摘要
通过优化柱温、载气流量、光电倍增管极化电压、氢气和空气流量比(氢空比)、检测器温度等条件,提出了气相色谱-火焰光度检测器(FPD)法测定高炉煤气中硫化氢、羰基硫,以及焦炉煤气中硫化氢、羰基硫、二硫化碳、甲硫醇、甲硫醚、乙硫醇、噻吩、二甲基二硫的含量.样品经不同程序稀释后,采用气相色谱仪分析.在分析高炉煤气时,以GDX-502色谱柱为固定相,在柱温60 ℃、载气流量30 mL·min-1、光电倍增管极化电压900 V、氢气流量80 mL·min-1、氢空比1∶0.67、检测器温度160 ℃条件下检测.在分析焦炉煤气时,以HF-Sulfur色谱柱作固定相,在柱程序升温条件下检测(除进样体积,其他条件和高炉煤气的一致).结果显示:高炉煤气、焦炉煤气中的各组分质量浓度的自然对数值均在一定范围内和对应的响应值的自然对数值呈线性关系.高炉煤气中两种组分的检出限为0.56～0.87 mg·m-3,相对误差(标准气体)为-4.6％～0.88％,测定值的相对标准偏差(RSD,n=5)为0.22％～2.4％;焦炉煤气中8种组分的检出限为0.711～1.145 mg·m-3,加标回收率为 94.4％～105％,测定值的 RSD(n=6)为 1.4％～8.8％.
Abstract
By optimizing the column temperature,carrier gas flow rate,photomultiplier polarization voltage,flow ratio of hydrogen to air(hydrogen-air ratio),and detector temperature,a method of gas chromatography with flame photometric detector(FPD)was proposed for the determination of hydrogen sulfide,carbonyl sulfur in blast furnace gas,and hydrogen sulfide,carbonyl sulfur,carbon disulfide,methyl mercaptan,methyl sulfide,ethyl mercaptan,thiophene,dimethyl disulfide in coke oven gas.The samples were diluted by different procedures and analyzed by gas chromatograph.In the analysis of blast furnace gas,the GDX-502 column was used as the stationary phase.The column temperature was 60 ℃,the carrier gas flow rate was 30 mL·min-1,the photomultiplier polarization voltage was 900 V,the hydrogen flow rate was 80 mL·min-1,the hydrogen-air ratio was 1∶0.67,and the detector temperature was 160 ℃.In the analysis of coke oven gas,HF-Sulfur column was used as the stationary phase,and detection was made under the condition of column temperature program(except for sampling volume,other conditions were consistent with those of blast furnace gas).It was shown that linear relationships between the natural logarithmic value of the mass concentration of each component in blast furnace gas and coke oven gas and the response value were kept in defite ranges.The detection limits of the two components in blast furnace gas ranged from 0.56 mg·m-3 to 0.87 mg·m-3,the relative errors(standard gas)ranged from-4.6％to 0.88％,and the RSDs(n=5)of the determined values ranged from 0.22％to 2.4％.The detection limits of 8 components in coke oven gas ranged from 0.711 mg·m-3 to 1.145 mg·m-3,the recoveries obtained by standard addition method were found in the range of 94.4％-105％,and the RSD(n=6)of the determined values ranged from 1.4％to 8.8％.
基金项目
山西省科技重大专项(2016)(MJH2016-03)
山西省优秀人才科技创新项目(2018)(201805D211037)
山西浙大新材料与化工研究院研发项目(2021)(2021ST-AT-002)
东莞市能源投资集团有限公司攻关项目()
NETL
NSTL
万方数据