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| 天然气中总硫GC-SCD测定不确定度评定研究 |
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朱华东1,2,3, 曾文平1,2,3, 黄灵1,2,3, 李晓红1,2,3
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1.中国石油西南油气田公司天然气研究院;2.国家市场监督管理总局重点实验室（天然气质量控制和能量计量）;3.中国石油天然气集团公司天然气质量控制和能量计量重点实验室
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| 摘要: |
| 目的 为解决GC-SCD天然气总硫测定方法缺乏不确定度评定应用案例的问题，开展实际样品测定的不确定度评价，提升测定数据的实用价值。方法 结合GC-SCD天然气总硫分析方法和实际检测经验，首次系统地分析了测量不确定度来源，依据JJF 1059.1—2012《测量不确定度评定与表示》，提出了不确定度评价方案。结果 实际样品总硫分析不确定度评定案例结果显示，样品1的总硫分析结果的扩展不确定度为0.19 mg/m3（k=2），主要来源于羰基硫（质量浓度为0.18 mg/m3，k=2）；样品2的总硫分析结果的扩展不确定度为0.14 mg/m3（k=2），主要来源于硫化氢（质量浓度为0.12 mg/m3，k=2）。结论 总硫分析和单个硫化合物分析不确定度主要来源为样品分析重复性和标准物质，其中硫化氢和羰基硫单个硫化合物分析不确定度为总硫分析不确定度的主要来源。建议根据实际工作情况可选择重复测定2次，或综合实际工作量适当提高重复测定次数和采用高准确度标准物质提升测量不确定度水平，并采用抗硫吸附材质的取样容器、管线阀门等元器件，减小硫化氢和羰基硫单个硫化合物分析不确定度，以保证数据准确。 |
| 关键词: 天然气 总硫 硫化合物 气相色谱 不确定度 |
| DOI：10.3969/j.issn.1007-3426.2025.03.017 |
| 分类号: |
| 基金项目:中国石油西南油气田公司科学研究与技术开发项目“天然气中H2S、CO2和C4H8S新型检测管法准确检测机理及设备研究”（2024D108-01-06） |
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| Study on uncertainty evaluation of GC-SCD determination of total sulfur in natural gas |
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ZHU Huadong1,2,3, ZENG Wenping1,2,3, HUANG Ling1,2,3, LI Xiaohong1,2,3
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1.Research Institute of Natural Gas Technology, PetroChina Southwest Oil & Gasfield Company, Chengdu, Sichuan, China;2.Key Laboratory of Natural Gas Quality Control and Energy Measurement, State Administration for Market Regulation, Chengdu, Sichuan, China;3.Key Laboratory of Natural Gas Quality Control and Energy Measurement, CNPC, Chengdu, Sichuan, China
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| Abstract: |
| Objective The uncertainty evaluation of actual sample measurement was carried out to provide an application case for the determination of total sulfur in natural gas using GC-SCD method, thus enhancing the practical value of the determination data. Method Combining with the practical testing experience of the GC-SCD method, the sources of uncertainty in measurement were systematically analysed at the first time. An uncertainty evaluation scheme was proposed based on the JJF 1059.1－2012 Evaluation and Expression of Uncertainty in Measurement. Result The results of the uncertainty evaluation for total sulfur determination of actual samples showed that the extended uncertainty of sample 1 was 0.19 mg/m3 (k=2), mainly derived from carbonyl sulfide at 0.18 mg/m3 (k=2), while the extended uncertainty of sample 2 was 0.14 mg/m3 (k=2), mainly derived from hydrogen sulfide at 0.12 mg/m3 (k=2). Conclusion The main sources of uncertainty in total sulfur and individual sulfur compound measurement are sample analysis repeatability and standard substances, and the uncertainty of hydrogen sulfide and carbonyl sulfide mainly contribute to the uncertainty of total sulfur. Twice repeated measurements according practical work are recommended, as increasing repeated measuring times, and using high accuracy standards are recommended to improve the level of measurement uncertainty, it is suggested to use sampling containers, pipeline valves, and other components made with sulfur-resistant adsorption materials, so as to reduce the uncertainty of hydrogen sulfide and carbonyl sulfide individual sulfur compound measurement and ensure data accuracy. |
| Key words: natural gas total sulfur sulfur compound gas chromatography uncertainty |
