Chemical composition of the melting surface on the Urumqi No.1 Glacier, Tien Shan Mountains

第4回極域科学シンポジウム個別セッション：[OM] 気水圏11月15日（金） 国立極地研究所 ３階ラウン

直接电位分析法的定位校准和斜率校准

本文阐述了直接电位分析法定位和斜率校准的理论与测量原理。Eemf pM标准曲线法不必考虑定位和斜率校准问题 ;单点定位pMX 直读法 ,只进行定位校准 ,没有完全校正电极理论与实际斜率不一致所产生的测量误差 ;双点定位pMX 直读法在pMS1～pMS2 之间同时进行定位与斜率校准 ,测量的相对误差较

Multiresidue Determination of Organophosphorus Pesticides in Fruits and Vegetables by Gas Chromatography-Negative Chemical Ionization-Mass Spectrometry

建立同时分析果蔬中多种有机磷农药残留。果蔬样品经乙酸乙酯提取剂提取与flOrISIl硅藻土层析柱净化后,以乙硫磷为内标物,采用气相色谱-负化学离子化-质谱法同时的选择离子监测方式对多种有机磷农药残留进行定性与定量分析。结果表明:此方法快速、简便、灵敏度高和选择性好;9种有机磷农药残留的检测限为0.12~1.21μg/kg,平均回收率为76.5%~112%,相对标准偏差为1.45%~11.0%。A gas chromatography-negative chemical ionization-mass spectrometry(GC-NCI-MS) method was established to simultaneously determine 9 organophosphorus pesticide residues in fruits and vegetables.Samples were extracted with ethyl acetate and cleaned up on a Florisil column before GC-NCI-MS analysis in a selective ion-monitoring(SIM) mode.The internal standard used was ethion.The presented method was rapid,simple,sensitive and selective.The detection limits of this method for 9 organophosphorus pesticides were in the range of 0.12-1.21 μg/kg.The average recovery rates of 9 organophosphorus pesticides varied from 76.5% to 112% with a relative standard deviation of 1.45%-11.0%.江西省自然科学基金项目(2009GQH0018);江西省教育厅科学技术研究项目(GJJ09580

GC Determination of Decabromodiphenyl Ether in Electronic Products

提出了气相色谱法测定电子产品中十溴联苯醚的方法。样品先后用甲苯超声提取和浓硫酸提取,所得有机相经硅胶层析柱净化和二氯甲烷洗脱后,以PCb-103为内标物,采用气相色谱法,用电子捕获检测器检测。十溴联苯醚与内标峰面积的比值对十溴联苯醚与内标物质量浓度比值在0.01--10.0 Mg.l-1范围内呈线性,检出限(3S/n)为8.0μg.kg-1。方法用于电视机塑料外壳中十溴联苯醚的测定,相对标准偏差(n=5)为2.2%--8.9%,回收率在92.1%--95.3%之间。Contents of decabromodiphenyl ether(BDE-209) in electronic products was determined by GC.The sample was extracted with toluene and con.H2SO4 in succession.The organic phase was purified and concentrated on silica-gel chromatographic column and eluted with dichloromethane.The dluate was used for GC-ECD analysis after adding PCB-103 as internal standard.Linear relationship between values of peak area ratios of the BDE-209 standard to internal standard and mass concentration of BDE-209 was obtained in the range of 0.01-10.0 mg·L-1,with detection limit(3S/N) of 8.0 μg·kg-1.The proposed method was applied to the analysis of plastic shells of TV-sets,giving values of RSD′s(n=5) in the range of 2.2%-8.9% and recovery in the range of 92.1%-95.3%.国家基础科学人才培养基金(J0630429

The Analytical Application of Moore Absorption Coefficient in Molecule Fluorescence Spectra

阐述摩尔吸光系数、入射光强度、荧光强度、检测器的灵敏度和仪器的光学系统损耗与入射光波长的函数关系， 初步提出了较为完整的分子荧光定性、定量理论表达式.This paper expound the relations between Moore absorption coefficient,intensity of incidence light,intensity of fluorescence,sensitivity of detector,lose of instrument optics system end wavelength.The more complete qualitative and quantitative formula of molecule fluorescence was put forward

Determination of 19 Organophosphorous Pesticides Residues in Milk Drink and Milk Powder by Gas Chromatography-Negative Chemical Ionization-Mass Spectrometry

将气相色谱-负离子化学源质谱法(GC-NCIMS)应用于牛奶饮品和奶粉中19种有机磷农药残留的同时分析。牛奶饮品和奶粉经乙腈提取剂超声提取、Florisil硅藻土和中性氧化铝双净化剂同时净化及正己烷-乙酸乙酯(体积比1∶1)混合洗脱剂洗脱后,以三苯基磷酸酯为内标物,采用GC-NCI MS的选择离子监测方式(SIM)定性与定量分析。当牛奶饮品和奶粉的加标浓度水平为20、100、500μg/kg时,平均加标回收率为64.5%~129%,相对标准偏差为2%~20%;除喹硫磷的方法检出限(MDL)为2.4μg/kg外,其余18种有机磷农药的MDL均小于1.0μg/kg;线性范围为10~500μg/kg,相关系数均大于0.9988,此分析方法成功地应用于牛奶饮品和奶粉中多种痕量有机磷农药残留的分析。A rapid method was developed for the determination of 19 organophosphorous pesticides residues in commercial milk drink and milk powder.Under optimized conditions,the pesticides were extracted from milk drink or milk powder with acetonitrile in an ultrasonic bath and cleaned up on a Florisil and neutral alumina column,and were determined by gas chromatography with negative chemical ionization mass spectrometric detection in the selected ion monitoring mode with triphenyl phosphate as internal standard.The recoveries for all the pesticides studied ranged from 64.5% to 129% with a relative standard deviation range of 2%-20%.The detection limit of the method was less than 1.0 μg/kg for most of the pesticides except for the quinolphos.The linear ranges of the calibration curves ranged from 10 μg/kg to 500 μg/kg with correlation coefficients of 0.998 8.The proposed method was successfully applied to the analysis of these compounds in milk drink and milk powder

Determination of Five Polybrominated Diphenyl Ether Residues in Deep-Sea Fish Oil Using Gas Chromatography-Negative Chemical Ionization/Mass Spectrometry

建立了气相色谱-负离子化学电离质谱法(GC-NCI/MS)同时分析深海鱼油食品中5种多溴联苯醚残留的分析方法。深海鱼油食品用正己烷超声提取、中性与酸性硅胶色谱柱净化和正己烷洗脱后,以PCB103为内标物,采用GC-NCI/MS的选择离子监测方式(SIM)分析;同时探讨了5种多溴联苯醚的NCI/MS特征离子的断裂机理。当空白深海鱼油食品的加标浓度为20.0和100.0μg/kg时,加标回收率为88.6%-111.3%,相对标准偏差为3.8%-13.5%,方法的检测限为0.77-1.34μg/kg,线性范围为1.0-500.0μg/kg,相关系数均大于0.999 2。此方法已成功地应用于深海鱼油食品中5种痕量多溴联苯醚残留的同时分析。Polybrominated diphenyl ethers(PBDEs) are a kind of brominated flame retardants(BFRs),which refer to compounds used in some plastics to impede or even suppress the combustion process.As the emission or disposal of plastics,PBDE residues have been found in both environment and biota.In this work,an analytical method was developed for the simultaneous determination of 5 PBDE residues in deep-sea fish oil.PBDEs were extracted from deep-sea fish oil with n-hexane,cleaned up on a silical gel column,and determined by using gas chromatography-negative chemical ionization/mass spectrometry(GC-NCI/MS) in the selected ion-monitoring(SIM) mode,with PCB103 as the internal standard.Meanwhile,the characteristic ion and fragmentation mechanism of some PBDEs in NCI/MS were evaluated.Recovery studies were performed at 20.0 and 100.0 μg/kg fortification levels for each PBDE,and the recoveries ranged from 88.6% to 111.3% with relative standard deviations between 3.8% and 13.5% for different PBDEs.The limits of detection(LOD) were from 0.77 to 1.34 μg/kg for different PBDEs.The developed method was linear over the range assayed,1.0-500.0 μg/kg,with correlation coefficients larger than 0.999 2.The developed method has also been successfully applied to the determination of PBDEs in several deep-sea fish oil samples and the three most abundant PBDEs(PBDE-47,PBDE-99 and PBDE-100) were found