An ion chromatographic method with a valve switching facility was developed to determine trace nitrate concentrations in seawater using two pumps, two different suppressors, and two columns. A carbohydrate membrane de...An ion chromatographic method with a valve switching facility was developed to determine trace nitrate concentrations in seawater using two pumps, two different suppressors, and two columns. A carbohydrate membrane desalter was used to reduce the high concentrations of sodium salts in samples. In this method, trace nitrate was eluted from the concentrator column to the analytical columns, while the matrix fl owed to waste. Neither chemical pre-treatment nor sample dilution was required. In the optimized separation conditions, the method showed good linearity( R >0.99) in the 0.05 and 50 mg/L concentration range, and satisfactory repeatability(RSD<5%, n =6). The limit of detection for nitrate was 0.02 mg/L. Results showed that the valve switching system was suitable and practical for the determination of trace nitrate in seawater.展开更多
A method was developed for the determination of tetraethyl ammonium （TEA） by reversed-phase ion- pair chromatography with indirect ultraviolet detection, Chromatographic separation was achieved on a reversed-phase C...A method was developed for the determination of tetraethyl ammonium （TEA） by reversed-phase ion- pair chromatography with indirect ultraviolet detection, Chromatographic separation was achieved on a reversed-phase C18 column using background ultraviolet absorbing reagent - ion-pair reagent - organic solvent as mobile phase. The effects of the background ultraviolet absorbing reagents, detection wavelength, ion-pair reagents, organic solvents and column temperature on the determination method were investigated and the retention rules discussed. Results found that TEA could be successfully analyzed by using 0.7 mmol/L 4-aminophenol hydrochloride and 0.15 mmol/L 1-heptanesulfonic acid sodium mixed with 20% （v/v） methanol as mobile phase at a UV detection wavelength of 230 nm. Under these conditions, the retention time of tetraethyl ammonium was 2.85 min. The detection limit （S/N = 3） for TEA was 0.06 mg/L. The relative standard deviations （n = 5） for peak area and retention time were 0.35% and 0.02%, respectively. The method has been successfully applied to the determination of synthesized tetraethyl ammonium bromide. Recovery of tetraethyl ammonium after spiking was 99.1%.展开更多
为建立一种离子色谱-质谱法检测血液中γ-羟基丁酸(GHB)、氟乙酸钠、亚硝酸钠、草甘膦和草铵膦五种水溶性毒物的方法,选用AS19阴离子色谱柱进行分离,以在线产生的50 mmol/L氢氧化钠为淋洗液等度淋洗,飞行时间质谱仪作检测器,采用电喷雾...为建立一种离子色谱-质谱法检测血液中γ-羟基丁酸(GHB)、氟乙酸钠、亚硝酸钠、草甘膦和草铵膦五种水溶性毒物的方法,选用AS19阴离子色谱柱进行分离,以在线产生的50 mmol/L氢氧化钠为淋洗液等度淋洗,飞行时间质谱仪作检测器,采用电喷雾电离源负离子模式、选择离子监测模式(Selected Ion Monitor,SIM)进行分析,外标法定量。利用离子色谱-质谱法检测五种水溶性毒物简单快速、专属性强、灵敏度高,可为司法鉴定实践提供重要的科学支撑。展开更多
An off-line chelation system combined with ICP-MS technique was developed for the quantitative determination of trace elements in seawater,namely V,Co,Ni,Cu,Zn,Mo,Cd,Pb,U and rare earth elements（REEs）.The system was...An off-line chelation system combined with ICP-MS technique was developed for the quantitative determination of trace elements in seawater,namely V,Co,Ni,Cu,Zn,Mo,Cd,Pb,U and rare earth elements（REEs）.The system was built based on an ion chromatography equipped with MetPac CC-1 chelation columns which had a strong selective chelation to these target elements within a pH range 5.2—5.6.Acidified seawater samples and NH4Ac（2 mol/L） were blended to meet suitable pH before being injected into the chelation column,thus target elements were retained while alkali and alkaline metals were excluded.Then chelated elements were eluted by HNO3（1 mol/L） and samples were collected for ICP-MS analysis.Varying the ratio of input（gen.200 mL） to output（gen.5 mL）,the target elements which were concentrated as 40 times as their concentrations were far beyond instrumental quantification limits.At last,a certificated seawater CASS-4 was introduced and our detected values were in good agreement with those certified values.展开更多
基金Supported by the National Special Fund for Major Research Instrumentation Development(No.2012YQ090229)the Instrument Functional Exploitation and Technical Innovation Fund,Chinese Academy of Sciences(No.yg2010072)the Shandong Provincial Technology Development Plan Fund(Nos.2011SJGZ06,2012SJGZ12,2012424012)
文摘An ion chromatographic method with a valve switching facility was developed to determine trace nitrate concentrations in seawater using two pumps, two different suppressors, and two columns. A carbohydrate membrane desalter was used to reduce the high concentrations of sodium salts in samples. In this method, trace nitrate was eluted from the concentrator column to the analytical columns, while the matrix fl owed to waste. Neither chemical pre-treatment nor sample dilution was required. In the optimized separation conditions, the method showed good linearity( R >0.99) in the 0.05 and 50 mg/L concentration range, and satisfactory repeatability(RSD<5%, n =6). The limit of detection for nitrate was 0.02 mg/L. Results showed that the valve switching system was suitable and practical for the determination of trace nitrate in seawater.
基金supported by the Natural Science Foundation of Heilongjiang Province(Grant No.B201307)the Ministry of Education of Heilongjiang Province(No.12531192)the Program for Scientific and Technological Innovation Team Construction in Universities of Heilongjiang Province(No. 2011TD010)
文摘A method was developed for the determination of tetraethyl ammonium （TEA） by reversed-phase ion- pair chromatography with indirect ultraviolet detection, Chromatographic separation was achieved on a reversed-phase C18 column using background ultraviolet absorbing reagent - ion-pair reagent - organic solvent as mobile phase. The effects of the background ultraviolet absorbing reagents, detection wavelength, ion-pair reagents, organic solvents and column temperature on the determination method were investigated and the retention rules discussed. Results found that TEA could be successfully analyzed by using 0.7 mmol/L 4-aminophenol hydrochloride and 0.15 mmol/L 1-heptanesulfonic acid sodium mixed with 20% （v/v） methanol as mobile phase at a UV detection wavelength of 230 nm. Under these conditions, the retention time of tetraethyl ammonium was 2.85 min. The detection limit （S/N = 3） for TEA was 0.06 mg/L. The relative standard deviations （n = 5） for peak area and retention time were 0.35% and 0.02%, respectively. The method has been successfully applied to the determination of synthesized tetraethyl ammonium bromide. Recovery of tetraethyl ammonium after spiking was 99.1%.
文摘为建立一种离子色谱-质谱法检测血液中γ-羟基丁酸(GHB)、氟乙酸钠、亚硝酸钠、草甘膦和草铵膦五种水溶性毒物的方法,选用AS19阴离子色谱柱进行分离,以在线产生的50 mmol/L氢氧化钠为淋洗液等度淋洗,飞行时间质谱仪作检测器,采用电喷雾电离源负离子模式、选择离子监测模式(Selected Ion Monitor,SIM)进行分析,外标法定量。利用离子色谱-质谱法检测五种水溶性毒物简单快速、专属性强、灵敏度高,可为司法鉴定实践提供重要的科学支撑。
文摘An off-line chelation system combined with ICP-MS technique was developed for the quantitative determination of trace elements in seawater,namely V,Co,Ni,Cu,Zn,Mo,Cd,Pb,U and rare earth elements（REEs）.The system was built based on an ion chromatography equipped with MetPac CC-1 chelation columns which had a strong selective chelation to these target elements within a pH range 5.2—5.6.Acidified seawater samples and NH4Ac（2 mol/L） were blended to meet suitable pH before being injected into the chelation column,thus target elements were retained while alkali and alkaline metals were excluded.Then chelated elements were eluted by HNO3（1 mol/L） and samples were collected for ICP-MS analysis.Varying the ratio of input（gen.200 mL） to output（gen.5 mL）,the target elements which were concentrated as 40 times as their concentrations were far beyond instrumental quantification limits.At last,a certificated seawater CASS-4 was introduced and our detected values were in good agreement with those certified values.
