A new detection system consisted of a flame ionization detector（FID） and a sulfur chemiluminescence detector（SCD） was developed for sensitive and interference free determination of total sulfur in natural gas by n...A new detection system consisted of a flame ionization detector（FID） and a sulfur chemiluminescence detector（SCD） was developed for sensitive and interference free determination of total sulfur in natural gas by non-separation gas chromatography. In this system, sulfur containing compounds and hydrocarbons were firstly burned in the FID using oxygen rich flame and converted to SO_2, CO_2 and H_2O, respectively. The products from FID were transported into the SCD with hydrogen rich atmosphere wherein only SO_2 could be reduced to SO and reacted with O_3 to produce characteristic chemiluminescence. Therefore, the chemiluminescence of CO found in conventional SCD were eliminated because CO_2 could not be reduced to CO under these conditions. The experimental parameters were systematically investigated. Limit of detection obtained by the proposed system is better than 0.5 mmol/mol for total sulfur and superior to those previously reported. The proposed method not only retains the advantages of the conventional SCD but also provides several unique advantages including no hydrocarbon interference, better stability, and easier calculation. The utility of this technique was demonstrated by the determination of total sulfur in real samples and two certified reference materials（GBW 06332 and GBW（E） 061320）.展开更多
采用硫化学发光检测器(SCD)-气相色谱仪,建立了甲硫醇、乙硫醇、甲硫醚、乙硫醚、二甲基二硫5种有机硫化合物的分析方法。优化色谱柱种类、进样管线材质、配气方式、样品保存时间等参数,考察方法性能指标。结果表明:在最优条件下,5种有...采用硫化学发光检测器(SCD)-气相色谱仪,建立了甲硫醇、乙硫醇、甲硫醚、乙硫醚、二甲基二硫5种有机硫化合物的分析方法。优化色谱柱种类、进样管线材质、配气方式、样品保存时间等参数,考察方法性能指标。结果表明:在最优条件下,5种有机硫化合物线性回归方程相关系数均为0.998以上。定量环进样为1.0 m L时,方法检出限为0.005~0.016 mg/m3;相对标准偏差为0.7%~3.8%。中、高浓度准确度较好,适用于有机硫化合物的测定。展开更多
基金the National Science and Technology Supporting Plan(No.2013BAK12B04)for financial support
文摘A new detection system consisted of a flame ionization detector（FID） and a sulfur chemiluminescence detector（SCD） was developed for sensitive and interference free determination of total sulfur in natural gas by non-separation gas chromatography. In this system, sulfur containing compounds and hydrocarbons were firstly burned in the FID using oxygen rich flame and converted to SO_2, CO_2 and H_2O, respectively. The products from FID were transported into the SCD with hydrogen rich atmosphere wherein only SO_2 could be reduced to SO and reacted with O_3 to produce characteristic chemiluminescence. Therefore, the chemiluminescence of CO found in conventional SCD were eliminated because CO_2 could not be reduced to CO under these conditions. The experimental parameters were systematically investigated. Limit of detection obtained by the proposed system is better than 0.5 mmol/mol for total sulfur and superior to those previously reported. The proposed method not only retains the advantages of the conventional SCD but also provides several unique advantages including no hydrocarbon interference, better stability, and easier calculation. The utility of this technique was demonstrated by the determination of total sulfur in real samples and two certified reference materials（GBW 06332 and GBW（E） 061320）.
文摘采用硫化学发光检测器(SCD)-气相色谱仪,建立了甲硫醇、乙硫醇、甲硫醚、乙硫醚、二甲基二硫5种有机硫化合物的分析方法。优化色谱柱种类、进样管线材质、配气方式、样品保存时间等参数,考察方法性能指标。结果表明:在最优条件下,5种有机硫化合物线性回归方程相关系数均为0.998以上。定量环进样为1.0 m L时,方法检出限为0.005~0.016 mg/m3;相对标准偏差为0.7%~3.8%。中、高浓度准确度较好,适用于有机硫化合物的测定。
