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1.
利用气相色谱-质谱联用仪(GC-MS)系统地分析了阿萨巴斯卡地区Mildred泥炭柱37个样品的脂类化合物,研究了它们的组成特征及可能来源。结果表明,样品中检出的正构烷烃、正烷酮、正烷醛、正烷醇、脂肪酸和脂肪酸甲酯均由高碳数化合物构成,并具明显的奇碳或偶碳优势,GC-MS质量色谱图中甾类和萜类极性化合物呈现显著的高峰。根据泥炭分子地球化学分析,Mildred泥炭柱沉积有机质主要来源于原地堆积的高等植物,苔藓类、水生植物对泥炭有机质也有一定程度的贡献,其中松柏、杜鹃花科等木本植物、莎草科草本植物以及泥炭藓类是主要的成炭植物。萜类和甾类极性化合物的分布存在明显差异,萜类化合物主要集中于剖面的上部,其形成与泥炭藓类植物存在联系;甾类化合物来源不具专属性,多与高等植物的输入有关,也可能是受微生物的改造作用而形成。  相似文献   

2.
佟玲  田芹  杨志鹏  潘萌 《岩矿测试》2020,39(4):587-596
近年人工合成麝香在环境中污染状况加剧,该类化合物具有潜在致癌和环境激素作用,对人类健康构成了威胁,因此越来越受到科学工作者的重视。水和土壤等环境样品中的人工合成麝香检测技术发展迅速,并朝着快速绿色的方向发展。人工合成麝香在沉积物中的浓度达到了几个到几千个ng/g的水平,但对于沉积物复杂基质中的多种类人工合成麝香,采取同步提取与净化,并快速分析的方法还有待研究。本文建立了沉积物样品中硝基麝香、多环麝香和大环麝香共三类、14种典型人工合成麝香的快速分析方法。通过实验优化了提取溶剂、提取温度、在线净化吸附剂等条件,大大降低了样品的前处理成本。最终确定样品采用加速溶剂萃取,萃取池中依次装入净化吸附剂(0.4g GCB和1.0g SAX)及5.0g沉积物样品,在80℃条件下采用提取溶剂正己烷-丙酮(4∶1,V/V)循环提取2次,提取液浓缩后采用气相色谱-三重四极杆串联质谱(GC-MS/MS)进行测定。结果表明:14种目标化合物的线性范围为5~200ng/mL,平均添加回收率为70.6%~121.5%,相对标准偏差(RSD,n=7)为0.97%~19.5%。替代物回收率为72.2%~116.8%,方法检出限为硝基麝香0.10~0.19ng/g,多环麝香0.09~0.14ng/g,大环麝香0.11~1.93ng/g。该方法能够满足复杂基质沉积物样品的分析要求。  相似文献   

3.
刘娇  吴淑琪  贾静  佟玲 《华东地质》2019,(4):309-316
文章研究了吹扫捕集-气相色谱-质谱法测定土壤中挥发酚的方法,分析了吹扫捕集各参数对挥发酚测定的影响,优化了吹扫捕集条件和气相色谱-质谱条件。通过与索氏提取技术对比,证明吹扫捕集-气相色谱-质谱法在实际样品检测中具有操作简便、分析周期短、试剂用量少、干扰小等优点,适用于测定沸点较低、溶解度较小的挥发酚,推荐选择经典的索氏提取技术测定沸点较高、溶解度较大的挥发酚。  相似文献   

4.
塔里木盆地海相碳酸盐岩沥青"A"的地球化学特征   总被引:2,自引:0,他引:2  
塔里木盆地采集的海相碳酸盐岩样品经粉碎后在索氏抽提器中用氯仿溶液抽提,正己烷沉淀沥青质后,可溶有机质进行柱色层族组成分离,获得饱和烃、芳烃、非烃,饱和烃和芳烃直接进行气相色谱-质谱分析,非烃经三氟化硼-甲醇混合液酯化后进行气相色谱-质谱分析。结果显示,样品有机质的演化程度高,母质类型以水生生物为主,台地相成烃古环境为富含单质硫的微生物发育的咸化深水还原环境。样品有机质经历过强烈的环化-芳构化过程和去甲基化过程有利于以甲烷为主的天然气的生成。样品的芳烃馏分中检测到C31-16-one、C33-16-one和C35-18-one长链中位酮化合物,推断这些长链中位酮可能是有机酸盐存在的特征生物标识化合物。  相似文献   

5.
佟玲  杨佳佳  吴淑琪 《岩矿测试》2012,31(6):1021-1027
对于复杂基质的样品,采用气相色谱法、气相色谱-质谱法( GC - MS)不能满足当前痕量水平分析的要求,串联质谱已发展成一种有机分析测试的成熟技术可应用于地质调查样品分析.本文建立了气相色谱-串联质谱技术( GC - MS - MS)分析植物样品中有机氯农药及多氯联苯的方法,通过对植物样品(圆白菜、菠菜、胡萝卜、橘子)分析,系统比较了GC- MS-MS与气相色谱-电子捕获检测器(GC-ECD)和气相色谱-选择离子-质谱( GC - SIS - MS)三种分析技术的检出限、定性定量分析结果,确认了分析方法的适用性.GC- MS-MS方法的检出限为0.03~0.29 ng/g,大部分化合物均低于GC -ECD的检出限,是GC - SIS -MS检出限的0.4倍.GC- MS-MS分析表明,圆白菜不含反式-氯丹,排除了GC-ECD的假阳性检出;检测胡萝卜等基质复杂、净化困难的样品,GC- MS-MS也表现出良好的定性定量能力;检出低含量水平样品菠菜含有0.26 ng/g六氯苯,而气相色谱未检出,表明GC- MS-MS显著提高了分析灵敏度,能够对样品中低含量的化合物进行准确定量.在三种分析技术中,GC- MS-MS在样品的准确定性、复杂基质样品分析灵敏度、低含量水平准确定量等方面都具有独特的优势,同时能够应用于复杂样品检测结果的确证.  相似文献   

6.
多氯联苯的环境特性及分析测试进展   总被引:2,自引:2,他引:0  
杨佳佳  吴淑琪  佟玲 《岩矿测试》2009,28(5):444-451
由于多氯联苯(PCBs)在环境样品中残留浓度低,基质复杂干扰多,必须对环境样品进行预处理,并且结合先进的分析测试方法进行分析。文章综述了PCBs的性质及其主要来源;近年来分析PCBs的前处理方法,主要包括加速溶剂萃取、超临界流体萃取、微波萃取、固相微萃取、基质分散固相萃取等提取方法和固相萃取小柱、凝胶渗透色谱等净化方法;目前气相色谱和气相色谱-质谱联用技术发展以及一些新技术在分析PCBs方面的应用,包括全二维气相色谱法、快速气相色谱法、气相色谱-离子肼串联质谱法、高分辨气相色谱-高分辨质谱法等。总结了国内外PCBs的研究现状。  相似文献   

7.
气相色谱-质谱在地下水检测过程中的重要性   总被引:1,自引:1,他引:0  
李松  饶竹  宋淑玲  田芹  赵威 《岩矿测试》2010,29(5):518-522
采用气相色谱法、高效液相色谱法、气相色谱-质谱法对地下水样品中α-HCH、β-HCH、γ-HCH、δ-HCH、p,p’-DDE、p,p’-DDD、o,p’-DDT、p,p’-DDT、六氯苯、苯并(a)芘等组分进行测定时,通过气相色谱-质谱在测量复杂基体待测样品组分中的识别作用、在高浓度待测样品组分检测中的确认作用以及对样品检测结果假阳性现象的判断作用等内容,论证了气相色谱-质谱技术在测定复杂基体或高浓度地下水样品过程中的重要性,确保了地下水调查项目测量数据准确可靠。  相似文献   

8.
建立了一种快速、批量测定盐湖水中碘含量的气相色谱法。碘离子与丁酮通过卤代衍生反应生成碘丁酮,由气相色谱(GC)-电子捕获检测器(ECD)进行定量测定。通过气相色谱-质谱法(GC-MS)确认了3-碘-2-丁酮和1-碘-2-丁酮两种异构体产物。采用两种异构体峰面积之和进行定量计算,标准曲线线性相关系数r20.999,方法的检出限为0.2 ng·L-1,10次重复测定RSD小于2%,加标回收率为94.7%~102%。方法可满足盐湖卤水中微量碘的测定,经验证该方法也可推广至海水、油田卤水、沉积物压榨水和孔隙水等水体中碘离子的快速测定。  相似文献   

9.
田芹  吴淑琪  佟玲  罗代洪 《岩矿测试》2015,34(2):238-244
目前我国有1个有机氯农药(OCPs)分析标准物质,3个多氯联苯(PCBs)分析标准物质;欧洲有1个OCPs分析标准物质和2个PCBs分析标准物质。美国、国际原子能机构和日本等组织研制了沉积物中OCPs、PCBs和多环芳烃的有机分析标准物质,这些标准物质的基质性质、浓度水平与我国地质样品基质性质、实际污染情况不符。本文针对我国土壤类型的分布特点、污染特征及实际样品检测情况,采集典型地区的土壤作为候选物,利用传统的气相色谱-质谱法、气相色谱-串联质谱法、气相色谱-电子捕获检测器法和现代分析技术方法——同位素稀释质谱法,严格按照国家一级标准物质技术规范和相关标准研制了6个土壤有机分析标准物质(编号为GBW07469~GBW07474),基本涵盖了我国典型土壤类型,包括褐土、水稻土、黄壤土和草甸土;定值化合物包括全国地质大调查必测的8种OCPs(α-HCH、β-HCH、γ-HCH、δ-HCH、p,p’-DDE、p,p’-DDD、o,p’-DDT、p,p’-DDT)和选测的7种PCBs(PCB28、52、101、118、153、138、180),含量范围为3.9μg/kg~2.31 mg/kg。此批标准物质的基质性质、目标组分的浓度水平和污染特征与实际环境样品具有较好的一致性,而且目标物种类多,含量范围宽,可以满足我国不同地区、不同程度污染的土壤样品中OCPs和PCBs同时测定的质量监控需求。  相似文献   

10.
植物化石角质层生物标志化合物分析   总被引:1,自引:0,他引:1  
简要介绍了植物化石角质层生物标志化合物研究方法。采用索氏抽提和超声抽提等方法提取出吉林长白八道沟中新世硅藻土中的植物化石角质层和德国Schrotzburg中新世植物化石角质层的溶解有机质,并进行了气相色谱-质谱(GC-MS)分析等实验。结果表明:有机物中只含有少量的正构烷烃、类异戊二烯烷烃、萜类化合物和甾类化合物;植物化石角质层生物标志化合物的采样和化学处理中应注意避免污染,同时应考虑岩相及岩性。  相似文献   

11.
This study assessed the state of waters in Belgrade regarding pollution with musk compounds as the target contaminants. Eleven of these compounds were alicyclic, two were macrocyclic, and one was polycyclic. Solid-phase microextraction was used for the isolation of these compounds from waste, surface and underground waters and from processed water prepared for drinking, while comprehensive orthogonal two-dimensional gas chromatography with mass spectrometry was used as the final analytical method. In wastewater samples, galaxolide was detected in concentrations of 1.13 and 0.40 μg/L, while in the Sava River and underground water its concentrations were 0.09 and 0.038 μg/L. The lowest concentrations of the investigated musk compounds were detected in underground water samples, indicating that this is the cleanest water of all the analyzed sources with respect to musk compounds. Comparing the results of musk compound concentrations determined in surface river water samples and clean river water samples utilized for drinking, a lower concentration of these compounds was detected in the clean river water samples. The majority of musk compounds were found in waters utilized for drinking. Based on the concentration values, we conclude that the analyzed waters are moderately polluted with these compounds.  相似文献   

12.
为了实现自动处理有机色谱分析数据,以Agilent 6890/5973N气相色谱-质谱仪检测地下水中挥发性有机化合物和多环芳烃的数据源为基础,编写了EXCEL应用程序,按批进行数据自动汇总、定性确认和结果计算,设置了对误确认数据的可逆恢复功能;对实验室空白、野外空白、实验室空白加标、实验室平行样、样品基体加标和质控样品回收率等各项质量控制指标进行统计和评价,并对分析方法长期性能的稳定性进行评价;同时生成质量控制报告,提供向数据库录入数据功能。  相似文献   

13.
The distribution of the aromatic steroids and hopanoids in six crude oils was determined using comprehensive two dimensional gas chromatography time-of-flight mass spectrometry (GCxGC-TOFMS) in order to improve their identification and application in geochemical studies. Co-elution between monoaromatic and triaromatic steroids and benzohopanes and their methylated homologues, which are commonly observed in 1D conventional GC, were resolved, with GCxGC facilitating recognition of the compounds. One important feature was that, despite the oils showing mid-oil window maturity characteristics, the distribution of long chain aromatic steroids decreased in lacustrine samples vs. marine samples. This difference in the distribution of long chain and short chain aromatic steroids may reflect the different origins of these oils although this aspect needs further evaluation.  相似文献   

14.
利用内标物,固相萃取剂和选择离子监测气相色谱-质谱分析方法对自然水体和土壤中氯代烃和芳香烃类化合物进行定量检测。分析结果显示,水样的平均误差基本在25%以内,土壤样品在10%以内,误差随着化合物浓度的降低而增大。方法简化了样品处理程序。  相似文献   

15.
黔北务川-正安-道真地区铝土矿位于石炭系黄龙组和二叠系梁山组之间,主要属于沉积型铝土矿。通过气相色谱(GC)与气相色谱-质谱(GC-MS)手段分析铝土矿系钻孔岩心中的生物标志物,发现了含量丰富的正构烷烃、类异戊二烯烷烃、萜类化合物与甾类化合物。对10个样品饱和烃组分GC分析表明,正构烷烃主要呈双峰式分布特征,碳数分布n-C14~n-C35,CPI值范围为0.90~3.45,表现出奇偶优势。姥鲛烷/植烷(Pr/Ph)值为0.38~077,表现出明显植烷优势。对3个样品饱和烃组分GC-MS分析表明,萜烷类化合物以C30藿烷占优势,相对丰度由大到小依次为五环三萜烷、三环萜烷、四环萜烷,并检测出少量的γ-蜡烷。规则甾烷C27-C28-C29呈近L型或V型分布,并含少量4-甲基甾烷。根据生物标志物特征参数,结合岩心样品岩相学特征,确定了铝土矿系中有机质的陆上植物与低等菌藻类双重来源,铝土质沉积时为偏酸性较还原环境,明确了铝土矿系的形成过程受到来自陆上与沉积水体内两个古生态系统的双重作用。  相似文献   

16.
Groundwater samples were collected from 25 sampling sites of the Oropos–Kalamos basin aiming to describe the groundwater quality in relation to geology, lithology and anthropogenic activities of the study area. Chromium speciation analysis, factor analysis, GIS database and geochemical data proved successful tools for the identification of natural and anthropogenic factors controlling the geochemical data variability and for the identification of the redox couple controlling Cr speciation. A Durov diagram is used to classify groundwater quality into five types: Ca–HCO3, Mg–HCO3, Na–Cl, Mg–Cl and Ca–Cl. The groundwater quality of Oropos–Kalamos is influenced by various natural and anthropogenic factors. Evaluation of water quality for drinking and irrigation purposes is discussed.  相似文献   

17.
The karst of the Cradle of Humankind World Heritage Site plays a major role in the assimilation or carrying of acid mine drainage, sewage effluent return flow and agricultural run-off. Infiltration of contaminated water has altered the chemical composition of the natural waters of the karst system. A multivariate statistical method in combination with conventional geochemical and spatial analysis was applied on groundwater and surface water quality samples to determine the spatial extent of hydrochemical impacts from different anthropogenic sources. The application of hierarchical cluster analysis of the major ions (148 samples) recognised three distinct hydrochemical regimes. Cluster 1 is moderately mineralized, especially with regard to chloride, nitrate and sulphate, cluster 2 has a low mineralization with all elements well within the recommended drinking water limits of South Africa and cluster 3 represents highly mineralized samples taken in the vicinity of decanting mineshafts. The cluster solution is confirmed by a simple mixing model, indicating varying contributions of three identified end members (acid mine drainage, treated sewage effluents and pristine dolomitic groundwater) to the groundwater quality in the catchment. The combination of statistical, geochemical and spatial methods in conjunction with end-member mixing analysis provides a reliable method to understand the processes responsible for the groundwater quality variations and to assist in the identification of anthropogenic impacts.  相似文献   

18.
This work characterizes the source rock potential of the Tarfaya Basin and enabled us to reconstruct its geochemical history. Outcrop samples covering different stratigraphic intervals, plus the northwestern part of the Zag/Tindouf Basin (Bas Draa area), were analyzed for total organic carbon (Corg) and total inorganic carbon contents and total sulfur content. Rock-Eval analysis and vitrinite reflectance measurements were performed on 56 samples chosen on the basis Corg content. A set of 45 samples were extracted and non-aromatic hydrocarbons were analyzed by way of gas chromatography-flame ionization detection (GC-FID) and GC-mass spectrometry (GC-MS). Non-isothermal open system pyrolysis at different heating rates was applied to obtain kinetic parameters for modelling petroleum generation from four different source rocks.High quality petroleum source rocks with high Corg content and hydrogen index (HI) values were found for samples of Eocene, Coniacian, Turonian and Cenomanian age. Most samples were carbonate rich and organic/sulfur values were high to moderate. Various maturity parameters indicated immature or possibly early mature organic matter. Based on organic geochemical and petrological data, the organic matter is of marine/aquatic origin (Cenomanian) or a mixture of aquatic and terrigenous material (Eocene). The Early Cretaceous interval did not contain high quality source rocks, but indications of petroleum impregnation were found.  相似文献   

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