分散液液微萃取-气相色谱/质谱法测定水中阿特拉津

建立了简便、快速、有效的分散液液微萃取(DLLME)-气相色谱/质谱技术萃取水样中痕量阿特拉津的新方法。通过试验确定最佳萃取条件。     

样品保存方法对阳极溶出伏安法测定时的影响

对海水中Cu、Pb、Zn、Cd的日常监测分析方法进行了调查,结果表明在调查范围内阳极溶出伏安法使用数量最高。通过实验研究了不添加保存剂、加浓HNO3、加浓HClO4对阳极溶出伏安法测定海水Cu、Pb、Zn、Cd的影响。发现不添加保存剂时4种金属峰电位变化范围大、出现频次分散,分析方法灵敏度下降。不同类型酸对阳极溶出伏安法测定Pb、Zn、Cd时的峰电位变化影响不大,加浓HNO3时Cu的峰电位变化小于加浓HClO4。根据实验结果,推荐使用保存剂为浓HNO3。     

间接竞争ELISA方法测定水中2，4-D的研究

以2,4-D-BSA为包被抗原,采用自行制备的2,4-D单克隆特异性抗体6D11建立了水中2,4-D的间接竞争 ELISA检测方法．本研究比较了包被抗原2,4-D-BSA浓度分别为240ng·mL-1、120ng·mL-1和60ng·mL-1的反应体系和竞争反应时间为60min和15min的间接竞争ELISA剂量-反应曲线,确定了当包被抗原浓度为60 ng·mL-1、竞争反应时间为15min时,剂量-反应曲线的IC50值较低．采用上述实验条件分别测定了由PBS缓冲溶液、饮用水、清华大学地下水和圆明园福海地表水配制的2,4-D标准溶液的剂量．反应曲线,发现实际水样的基质效应对检测结果的影响较大;采用实际水样和PBS缓冲溶液配水在含有5％乙醇的PBS缓冲体系中反应的方法,基本上消除了基质效应对检测结果的干扰．采用上述优化试验条件,测定2,4-D浓度分别为0．5mg·L-1、0．125mg·L-1和0．03mg·L-1的加标样品,测定数据的准确度符合痕量有机污染物定量检测对准确度的要求,但是平行样品测定数据之间的变异系数较大,需要进一步改进检测方法,用于实际水样的检测．     

顶空固相微萃取-气相色谱法测定水中四乙基铅

建立了水中四乙基铅的测定方法——顶空固相微萃取-气相色谱法,探讨了影响水中四乙基铅萃取效率的温度、转速和萃取时间等因素。实验结果表明,在0.08～10μg/L范围内线性关系良好,方法检出限为0.02μg/L,实际水样加标回收率为96.2%～98.3%。     

国产脱硝催化剂在国电长源荆州电厂2×300MW机组上的应用

随着新火电厂大气污染物排放标准的出台,NOx排放标准提高,现有的脱硝技术难以满足要求,需要增加后端烟气脱硝处理技术.选择性催化还原法是较成熟的烟气脱硝技术,催化剂是SCR技术的核心.针对国内某催化剂在国电长源荆州电厂的应用情况,详细描述了催化剂的设计选型过程.运行结果表明,该催化剂完全可以满足长源荆州电厂的性能要求,说明国产脱硝催化剂的设计选型、生产以及运行等技术能力已达到要求.     

Estimation of Efficiency of Processing Soil Samples for Pesticide Residues Analysis

The efficiency of four sample processing methods was tested with eight different types of soils representing the major proportion of cultivated soils. The principle of sampling constant was applied for characterizing the efficiency of the procedures and testing the well-mixed status of the prepared soil. The test material was 14C-labeled atrazine that enabled keeping the random error of analyses ≤ about 1%. Adding water to the soil proved to be the most efficient and generally applicable procedure resulting in about 6% relative sample processing uncertainty for 20 g test portions. The expected error is inversely proportional to the mass of test portion. Smashing and manual mixing of soil resulted in about four times higher uncertainty than mixing with water. Grinding of soil is applicable for dry soils only, but the test procedure applied was not suitable for estimating a typical uncertainty of processing dry soil samples. Adding dry ice did not improve the efficiency of sample processing.     

Trace phthalate and adipate esters contaminated in packaged food

A method for trace analysis of two plasticizers, di-2-ethylhexyl phthalate (DEHP) and di-2-ethylhexyl adipate (DEHA), contaminated in packaged curry paste were investigated by gas chromatography with flame ionization detector (GC-FID). Curry paste samples were extracted by ultrasonic and solid phase extraction using Florisil® cartridge. Analysis by the GC-FID system provided limits of detection for DEHA and DEHP at 12 and 25 μ g L^{? 1} and a linear dynamic range between 25 μ g L^{? 1} to 60 mg L^{? 1} with a coefficient of determination (R²) greater than 0.99. High recoveries were obtained, ranged from 91 to 99% and 88 to 98% for DEHP and DEHA with RSD lower than 7 and 10% respectively. The method detection limit and limits of quantitation were ranged from 27 to 30 and 90 to 100 μ g L^{? 1}. The analysis of curry paste samples showed concentrations of DEHP and DEHA in the range of 4.0 ng g^{? 1} to 0.61 μg g^{? 1}.     

Comparison of two sample preparation methods for analysis of organochlorine pesticides residues in fish muscle

The aim of this study was to compare recoveries of organochlorine pesticides (heptachlor, α-HCH, β-HCH, γ-HCH, op′-DDD, pp′-DDD, pp′-DDE, op′-DDT, pp′-DDT) from fish muscle dried by two alternative methods: (i) grinding with anhydrous sodium sulphate and (ii) freeze drying. Pesticide residues content was determined by gas chromatography-mass spectrometry (GS-MS) method. For four pesticides (γ-HCH, α-HCH, heptachlor and pp;-DDD) in four of five fish species, higher recoveries were obtained from the freeze-dried samples. For five remaining pesticides, correlations between fish species and drying method were not found. The results of this study do not clearly indicate which drying method caused lower losses of analytes. Recoveries from the freeze-dried samples ranged from 69.9 to 117.6 %, while recoveries from the samples ground with sodium sulphate varied from 64.4 to 126.7 %. Either of the methods gave satisfactory recoveries and they both can be used interchangeably.     

Much Ado: How Big Is the Problem of Hydrolysis of Methyl Tertiary Butyl Ether (MtBE) to Form Tertiary Butyl Alcohol (tBA)?

Groundwater contaminated by the gasoline additive methyl tertiary butyl ether (MtBE) is also frequently impacted by tertiary butyl alcohol (tBA). The USEPA recently sponsored a study that discusses the possibility of hydrolysis of MtBE to form tBA during analytical procedures. This finding is important because it suggests that existing tBA data may not accurately depict tBA or MtBE concentrations in groundwater. This article discusses the mechanism and kinetics of MtBE hydrolysis, then presents three case studies of analytical results from sites in California, USA. Although these case studies are limited in scope, the data do not support the occurrence of the hydrolysis of MtBE to form tBA due to acid preservation of groundwater samples. At a minimum, this suggests that MtBE hydrolysis may not be as pervasive a problem as suggested in USEPA's study; therefore, concerns about the validity of historical tBA data may not be warranted. The reason for this result may be simple: there are two necessary factors that promote hydrolysis: low pH and high temperature (above 40°C). Although the static headspace analysis method used to obtain the data in the White et al. study may require heating to achieve adequate sensitivity, many laboratories perform purge-and-trap analyses without heating. Under those conditions, hydrolysis may not occur. However, it may be prudent to preserve samples with alkaline preservatives, to eschew high temperatures during the analysis of groundwater samples, or to neutralize the sample pH before heating.     

嗅觉实验配气方法的改进及影响因素研究

配制气体样品是异味测试及相关研究的基础工作,配气稳定性直接影响测试结果准确度。三点比较式臭袋法使用微量进样针量取并转移液体标准物质到3L无臭气袋的传统配气方法。对于异味阈值较小物质或样品浓度处于较低范围时,为了降低取样体积波动对配气精度和稳定性的影响。提出先将标准注入100mL玻璃注射器,充分挥发混匀后再转移部分气体到无臭气袋的两步式配气方法。结果表明,2种配气方法的准确度不存在显著差异,但两步式配气法的配气稳定性明显优于传统方法。此外,研究还发现,常见异味物质在被注人气袋后3min内便能完全挥发并混合均匀。除一些挥发性和吸附性极强的物质外,气袋内的异味物质气体浓度能在配好后20min内基本保持不变。