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物探与化探  2020, Vol. 44 Issue (6): 1435-1440    DOI: 10.11720/wtyht.2020.1589
  方法研究·信息处理·仪器研制 本期目录 | 过刊浏览 | 高级检索 |
氧化燃烧—气相色谱法测定土壤中的有机碳含量
胡梦颖1,2(), 徐进力1,2(), 朱颖涛3, 张鹏鹏1,2, 张灵火1,2, 徐红纳4, 白金峰1,2, 张勤1,2
1.中国地质科学院 地球物理地球化学勘查研究所,河北 廊坊 065000
2.联合国教科文组织全球尺度地球化学国际研究中心,河北 廊坊 065000
3.交通运输部 天津水运工程科学研究所, 天津 300456
4.牡丹江医学院 药学院,黑龙江 牡丹江 157011
A method for determination of total organic carbon in soil by oxidative combustion and gas chromatography
HU Meng-Ying1,2(), XU Jin-Li1,2(), ZHU Ying-Tao3, ZHANG Peng-Peng1,2, ZHANG Ling-Huo1,2, XU Hong-Na4, BAI Jin-Feng1,2, ZHANG Qin1,2
1. Institute of Geophysical and Geochemical Exploration, Chinese Academy of Geological Sciences, Langfang 065000, China
2. United Nations Educational-Scientific and Cultural Organization, International Center on Global-Scale Geochemistry,Langfang 065000, China
3. Tianjin Research Institute for Water Transport Engineering, Ministry of Transport, Tianjin 300456, China
4. School of Pharmacy, Mudanjiang Medical College, Mudanjiang 157011, China
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摘要 

土壤有机碳作为多目标区域地球化学调查中必须分析的元素,其含量高低影响其他元素在土壤中的迁移和转化过程,是评价土壤质量的重要指标。传统测定土壤有机碳的方法包括了重铬酸钾氧化法和燃烧法等,但前者在实际应用中操作繁琐复杂,对环境也有一定的污染。本文主要采用磷酸(H3PO4)对土壤进行前处理,去除无机碳干扰,再详细探讨了分析仪器工作过程中的最佳条件,包括氧化炉温度、加氧量、氧气压力以及载气压力等,综合建立并优化了使用氧化燃烧—气相色谱法直接固体进样测定土壤中的总有机碳含量的分析方法。实验结果表明,校准曲线相关系数R2良好,达到0.999 9,检出限为0.012%。经国家一级土壤成分分析标准物质验证,测定值与认定值吻合,精密度(RSD, n=12)范围为1.10%~4.11%。该方法分析效率高,操作简单,适用于不同类型、含量的土壤样品有机碳测定。

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胡梦颖
徐进力
朱颖涛
张鹏鹏
张灵火
徐红纳
白金峰
张勤
关键词 土壤有机碳氧化燃烧气相色谱    
Abstract

Soil organic carbon (SOC), as an important element to be analyzed in multi-purpose regional geochemical survey, affects the migration and transformation of other elements in the soil. Therefore, it is a significant index in evaluating the soil quality. The traditional methods of measuring SOC include potassium dichromate oxidation method and combustion method.The former is complicated to operate in practical application and there is also some pollution to the environment. Through the pretreatment of soil with H3PO4 to remove the interference of inorganic carbon, and the detailed discussion of the best conditions in the working process of the analytical instrument, which include the temperature of the oxidation furnace, oxygen adding quantity, oxygen pressure and the carrier gas pressure and some other factors, an analytical method for the direct solid injection and determination of total organic carbon in soil by oxidative combustion and gas chromatographywas established and optimized in this paper. The experimental results show that the correlation coefficient R2 of this method is 0.9999, and the detection limit is 0.012%. According to the verification of the Certified Reference Materials for the Chemical Composition of Soils, the measured value is consistent with the certified value with the precision of 1.10%~4.11% (n=12). This method has the advantages of high efficiency and simple operation, and is suitable for the determination of organic carbon in different types and values of soil samples.

Key wordssoil    organic carbon    oxidative combustion    gas chromatography
收稿日期: 2019-12-16      出版日期: 2020-12-29
ZTFLH:  P632  
基金资助:中国地质调查局地质调查项目(DD20190518)
通讯作者: 徐进力
作者简介: 胡梦颖(1993-),女,硕士,助理工程师,主要从事地球化学样品配套分析方法的研究工作。Email:524682527@qq.com
引用本文:   
胡梦颖, 徐进力, 朱颖涛, 张鹏鹏, 张灵火, 徐红纳, 白金峰, 张勤. 氧化燃烧—气相色谱法测定土壤中的有机碳含量[J]. 物探与化探, 2020, 44(6): 1435-1440.
HU Meng-Ying, XU Jin-Li, ZHU Ying-Tao, ZHANG Peng-Peng, ZHANG Ling-Huo, XU Hong-Na, BAI Jin-Feng, ZHANG Qin. A method for determination of total organic carbon in soil by oxidative combustion and gas chromatography. Geophysical and Geochemical Exploration, 2020, 44(6): 1435-1440.
链接本文:  
http://www.wutanyuhuatan.com/CN/10.11720/wtyht.2020.1589      或      http://www.wutanyuhuatan.com/CN/Y2020/V44/I6/1435
Fig.1  仪器工作原理
Fig.2  炉温与碳信号强度的关系
Fig.3  加氧量和碳百分质量与其认定值比值的关系
Fig.4  氧气压力和碳百分质量与其认定值比值的关系
Fig.5  载气压力和碳百分质量与其认定值比值的关系
指标参数 设置条件
载气压力/kPa 120
吹扫气流速/(mL·min-1) 80
氧气注入量/mL 18
氧气压力/kPa 35
氧化时间/s 7.9
进样延迟/s 10
分析时间/s 170
前加热炉温度/℃ 1000
后加热炉温度/℃ 700
柱温箱温度/℃ 80
Table 1  仪器参数设置
Fig.6  碳标准曲线
样品 12次测定结果/% 平均值
/%
标准值
/%
RSD/%
1 2 3 4 5 6 7 8 9 10 11 12
GSS3 0.51 0.52 0.52 0.52 0.53 0.54 0.53 0.53 0.53 0.53 0.53 0.53 0.53 0.51 1.10
GSS19 0.99 0.99 0.99 0.96 0.97 1.00 0.99 0.99 0.98 1.01 0.99 0.99 0.99 1.00 1.29
GSS29 1.06 1.12 1.08 1.12 1.10 1.12 1.08 1.09 1.06 1.12 1.10 1.08 1.09 1.12 1.93
GSS31 0.94 1.06 1.03 0.98 0.96 1.01 1.05 0.95 0.97 1.03 1.03 0.97 1.00 1.02 4.11
GSS35 2.08 2.03 1.97 2.03 2.07 2.00 2.01 2.07 2.07 1.94 2.02 2.05 2.03 2.00 2.08
Table 2  方法精密度结果
样品号 推荐值/% 测定值/% RE/%
GSS3 0.51 0.52 2.16
GSS10 1.35 1.36 0.52
GSS11 1.07 1.07 -0.09
GSS13 0.62 0.65 5.00
GSS19 1.00 1.00 -0.04
GSS23 (0.50) 0.48 -3.4
GSS25 0.58 0.55 -4.48
GSS27 (0.90) 0.85 -5.78
GSS29 1.12 1.10 -1.70
GSS30 1.02 0.98 -3.63
GSS31 1.02 1.01 -0.59
GSS32 (0.30) 0.29 -2.67
GSS34 0.79 0.77 -2.15
GSS35 2.00 2.05 2.50
Table 3  方法准确度结果
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