近岸海水中全氟化合物的液相色谱-离子阱质谱法测定

建立了利用高效液相色谱-电喷雾离子阱质谱(HPLC-ESI-IT-MS/MS)测定近岸海水中多种常见全氟化合物(PFCs)的分析方法.采用固相萃取法(SPE)对海水中的PFCs净化富集,用HPLC-ESI-IT-MS/MS多反应离子监测(MRM)模式对各组分(全氟己烷磺酸、全氟辛烷磺酸、全氟辛烷磺酰胺、全氟己酸、全氟庚酸、全氟辛酸、全氟壬酸、全氟癸酸、全氟十一酸、全氟十二酸)进行测定.在最佳实验条件下,采用基质匹配标准曲线法定量,以消除海水基质的影响,8种目标化合物的检出限介于0.50—1.00 ng·L-1,9种PFCs的回收率在71.0%—130.2%之间,能满足近岸海水中多种PFCs检测的要求.青岛沿岸表层海水样品测定结果显示,全部采样站点的海水样品中均检测到≥4种PFCs,说明青岛沿岸海水中已有一定程度的PFCs污染.     

Optimization of the ionization conditions for the trace analysis of PCDD/PCDF with ion trap MS/MS

Commercial ion trap mass spectrometer provides easy-to-operate MS/MS analysis for the determination of PCDD/PCDF. The limit of quantification is appropriately low (0.2 pg for 23478-P5CDF) because all the stages are performed in the trap and sample losses associated with the ion transportation are minimized. However, if excessive ions are injected into the trap, its electrical fields are distorted and an overall reduction in performance arises. Ionization condition is an important parameter as it affects the amount of the total ions produced. If the amount of interfering compounds are negligible, such as standard solution or cleaned-up sample, lower ionization condition (e.g. electron energy: 30 eV, emission current (EC): 150 μA) is preferable. On the contrary, in case excessive interfering ions are coexisting with PCDD/PCDF, such as crude extract or semi-cleaned-up sample, the ionization condition should be high (e.g. electron energy: 90 eV, EC: 350 μA) for the reproductive quantification.     

吹扫捕集-气相色谱/质谱联用法测定地表水中氯丁二烯

采用吹扫捕集-气相色谱/质谱联用法测定地表水中氯丁二烯。当进样体积为20 mL时,方法在0.100μg/L~50.0μg/L范围内线性良好,检出限为0.05μg/L,标准溶液平行测定的RSD≤3.7%,地表水样加标回收率为91.0%~101%,方法可用于地表水中卤代烃、苯系物等其他21种挥发性有机物的同时测定。     

吹扫捕集- GC/MS法测定水中卤代烃的质量控制指标研究

采用吹扫捕集-气相色谱/质谱联用法,通过实际样品测试及全国多家实验室测定数据统计两种方法,针对水中三氯甲烷、四氯化碳、溴仿、二氯甲烷、1,2-二氯乙烷、1,1-二氯乙烯、三氯乙烯、四氯乙烯等8种卤代烃的平行样测定相对偏差、空白加标回收率及实际样品加标回收率等3个指标,研究了每种卤代烃的质控指标评价标准,提出其平行样测定...     

吹扫捕集-GC/MS-SIM法测定海水中挥发性有机污染物

采用吹扫捕集 -GC/MS -SIM法测定水中挥发性有机物 ,具有定量准确、操作简便等特点 ,检测限可达ng/L级 ,适合环境水中低浓度挥发性有机物的测定。测定实际海水样品 ,其浓度范围在 0 4ng/L～ 1 0 0 0ng/L之间。     

Emission reduction characteristics of a catalyzed continuously regenerating trap after-treatment system and its durability performance

The primary purpose of this study was to investigate the effect of a catalyzed continuously regenerating trap(CCRT)system composed of a diesel oxidation catalyst(DOC)and a catalyzed diesel particulate filter(CDPF)on the main gaseous and particulate emissions from an urban diesel bus,as well as the durability performance of the CCRT system.Experiments were conducted based on a heavy chassis dynamometer,and a laboratory activity test as well as X-ray photoelectron spectroscopy(XPS)test were applied to evaluate the changes of the aged CCRT catalyst.Results showed that the CCRT could reduce the CO by 71.5%and the total hydrocarbons(THC)by 88.9%,and meanwhile promote the oxidation of NO.However,the conversion rates for CO and THC dropped to 25.1%and 55.1%,respectively,after the CCRT was used for one year(～60,000 km),and the NO oxidation was also weakened.For particulate emissions,the CCRT could reduce 97.4%of the particle mass(PM)and almost 100%of the particle number(PN).The aging of the CCRT resulted in a reduced PM trapping efficiency but had no observable effect on the PN;however,it increased the proportion of nucleation mode particles.The activity test results indicated that the deterioration of the CCRT was directly relevant to the increase in the light-off temperatures of the catalyst for CO,C_3H_8 and NO_2.In addition,the decreased concentrations of the active components Pt~(2+) and Pt~(4+) in the catalyst are also important factors in the CCRT deterioration.     

用于气相色谱分析的样品导入技术及其应用

综述了几种用于气相色谱分析的绿色环保型样品导入技术,如静态顶空技术、吹扫捕集技术、固相微萃取技术和热脱附技术的原理及应用情况,并对这几种方法进行了比较。     

吹扫—捕集/气相色谱法测定水中挥发性卤代烃

建立了吹扫—捕集 /气相色谱 /电子捕获检测器联用测定水中 5种挥发性卤代烃分析方法 ,且按国家水质分析标准方法 (GB/T 1 71 3 0 -1 997)所确定的三氯甲烷、四氯化碳、三氯乙烯、四氯乙烯、三溴甲烷 5种挥发性卤代烃进行实验 ,采用 Supelcoport担体层析柱对去离子水处理 ,所获得的纯水无色谱干扰峰 ,本法按国家水质分析标准方法列出的 5种挥发性卤代烃进行测定在国内尚未见报导。当纯水的进样体积为 5 .0 ml时 ,其最低检出浓度为 1× 1 0 - 2～ 6× 1 0 - 4(μg/L)之间 ;相对误差在 1 .1 %～ 2 .4%之间 ;加标回收率在 82 .5 %～ 1 0 8%之间 ;相关系数在 0 .9980～ 0 .9999之间。可快速、高灵敏度、简便、准确、精密地测定水中 5种挥发性卤代烃 ,本法适用于饮用水和地表水中挥发性卤代烃的测定     

燃煤电站湿法烟气脱硫的颗粒物脱除效果

伴随着我国燃煤电站污染物严峻形势,湿法烟气脱硫协同捕集颗粒物越来越受到工程应用部门的重视。从基本理论出发,引入捕集体与颗粒碰撞、拦截与扩散的基本方程,推导并建立多液滴对多颗粒的捕集模型。研究结果表明：直径245 μm的液滴,沉降速度小于气流速度,会被携带出脱硫塔;液滴对PM0.1、PM1、PM2.5、PM5、PM10颗粒物的去除效率为U型曲线,910 μm液滴对颗粒物的去除效率比4 666 μm液滴高近百倍;同等质量浓度,不同粒度分布,脱硫塔除尘性能仍然差异较大。     

Hg-CEMS系统中元素汞发生器的溯源和质控方法研究

参考借鉴美国IEMGTP元素汞溯源协议中规定的4个溯源传递层级以及4种常用的成熟溯源质控方法,研究了在中国现有技术条件下,各种质控方法针对Hg-CEMS中元素汞发生器User generator进行质控的适用性。通过对不同质控方法的测试,显示通过可吸附元素汞的活性炭吸附管采样分析（美国EPA 30B方法）和通过汞渗透源两种对元素汞发生器进行质控的方法在中国目前是可行且科学、可靠的。同时对建立和完善中国的元素汞溯源协议和元素汞发生器质控方法提出了建议。