼和浩特 010031)])], figs=[ArticleFig(id=1154353358832918589, tenantId=1146029695717560320, journalId=1146119944283992078, articleId=1149789897323671600, language=EN, label=null, caption=null, figureFileSmall=tn8+IV0jJlmDNuEQ8fmKkw==, figureFileBig=8WfuetuRhgVa7qhnJKk2Bw==, tableContent=null), ArticleFig(id=1154353358920998974, tenantId=1146029695717560320, journalId=1146119944283992078, articleId=1149789897323671600, language=CN, label=图 1, caption=
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不同超声浸提温度硫酸盐硫的测定值, figureFileSmall=VAvVJvfzgaNAFgeWITsoXw==, figureFileBig=unzBydDGv8udzne6sEn61g==, tableContent=null), ArticleFig(id=1154353359655002182, tenantId=1146029695717560320, journalId=1146119944283992078, articleId=1149789897323671600, language=EN, label=null, caption=null, figureFileSmall=AEPaKNgtji1kqpDTKMc3SA==, figureFileBig=7h13yr8qeV2Nl3p3z78vZw==, tableContent=null), ArticleFig(id=1154353359759859785, tenantId=1146029695717560320, journalId=1146119944283992078, articleId=1149789897323671600, language=CN, label=图 4, caption=
不同超声浸提温度硫化铁硫的测定值, figureFileSmall=AEPaKNgtji1kqpDTKMc3SA==, figureFileBig=7h13yr8qeV2Nl3p3z78vZw==, tableContent=null), ArticleFig(id=1154353359831162958, tenantId=1146029695717560320, journalId=1146119944283992078, articleId=1149789897323671600, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
| 分析谱线 | BEC/(mg/L) | 响应强度 | 信噪比 |
| S 180.669 | 0.56 | 4044.1 | 68.7 |
| S 181.975 | 0.78 | 2359.5 | 42.6 |
| S 182.563 | 1.90 | 890.6 | 15.3 |
| S 189.965 | 2.35 | 919.7 | 15.9 |
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硫元素不同分析谱线下仪器响应值, figureFileSmall=null, figureFileBig=null, tableContent=
| 分析谱线 | BEC/(mg/L) | 响应强度 | 信噪比 |
| S 180.669 | 0.56 | 4044.1 | 68.7 |
| S 181.975 | 0.78 | 2359.5 | 42.6 |
| S 182.563 | 1.90 | 890.6 | 15.3 |
| S 189.965 | 2.35 | 919.7 | 15.9 |
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| 项目 | 样品号 | 本方法 | 标准方法 | 相对偏差 RE/% | 值 |
| 测定 平均值 /% | 相对标准 偏差 RSD/% | 加标 回收率 /% | 测定 平均值 /% | 相对标准 偏差 RSD/% |
| 硫酸盐硫 | M9964 | 0.735 | 0.63 | 95.2 | 0.721 | 1.56 | 1.92 | 2.07 |
| M9965 | 0.233 | 1.33 | 93.2 | 0.226 | 2.25 | 3.05 | 2.11 |
| M9967 | 0.064 | 1.34 | 107.5 | 0.066 | 3.13 | 3.08 | 1.61 |
| M0074 | 0.038 | 2.38 | 94.5 | 0.040 | 3.54 | 5.13 | 2.14 |
| M8935 | 0.024 | 3.24 | 105.4 | 0.023 | 4.44 | 4.26 | 1.40 |
| M8956 | 0.027 | 2.02 | 88.5 | 0.026 | 4.16 | 3.77 | 1.48 |
| M8957 | 0.041 | 1.75 | 103.8 | 0.040 | 3.55 | 2.47 | 1.13 |
| M8959 | 0.082 | 2.76 | 109.8 | 0.079 | 2.86 | 3.73 | 1.69 |
| M1168 | 0.022 | 3.40 | 98.7 | 0.021 | 4.08 | 4.65 | 1.58 |
| M1169 | 0.020 | 3.97 | 93.4 | 0.021 | 3.94 | 4.88 | 1.57 |
| M1170 | 0.245 | 1.87 | 92.5 | 0.238 | 2.31 | 2.90 | 1.76 |
| M1171 | 0.020 | 4.55 | 102.0 | 0.021 | 4.42 | 4.88 | 1.38 |
| 硫化铁硫 | M9964 | 0.255 | 1.75 | 104.7 | 0.262 | 1.53 | 2.71 | 2.10 |
| M9965 | 0.428 | 1.96 | 97.5 | 0.441 | 2.15 | 2.99 | 1.85 |
| M9967 | 0.397 | 2.23 | 96.4 | 0.414 | 3.14 | 4.19 | 1.94 |
| M0074 | 0.485 | 2.07 | 91.3 | 0.499 | 2.26 | 2.85 | 1.67 |
| M8935 | 0.399 | 2.25 | 94.4 | 0.404 | 3.11 | 1.25 | 0.58 |
| M8956 | 1.653 | 2.85 | 95.9 | 1.634 | 2.05 | 1.16 | 0.59 |
| M8957 | 0.537 | 2.25 | 89.4 | 0.553 | 2.36 | 2.94 | 1.62 |
| M8959 | 1.771 | 2.11 | 93.5 | 1.723 | 2.49 | 2.75 | 1.52 |
| M1168 | 0.724 | 3.52 | 99.2 | 0.738 | 4.55 | 1.92 | 0.60 |
| M1169 | 0.188 | 1.52 | 106.1 | 0.182 | 2.59 | 3.24 | 1.96 |
| M1170 | 0.963 | 1.38 | 99.9 | 0.993 | 3.67 | 3.07 | 1.39 |
| M1171 | 0.627 | 2.78 | 98.2 | 0.646 | 3.23 | 2.99 | 1.26 |
| 有机硫 | M9964 | 0.323 | 2.98 | 108.3 | 0.343 | 4.35 | 6.01 | 2.02 |
| M9965 | 0.293 | 2.14 | 99.3 | 0.307 | 3.76 | 4.67 | 1.92 |
| M9967 | 0.300 | 1.98 | 90.0 | 0.313 | 2.99 | 4.24 | 2.11 |
| M0074 | 0.204 | 2.71 | 92.5 | 0.215 | 3.67 | 5.25 | 2.05 |
| M8935 | 0.432 | 0.72 | 85.5 | 0.441 | 2.19 | 2.06 | 1.59 |
| M8956 | 1.081 | 1.22 | 96.7 | 1.103 | 1.76 | 2.01 | 1.68 |
| M8957 | 0.576 | 1.55 | 87.5 | 0.585 | 4.33 | 1.55 | 0.60 |
| M8959 | 0.585 | 3.56 | 94.7 | 0.579 | 3.85 | 1.03 | 0.35 |
| M1168 | 0.473 | 2.34 | 98.8 | 0.467 | 2.93 | 1.28 | 0.61 |
| M1169 | 0.221 | 2.98 | 89.2 | 0.232 | 3.25 | 4.86 | 1.97 |
| M1170 | 0.885 | 2.40 | 95.8 | 0.867 | 2.72 | 2.05 | 1.02 |
| M1171 | 1.241 | 1.35 | 98.1 | 1.233 | 1.77 | 0.65 | 0.52 |
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方法精密度和准确度, figureFileSmall=null, figureFileBig=null, tableContent=
| 项目 | 样品号 | 本方法 | 标准方法 | 相对偏差 RE/% | 值 |
| 测定 平均值 /% | 相对标准 偏差 RSD/% | 加标 回收率 /% | 测定 平均值 /% | 相对标准 偏差 RSD/% |
| 硫酸盐硫 | M9964 | 0.735 | 0.63 | 95.2 | 0.721 | 1.56 | 1.92 | 2.07 |
| M9965 | 0.233 | 1.33 | 93.2 | 0.226 | 2.25 | 3.05 | 2.11 |
| M9967 | 0.064 | 1.34 | 107.5 | 0.066 | 3.13 | 3.08 | 1.61 |
| M0074 | 0.038 | 2.38 | 94.5 | 0.040 | 3.54 | 5.13 | 2.14 |
| M8935 | 0.024 | 3.24 | 105.4 | 0.023 | 4.44 | 4.26 | 1.40 |
| M8956 | 0.027 | 2.02 | 88.5 | 0.026 | 4.16 | 3.77 | 1.48 |
| M8957 | 0.041 | 1.75 | 103.8 | 0.040 | 3.55 | 2.47 | 1.13 |
| M8959 | 0.082 | 2.76 | 109.8 | 0.079 | 2.86 | 3.73 | 1.69 |
| M1168 | 0.022 | 3.40 | 98.7 | 0.021 | 4.08 | 4.65 | 1.58 |
| M1169 | 0.020 | 3.97 | 93.4 | 0.021 | 3.94 | 4.88 | 1.57 |
| M1170 | 0.245 | 1.87 | 92.5 | 0.238 | 2.31 | 2.90 | 1.76 |
| M1171 | 0.020 | 4.55 | 102.0 | 0.021 | 4.42 | 4.88 | 1.38 |
| 硫化铁硫 | M9964 | 0.255 | 1.75 | 104.7 | 0.262 | 1.53 | 2.71 | 2.10 |
| M9965 | 0.428 | 1.96 | 97.5 | 0.441 | 2.15 | 2.99 | 1.85 |
| M9967 | 0.397 | 2.23 | 96.4 | 0.414 | 3.14 | 4.19 | 1.94 |
| M0074 | 0.485 | 2.07 | 91.3 | 0.499 | 2.26 | 2.85 | 1.67 |
| M8935 | 0.399 | 2.25 | 94.4 | 0.404 | 3.11 | 1.25 | 0.58 |
| M8956 | 1.653 | 2.85 | 95.9 | 1.634 | 2.05 | 1.16 | 0.59 |
| M8957 | 0.537 | 2.25 | 89.4 | 0.553 | 2.36 | 2.94 | 1.62 |
| M8959 | 1.771 | 2.11 | 93.5 | 1.723 | 2.49 | 2.75 | 1.52 |
| M1168 | 0.724 | 3.52 | 99.2 | 0.738 | 4.55 | 1.92 | 0.60 |
| M1169 | 0.188 | 1.52 | 106.1 | 0.182 | 2.59 | 3.24 | 1.96 |
| M1170 | 0.963 | 1.38 | 99.9 | 0.993 | 3.67 | 3.07 | 1.39 |
| M1171 | 0.627 | 2.78 | 98.2 | 0.646 | 3.23 | 2.99 | 1.26 |
| 有机硫 | M9964 | 0.323 | 2.98 | 108.3 | 0.343 | 4.35 | 6.01 | 2.02 |
| M9965 | 0.293 | 2.14 | 99.3 | 0.307 | 3.76 | 4.67 | 1.92 |
| M9967 | 0.300 | 1.98 | 90.0 | 0.313 | 2.99 | 4.24 | 2.11 |
| M0074 | 0.204 | 2.71 | 92.5 | 0.215 | 3.67 | 5.25 | 2.05 |
| M8935 | 0.432 | 0.72 | 85.5 | 0.441 | 2.19 | 2.06 | 1.59 |
| M8956 | 1.081 | 1.22 | 96.7 | 1.103 | 1.76 | 2.01 | 1.68 |
| M8957 | 0.576 | 1.55 | 87.5 | 0.585 | 4.33 | 1.55 | 0.60 |
| M8959 | 0.585 | 3.56 | 94.7 | 0.579 | 3.85 | 1.03 | 0.35 |
| M1168 | 0.473 | 2.34 | 98.8 | 0.467 | 2.93 | 1.28 | 0.61 |
| M1169 | 0.221 | 2.98 | 89.2 | 0.232 | 3.25 | 4.86 | 1.97 |
| M1170 | 0.885 | 2.40 | 95.8 | 0.867 | 2.72 | 2.05 | 1.02 |
| M1171 | 1.241 | 1.35 | 98.1 | 1.233 | 1.77 | 0.65 | 0.52 |
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