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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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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.
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Received: 16 December 2019
Published: 29 December 2020
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Corresponding Authors:
XU Jin-Li
E-mail: 524682527@qq.com;80368070@qq.com
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Working principle of the instrument
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Relationship between furnace temperature and signal intensity of carbon
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Relationship between oxygen adding quantity and the ratio of measured value to the certified value
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Relationship between oxygen pressure and the ratio of measured value to the certified value
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Relationship between carrier gas pressure and the ratio of measured value to the certified value
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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 |
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Instrument parameter setting
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Standard curve of carbon
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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 |
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Precision of the method
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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 |
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Accuracy of the method
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