气相色谱法测定环境空气和废气中乙酸

以蒸馏水吸收环境空气或工业废气中的乙酸,用5%PEG20M+0 5%H3PO4ChromosorbHP80目～100目、2m×2mm玻璃填充柱分离,氢火焰离子化检测器检测,样品直接进气相色谱仪测定。方法最低检出质量浓度为0 16mg/m3,相对标准差为2%～5%,加标回收率在85%～106%之间。方法操作简便、快速。     

柳州市大气颗粒物中多环芳烃的种类和时空分布特征及来源

采用气相色谱/质谱联用技术(GC/MS)检测了柳州市大气颗粒物样品中的PAHs,比较了柳州市各区大气颗粒物中多环芳烃含量的差异以及不同季节对多环芳烃含量的影响,讨论了其分布规律及污染源.     

等温气相色谱法测定土壤中甲基汞

样品采用碱消化，室温下在pH＝4．9时进行乙基化反应，氢气为载气，Carbotrap富集有机态汞，等温气相色谱（GC）分离，用冷原子萤光仪（CVAFS）测定。方法检出限20pg。线性范围100～600pg。回收率在95％～105％之间。     

Determination of methyl tert-butyl ether (MTBE) in Chinese fuels by gas chromatography/mass spectrometry and gas chromatography/flame ionization detector

A method was developed to determine the concentration of methyl tert-butyl ether(MTBE) in gasoline,diesel and heating oil by gas chromatography(GC) with mass spectrometry(GC-MS) or flame ionization detection(FID). The diluted gasoline was directly injected into the GC, and the complete separation of MTBE from co-eluting hydrocarbons was not required. GC/MS or GC/FID method can be used to analyze MTBE in different concentration range and have good consistency.     

Characterization of fine organic particulate matter from Chinese cooking

PM2.5 samples were collected by a three-stage cascade impactor at two kinds of Chinese restaurants to characterize fine organic particulate matter from Chinese cooking sources. Major individual organic compounds have been quantified by GC/MS, including series of alkanes, n-alkanoic acids, n-alkanals, alkan-2-0nes and PAHs.Alkanes and ketones make up a significant fraction of particle-phase organic compounds, ranging from C11 to C26,and (C9 to C19, respectively. In addition, other organic compound classes have been identified, such as alkanols,esters, furans, lactones, amides, and nitriles. The mass concentrations of fine particles, alkanes, n-alkanoic acids and PAHs in air emitted from the Uigur style cooking are hundreds times higher than ambient PM2.5in Beijing.     

基质固相分散-快速溶剂萃取-GC/MS法同时测定土壤中有机氯农药和多环芳烃

建立了基质固相分散-ASE提取-GC/MS法同时测定土壤中8种有机氯农药和16种多环芳烃的方法。对方法的线性、检出限、精密度、回收率及土壤质控样品进行了分析,结果表明,8种有机氯农药和16种多环芳烃线性良好,相关系数为0.997 5～0.999 8,方法检出限为0.39～1.57μg/kg,空白加标样品的相对标准偏差小于20%,实际土壤样品加标回收率为60.6%～125%,土壤质控样品结果均在范围内。该方法能够满足土壤中8种有机氯农药和16种多环芳烃的检测要求。     

小体积液液萃取-GC/MS法测定地表水中有机磷农药

采用小体积液液萃取-气相色谱/质谱联用法测定地表水中有机磷农药,以1.2 mL正己烷为萃取剂,磷酸三苯酯为内标,对8种目标化合物的富集倍数达156～436.方法在1.00 μg/L～20.0 μg/L范围内线性良好,8种有机磷农药的检出限均为0.2 μg/L,实际水样平行测定的RSD为2.1%～9.7%,平均加标回收率...     

顶空固相微萃取-气相色谱法测定饮用水中的百菌清

建立了顶空固相微萃取(HS-SPME)-气相色谱法(GC-ECD)分析饮用水中百菌清的方法。对HS-SPME的各项参数进行了优化:萃取纤维应选择弱极性的聚二甲基硅氧烷(PDMS,100μm),水样分析前应加入一定量的H2SO4溶液和Na Cl固体,调节pH和离子强度,可显著提高萃取效率。萃取温度70℃,萃取时间30 min,搅拌速度250 r/min,解吸时间3 min。根据优化后的条件,从线性、检出限、回收率、精密度等方面对整个方法进行了验证,结果表明,该方法线性良好,相关系数大于0.999,回收率与精密度均符合要求。取样量为10.0 mL时,检出限为0.09μg/L,可完全满足饮用水分析的需要。     

Determination of polycyclic aromatic hydrocarbons and substitutes (Nitro-, Oxy-PAHs) in urban soil and airborne particulate by GC-MS and NCI-MS/MS

A method involving high resolution gas chromatography combined with ion trap (HRGC-MS/MS) and negative chemical ionisation (NCI) was developed for the determination of nitrated or oxygenated polycyclic aromatic hydrocarbons (nitro-PAHs, oxy-PAHs) and other electrophilic substitutes in soil samples. Efficient clean-up was achieved by a combination of methods for the determination of PAHs in soil and nitro-PAHs in aerosol using solid phase extraction (SPE) and semipreparative high performance liquid chromatography (HPLC). In samples of surface soil from the city of Basle (Switzerland), nitro-PAHs (mainly 3-nitrofluoranthene and 1-nitropyrene) were found in concentrations between 30 and 800 ng/kg dry weight. Oxy-PAHs and parent PAHs revealed 10²-10⁴-fold higher levels. Nitro-PAHs which are up to 10⁵ times more mutagenic seem to be less persistent in soil than the parent forms, although their entire mutagenic potential has to be estimated as being on the same order of magnitude. In urban air particulate matter, the amounts of nitro-PAHs (2–62 pg/m³) were 10–100 times lower than oxyPAHs and parent PAHs which were both found in a similar range. 3-nitrobenzanthrone, a recently described suspected human carcinogen has not yet been detected. Using multivariate statistical analysis, it was possible to elucidate similarities or special characteristics of substances in a given matrix reflecting their chemical properties or specific emission sources.     

水相中三丁基锡预富集方法研究

首次用x－5树脂吸附三丁基锡（TBT）化合物。结果表明,X－5树脂吸附TBT化合物具有吸附容量大、吸附速度快等优点,符合Freundlich吸附等温式;用自制的吸附注（长度为11cm,内径为0.55cm的玻璃管,内装x－5大孔网状树脂,约0.7g）作TBT吸附剂,研究各种因素对吸附及脱附效率的影响。结果表明,吸附率主要取决于柱长及流速,而溶液的盐度及pH值影响不大;脱附率主要取决于洗脱剂的流速,而pH值影响不大;实际样品的回收率超过90％。