超高效液相色谱测定地表水中超痕量苯并(a)芘及其前处理干扰研究

本研究采用液液萃取-超高效液相色谱仪接荧光检测器测定地表水中超痕量的苯并(a)芘,仪器检出限为0.005ng/m L,水样分析方法检测限为0.05ng/L,可对地表水中超痕量的苯并(a)芘实现定量检测。通过验证试验发现在实验室分析水样时,二氯甲烷等萃取溶剂中含有少量的苯并(a)芘是导致空白干扰的主要因素,溶剂经蒸馏提纯后可排除干扰。     

超声波萃取-高效液相色谱法测定总悬浮颗粒物中的多环芳烃

研究了一种用中流量采样器采样,超声波萃取,硅镁型吸附剂柱层析预分离.高效液谱测定总悬浮颗粒物的实验方法,在16分内可分高萘、蒽、芘、苯并(a)芘、苯并(ghi)苝等15种多环芳烃.已在大气环境的实际监测中得到应用.     

沥青烟中苯并(a)芘的等速采样与监测

新的大气污染综合排放标准对沥青及碳素制品生产和加工制定了沥青烟和苯并(a)芘的排放标准,然而空气和废气监测分析方法没有给出沥青烟气中苯并(a)芘的分析方法.为此,用色谱固定液滤筒及新设计的富集器等速采样,进行沥青烟苯并(a)芘的分析,为执行新的大气污染综合排放标准提供了实用技术.     

液液萃取—气相色谱/质谱联用法测定地表水中的四乙基铅

建立了液液萃取气相色谱质谱法测定地表水中痕量四乙基铅的分析方法。用正己烷萃取水样,不经浓缩直接进样,有效避免了萃取浓缩过程中四乙基铅的损失,并对实际样品进行测定。方法的检出限为0.005μg/L,水样的加标回收率为89.4%~102%,精密度(RSD,n=6)为4.80%~6.15%。实验结果表明,该方法准确可靠、灵敏度好,适用于地表水中痕量四乙基铅的检测分析。具有有机溶剂用量少、方法环保、萃取操作简单、快速等优点。     

高效液相色谱法测定烟道沥青烟中苯并(a)芘

用玻璃纤维滤料在烟道外部(或内部)采集颗粒物,用有机溶剂连续提取或超声波提取,碱性氧化铝净化样品,高压液相色谱分离、荧光检测器检测的方法快速测定烟道气中苯并(a)芘(BaP)平均回收率104.6％。合并变异系数为6.5％,检测下限为2PgBap。     

煤化工厂烟气中苯并(a)芘现状监测分析

通过试验建立了煤化工厂烟气中苯并(a)芘的液相色谱监测分析方法.通过条件优化,用配有荧光检测器的高效液相色谱仪分析烟气样品中苯并(a)芘的含量,该方法以乙腈、水梯度比例混合作为流动相;流速为1.0 ml/min;激发波长为255nm、发射波长为420nm;保留时间为27.38 min,测定检出限为2×10-3μg/m3...     

液相色谱法测定土壤中苯并(a)芘

用快速溶剂萃取法ASE300对土壤样品进行前处理,以配有荧光检测器的高效液相色谱仪分析土壤样品中苯并(a)芘的含量,该方法以乙腈、水梯度比例混合作为流动相,流速为1.0 ml/min;激发波长和发射波长分别为255 nm和420 nm;保留时间为27.58 min。样品的称样量为25 g时,测定检出限为8.28×10-5mg/kg,相对标准偏差(RSD)为1.0%~12%,回收率为60%~87%,以上指标均能满足环境中土壤样品的检测要求。     

河南省主要城市饮用水源水中多环芳烃污染状况的研究

对河南省主要城市饮用水源水中多环芳烃的污染状况进行了初步研究 ,结果表明 ,河南省主要城市饮用水源水普遍受到多环芳烃的污染 ,主要污染因子为萘、蒽、菲、芘、荧蒽、芴以及强致癌性物质苯并 (a)芘 ,而且苯并 (a)芘有超标情况出现     

乙醇提纯4-氨基安替比林试剂

用4-氨基安替比林(4-AAP)萃取光度法。测定水中挥发酚,由于4-AAP试剂易潮解氧化变质,使空白值偏高,且波动幅度大,从而影响测定结果的精确度和方法检测限。用苯清洗4-AAP苯毒性较大,对环境和操作人员均有影响。现使用乙醇提纯4-AAP晶体,取得了较好的效果。     

离子交换——石墨炉原子吸收法测定地表水及废水中痕量六价铬

在目前实行的测定六价铬的方法中,二苯碳酰二肼比色法是作为标准方法,它的检测限为4ppb,不能检出地表水中的痕量六价铬。若要用石墨炉原子吸收法进行测定,其检出限也不能满足测地表水的要求,而且要用特殊型号的树脂进行分离浓缩,不宜普及使用。 本工作采用了最普通的721阴离子交换树脂(市面有售)对水中的六价铬进行分离富集,用抗坏血酸还原淋洗,而后用石墨炉     

Evaluation of a tape-stripping technique for measuring dermal exposure to pyrene and benzo(a)pyrene

Epidemiological studies have shown an increased incidence of cancer among workers occupationally exposed to polycyclic aromatic hydrocarbons (PAHs). As the dermal route is considered important for exposure to PAHs in the workplace, the aim of this study was to develop and evaluate a tape-stripping technique for monitoring dermal exposure to pyrene and benzo(a)pyrene. The tape-stripping method was evaluated by applying different concentrations of pyrene and benzo(a)pyrene directly onto tape strips (spiked tapes), clean glass plates, and on the skin of five volunteers. The glass plates were stripped using a single strip of tape and the skin of the volunteers was stripped with five consecutive strips of tape after 0 and 30 minutes. The method was also tested on five chimney sweeps at three exposure sites. High-performance liquid chromatography with fluorescence detection was employed for the quantification of pyrene and benzo(a)pyrene. The mean recovery from the spiked tapes was 97% for pyrene and 93% for benzo(a)pyrene. The mean overall recovery from the glass plates was 88% and 76% for pyrene and 88 and 85% for benzo(a)pyrene. The recovery from human skin was 70% and 63% for pyrene and 60 and 54% for benzo(a)pyrene, after 0 and 30 minutes, respectively. A concentration gradient was clearly detected between the five consecutive strips. Detectable amounts of pyrene and benzo(a)pyrene were found on all chimney sweeps at all exposure sites. This method can thus be used to detect and quantify dermal exposure to pyrene and benzo(a)pyrene. The results also show that pyrene and benzo(a)pyrene may be taken up by the skin.     

公园地表土中多环芳烃的分离提取及含量分析

比较加压液体萃取法、超声波辅助萃取技术和微波辅助提取技术对公园地表土中多环芳烃的提取效率,并对目标化学成分进行分析鉴定。以超高效液相色谱-三重四极杆质谱作为分析方法,共分离检测出16种多环芳烃类化合物,分别为萘、苊、苊烯、氟、菲、蒽、荧蒽、芘、苯并[a]蒽、艹屈、苯并[b]荧蒽、苯并[k]荧蒽、苯并[a]芘、二苯并[a,h]蒽、茚并[1,2,3-cd]芘和苯并[ghi]苝。结果表明:加压液体萃取法、超声波辅助萃取技术和微波辅助提取技术均可以有效提取公园地表土中多环芳烃类成分。超高效液相色谱-质谱联用技术可以有效地分析公园地表土中多环芳烃类成分。     

5-氯-2-(吡啶偶氮)-1,3-二氨基苯分光光度法测定水质钴

采用5-氯-2-(吡啶偶氮)-1,3-二氨基苯分光光度法测定水质钴。对分析方法的样品前处理、样品保存、样品分析条件、干扰消除、检出限及测定范围、实际样品测定进行了深入研究和技术改进。水样经消解后测定的方法检出限为0.009 mg/L,经富集后测定的方法检出限为4×10-4mg/L,干扰消除实验的回收率为96%~101%,地表水、地下水、生活污水及工业废水等4种类型水样的加标回收率为92%~103%。     

Assessment of hydrocarbons concentration in marine fauna due to Tasman Spirit oil spill along the Clifton beach at Karachi coast

On 27 July 2003, Tasman Spirit spilled 31,000 tonnes of crude oil into the sea at the Karachi coast. This disaster badly affected the marine life (Flora and Fauna.) Present research has been proposed to ascertain the level of Polycyclic Aromatic hydrocarbons (PAHs) contamination in different fisheries including Fishes, Crustaceans; Crabs and Shrimps, Mollusks and Echinoderms along with passing time. Heavier components of crude oil such as Polycyclic Aromatic Hydrocarbons (PAHs) appear to cause most damages as these are relatively unreactive and persist in water. High concentrations of toxic PAHs were observed in all the fisheries and shellfishes caught form oil-impacted area. In this study fishes were found most contaminated than shellfishes i.e. summation operator 16 PAH = 1821.24 microg/g and summation operator 1164.34 microg/g, respectively. Naphthalene was found in the range of 0.042-602.23 microg/g. Acenaphthylene, acenaphthene, fluorene, phenanthrene and anthracene were detected in the range 0.008-80.03 microg/g, fluoranthene, pyrene, benzo(a)anthracene and chrysene 0.0008-221.32 microg/g, benzo(b) fluoranthene, benzo(k)fluoranthene and benzo(a) pyrene 0.0005-7.71 microg/g, benzo(g,h,i)perylene and indeno(1,2,3-c,d)pyrene 0.02-503.7 microg/g. Dibenzo(a,h)anthracenre was not detected in any specie.     

高效液相色谱法测定地表水中四乙基铅

系统研究了地表水中四乙基铅的液相色谱分析方法,水中四乙基铅经二氯甲烷萃取浓缩后,用高压液相色谱柱分离,在280 nm波长处检测,根据保留时间定性,外标法定量,检出限及测定下限分别为0.02μg/L和0.06μg/L,低于地表水限值0.1μg/L,地表水平行测定的相对标准偏差均小于5%,地表水和废水样品加标回收率分别为79.4%～82.0%和62.5%～106.6%。     

Chemometric application in identifying sources of organic contaminants in Langat river basin

Increasing urbanization and changes in land use in Langat river basin lead to adverse impacts on the environment compartment. One of the major challenges is in identifying sources of organic contaminants. This study presented the application of selected chemometric techniques: cluster analysis (CA), discriminant analysis (DA), and principal component analysis (PCA) to classify the pollution sources in Langat river basin based on the analysis of water and sediment samples collected from 24 stations, monitored for 14 organic contaminants from polycyclic aromatic hydrocarbons (PAHs), sterols, and pesticides groups. The CA and DA enabled to group 24 monitoring sites into three groups of pollution source (industry and urban socioeconomic, agricultural activity, and urban/domestic sewage) with five major discriminating variables: naphthalene, pyrene, benzo[a]pyrene, coprostanol, and cholesterol. PCA analysis, applied to water data sets, resulted in four latent factors explaining 79.0% of the total variance while sediment samples gave five latent factors with 77.6% explained variance. The varifactors (VFs) obtained from PCA indicated that sterols (coprostanol, cholesterol, stigmasterol, β-sitosterol, and stigmastanol) are strongly correlated to domestic and urban sewage, PAHs (naphthalene, acenaphthene, pyrene, benzo[a]anthracene, and benzo[a]pyrene) from industrial and urban activities and chlorpyrifos correlated to samples nearby agricultural sites. The results demonstrated that chemometric techniques can be used for rapid assessment of water and sediment contaminations.     

二氯甲烷萃取与气相色谱—质谱结合新方法测定饮用水源地水中的苦味酸

为建立饮用水源地中苦味酸分析测定的新方法,将10 ml水样中的苦味酸氯化后,以二氯甲烷萃取,用气相色谱—质谱法(GC—MSD)测定水中苦味酸的含量,采用保留时间定性,外标法定量。结果表明,最佳萃取时间为4 min,最佳萃取剂用量为1.5 ml,该法能快速而有效的提取并测定水中苦味酸,检出限低(0.4μg/L)、精密度(RSD=1.8%)和准确度高(加标回收率93.16%)、标准曲线线性(r=0.999)较好,能满足饮用水源地水中苦味酸的测定要求。     

隧道路面沥青摊铺过程空气中TSP和多环芳烃污染研究

分析了隧道沥青摊铺过程环境空气中的TSP及多环芳烃质量浓度。TSP用膜法,中流量采样器采样15 min,重量法分析;超声波萃取,高效液相色法分析多环芳烃。结果表明,摊铺机周围空气中TSP超过8 mg/m3,道路空气中TSP超过3 mg/m3;环境空气中苊烯等12种多环芳烃均有检出,苊烯和艹屈质量浓度较高,苯并[a]芘和二苯并[a,h]蒽质量浓度较低。苯并[a]蒽、苯并[a]芘和二苯并[a,h]蒽超标,对人体健康危害较大。建议加强相关行业PAHs的排放水平及其健康风险研究,制定相关限值标准和沥青摊铺过程环境空气的沥青烟监测方法标准。     

五种多环芳烃化合物对鲤鱼肝微粒体芳烃羟化酶的诱导

以鲤鱼肝微粒体为实验体系,研究了被五种多环芳烃(PAH)化合物菲、9,10-菲醌、芘、1-羟基芘、苯并芘污染后,其芳烃羟化酶(AHH)的活性变化,发现多环芳烃对AHH的诱导具有良好的剂量效应关系.AHH活性升高的大小可以作为监测多环芳烃对水体污染程度的一种生物指标.五种多环芳烃对AHH诱导能力的大小为1-羟基芘＞苯并芘;9,10-菲醌＞芘＞菲,与其毒性大小相关.     

气相色谱-质谱法测定废酸油渣中的16种多环芳烃

建立了废酸油渣中16种多环芳烃超声萃取、Florisil萃取柱净化、气相色谱-质谱测定的方法。笔者对提取方式、提取剂类型和体积、提取时间和次数、净化方式等进行研究,采用无水硫酸钠分散,二氯甲烷作为提取剂超声40 min,提取液经纯水清洗、离心后取适量有机相经过3 g Florisil萃取柱净化,采用气相色谱-质谱选择离子模式(SIM),加入内标进行定量分析。结果表明:二氯甲烷提取效率比正己烷好,丙酮可能引起酸性样品中多环芳烃的降解,丙酮超声萃取时加入无水硫酸钠能在一定程度上防止目标物降解,但萃取效率不可控制,宜采用二氯甲烷作为萃取剂。分散提取能有效减少提取时间,超声清洗仪超声40 min提取效率为86.2%～104%。3g Florisil萃取柱净化比1 g Florisil萃取柱净化和GPC净化效果略好。方法检出限为0.4～1.3 mg/kg,6次空白加标的相对标准偏差为2.3%～15.3%,6个实际样品测定结果的相对标准偏差为1.2%～27.3%,基体加标回收率为51.3%～126%,连续校准稳定。该方法适用于废酸油渣样品中16种多环芳烃的检测,比直接溶解有效,比加速溶剂萃取、索氏提取、微波萃取和超声探头萃取简单、快捷,能有效减少设备污染和腐蚀,净化方法有效,测定结果准确可靠,是实现大批量样品检测的可行方法。