超高压液相色谱/质谱联用法测定地表水中特定污染物

采用超高压液相色谱/质谱联用法测定地表水特定项目中包括微囊藻毒素-LR在内的13种污染物,对测定条件进行优化,使得各目标化合物均能在3min内检测完毕.试验表明,方法在各测定范围内线性良好,相关系数均〉0.99,各目标化合物的方法检出限为0.12μg/L～8.40μg/L,地表水样的加标回收率在62.0% ～104%之间,6次平行测定的RSD〈6%.用该方法测实际水样,阿特拉津和马拉硫磷被检出,质量浓度分别为0.6μg/L和0.7μg/L.     

吹脱捕集GC/FID法测定海河水中挥发性有机物

采用吹脱捕集GC/FID法对海河干流水中挥发性有机物进行定性、定量分析。共检测出 39种挥发性有机物 ,不同化合物的回收率为 84 2 %～ 143 2 % ,相对偏差为 1 5 %～ 9 6 %。当水样体积为 2 5mL时 ,方法检测限为 0 0 0 1μg/L～ 0 4μg/L。     

气相色谱/负离子化学电离质谱法测定地表水中硫丹及其代谢物

采用气相色谱/负离子化学电离质谱法测定地表水中的硫丹及其代谢物,用正己烷提取,外标法定量。α-硫丹、β-硫丹及硫丹硫酸酯在0.200μg/L～10.0μg/L范围内线性良好,方法检出限分别为0.010μg/L、0.008μg/L及0.010μg/L,空白加标平行测定的RSD为3.9%～4.8%,地表水样品加标回收率为85.5%～93.8%。     

UPLC-MS/MS法测定尿液中的反-反黏糠酸和苯巯基尿酸

采用超高效液相色谱-串联质谱法(UPLC-MS/MS)测定尿液中的苯代谢产物反-反黏糠酸与苯巯基尿酸,通过优化前处理和测定条件,使反-反黏糠酸在10.0μg/L～1 000μg/L范围内,苯巯基尿酸在0.500μg/L～50.0μg/L范围内线性良好,方法检出限为1.4μg/L和0.08μg/L。将该方法用于实际尿样的加标回收试验,结果加标回收率为90.6%～108%,6次测定结果的RSD为1.5%～4.2%,有证标准物质测定结果在规定范围内。     

UPLC-MS/MS法同时测定地表水中多种有机污染物

采用超高效液相色谱-串联质谱法直接进样测定地表水中26种有机污染物,通过优化试验条件,使各目标化合物在1.00μg/L^100μg/L范围内线性良好,相关系数(r 2)>0.995,方法检出限为0.003μg/L^1.0μg/L。将该方法用于地表水样的测定,加标回收率为79.0%~120%,6次测定结果的RSD均<15%。     

气相色谱-电子捕获法直接测定水体中的五氯酚钠

建立了不经衍生直接测定水体中五氯酚钠残留量的气相色谱-电子捕获(GC-ECD)方法。用乙酸乙酯提取目标化合物,浓缩后上机测定。五氯酚钠标准溶液的线性范围在0.35～400μg/L之间,相关系数为0.9992;池塘水中五氯酚钠的添加浓度为1.0、5.0、10.0μg/L时,其加标回收率为95.8%～98.7%,相对标准偏差≤3.6%;检出限(信噪比为3时)为0.35μg/L,定量限(信噪比为10时)为1.0μg/L。     

原子荧光光谱法同时测定环境水体中痕量锡和锌

采用原子荧光光谱法同时测定环境水样中痕量锡和锌,优化了试验条件。锡在1.00μg/L～10.0μg/L、锌在20.0μg/L～200μg/L范围内线性良好,方法检出限锡为0.13μg/L,锌为1.76μg/L,锡和锌标准溶液测定的相对标准偏差分别为2.9%和4.0%,环境水样加标回收率锡为96.4%～106%,锌为92.0%～111%。     

固相萃取/高效液相色谱法测定地表水中氨基甲酸酯类农药

通过固相萃取法提取地表水中10种氨基甲酸酯类农药,萃取溶液经浓硫酸脱色,佛罗里硅土柱除杂,用柱后衍生高效液相色谱法测定.在5μg/L～500μg/L范围内,标准曲线线性关系良好,仪器检出限低于1μg/L,水样平均加标回收率为90.0%～101%,RSD为1.1%～9.2%.     

吹扫捕集-GC/MS法测定饮用水中致嗅物质

采用吹扫捕集-气相色谱/质谱联用法测定饮用水中6种致嗅物质,优化了吹扫捕集条件。方法线性良好,甲硫醚、二甲二硫、甲苯、异佛尔酮、癸醛、β-环柠檬醛的检出限分别为10.5μg/L、0.558μg/L、0.862μg/L、47.4μg/L、4.75μg/L、3.77μg/L,标准溶液平行测定的RSD≤10.9%,加标回收率为71.0%～125%。     

固相萃取气相色谱法测定水中15种硝基苯类化合物

使用Oasis HLB固相萃取柱,以正己烷/丙酮混合溶剂(体积比为3∶1)为洗脱溶剂,采用毛细管柱气相色谱电子捕获检测器同时测定水中15种硝基苯类化合物,以保留时间定性,外标标准曲线法定量。硝基苯和硝基甲苯在50.0μg/L～1 000μg/L、其他硝基苯类化合物在5.00μg/L～100μg/L范围内线性良好,检出限硝基苯和硝基甲苯为0.035μg/L～0.052μg/L,其他硝基苯类化合物为0.003 5μg/L～0.005 6μg/L,加标水样平行测定的RSD为1.4%～4.0%,平均回收率为92%～100%。     

Monitoring priority substances of directives 76/464/EEC and 2000/60/EC in Greek water bodies

The priority substances of List I, 76/464/EEC Directive, some of which belong to the new Water Framework Directive 2000/60/EC, have been monitored in the surface waters of Greece through the developed network of 53 sampling stations. The analytical methods used for the determination of these substances included Purge and Trap-Gas chromatography-Mass spectrometry for volatile and semivolatile organic compounds, Gas Chromatography-Electron Capture Detection for organochlorine insecticides, High Performance Liquid Chromatography for pentachlorophenol and Atomic Absorption Spectrometry for metals. The results have shown the presence of several priority substances in Greek surface waters, in most cases at concentrations well below the regulatory limits. However, non-compliance was observed for a limited number of compounds. The monitoring network and the analytical determinations have to be expanded to more water bodies and more priority substances, in order to safeguard the quality of Greek surface waters.     

HS/SPME-GC/MS/MS法测定水中痕量2-甲基异莰醇和土臭素

建立了测定水中痕量2-甲基异莰醇(2-MIB)和土臭素(GSM)的顶空固相微萃取-气相色谱/二级质谱联用法(HS/SPME-GC/MS/MS),并对HS/SPME条件进行优化。优化后的方法 2-MIB和GSM在1.00~50.0 ng/L范围内,线性良好(r≥0.999 4),RSD分别为7.36%和7.75%,方法检出限分别为0.226和0.239 ng/L,加标回收率分别为87.0%~97.0%和85.2%~112%。结果表明,所建立的方法操作简便、准确度高、重现性好、灵敏度高,无需有机溶剂,适用于水中痕量2-MIB和GSM的测定。     

多氯联苯的气相色谱/质谱/质谱(GC/MS/MS)法测定

采用气相色谱/质谱/质谱(GC/MS/MS)法测定多氯联苯(PCB),具有良好的灵敏度和选择性,在地表水样品检测时,样品只须进行简单的液液萃取-浓缩,不须任何净化过程即可上机分析,方法检出限低于ng/L级。     

Water quality monitoring in Washington's Timber/Fish/Wildlife program

The Timber, Fish, and Wildlife program (TFW) in Washington is a consensus approach to implementing reforms in forest practice regulations involving industrial timberland owners, state agencies, environmental groups, Indian tribes, and non-industrial forest landowners. A cooperative monitoring and research effort (CMER) has been included as a part of this program. Technical projects undertaken by CMER are overseen by a series of steering committees, one of which is the Water Quality Steering Committee. Projects currently being addressed by the Water Quality Steering Committee include: forestry impacts on water temperature, water quality impacts from forestry derived sediment, use of bio-indicators to assess the water quality impacts of forest practices, and the effect of forest chemical applications on water quality. A close link between the research efforts in TFW and the procedure for implementing regulatory change has greatly improved the responsiveness of the rule making process to new information. Results from the water temperature and forest chemical work is currently being incorporated into the forest practice regulations.     

顶空便携气相色谱测定水中苯系物

研究了分配常数、气液相比、温度和无机盐等对顶空分析灵敏度的影响.结果表明,这些参数对不同组分顶空灵敏度的影响有显著差异.气液相比对分配常数小的组分影响大,而温度和无机盐对分配常数大的组分影响大.提出了静态顶空/吸附热解吸/SENTEX便携气相色谱仪/微氩离子检测器测定水中4个苯系物的方法,平均相对标准偏差7.38%,平均相对误差3.46%,与标准方法比较,没有显著差异,而方法检出限低于标准方法1～2数量级.     

气质联用法测固定污染源中三氟甲烷、四氟甲烷、六氟乙烷和六氟化硫

建立了固定污染源排气中三氟甲烷、四氟甲烷、六氟乙烷和六氟化硫的采样和气质联用分析方法,检出限分别为0.06、0.15、0.21、0.71 mg/m3,精密度在3.2%以下,相关系数大于0.999 6,并对浙江省内2家典型企业排放的温室气体进行了监测,实际样品监测结果表明,该方法能够满足废气中4种温室气体的监测要求。     

水中微囊藻毒素的超高效液相色谱-串联质谱法研究

建立测定水体中微囊藻毒素(MCYST)的超高效液相色谱-串联质谱分析方法.水样通过固相萃取富集净化,采用超高效液相色谱-串联质谱测定,6min内完成3种MCYST的分离及检测.MCYST-LR、MCYST-RR、MCYST-YR检出限分别为3.5、2.5、5.0ng/L,回收率为85.6％～107.9％,为水质微囊藻毒素监测提供了一种快速、准确、灵敏的分析方法.     

便携式顶空/气相色谱/质谱联用法快速测定水中苯系物

建立了以便携式顶空/气相色谱/质谱联用技术快速测定水中苯系物的方法,该方法适用于水中苯系物的应急监测。     

工业废水BOD5与CODCr相关关系以及BOD5测定的简化法

通过研究BOD5与CODCr的相关性,用线性函数BOD5=a+bCODCr的形式进行一元回归,间接求出BOD5或指导BOD5的测定,验证BOD5结果的准确性以及通过对稀释法公式的推导得出简化法的公式,并与稀释法进行比较,结果表明,简化后的方法与稀释法无显著差异,精密度、准确度较好.     

Water quality in Minho/Miño River (Portugal/Spain)

Minho River, also called Miño (in Spain), extends to about 300 km from Spain to Portugal. The source of the river lies in Spain and in the last 75 km, the river defines the border between Portugal and Spain. Under the scope of a cooperation project between North Portugal and Galicia region of Spain, titled: “Valorization of the natural resources of the Minho/Miño drainage basin”, seven water-sampling campaigns were carried out during the last 2 years in Minho River basin. Seven sampling sites were selected along the international stretch, and five were chosen in the main Portuguese and Spanish tributaries of Minho River. Water quality based on the physicochemical and microbial parameters was assessed. According to the Portuguese legislation for surface waters, the international section of Minho River presents a reasonably good water quality (BOD₅ <5 mg/L, TNK <2 mg/L, and total phosphorous <1 mg P/L). Valença and Louro were found to be the most polluted sampling sites and Louro the most polluted tributary (maximum values observed: TSS?=?26 mg/L, BOD₅?=?6.6 mg O₂/L, COD?=?20.8 mg O₂/L, total nitrogen?=?9.9 mg N/L; minimum value observed: OD?=?1.3 mg O₂/L). A one-dimensional stream water quality model QUAL2Kw was calibrated using data measured in field surveys along the international stretch of Minho River. QUAL2Kw was also used to predict the impact of flow conditions, discharges, and tributaries on the water quality of international stretch of Minho River, essential to establish proposals for management and planning of Minho River Basin.