DPX快速萃取程序升温大体积进样GC/MS法测定水中19种多溴联苯化合物

建立DPX快速吸附萃取、程序升温(PTV)大体积进样与气相色谱/质谱(GC/MS)联用,SIM模式同时测定水中19种多溴联苯(PBBs)单体的方法。该方法在PBBs质量浓度1~50μg/L范围内线性良好,19种PBBs单体检出限为0.147~0.230μg/L,相对标准偏差为6.61%~10.5%,加标回收率为61.5%~82.6%。     

气相色谱-质谱法测定沉积物中的有机氯和多氯联苯

采用加速溶剂萃取法提取沉积物中的有机氯和多氯联苯,提取液用凝胶色谱法净化后用气相色谱-质谱法测定。方法在5.00μg/L~200μg/L范围内线性良好,当取样量为10.0 g时,方法检出限为0.03μg/kg~0.37μg/kg,空白样品2个质量比水平的加标回收率为70.8%~121%,测定结果的RSD为2.7%~11.5%。用该方法测定实际样品,结果 12个抽检的沉积物样品中多氯联苯均未检出,9个样品中有机氯检出。     

HPLC和HPLC-MS/MS测定地表水中酚类化合物

采用高效液相色谱法(HPLC)和高效液相色谱-三重四级杆质谱联用法(HPLC-MS/MS)测定地表水及饮用水中11种酚类化合物,通过优化测定条件,使HPLC法在0.020 mg/L~50.0 mg/L范围内,HPLC-MS/MS法在0.500μg/L~250μg/L范围内线性良好,方法检出限分别为0.005μg/L~0.031μg/L和0.005μg/L~1.56μg/L。未检出的实际样品加标回收率分别为57.2%~96.7%和81.3%~113%,RSD分别为1.5%~5.3%和3.9%~17.7%。     

固相萃取-GC/MS法测定水中持久性有机污染物

采用Envi-18固相萃取小柱富集水样,用正己烷/丙酮混合溶剂洗脱水样中42种POPs化合物,再用气质联用法测定。通过优化仪器监测条件,使目标物在0.250 mg/L~5.00 mg/L范围内线性良好。方法检出限为50.9 ng/L~11 640 ng/L,实际水样加标回收率为57.1%~129%,测定结果的RSD为0.1%~13.8%。将该方法用于测定浙江省东苕溪流域的45份水样,结果滴滴涕、六六六等有机氯农药的检出率较高,其他POPs的检出率较低。     

氨基化有机-无机杂化整体柱分离富集环境水中五价砷

将四乙氧基硅烷(TEOS)和N-(β-氨乙基)-γ-氨丙基三乙氧基硅烷(AEAPTES)作为共聚前体,采用在毛细管内原位聚合的方式制备得到氨基功能化的有机-无机杂化整体柱,将其作为针式固相微萃取(SPME)介质,建立了现场分离富集环境水中As(V)的SPME方法,优化了有机-无机杂化整体柱富集As(V)的实验条件,并研究了整体柱对As(V)的吸附/洗脱性能和富集能力,实现了环境水样中As(V)的高效、快速、高选择性检测。     

M3法测定土壤有效态Cd、Cr、Pb和Ni

通过M3法对耕地土壤重金属的联合测定,为土壤重金属污染监测应用提供快速联合测定的方法。用M3法测定北方耕地土壤的有效Cd、Cr、Pb和Ni,通过对M3法与其他方法进行有效重金属测定值差异性及其相关性比较,与全量的浸出率分析等探讨M3法对耕地土壤有效重金属测定的特征。结果表明,M3法在《土壤环境质量标准》(GB 15618—1995)的土壤重金属含量范围内可以测定土壤有效态重金属Cd、Cr、Pb和Ni,且呈线性极显著相关。M3法与其他方法有效Cd、Cr、Pb和Ni有较好的相关性,与DTPA法呈极显著相关;与NaNO₃法除有效Pb外,呈极显著和显著相关;与HCl法除褐土和潮土的有效Pb外,也呈极显著和显著相关。M3法的有效态Cd、Cr、Pb和Ni的测定值均为最大。M3法对4种耕地土壤有效Cd、Cr、Pb和Ni的浸出率,因土壤类型不同,有效重金属含量所占比率不同,但利用M3法测定的有效态Cd、Cr、Pb和Ni的浸出率最大。     

Solid‐phase extraction and GC analyses of select agricultural pesticides and metabolites in stream water

Abstract

The occurrence of agricultural pesticides in surface waters around the USA has created a concern over the status of safe drinking water. Solid‐phase extraction (SPE) or liquid‐liquid extraction (LLE) is usually employed to concentrate trace levels of pesticides in water samples to concentrations that are measurable with advanced chromatographic instruments. We describe here a SPE and capillary gas chromatographic (GC) procedure to extract and concentrate trace levels of select agricultural pesticides and metabolites from stream water. Our SPE and GC method provides high sensitivity, with recoveries between 85% to 95%, and high reproducibility for 9 of the pesticides studied. The described method provided marginal recoveries of 19 and 60% for the atrazine metabolites.     

U型工作面上隅角埋管瓦斯抽采数值模拟研究

传统的U型通风工作面上隅角瓦斯积聚现象经常出现，严重制约着矿井正常生产能力的有效发挥，对矿井安全生产造成重大威胁。基于前人对采空区非均质多孔介质气体运移理论的研究，采用Fluent软件数值模拟研究了U型和上隅角埋管条件下U型通风系统的静压力场和瓦斯浓度场。研究结果表明：在相同的模型参数条件下，U型通风容易造成上隅角瓦斯积聚，上隅角瓦斯超限问题十分严重；采空区5m处埋管，治理上隅角瓦斯积聚的效果欠佳，达不到安全开采的条件；15m处埋管可以较好的解决上隅角瓦斯超限问题，工作面没有出现瓦斯积聚现象，工作面和回风巷的瓦斯浓度始终处于1％以下；25m处埋管的效果与15m基本相同，没有表现出更好的瓦斯治理效果。综合数值模拟的结果，确定了上隅角埋管抽放采空区瓦斯的理想抽放位置为距离地板垂高1．2m、沿走向深入采空区15m处。     

RUNOFF PREDICTION USING REMOTE SENSING IMAGERY1

ABSTRACT: Percent imperviousness is an important parameter in modeling the urban rainfall-runoff process and is usually determined using manual methods such as random sampling or conventional accounting methods. In this study two computerized methods are used for estimating the percent imperviousness of urban watersheds using high altitude remote sensing imagery. These methods include the Laser Image Processing Scanner and the Video-Tape Camera system. Imperviousness is directly estimated in the former method while in the latter it is estimated as a function of the statistics of the responses on emulsions of the imagery. The percent imperviousness computed by utilizing remote sensing imagery was used with the conceptual models of rainfall-runoff models. The models were applied to four urban watersheds and the runoff prediction results indicate that imperviousness determined by using remote sensing imagery was as accurate as that obtained by the manual methods, and that the use of remote sensing imagery requires significantly less time and money.     

催化裂化废水萃取脱酚预处理研究

选用焦化粗柴油为萃取剂,对催化裂化含酚废水进行脱酚预处理,结果表明,最佳萃取条件为：ｐＨ７．０－８．５,温度１５－４０℃,油水体系比１．７－２．１,理论萃取级数４－７级。在上述条件下,出水酚质量浓度为５０ｍｇ／Ｌ。萃取后的粗柴油用于炼油厂加氢精制装置。