GC-MS/MS法测定水中多种N-亚硝胺类化合物

采用固相萃取-GC-MS/MS法测定水中10种N-亚硝胺类化合物,通过试验优化前处理和测定条件,使方法在0. 500μg/L～100μg/L范围内线性良好。方法检出限为0. 6 ng/L～2. 1 ng/L,混合标准溶液6次测定结果的RSD 5%。将该方法用于测定实际水样,结果除N-亚硝基二甲胺、N-亚硝基甲基乙基胺和N-亚硝基二丙胺以外,其余目标物均为未检出,加标回收率为73. 1%～97. 6%。     

水环境中26种类固醇激素的分析方法研究

建立了固相萃取-超高效液相-串联质谱法同时测定水环境中26种类固醇激素的分析方法。明确了取样体积为500 m L,Cleanert PEP为富集柱,乙酸乙酯为洗脱剂,甲醇为溶剂进行提取操作。选择了正离子模式,以0. 1%甲酸/甲醇-水为流动相,负离子模式以0. 1%氨水/乙腈-水为流动相,试样经AcquityTMUPLC BEH C18色谱柱分离后,选用质谱检测模式进行定性、定量分析。通过方法验证,26种类固醇激素的方法检出限为0. 3～1. 5 ng/L,测定下限为1. 2～6. 0 ng/L,代表性样品测定结果的相对标准偏差为2. 6%～13. 7%(n=6),加标回收率为71. 2%～121%。该方法操作便捷,灵敏度高,精密度和准确度良好,可适用于水环境中多种痕量、超痕量类固醇激素的定性定量分析。     

动态固相微萃取-气相色谱质谱法测定水中多种异味有机物

采用动态固相微萃取技术富集水样中2-异丙基-3-甲氧基吡嗪、2-异丁基-3-甲氧基吡嗪、2-MIB、β-环柠檬醛、2,4,6-三氯苯甲醚、GSM、α-紫罗酮和β-紫罗酮等8种异味有机物,并用气相色谱质谱法测定。通过优化试验条件,使方法在2. 00 ng/L～100 ng/L范围内线性良好,方法检出限为1. 0 ng/L～4. 4 ng/L。空白水样3个质量浓度水平的加标回收率为81. 0%～121%,6次测定结果的RSD为1. 7%～8. 9%。将该方法用于一水库实际水样的测定,结果 2-MIB、β-环柠檬醛、α-紫罗酮和β-紫罗酮检出,其余均为未检出。     

负吸光度法测定微量氟化物

研究了 F- 与茜素磺酸锆的褪色反应条件 ,建立了一种负吸光度法测定微量氟化物的新方法 ,F- 量在 0～ 1 5μg/2 5 ml范围内与负吸光度值呈线性关系 ,方法已用于环境水中微量氟的测定 ,RSD为 0 .2 5 %～ 4 .2 % ( n=5 ) ,回收率为93.1 %～ 1 0 2 .0 %。     

U PLC- ESI- MS/MS法同时测定水中7种抗生素

采用超高效液相色谱-电喷雾二级质谱联用技术同时测定水中7种抗生素,优化了试验条件.磺胺甲恶唑、诺氟沙星、环丙沙星、氧氟沙星、四环素在1.00 ng/L～1000 ng/L范围内线性良好,定量下限为1 ng/L,土霉素、金霉素在10.0 ng/L-2 000 ng/L范围内线性良好,定量下限为10 ng/L,去离子水和地表水样加标回收率为72.1%-112%,RSD为0.6%～9.2%.     

在线固相萃取-高效液相色谱-串联质谱法测定饮用水中4种兴奋剂

可替宁、可待因、1,7-二甲基黄嘌呤和咖啡因作为药物及其代谢产物广泛应用于日常生活中,其在环境中的残留物可能对人类健康和生态环境安全造成威胁。采用在线固相萃取法进行前处理,酸性条件(0. 1%甲酸水溶液)上样,水样加硫代硫酸钠(1 L水样加0. 1 g硫代硫酸钠)除去余氯后用高效液相色谱-串联质谱法测定饮用水中可替宁、可待因、1,7-二甲基黄嘌呤和咖啡因这4种兴奋剂。当进样体积为1. 0 m L时,方法检出限为0. 633～1. 75 ng/L,测定下限为2. 53～6. 98 ng/L,饮用水样品加标回收率为80. 0%～129%,多次测定均值的相对标准偏差(RSD)5%。方法检出限低,精密度和准确度好,能满足饮用水样品中4种兴奋剂的日常检测。     

甲基汞在鲳鱼中的积累规律初探

建立了气相色谱-冷原子荧光光谱法测定鲳鱼中甲基汞质量比的方法,并通过比较南通海域常见鲳鱼的鱼肉、鱼皮、鱼鳃和鱼内脏的甲基汞质量比水平,初步推断其在鲳鱼体内的富集规律。结果表明:在0～1 000 pg范围内甲基汞标准曲线为y=567. 354 3 x-545. 733 8,r≥0. 999 9,检出限为0. 03 ng/kg。甲基汞在鲳鱼各部位的质量比为2. 11～20μg/kg,RSD 5. 0%,加标回收率为74. 6%～81. 0%,且分布规律为鱼肉鱼皮鱼鳃鱼内脏。该方法前处理简单、精密度和准确度较好,适用于鲳鱼中甲基汞的测定。     

海水、地面水中磷酸盐测定方法

以人工海水、纯水为介质 ,采用先加钼酸盐后加抗坏血酸进行显色 ,在 70 0 nm波长下测定校准曲线 ,线性较好且没有显著性差异 ,方法稳定 ,可同时测定海水和地表水无机磷、地表水总磷。检出限低于 0 .0 1 mg/L;测定天然水样 ,相对标准偏差5.1 %～ 0 .9% ;测定加标水样加标回收率为 95%～ 1 0 5% ;重复测定加标回收率相对标准偏差为1 .3%～ 2 .7% ;重复测定质控样品和标准样品误差范围 - 0 .0 0 2～ + 0 .0 0 5mg/L、- 0 .0 0 8～ +0 .0 0 4 mg/L、- 0 .0 8～ + 0 .0 0 7mg/L,相对标准偏差 0 .8%、1 .2 %、1 .3% ,精密度、准确度可满足方法要…     

我国4个大城市空气PM_(2.5)、PM_(10)污染及其化学组成

报告了 1 995～ 1 996年在中国的广州、武汉、兰州、重庆 4大城市 8个采样点 PM2 .5 、PM2 .5～ 1 0 和 PM1 0 的监测结果。结果表明 ,1 995年 PM2 .5 年均值浓度为 57～ 1 60 μg/m3,比美国 1 997年颁布的标准值 (1 5μg/m3)高 2 .8～ 9.7倍。PM1 0 年日均值为 95～ 2 73μg/m3。除武汉市 1个对照点外 ,其余 7个监测点的 PM1 0 均超过我国空气质量二极标准 (1 0 0μg/m3)2 8%～ 1 73 % ,比美国标准 (50μg/m3)超过更多 ,说明污染是相当严重的。用 XRF分析了 PM2 .5 、PM2 .5～ 1 0 中 4 2种化学元素 ,结果表明 ,燃煤、燃油和其它工业污染的元素 As、Pb、Se、Zn、Cu、Cl、Br、S在这些颗粒物中有明显富集 ,特别是在PM2 .5 中的富集倍数达数十倍至数万倍 ,对人体健康有很大危害     

AMA254汞分析仪测定颗粒物中痕量总汞的研究

采用AMA254汞分析仪测定大气颗粒物和煤中的痕量总汞,建立了直接测定颗粒物中痕量总汞的分析方法.测定结果表明,在汞绝对含量为0～35ng范围内线性良好,测定大气颗粒物和煤中的痕量总汞的检出限分别为0.06ng/m3和0.02ng/g,标准样品测定的RSD≤0.78%,加标回收率为92%～108%.该方法具有无需消解直接进样测定、极其简便、省时等特点,适合多种固体样品中痕量汞的测定.     

同步荧光光谱法测定环境水样中的多环芳烃

为了建立快速测定水体中多环芳烃的方法,用恒波长同步荧光法对14种多环芳烃混合标样进行了分析。在优化的实验条件下,对环境水样进行分析,可以鉴别出11种多环芳烃。14种PAHs在0～1000ng/ml范围内呈良好的线性关系,相关系数r均不小于0.9988,相对标准偏差(RSD)在1.06%～1.67%之间(n=6)。14种PAHs的检出限在0.072～3.9ng/ml之间。该方法应用于污水、样河水样、池塘水样中的多环芳烃检测取得了良好的效果,回收率分别为82.2%～111.0%、86.0%～107.0%、88.0%～106.2%(n=5)。     

Derivative spectrophotometric method for copper determination

A simple, sensitive and selective method by solvent extraction-first derivative spectrophotometry is described for the determination of microamounts of copper in water by means of its reaction and extraction at pH 8.0 with 3-(4-phenyl-2-pyridinyl-5-phenyl-1,2,4-triazine) (PPT) and picrate (2,4,6-trinitro-phenol) into 1,2-dichloroethane. Copper was thus determined in the range 7.5–350 ng/ml with a detection limits (3) of 2.3 ng/ml. The relative standard deviations were in all instances less than 2.0%. The proposed method was successfully applied for the determination of copper in several kinds of water.     

Microtrace Metalloids Speciation in Lakes Water Samples (Poland)

This paper presents the results of the determination of arsenic, antimony and selenium concentrations of inorganic speciation in surface water samples from Gniezno city (western Poland) and its neighborhood. The concentration of elements were up to 1.85 ng/ml for arsenic, 1.61 ng/ml for antimony and 0.45 ng/ml for selenium (detection limits: 0.04 ng/ml for As and Sb and 0.03 ng/ml for Se). A variety of concentrations for the determined elements has been obtained in waters from Gniezno city’s neighborhood and in water from down-town reservoirs which are under strong anthropogenic pressure.     

毛细管低温吸附气相色谱法同时测定空气中痕量甲硫醇和硫化氢

建立了毛细管低温吸附气相色谱同时测定空气中痕量甲硫醇和硫化氢的方法，介绍了冷冻吸附装置的制备方法和样品冷凝吸附流程。甲硫醇和硫化氢分别在0.467ng～5.16ng和0.327ng～3.60ng范围内线性良好，当进样体积为1L时，检出限为0．205μg/m^3和0．213μg／m^3，空白加标平均回收率为88．6％和90．2％，RSD为6.0％和6．5％。     

A new catalytic oxidation method for sensitive quantification of bromate in flours and bottled water using AgNPs

In this paper, a simple and sensitive spectrophotometric method for the determination of nanomolar level of bromate, based on the catalytic effect of silver nanoparticles on the oxidation of acid red 14 by potassium bromate, is described. The reaction rate was monitored spectrophotometrically by measuring the decrease in absorbance of acid red 14 at 516 nm. The detection limit of the method was 8 ng/mL, and the linear range was between 15 and 130 ng/mL. The effects of acidity, concentration of reactants and reaction time, and external ions were also discussed. The optimum reaction conditions were fixed, and some kinetic parameters determined. The relative standard deviation for the determination of bromate at the concentration of 50 ng/mL was calculated to be 0.996 % (n?=?10). The method has been successfully applied to the determination of bromate in flours and bottled waters.     

原子荧光光度法测定工业炉气中的砷

采用原子荧光光度法测定炉气中砷的含量。方法探讨了盐酸酸度对测定结果的影响 ,确定本方法的检测限为2 .1 3ng/ml,样品回收率为 95.2 %～ 97.6%。     

Development of an efficient and sensitive analytical method for the determination of copper at trace levels by slotted quartz tube atomic absorption spectrometry after vortex-assisted dispersive liquid-liquid microextraction in biota and water samples using a novel ligand

This study describes the determination of trace levels of copper by slotted quartz tube atomic absorption spectrometry after dispersive liquid-liquid microextraction. A ligand synthesized from the reaction of salicylaldehyde and 1-naphthylamine was used to form coordinate copper complex prior to extraction. All parameters that influence the output of complex formation, extraction, and instrumental measurement were optimized to enhance the absorbance signal of copper. Under the optimum conditions, about 104-fold enhancement in sensitivity was recorded over the conventional flame atomic absorption spectrometer, corresponding to a 0.51 ng/mL detection limit. The percent relative standard deviation calculated for the lowest concentration (4.8%) indicated high precision for the experimental procedure. Accuracy and applicability of the optimum method were determined by performing spiked recovery tests on urine, lake water, and mineral water samples. Satisfactory recovery results were obtained between 82.2 and 106.3% at four different concentrations. Matrix matching method was also performed to increase the accuracy of quantification, and the percent recovery calculated for 175 ng/mL was 105.14%.     

ASE萃取-SPE净化- HPLC法测定土壤中多环芳烃

建立了加速溶剂萃取-固相萃取净化-高效液相色谱测定土壤中16种多环芳烃的方法,优化了试验条件.方法线性关系良好,16种多环芳烃的检出限在0.412 ng/g～3.974 ng/g之间,空白加标试验的相对标准偏差在1.2%～12.7%之间,基质加标回收率在60.4%～126%之间.实际样品的测定结果表明该方法分离效果好,能够满足土壤分析的要求.     

石墨炉原子吸收光谱法测定土壤中的微量砷

土壤样品经ＨＮＯ３－ＨＣＩＯ４消解处理后，采用Ｎｉ作为基体改进剂，偏振塞曼效应扣去背景，实现了砷的石墨炉原子吸收法的直接测定。该方法操作简单，干扰少，灵敏度高，砷的检测下限为０．７ｎｇ／ｍｌ，样品分析回收率９４％－１０８％，相对标准偏差５．１％。     

三甲基氯硅烷及六甲基二硅氮烷水解产物分析方法研究

研究采用吹扫捕集-气相色谱-质谱法测定三甲基氯硅烷及六甲基二硅氮烷水解产物的分析方法。结果表明,两种物质遇水迅速水解,水解产物均为三甲基硅醇与六甲基二硅氧烷。以该方法测定六甲基二硅氧烷的检出限为0.02ng/ml,精密度为1.3%～10.6%,线性范围为0.05～60ng/ml。水解动力学研究结果表明,三甲基氯硅烷及六甲基二硅氮烷水解产物含量随时间减少而降低,强酸、强碱条件下测试未发现生成其他的水解产物。该方法可为同类污染物的应急测试提供参考。