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邱灵佳, 黄国林, 帅琴, 苏玉. 灼烧法中有机质与总有机碳换算关系的重建及其在页岩分析中的应用[J]. 岩矿测试, 2015, 34(2): 218-223. DOI: 10.15898/j.cnki.11-2131/td.2015.02.011
引用本文: 邱灵佳, 黄国林, 帅琴, 苏玉. 灼烧法中有机质与总有机碳换算关系的重建及其在页岩分析中的应用[J]. 岩矿测试, 2015, 34(2): 218-223. DOI: 10.15898/j.cnki.11-2131/td.2015.02.011
Ling-jia QIU, Guo-lin HUANG, Qin SHUAI, Yu SU. Reconstruction of the Conversion Relationship between Organic Matter and Total Organic Carbon in Calcination Method and Its Application in Shale Analysis[J]. Rock and Mineral Analysis, 2015, 34(2): 218-223. DOI: 10.15898/j.cnki.11-2131/td.2015.02.011
Citation: Ling-jia QIU, Guo-lin HUANG, Qin SHUAI, Yu SU. Reconstruction of the Conversion Relationship between Organic Matter and Total Organic Carbon in Calcination Method and Its Application in Shale Analysis[J]. Rock and Mineral Analysis, 2015, 34(2): 218-223. DOI: 10.15898/j.cnki.11-2131/td.2015.02.011

灼烧法中有机质与总有机碳换算关系的重建及其在页岩分析中的应用

Reconstruction of the Conversion Relationship between Organic Matter and Total Organic Carbon in Calcination Method and Its Application in Shale Analysis

  • 摘要: 有机质与总有机碳(TOC)的换算关系为wo=1.724×wTOC, 难以满足当前页岩气开发的现场测定要求, 需要作出修正。本文以鄂尔多斯盆地南部页岩样品为研究对象, 在传统灼烧法基础上, 采用X射线荧光光谱仪测定页岩组成, 得出影响烧失量的因素; 用热重-差热仪研究页岩灼烧情况, 确定了无机盐不分解而有机质分解的最佳灼烧温度和时间。通过线性拟合灼烧法测得的有机质含量与仪器法测得的有机碳含量间的换算关系, 建立了一种通过测定烧失量来换算总有机碳含量的新方法。在页岩最佳灼烧温度480℃, 灼烧时间1.5 h条件下线性拟合建立了两种新的换算关系, 获得TOC测定值与仪器法的标准值相对误差分别为1.691%、0.486%, 检出限分别为0.41%、1.60%。综合它们的优缺点, 可将测定页岩类样品的换算关系重建为wo=2.125×wTOC。重建的方法通过严格控制灼烧温度, 解决了传统灼烧法中烧失量因无机盐高温分解造成有机质代表性不足的问题, 可用于精确测定页岩中的有机质或有机碳含量。

     

    Abstract: The current function relationship (wo=1.724×wTOC) between organic matter and total organic carbon needs a correction because it is not suitable for the new materials. As a significant index of shale gas exploitations, the determination of total organic carbon needs close attention. In this paper, a description of a modified calcination method that has been used to study samples from the south of Ordos Basin is described. X-ray Fluorescence Analysis (XRF) has been applied to determine the compositions of shale in order to reveal the factor controlling the ignition loss of the calcination method. TG-DTA analysis has been used to determine the calcination conditions, which could distinguish mineral salt whether decomposed or not. A linear relationship could be established by fitting the ignition loss value of the calcination method and standard total organic carbon value (TOC) of the CS analyzer method, which could be applied to determine TOC by the conversion relationship between loss on ignition and TOC. Results show that the best calcination temperature is 480℃, and the preferred reaction time is 1.5 h. Two function conversion relationships have been established at the above-mentioned conditions. The relative errors between values from the conversion relationship and from the equipment analysis are 1.691% and 0.486% with detection limits of 0.41% and 1.60%, respectively. The traditional conversion relationship could be corrected to wo=2.125×wTOC. The proposed method avoids the ignition loss in traditional calcination method that results in under-representation of organic matters for the decomposition of mineral salt at high temperature, and can precisely measure the organic matters or organic carbon in shale.

     

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