固体吸附-热脱附/气相色谱-质谱法测定固定污染源废气中50种挥发性有机物

采用Tenax GR吸附-热脱附-气质联用法对固定污染源废气中50种挥发性有机物(VOCs)进行测定。结果显示,Tanax GR吸附管对于丙酮、环戊酮、2-庚酮、2-壬酮及六甲基二硅氧烷的吸附能力相对较差,但丙酮、环戊酮、2-庚酮、2-壬酮在2~30 ng范围内呈现良好的线性关系,且相关系数(R 2)>0.99,六甲基二硅氧烷在2~50 ng范围内呈现良好的线性关系,R^2=0.994,其他45种化合物在2~100 ng范围内呈现良好的线性关系,R^2>0.995。当采样体积为300 mL时,50种化合物的检出限为0.0003~0.0096 mg/m^3,测定下限为0.0011~0.0384 mg/m^3,相对标准偏差(RSD)<15.98%,加标回收率为78.15%~120.90%。该方法操作简单、灵敏度高、准确性好,能够满足固定污染源废气中痕量VOCs的快速检测。     

气相色谱法测定焦化厂废水中的挥发酚

焦化厂废水以苯酚、邻甲酚、对甲酚、间甲酚为主。因此,采用4—氨基安替比林比色法和引进来电子基团法都不适用焦化厂废水中挥发酚的测定。本文采用六甲基二硅胺烷和三甲基氯硅烷混合物作为硅醚化试剂,并对其操作方法进行了改进,提高了灵敏度,使之更适宜于测定焦化厂生化后外排水中的微量挥发酚。     

G C/MS法测定环境空气中痕量POPs类有机氯农药及降解产物

采用快速溶剂萃取-氟罗里硅土柱净化-气相色谱/质谱联用法测定环境空气中POPs类有机氯农药及其降解产物.艾氏剂、狄氏剂、异狄氏剂、六六六、滴滴涕,七氯、氯丹、灭蚁灵及其降解产物的检出限为2.0 ng～4.6 ng,空白加标回收率为62.1%～118%,RSD为6.8%～15.2%.     

新型介孔薄膜涂层固相微萃取-气相色谱法测定塑料浸取液中的邻苯二甲酸二(2-乙基己基)酯

自制新型介孔薄膜涂层固相微萃取头,结合顶空固相微萃取-气相色谱法(HS-SPME-GC),测定水溶液中的邻苯二甲酸二(2-乙基己基)酯(DEHP)。结果表明,该方法具有良好的线性范围(0.1～2000μgL),检出限为0.08μgL,相对标准偏差为5.5%(n=3)。将该法应用于检测塑料浸取液中DEHP,结果令人满意。     

双抗体夹心荧光免疫法测定水中的邻苯二甲酸环己二酯

用制备的邻苯二甲酸环己二酯(DCHP)抗体包被酶标板,以酶联免疫双抗夹心法为基础,以异硫氰酸荧光素为荧光探针,研究了双抗夹心免疫反应的条件,建立了邻苯二甲酸环己二酯抗体包被荧光免疫分析新方法,DCHP的最小检出限是0.5ng/ml,线性范围为10-5~10-1μg/ml。该方法灵敏度高,选择性好,线性范围宽。     

U PLC- ESI- MS/MS法同时测定水中7种抗生素

采用超高效液相色谱-电喷雾二级质谱联用技术同时测定水中7种抗生素,优化了试验条件.磺胺甲恶唑、诺氟沙星、环丙沙星、氧氟沙星、四环素在1.00 ng/L～1000 ng/L范围内线性良好,定量下限为1 ng/L,土霉素、金霉素在10.0 ng/L-2 000 ng/L范围内线性良好,定量下限为10 ng/L,去离子水和地表水样加标回收率为72.1%-112%,RSD为0.6%～9.2%.     

二安替比林基—（2—溴）苯基甲烷与铬（Ⅵ）的显色反应研究及应用

研究了二安替比林基—（2—漠）本基甲烷（DAOBM）与铬（Ⅵ）的显色反应的最佳条件．在Mn（Ⅱ）的诱导作用下，其摩尔吸光系数可达1．82×105L·mol-1·cm－1。显色反应在吐温—80存在下的磷酸介质中进行，铬量在1．0～60μg／25ml范围内符合比耳定律。该方法稳定性好．灵敏度高，具有很好的选择性．可用于电镀废水及处理废水中微量铬的测定．结果满意。     

UPLC-MS/MS法同时测定地表水中多种药物及个人护理品

采用快速液相色谱-三重四级杆串联质谱仪(UPLC-MS/MS)测定地表水中31种药物及个人护理品,通过优化分析条件,使方法在0.01μg/L～10.0μg/L范围内线性良好,方法检出限为0.2 ng/L～1.2 ng/L。地表水样品两个质量浓度水平的加标回收率为64.8%～125%,测定6次结果的RSD≤11%。将该方法用于上海市两条河道中10个水样的测定,结果地西泮、氟康唑、甘宝素、咖啡因、可替宁、氨基比林的测定值为6.56 ng/L～302 ng/L,其余PPCPs未检出。     

便携式催化氧化-FID法测定固定污染源废气中非甲烷总烃

对便携式催化氧化-FID法测定非甲烷总烃的检出限、精密度、准确度、催化效率等性能指标开展研究,考察该方法测定固定污染源废气中非甲烷总烃的适用性。结果表明：催化氧化装置的转化效率为98.1%～99.7%,方法检出限为0.05 mg/m3（以碳计）;2个质量浓度水平的甲烷和丙烷混合标准气体测定结果的相对误差分别为-6.4%～6.1%、-4.7%～-0.5%,实验室内、实验室间测定结果的RSD分别为2.9%～5.9%和1.6%～2.5%、1.5%和0.6%。用该方法和国标法同时测定实际样品,两种方法测定结果的相对误差为6.4%～21.4%。     

氢化物发生—电加热石英管原子吸收法测定环境水样中痕量铅的研究

研究了将氢化物发生技术用于电加热石英管原子吸收法测定环境水样中痕量铅 ,讨论了最佳测定条件和干扰元素的消除。方法的线性范围为 0～ 2 5 ng/m l,检出限为 0 .48ng/ml,相对标准偏差小于 2 .5 % ,回收率在 95 %～ 116%之间。     

Organochlorine pesticide (OCP) residues in cow??s, buffalo??s, and sheep??s milk from Afyonkarahisar region, Turkey

In this study, it was aimed to determine organochlorine pesticides (OCPs) in three types of milk (cow's, buffalo's, and sheep's milk) produced in Afyonkarahisar province of Turkey. The results indicated that these milk specimens were found to be contaminated by 21 different pesticides. Sixteen OCP residues were detected in sheep's milk and it was followed with 14 pesticides in buffalo's milk and 11 pesticides in cow's milk. Dominant pesticides in all samples examined were beta-HCH in buffalo's, cow's, and sheep's milk in the concentrations of 63.36, 91.32, and 122.98 ng/ml, respectively. Total OCP levels were found to be 243.81 ng/ml in sheep's milk, 151.02 ng/ml in cow's milk, and 133.38 ng/ml in buffalo's milk. Some of the pesticides detected were found to be in the excess amount of the acceptable level regarding the EU regulations.     

同步荧光光谱法测定环境水样中的多环芳烃

为了建立快速测定水体中多环芳烃的方法,用恒波长同步荧光法对14种多环芳烃混合标样进行了分析。在优化的实验条件下,对环境水样进行分析,可以鉴别出11种多环芳烃。14种PAHs在0～1000ng/ml范围内呈良好的线性关系,相关系数r均不小于0.9988,相对标准偏差(RSD)在1.06%～1.67%之间(n=6)。14种PAHs的检出限在0.072～3.9ng/ml之间。该方法应用于污水、样河水样、池塘水样中的多环芳烃检测取得了良好的效果,回收率分别为82.2%～111.0%、86.0%～107.0%、88.0%～106.2%(n=5)。     

Microtrace Metalloids Speciation in Lakes Water Samples (Poland)

This paper presents the results of the determination of arsenic, antimony and selenium concentrations of inorganic speciation in surface water samples from Gniezno city (western Poland) and its neighborhood. The concentration of elements were up to 1.85 ng/ml for arsenic, 1.61 ng/ml for antimony and 0.45 ng/ml for selenium (detection limits: 0.04 ng/ml for As and Sb and 0.03 ng/ml for Se). A variety of concentrations for the determined elements has been obtained in waters from Gniezno city’s neighborhood and in water from down-town reservoirs which are under strong anthropogenic pressure.     

A rapid and sensitive analytical method for the quantification of residues of endosulfan in blood

A new sensitive analytical procedure has been developed for the determination of residues of endosulfan in human blood samples. The method involves the extraction of residues of endosulfan from blood samples by the addition of 60% sulfuric acid at 10 degrees C, liquid/liquid partitioning by using hexane and acetone mixture (9:1) and quantification by using GC-ECD. Residues of endosulfan in blood samples were quantified as the sum of alpha-endosulfan, beta-endosulfan, endosulfan sulfate and endosulfandiol. The influence of temperature during the extraction has been studied. Recovery experiments were conducted over the concentration range 1.0-50 ng ml(-1) and the relative standard deviation calculated. The method was found to be sufficiently sensitive to quantify the residue of total endosulfan up to the 1.0 ng ml(-1) level. The recovery was 92% with a calculated relative standard deviation of 1.96%. Conversion of endosulfan to endosulfandiol is found to be less than 0.5% under the defined conditions. The method was applied to the analysis of residue contents of endosulfan and its metabolites in blood samples collected from the exposed population. The data obtained has been confirmed by GC-MS-EI in selective ion monitoring (SIM) mode.     

Residue levels of organochlorine pesticides in some ecosystem components of Manzala Lake

To evaluate the organochlorine pesticide (OCP) contamination of Manzala Lake, its ecosystem was investigated during the winter season (December to March). The studied ecosystem components were water, sediment, aquatic weeds, and fishes in four locations. The samples were analyzed by gas chromatography with electron capture detector. Pollutant levels of total OCPs showed significantly high levels in the water areas of Round road (46.253 ng/ml), Port-Said Damietta road (19.301 ng/ml), followed by Bughas El-Rasoah (5.539 ng/ml), then Ashtoum El Gamel (natural reserve area now) (0.289 ng/ml). Organochlorines were detected in sediment only in Round road (3.359 μg/kg) and Port-Said Damietta road (0.171 μg/kg) by significant order while they were undetectable in Ashtoum El Gamel and Bughas El-Rasoah. Total OCPs in aquatic weeds ranged between 0.194 μg/kg in Port-Said Damietta and 0.026 μg/kg in Ashtoum El Gamel. While OCPs were 0.160 and 0.153 μg/kg in Round road and Bughas El-Rasoah, respectively. Concerning fish muscles OCPs were significantly higher in the Round road area (0.397 μg/kg) followed by the Port-Said Damietta road (0.258 μg/kg), and finally, Ashtoum El Gamel samples (0.126 μg/kg). The results revealed the direct relation for the accumulation of OCPs between studied ecosystem parameters at the Manzala Lake during the winter season. Results also demonstrated that fish samples collected from the Manzala Lake in the studied areas were contaminated with levels of organochlorines, not higher than the maximum permissible level recorded by FAO/WHO, and that the public is not at risk with fish consumption.     

水样中痕量十溴联苯醚的分散液-液微萃取条件的优化

采用正交设计和Box-Penhnken响应面设计,对分散液-液微萃取技术萃取水样中痕量十溴联苯醚的条件进行了筛选和优化,得到最佳条件:四氯乙烯为萃取剂(10μl)、丙酮作分散剂(1ml)、pH范围5~9、离子强度,2%NaCl及萃取时间10min。此优化条件下分散液-液微萃取技术的萃取回收率可达92.37%~104.38%,富集倍数为508~611。优化条件下方法的线性范围为0.01~100ng/ml,检出限(S/N=2)为3.0pg/ml,加标回收率为96.25%~102.16%,精密度为5.44%~6.34%。     

原子荧光光度法测定工业炉气中的砷

采用原子荧光光度法测定炉气中砷的含量。方法探讨了盐酸酸度对测定结果的影响 ,确定本方法的检测限为2 .1 3ng/ml,样品回收率为 95.2 %～ 97.6%。     

Derivative spectrophotometric method for copper determination

A simple, sensitive and selective method by solvent extraction-first derivative spectrophotometry is described for the determination of microamounts of copper in water by means of its reaction and extraction at pH 8.0 with 3-(4-phenyl-2-pyridinyl-5-phenyl-1,2,4-triazine) (PPT) and picrate (2,4,6-trinitro-phenol) into 1,2-dichloroethane. Copper was thus determined in the range 7.5–350 ng/ml with a detection limits (3) of 2.3 ng/ml. The relative standard deviations were in all instances less than 2.0%. The proposed method was successfully applied for the determination of copper in several kinds of water.     

A chemosorptive cylindrical denuder designed for personal exposure measurements of isocyanates-evaluation on generated aerosols of 4,4'-methylenediphenyl diisocyanate

A denuder/filter system constructed for solvent-free personal exposure measurements was evaluated for separation of vapour and particulate 4,4'-methylenediphenyl diisocyanate (4,4'-MDI) generated from heated PUR-foam. The two different phases were collected in the denuder and on the filter, respectively, by chemosorption on a polydimethylsiloxane (SE-30)-dibutylamine (DBA) stationary phase. Both repeatability and the total mass concentration of 4,4'-MDI were similar to that obtained from the reference method, in this case an impinger/filter system. The penetration of particles through the denuder at 300 ml min(-1) was nearly 100% in the particle size range 25 to 700 nm, which fits well with the Gormley-Kennedy equation. Denuder/filter sampling of the 4,4'-MDI aerosol at 500 ml min(-1) yielded a phase distribution that was in accordance with the results from the reference method. The method limit of detection was 6 ng m(-3) and 4 ng m(-3) for the denuder and filter, respectively, when using an air sampling flow rate of 300 ml min(-1) and a sampling period of 15 min. This is well below the Swedish occupational exposure limit (OEL) of 50 and 100 microg m(-3) for an 8-hour working day and a 5-min period, respectively.