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1.
摘要:对颗粒物中常见有机污染物组成、来源及其分析技术进行总结。介绍了常见有机污染物的滤膜采样技术、前处理技术(溶剂萃取和热脱附)和色谱检测技术及所存在的问题。热脱附气相色谱-质谱联用技术在同时测定大气颗粒物中多环芳烃、正构烷烃等半挥发有机物方面具有明显优势。  相似文献   

2.
测定大气颗粒物中金属含量的样品预处理   总被引:3,自引:0,他引:3  
通过综合对比实验,从多种样品预处理方法中筛选出测定大气颗粒物中金属含量的样品预处理方法——HNO3-HClO4热消解提取法。该法操作简便、易于掌握,待测金属及其化合物提取率达90%以上(滤筒样品84%以上),而且空白值低,可与化学法及仪器法配套使用。  相似文献   

3.
成都地区大气颗粒物中复杂有机物的色谱-质谱分析   总被引:11,自引:0,他引:11       下载免费PDF全文
张世森  刘勇 《色谱》1991,9(4):236-241
〕本文报道了应用气相色谱和气相色谱-质谱联用法对成都地区大气颗粒物中复杂有机物的分析结果。实际分析中共鉴定出77种有机物,首次在成都地区大气颗粒物中发现含有烟碱这一新的污染物。同时对苯并[a]等28种主要污染物做了定量测定。结果表明,成都大气中的有机污染状况非常严重,急待采取有力措施加以改善。  相似文献   

4.
色谱分析中样品前处理技术的发展动态   总被引:2,自引:0,他引:2       下载免费PDF全文
黄维妮  林子俺 《色谱》2021,39(1):1-3
作为现代分析领域的重要手段之一,色谱可用于食品、环境、生物等复杂样品的定性与定量分析。而样品前处理是获得理想色谱分析结果的必要前提,它可有效消除基质干扰、浓缩目标分析物、改善分离效能以及延长色谱仪器使用寿命。本文主要依据2020年4-5月Anal Chem新发表和在线录用的有关论文,讨论色谱分析中涉及样品前处理技术方面的最新发展动态。  相似文献   

5.
样品前处理-色谱分析在线联用技术的研究进展   总被引:8,自引:0,他引:8       下载免费PDF全文
钟启升  胡玉斐  李攻科  胡玉玲 《色谱》2009,27(5):690-699
样品前处理是色谱分析中耗时最多、最容易引起误差的关键环节,因此有关样品前处理技术与色谱分析的在线联用的研究已成为分析化学的前沿课题。本文综述了近年来各种样品前处理技术与色谱分析在线联用的研究进展,包括固相萃取、固相微萃取与液相微萃取、膜辅助萃取、场作用辅助萃取、气相萃取、热解吸以及微芯片分离技术。  相似文献   

6.
临床样品微量元素分析过程中样品制备技术的进展   总被引:1,自引:0,他引:1  
对临床样品微量元素分析过程中的样品制备技术的最近进展进行了评述,主要从直接稀释、湿法消解、干式灰化及微量元素形态分析的样品预处理技术等几方面进行了分别介绍。  相似文献   

7.
微波能用于酵母中海藻糖高效液相色谱分析样品制备的研究   总被引:12,自引:0,他引:12  
利用微波能提取酵线中的海藻糖,建立了一种海藻糖分析样品的快速制备方法。高效液相色分析结果表明,无论是提取选择性、还是提取时间消耗,用微波法提取均具有常规提取法所无法比拟的优越性。经20s微波处理后,海藻糖酶已失活,故有效防止了提取过程中海藻糖的降解。微波提取不失为一种良好的样品的制备方法,尤其适用于对酵母低谢的研究。  相似文献   

8.
对近几年国内外大气颗粒物中Cr(VI)的采样、样品贮存、Cr(III)与Cr(VI)的分离技术及Cr(VI)的检测手段进行了系统介绍,并对大气中Cr(VI)的在线监测技术进行了初步探讨,为环保、卫生等部门进行大气颗粒物中Cr(VI)的监测及质量控制提供了参考。  相似文献   

9.
气相色谱-质谱法测定大气颗粒物中的有机胺类物质   总被引:1,自引:0,他引:1  
建立了大气颗粒物中有机胺类物质的气相色谱-质谱(GC-MS)分析方法.样品用超纯水超声萃取,然后在碱性条件下,用苯磺酰氯(Benzenesulfonyl chloride,BSC)衍生化,衍生物用二氯甲烷萃取,最后用DB-5MS色谱柱分离测定,实现了13种有机胺(包括7种脂肪胺、2种杂环胺和4种芳香胺)的同时测定.本方法的仪器检出限(S/N=3)和定量限(S/N=10)分别为0.00008~0.017 μg/mL和0.00026~0.0565 μg/mL; 标准曲线线性相关系数为0.9903~0.9996,相关性良好;相对标准偏差(RSD)均小于30%, 除低浓度加标水平的甲胺和苯甲胺,其余样品基质加标平均回收率为54.4%~159.7%,大部分胺具有较高的精密度与准确度.将本方法应用于广州城区PM2.5样品的检测, 共检出有机胺9种,其中甲胺、二甲胺和二丁胺约占9种有机胺总和的90%,是PM2.5中主要胺类物质,而丙胺浓度最低,浓度小于1.0 ng/m3.  相似文献   

10.
大气颗粒物的仪器分析方法   总被引:2,自引:0,他引:2  
对大气总颗粒物和单颗粒物仪器分析方法进行了简要介绍和评述,并对当前研究进展进行了综述,引用文献39篇。  相似文献   

11.
凹凸棒石是一种纤维状的硅酸盐黏土矿物,在中国储量丰富。凹凸棒石具有机械强度良好、比表面积大、离子交换容量适中和易修饰等优点。比如凹凸棒石表面的羟基可作为改性位点,有利于凹凸棒石的表面功能化。可通过水热改性、酸改性、热改性和表面功能化改性等方法实现对凹凸棒石的改性,使材料的分散性、导电性等性质发生变化,并提高复合材料的吸附性能和催化性能,从而设计制备多种改性凹凸棒石及其复合材料以扩展其应用范围。该文综述了上述凹凸棒石的改性方法和近5年来凹凸棒石及其复合材料在分离及传感分析中的应用研究进展,包括样品前处理、色谱分析、吸附净化等分离分析以及荧光、电化学、比色等传感器构建等方面。最后总结并提出了凹凸棒石未来的发展趋势。  相似文献   

12.
    
Capillary zone electrophoresis with indirect UV detection was developed for the simultaneous analysis of inorganic anions and organic acids using a mixed solution of 2,6-pyridinedicarboxylic acid and cetyltrimethylammonium hydroxide as the background electrolyte (BGE). The parameters which influence the separation, such as indirect UV detection wavelength, BGE conditions, applied voltage and extraction conditions were investigated. Thirteen inorganic anions and organic acids were detected within 20 min. The calibration curves of each analyte were linear with correlation coefficients greater than 0.991. The relative standard deviations (= 10) of the peak areas ranged from 0.6% to 3.3%. The detection limits for these species ranged from 0.4 to 1.4 mg/L at a signal-to-noise ratio of 3. The recovery rate of each analyte was more than 80% under optimised extraction conditions, except for nitrite. The proposed method was applied towards the analysis of inorganic anions and organic acids in the atmospheric particulate matter using an Andersen sampler. The particle size of the particulate matter was determined, but not the size of the anions.  相似文献   

13.
    
Aluminium is the most common substrate in studies using impactors for the measurement of the number or the weight of size-segregated atmospheric particulate matter (PM), as its characteristics perfectly fit impactor requirements. However, its use is not recommended by manufacturers when one of the purposes of the study is the determination of the metal content in the sample. The aim of this work was to develop an efficient analytical procedure for the removal and acid digestion of PM samples collected on aluminium foils by a cascade impactor to perform the determination of metals. The possibility of performing the trace metal analysis of PM samples collected using aluminium foils is of great importance, as it allows the determination of an accurate size distribution and the elemental composition of the PM collected on each impactor stage. Two procedures were optimised by using different digestion and analysis techniques. Both procedures were then applied to the two halves of several Dekati low-pressure impactor (DLPI) samples, and the results were critically compared. The two procedures proved to be effective in the determination of extremely low concentrations of a large suite of analytes in different size fractions of PM emitted by a brake system.  相似文献   

14.
静态灼烧氧化法制备有机碳同位素质谱分析样品   总被引:6,自引:0,他引:6       下载免费PDF全文
针对目前国内大多数实验室采用密封安瓶法制备有机碳同位素质谱分析样品所存在的不足之处,设计了呈套静态灼氧化法制备有机碳同位素质谱分析样品的实验系统,该系统具有实验精度高,操作方便,经济安全等特点,适合于在国内同位素实验室中推广应用。  相似文献   

15.
    
A novel multi-analyte method for the simultaneous determination of 46 compounds of environmental concern, most of them belonging to the category of persistent organic pollutants, was developed using high-performance liquid chromatography and the results were compared to those obtained by gas chromatography. This study was performed in perspective of a cumulative exposure assessment of substances of health concern in environments where high levels, relatively to airborne particulate matter, can be found. The target compounds included polychlorinated biphenyls, brominated flame–retardants and derivatives of polycyclic aromatic hydrocarbons.

The multi-analyte method was evaluated in air particulate matter in terms of reproducibility, linearity, recovery, limits of detection and quantification and matrix effect. The recovery was above 70% for all the analytes, whereas limits of quantification ranged between 23 and 390 pg?m?3 in liquid chromatography and less than ten times in gas chromatography–mass spectrometry.

Matrix effect was generally negligible for both the techniques, except the case of the detection of oxygenated derivatives of polycyclic aromatic hydrocarbons by gas chromatography.

In order to demonstrate the efficacy and to assess the method performances (accuracy and precision), both the techniques were applied to standard reference materials, and the results were compared, discussing their advantages and disadvantages.

The method was finally applied to a real sample of indoor airborne particulate matter with aerodynamic diameter ≤4 μm (PM4).

We demonstrated that liquid chromatography was the only technique able to analyse the 46 compounds, including thermally degradable ones, with a single chromatographic run without derivatisation steps. On the other hand, gas chromatography still presents higher sensitivity for the detection of some of the investigated compounds. This study can be considered only explorative and further improvements can be expected with new-generation LC-MS instruments (10–100 times more sensitive).  相似文献   

16.
    
Porous cage materials with certain dimensions, sizes, shapes, and functions have been regarded as promising materials for sample preparation, chromatographic separation, and detection process. In contrast to infinite frameworks such as metal-organic frameworks or covalent organic frameworks, porous cage materials are constructed from discrete molecules containing at least one internal cavity. The well-defined cavities in porous cage materials provide opportunities for non-covalent interactions. These interactions can be programmed into the ligand design or supramolecular cage constructing using the cages as building blocks, offering various host-guest recognition with great selectivity. In this review, we desire to elucidate the fundamental principles governing the design and fabrication of porous cage materials with well-defined cavities, good solvent processability, and modifiable groups, the applications of these porous cage materials in sample preparation, chromatographic separation, and detection were discussed. The recent advantages of porous cage materials for the analysis process were summarized. We state the potential of these materials and provide an outlook for further application strategies. We expect that this review can inspire interest in the porous cage materials research area for analysis.  相似文献   

17.
    
《Analytical letters》2012,45(2):231-258
Abstract

Interest in hair analysis as an alternativ or complementary approach to urinalysis for drug abuse detection has grown in recent years. Hair analysis can be particularly advantageous for drugs and their enantiomers.

More than hundred pharmaceuticals, drugs of abuse agents are reported to be detectable in human and animal hair. This article reviews the aalysis of drugs and drug metabolites by chromatographic procedures, incuding the pretreatment steps, and the xtraction methods. Tihe eneral tendency in the last years, to highly sophisticated techiques gas chromatography–mass spectrometry (GC–MS–NCI), high pressure liquid chromatography–mass spectrometry (HPLC–MS), gas chromatography–mass spectrometry–mass spectrometry (GC–MS–MS) well illustrates this constant fight for sensitivity.  相似文献   

18.
张成江  潘加亮  张卓旻  李攻科 《色谱》2014,32(10):1034-1042
微孔有机聚合物(microporous organic polymers,MOPs)是一类由轻元素组成的新型多孔材料,具有骨架密度低、比表面积大、孔尺寸可调控、表面可修饰、化学和物理性质稳定等优点。近年来,MOPs在样品前处理领域展现出巨大的应用潜力。本文综述了MOPs的结构类型及合成方法,以及MOPs在固相萃取、批处理吸附萃取、整体柱和传感膜等样品前处理技术中的应用。  相似文献   

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