水中溶解态甲烷的快速测定方法研究

    Research on the Rapid Measurement Method of Dissolved Methane in Water

    • 摘要: 为满足油气资源勘探、水环境动态监测等方面的测量需求,提高水中溶解烃类的测量精度和测量时效,研究了水中溶解态甲烷的快速测定方法。采用高纯甲烷气体标准物质制备甲烷饱和水,对甲烷饱和时间进行了优化,结果表明通气60 min后,水中甲烷完全达到饱和状态;通过稀释甲烷饱和水制备了水中甲烷标准溶液系列,用以建立校准曲线。比较了直接进样-气相色谱法、顶空进样-气相色谱法的分析效果,结果表明采用顶空进样分析水中溶解态甲烷时,重复性、灵敏度都要优于直接进样。对顶空进样器、气相色谱仪的测定条件进行了优化,建立了水中溶解态甲烷的快速测定方法,优化后的分析条件为:气液平衡温度70℃、气液平衡时间20 min、进样口温度200℃、柱箱温度80℃、FID 检测器温度230℃。采用顶空进样器-气相色谱仪对水中溶解态甲烷样品进行测定,分析结果显示,在1.16~11.6 mg/L范围内,甲烷的标准曲线呈一次线性相关,相关系数为R2 = 0. 9997,方法检出限为4.6 μg/L。该方法能实现水中溶解态甲烷的定量分析,标准溶液的制备时间短,分析时间仅为5 min,具有快速、准确、易操作的优势。

       

      Abstract: To meet the measurement requirements in aspects such as oil and gas resource exploration and dynamic monitoring of water environment, and to improve the measurement accuracy and timeliness of dissolved hydrocarbons in water, a rapid measurement method for dissolved methane in water is studied. Methane saturated water is prepared using high-purity methane gas standard substance, and the methane saturation time is optimized. The results show that after 60 minutes of ventilation, methane in the water completely reachs the saturated state. A series of standard solutions of methane in water are prepared by diluting saturated methane water to establish the calibration curve. The analytical effects of direct injection - gas chromatography and headspace injection - gas chromatography are compared. The results show that when headspace injection is used to analyze dissolved methane in water, both the repeatability and sensitivity are superior to those of direct injection. The measurement conditions of the headspace sampler and gas chromatograph are optimized, and a rapid determination method for dissolved methane in water is established. The optimized analytical conditions are as follows: gas-liquid equilibrium temperature of 70℃, gas-liquid equilibrium time of 20 min, injection port temperature of 200℃, column oven temperature of 80℃, and FID detector temperature of 230℃. The dissolved methane samples in water are measured by headspace sampler - gas chromatograph, The analysis results show that within the range of 1.16~11.6 mg/L, the standard curve of methane presents a first-order linear correlation, with a correlation degree of R2 = 0.9997, and the detection limit of the method is 4.6μg/L. This method can achieve quantitative analysis of dissolved methane in water. The preparation time of the standard solution is short, and the analysis time is only 5 minutes. It has the advantages of being rapid, accurate and easy to operate.

       

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