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1.
气相色谱-质谱联用法测定土壤中16种多环芳烃   总被引:1,自引:0,他引:1  
张小辉  王晓雁 《岩矿测试》2010,29(5):535-538
应用加速溶剂萃取气相色谱-质谱联用法测定土壤中16种多环芳烃。确定了二氯甲烷-丙酮(体积比1:1)作为提取溶剂,方法检出限为0.10~3.90ng/g,加标回收率为72.6%~123.5%。方法检出限较低,精密度好,适用于土壤样品中多环芳烃的分析。  相似文献   

2.
本文建立了S-916快速溶剂萃取仪(Buchi瑞士)快速萃取-气相色谱-质谱仪(GC-MS)联用测定土壤中15种多环芳烃(PAHs)含量的方法。土壤样品经正己烷、丙酮快速溶剂萃取,除水浓缩后,利用硅酸镁小柱进行净化,直接进GC-MS测定。结果表明,在5.01000.0μg/L浓度范围内,15种PAHs的相关系数均在0.996以上,RF RSD<12%,加标回收率在80%117%之间,15种PAHs的最低检出限均低于0.40μg·kg^-1.该方法灵敏、快速、准确可靠,完全满足实验室对土壤中PAHs的检测要求,可为土壤中多环芳烃(PAHs)的污染情况提供快速检测依据。  相似文献   

3.
杨清 《岩矿测试》2022,(3):404-411
多环芳烃(PAHs)是一类具有致癌、致突变、致畸的碳氢化合物,具有较高的辛醇-水分配系数,易被土壤颗粒吸附而影响环境和人体健康。过硫酸钠(Na2S2O8)氧化法是近些年来国内外修复PAHs污染土壤较为常用的方法,但现阶段在测定修复后土壤中PAHs含量、进行土壤修复效果评估时亟待解决的问题是:经该方法修复的土壤,若土壤中残留有过硫酸钠,在样品前处理过程中由于提取温度较高,可能会进一步加速多环芳烃的氧化反应,从而影响土壤中PAHs的准确测定。本文建立了一种在修复后土壤中加入还原剂抗坏血酸,与残留的过硫酸钠反应生成脱氢抗坏血酸,采用索氏提取结合气相色谱-质谱法(GC-MS)同时测定土壤中16种PAHs的方法,PAHs加标回收率为76.2%~110.0%。而修复后土壤若不加还原剂直接进行索氏提取,用GC-MS测定,可能会使部分PAHs及替代物的测定不准确,PAHs加标回收率仅为6.0%~72.4%。通过对比分析表明,在样品提取前加入还原剂,可以有效地消除残留过硫酸钠的影响,提高测定修复后土壤中PAHs含量的准确性。  相似文献   

4.
为了解广州地区蔬菜基地有机污染物的分布情况,选取了6个代表性基地进行调查采样,测试分析了表层土壤、蔬菜及灌溉水中15种邻苯二甲酸酯(PAEs)化合物、16种多环芳烃(PAHs)化合物和19种有机氯农药(OCPs)化合物的质量分数及质量浓度.结果表明:在15种PAEs化合物的总质量分数(w(ΣPAEs))中,土壤样品为158.0~4 321.0 ng/g,蔬菜样品为1 134.0~48 576.0 ng/g;水样中15种PAEs化合物的总质量浓度(ρ(ΣPAEs))为632.0~14 271.0 ng/L;就单个化合物而言,以DiBP、DBP、DEHP三种污染物为主,其三项之和占所有PAEs质量分数的97.5%~99.1%;在16种PAHs化合物的总质量分数(w(ΣPAHs))中,土壤样品为28.48~1 121.96 ng/g,蔬菜样品为238.09~1 000.61 ng/g;水样中16种PAHs化合物的总质量浓度(ρ(ΣPAHs))为338.21~1 239.78 ng/L;在19种OCPs化合物的总质量分数(w(ΣOCPs))中,土壤为0.04~71.28 ng/g,蔬菜为1.08~9.18 ng/g.总体上看,各基地土壤中DBP质量分数均超标,多环芳烃类在灵山、花东、黄埔菜地土壤中存在轻微污染,有机氯农药均未出现污染.  相似文献   

5.
The purpose of this study is to determine the degree of contamination caused by polycyclic aromatic hydrocarbons (PAHs) in oily sludge and soils around it in the Zhongyuan Oilfield. The contents of polycyclic aromatic hydrocarbons in oily sludge samples were determined with HPLC. The contents of PAHs of oily sludge from three different oil production plants vary from high to low in the order of the Wenming oily sludge dumping site of No. 3 Oil Production Plant (3W)>the Mazhai oily sludge dumping site of No. 3 Oil Production Plant (3M)>the Wen’er oily sludge dumping site of No. 4 Oil Production Plant (4W). Naphthalene, acenaphthylene, acenaphthene, fluorine and phenanthrene are the major pollutants of PAHs in oily sludge. The contents of PAHs in soil samples around the oily sludge dumping sites vary widely from 434.49 to 2408.8 ng/g. Naphthalene, acenaphthene, fluorine, phenanthrene and pyrene are the characteristic factors of PAHs in soil samples of 3M and 3W, and naphthalene, acenaphthene, fluorine and phenanthrene are the characteristic factors of PAHs in soil samples of 4W. According to these data and the ratios of Fl/Py, PAHs in oily sludge samples come mainly from petrogenic sources, and soil samples are divided into petrogenic soil samples and mixed-source soil samples, and both petrogenic and pyrogenic soil samples in terms of the sources of PAHs. The classification by Nemero index P indicates that soils around the oily sludge dumping sites have been seriously polluted.  相似文献   

6.
An investigation for the analysis of polycyclic aromatic hydrocarbons in airborne particulates using thermal desorption and gas chromatography-mass spectrometry is described. Samples are obtained from ambient air using fibreglass filters and the volatile material from the filter is thermally desorbed to gas chromatograph. A 30 meter capillary column is used to separate the hydrocarbons and eight polyaromatic hydrocarbons are used to test the method and recovery is >95%. The eight polycyclic aromatic hydrocarbons anthracene, phenanthrene, fluoranthrene, pyrene, benzo (a) anthracene, chrysene, benzo (a) pyrene and benzo (e) pyrene were the most abundant PAHs found in the samples of ambient air with current method at Uxbridge-London. Application of the measurement of polycyclic aromatic hydrocarbons in ambient air samples shows that the hydrocarbons trapped in the particle phase to a lesser degree at higher ambient temperature. In conclusion a method has been developed to transfer the PAHs in particle phase from a filter to GC-MS by thermal desorption. A standard mixture of PAHs, when absorbed onto the filter, did lead to strong analyte absorbent interactions by the high percent recovery of the sample.  相似文献   

7.
A study of polycyclic aromatic hydrocarbons pollution in roadside soil was conducted in developing city environment of northern India during autumn and winter season to ascertain the contamination levels and their distribution behavior in soil. The concentration of polycyclic aromatic hydrocarbons was determined at ten locations of Jalandhar city, Punjab in India at 1, 2 and 3 m distances from roadside in soil covering all the major traffic intercepts within city. The samples were extracted in acetone and dichloromethane (1:1) using soxhlet extraction. The extracts were then filtered on a silica gel micro column to remove impurities and elute was subjected to GC-FID. The total average concentration (city average) was found to be 4.04 ?g/g and 16.38 ?g/g during winter and autumn respectively. DiBenzo (ah) Anthracene and Benzo (a) Pyrene were the individual polycyclic aromatic hydrocarbons found in highest concentration at all the intercepts ranging between 0.008 to 28.4 ?g/g during winter and 0.01 to 252.55 ?g/g during autumn. Average concentration of non-carcinogenic and carcinogenic polycyclic aromatic hydrocarbons during winter and autumn was found to be 2.1 and 6.4 and 4.74 and 35.08 ?g/g respectively. The average ratio of non-carcinogenic and carcinogenic Polycyclic Aromatic Hydrocarbons was found to be 1:3 during winter, and 1:7.6 during autumn at most of the intercepts. Total carcinogenic polycyclic aromatic hydrocarbons concentration was found quite high (80 %) in comparison to non-carcinogenic polycyclic aromatic hydrocarbons (20 %) at most of the intercepts.  相似文献   

8.
A solvent–water extraction method was proposed as an assessment tool to estimate the bioavailability of polycyclic aromatic hydrocarbons in coal–tar-contaminated soils. The approach taken was to measure the percent of polycyclic aromatic hydrocarbons extracted by a solvent–water mixture and comparing the results with the percent of polycyclic aromatic hydrocarbons degraded in a soil slurry reactor. Five soil samples from three former manufactured gas plant sites and a coal–tar disposal site which were operated between 1880 and 1947, and 1945 and 1950, respectively, in Iowa, USA were used in this study. Extraction experiments were conducted using acetone–water or ethanol–water mixtures with solvent volume fractions ranging from 1.0 to 0.4 (v/v). The percent of polycyclic aromatic hydrocarbons extracted from the various soils decreased as the volume fraction of the solvent in the solvent–water mixture was reduced. An acetone–water mixture of 0.6 was found to be appropriate in correlating the percent of polycyclic aromatic hydrocarbons degraded to the percent of polycyclic aromatic hydrocarbons extracted. For the first correlation, the percent extracted and the percent biodegraded were modified by using the molecular weights and log K ow of polycyclic aromatic hydrocarbons, respectively. For the second correlation, the equation relating the percent extracted and the percent biodegraded was modified using soil properties such as organic carbon content and percent of clay and silt. Although the experiments were conducted for a limited number of soils, the extraction method appeared to be a good starting point in estimating the bioavailability of polycyclic aromatic hydrocarbons in coal–tar-contaminated soils.  相似文献   

9.
湖州市不同土地利用类型土壤中多环芳烃的分布及来源   总被引:1,自引:1,他引:0  
林琳  郑俊  杨晓红  缪丽娜  许健  杨笑 《岩矿测试》2010,29(6):687-690
建立了原子发射光谱法测定独居石矿物中钇组稀土元素的分析方法。在260.00~360.00 nm波段内,选择不受干扰的分析谱线,用炭粉作缓冲剂,钪作内标元素,样品不需要化学处理,不需分离,可直接采用原子发射光谱法测定钇组稀土元素。方法相对标准偏差(RSD,n=12)为1.6%~6.2%,相对误差RE<±12.0%,方法简单、快速、可行。  相似文献   

10.
研究了海洋沉积物提取液中28种多氯联苯(PCBs)、16种多环芳烃(PAHs)和21种有机氯农药(OCPs)在硅胶-氧化铝复合净化柱上的同时净化与分离效果,结果表明:在充填4 cm3%去活化氧化铝-6 cm 3%去活化硅胶的8 mm i.d×15 cm固相萃取净化柱上,使用10 mL正己烷作为淋洗PCBs的分割点,可实现PCBs、PAHs和OCPs的满意分离,更有利于PCBs与高环数PAHs、极性较强OCPs的分离。继续用20 mL正己烷-二氯甲烷混合液(体积比1∶1)洗脱,28 PCBs、16种PAHs和21种OCPs均可获得有效回收,回收率分别为75%~110%、76%~115%、75%~130%。经海洋沉积物标准参考物质验证,该方法实用、可靠,流程简单,试剂消耗少,成本低,适用于海洋环境地质调查中基质复杂沉积物样品的定量分析。  相似文献   

11.
水体悬浮颗粒物的扫描电镜与X射线能谱显微分析   总被引:3,自引:0,他引:3  
盛东  胡忻  刘锡尧 《岩矿测试》2010,29(6):683-686
通过对湖州地区74个土壤样品多环芳烃含量的测定,分析了湖州市不同土地利用类型土壤中多环芳烃(PAHs)的含量特征及污染水平。结果表明,湖州地区PAHs各组分的含量均有检出,各种土地利用类型表层土壤均受到一定程度的PAHs污染,但均小于荷兰土壤修复标准;湖州市区耕地中PAHs的含量最高;从PAHs低环/高环比值小于1以及芘/苯并(a)芘比值小于2,反映了湖州地区土壤中PAHs主要是由燃煤和生活污染产生的。  相似文献   

12.
An off-line solid-phase extraction procedure followed by high-performance liquid chromatography with ultraviolet detection for the determination of 16 priority polycyclic aromatic hydrocarbon pollutants in aqueous matrices was described. Diverse aspects determining extraction efficiency such as packing type (disk or cartridge), elution solvents and addition of organic modifiers to the sample were evaluated. Elution with acetonitrile yields the highest recoveries. Rinsing the sample bottle with acetonitrile and combining the rinse with the sample extract avoids the adsorption of polycyclic aromatic hydrocarbons on the walls of the water containers. The use of isopropanol or methanol 10 % (V/V) was the most appropriate amount for the enrichment of 2- to 6-ring aromatic compounds only on C18 cartridge. The recoveries for all studied polycyclic aromatic hydrocarbons are ranged from 71.4 to 95.2 % for a treated water samples of 500 mL. The proposed method gives very low detection limits (subnanograms per liter) and it has been applied to drinking water, surface water and industrial effluent (oil refinery) samples with good results.  相似文献   

13.
南黄海中部海水中多环芳烃的分布特征   总被引:1,自引:0,他引:1  
2007年9月进行了2007南黄海海洋环境调查,并采集各个调查站位的表层、中层、底层海水及表层沉积物。利用液-液萃取法对采集到的样品进行前处理,并用气相色谱-质谱法检测海水中的多环芳烃。结果显示,监测站位中表层海水中总多环芳烃的含量范围是15.76~233.39ng/L,南黄海中部海水中多环芳烃的组成以2环的萘为优势组分;各种多环芳烃的含量与国际生物学组织或国家制定的评价水生生物暴露于水体的安全食用标准相比虽未超标,但个别组分如荧蒽的含量已达到生态毒理评价标准。  相似文献   

14.
土壤pH值对土壤多环芳烃纵向迁移影响的模拟实验研究   总被引:6,自引:0,他引:6  
康耘  葛晓立 《岩矿测试》2010,29(2):123-126
影响土壤多环芳烃(PAHs)纵向迁移行为的环境因素很多。文章以氧化钙和冰乙酸改变采自徐州土壤的pH值水平,人工装填土柱进行纵向淋滤试验,研究pH值对土壤PAHs纵向迁移行为的影响。结果表明,土壤pH值的变化加强了PAHs在土柱中的纵向淋滤能力,表层土壤中的PAHs可迅速向底层转移;不同种类的PAHs淋滤特性表现不同,pH值增加更能增强低环PAHs的迁移淋滤能力,pH值降低则更能促进高环PAHs从土壤表层向深部迅速迁移。  相似文献   

15.
建立了用加速溶剂萃取,气相色谱-质谱法同时测定河流沉积物中16种多环芳烃和19种有机氯农药的分析方法,优化了萃取溶剂、萃取温度和时间、凝胶渗透色谱收集时间、固相萃取洗脱溶剂和洗脱体积等条件。16种多环芳烃的方法检出限在0.15~0.59 ng/g,加标回收率为82%~102%,相对标准偏差(RSD,n=5)为1.1%~4.5%。19种有机氯农药的方法检出限在0.14~2.23 ng/g,加标回收率为71%~108%,相对标准偏差(RSD,n=5)为1.0%~4.5%。实际样品的测定结果表明,该方法分离效果较好,能够满足沉积物样品中多环芳烃和有机氯农药的分析要求。  相似文献   

16.
Studies of polycyclic aromatic hydrocarbons (PAHs) in the surface soil were conducted in Huizhou City, which is located in the Pearl River Delta, South China. Sixteen PAHs in 42 soil samples were detected. The results showed that 4 components of PAHs were detectable in all soil samples, and other 12 components were also detectable to some extent. The total PAHs contents range from 35.40 to 534.5 μg/kg with the mean value of 123.09 μg/kg. Soil in Huizhou was slightly polluted by PAHs according to Maliszewska-Kordybach’s study. It can be confirmed that the increase of PAHs contents in the surface soil of Huizhou City is closely connected to human activities. Multivariate analysis was also made in this study. Principal component analysis was used to constrain their origins, and 3 principal components (PCs) were extracted. The results showed that coal combustion and oil spilling made the major contributions to PAHs. Cluster analysis was made and 16 priority PAHs were classified as 4 sorts, and the result revealed the differences in environmental behavior, chemical properties and sources of PAHs.  相似文献   

17.
Doklady Earth Sciences - The content of polycyclic aromatic hydrocarbons (PAHs) in soil and snow cover near the carbon black plants in Moscow, Omsk, and Samara regions was studied. The differences...  相似文献   

18.
Polycyclic aromatic hydrocarbons and polychlorinated biphenyls were investigated in sediment of bitumen deposit impacted area of Agbabu, Nigeria, to determine the present level of contamination with these toxic compounds prior to exploitation. Samples were collected during the dry season (March) and the wet season (August) of year 2008. Analysis was carried out with gas chromatography using mass spectrometry detector for polycyclic aromatic hydrocarbons and flame ionization detector for polychlorinated biphenyls. In the dry season sum of concentration of PAHs ranged from zero to 0.12 ± 0.06 ppm, while in the wet season the minimum was 0.18 ± 0.07 ppm and the maximum was 1.04 ± 0.16 ppm. Most of these values were higher than sum of polycyclic aromatic hydrocarbons concentrations of 1–10 μg/kg indicating that they were likely to come from anthropogenic sources. Average concentrations of PAHs such as naphthalene and benzo (a) pyrene obtained in sediment in the wet season in some of the stations were higher than recommended limits. The linear regression analysis between sum of concentrations and percentage organic carbon showed no significant correlation in sediment in the dry season (r2 = 0.0025) and in the wet season (r2 = 0.1345). The predominance of 4–6 ringed polycyclic aromatic hydrocarbons and the ratios between pairs of individual polycyclic aromatic hydrocarbons showed that they are likely to have come from pyrolytic sources. No polychlorinated biphenyl congener was detected in the samples.  相似文献   

19.
为研究广西三娘湾海域表层沉积物有机质中烃类化合物的分布特征及来源,于2019年10月在三娘湾海域采集了表层沉积物样品,利用加速溶剂萃取GC-MSD法对沉积物中的16种多环芳烃(PAHs)进行了分析。结果表明: 三娘湾海域表层沉积物样品中多环芳烃的含量为37~241.8 ng/g,总体处于含量较低的水平,但与往年相比研究区PAHs含量增加明显。通过组分分析等方法进行PAHs的来源分析,结果指示其主要来源为燃烧源,夹杂石油源的混合来源; 通过效应区间法对多环芳烃进行生态风险评价,认为其总体处于风险较低的水平。综合研究表明,三娘湾海域总体生态环境较好,但人类活动对多环芳烃含量及分布特征的影响较明显,需要持续关注。  相似文献   

20.
曹攽  马军  李云木子 《岩矿测试》2010,29(5):539-542
应用荧光-紫外检测器联用的高效液相色谱法分析地下水中16种多环芳烃。对高效液相色谱条件进行优化,建立了分析方法,并用于实际水样分析。在较佳的实验条件下,加标回收率为86.3%~105%,方法精密度(RSD,n=7)为0.39%~2.55%,检出限为0.001~0.010μg/L。分析16种PAHs仅用20min,比EPA8310方法中采用的液相色谱法缩短了17min。方法灵简便、准确,灵敏度高,分析时间短,适用于大批量地下水中痕量多环芳烃的分析。  相似文献   

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