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
One of the contaminants in coal is sulphur. The adverse impact of sulfur on coal, such as environmental pollution, degradation of steel quality, and reduction of coal’s thermal value, has led to the attention of sulf...One of the contaminants in coal is sulphur. The adverse impact of sulfur on coal, such as environmental pollution, degradation of steel quality, and reduction of coal’s thermal value, has led to the attention of sulfur separation methods in recent decades. Leaching (chemical dissolution) is one of the best methods for desulfurising coal, reducing sulfur in coal. In this study, hydrogen peroxide as an oxidising agent on sulfuric acid yield in reducing sulfur types of coal and chemical structure and the organic texture of high sulfur coal was investigated. The experiments were designed using a three-level response surface methodology with four duplicate points and 27 experiments. The independent variables studied were temperature, time, stirring speed and ratio of sulfuric acid to hydrogen peroxide. Dependent variables included reduction percentage of total, pyritic and organic sulfur. This study showed that 99.99% of total sulfur, 30.11% of pyritic sulfur and 69.08% of organic sulfur were reduced. These values were obtained at a temperature of 60°C, time 120 min, stirring speed 200 rpm and 3:1 ratio of sulfuric acid to hydrogen peroxide. Significant changes were observed by infrared spectroscopy (FTIR) of the coal structure before and after desulphurisation. On the other hand, the studies showed no specific changes in the bonds related to the organic coal matrix. The results showed that this method could be used as a secure process for removing inorganic and organic sulfur without destroying the organic coal matrix.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One of the contaminants in coal is sulphur. The adverse impact of sulfur on coal, such as environmental pollution, degradation of steel quality, and reduction of coal’s thermal value, has led to the attention of sulfur separation methods in recent decades. Leaching (chemical dissolution) is one of the best methods for desulfurising coal, reducing sulfur in coal. In this study, hydrogen peroxide as an oxidising agent on sulfuric acid yield in reducing sulfur types of coal and chemical structure and the organic texture of high sulfur coal was investigated. The experiments were designed using a three-level response surface methodology with four duplicate points and 27 experiments. The independent variables studied were temperature, time, stirring speed and ratio of sulfuric acid to hydrogen peroxide. Dependent variables included reduction percentage of total, pyritic and organic sulfur. This study showed that 99.99% of total sulfur, 30.11% of pyritic sulfur and 69.08% of organic sulfur were reduced. These values were obtained at a temperature of 60°C, time 120 min, stirring speed 200 rpm and 3:1 ratio of sulfuric acid to hydrogen peroxide. Significant changes were observed by infrared spectroscopy (FTIR) of the coal structure before and after desulphurisation. On the other hand, the studies showed no specific changes in the bonds related to the organic coal matrix. The results showed that this method could be used as a secure process for removing inorganic and organic sulfur without destroying the organic coal matrix.
