液上空间法分析水中卤代烃

实验建立了利用气液两相平衡对水样中卤代烃含量进行测定的液上空间法。试验了与气液两相平衡有关的因素:温度、压力、气液体积比及平衡时间对测定的影响。对十一个样品进行测定的相对标准偏差为,氯仿:4.2％,四氯化碳:5.3％。方法可检知水样中卤代烃的最低浓度为,氯仿:8×10~(-2)μg/1,四氯化碳:3×10~(-3)μg/1。     

自配消解液分光光度法测定污水中的COD

以自配消解液代替ThermoFisher公司AQ4001COD测定系统的专用消解液，比较了自配消解液分光光度法与国家标准重铬酸钾法(GB 11914-1989)测定化学需氧量(COD)的差异。对比试验表明，自配消解液分光光度法测定COD的结果精确度和准确度高，与国家标准方法无显著性差异。自配消解液分光光度法测定水样COD值的相对标准偏差;低量程(30～150 mg/L)为1.38%～2.53%，中量程(0～1 500 mg/L)为0.47%～3.63%，高量程（2 000～15 000 mg/L）为0.17%～3.53%，在国家标准方法测试水样COD值的允许误差范围内。除制革废水外，自配消解液可以代替AQ4001COD测定系统的专用消解液，适用不同量程范围内污水COD的测定。自配消解液分光光度法具有试剂使用量少、速度快、经济、二次污染小等优点，值得在环境科学领域及废水水质监测中推广应用。     

气相色谱/质谱测定苯酚丙酮生产废水中半挥发性有机物

建立了用二氯甲烷液液萃取对苯酚丙酮生产废水进行预处理,气相色谱/质谱法同时测定废水中半挥发性有毒有机物异丁酸、异丙苯、α-甲基苯乙烯、2-苯基丙醛、苯乙酮、2-苯基-2-丙醇、α-甲基苯甲醇、苯酚和苯甲酸等的定性定量分析方法。色谱条件为:DB-17MS型色谱柱,程序升温,进样量为1μL,质量选择检测器(MSD)。实验结果表明,该色谱条件对苯酚丙酮生产废水中各半挥发性组分具有较好的分离效果。而对9种组分的最低检出限均低于0.04mg/L,精密度实验相对标准偏差2.14%～5.15%,实际水样的加标回收率稳定。苯酚丙酮生产废水中的主要污染物为2-苯基-2-丙醇,其次为苯酚、异丁酸和异丙苯。     

液液萃取 — 超高效液相色谱 — 三重四级杆质谱测定地表水中19种磺胺类药物残留

建立了液液萃取—超高效液相色谱—三重四级杆质谱技术,测定地表水中19种磺胺类药物。通过乙酸乙酯超声萃取水样中的磺胺类药物,并用0.1%(体积分数)甲酸水溶液-甲醇作为流动相,C18色谱柱分离,在多反应监测(MRM)模式下测定。优化了萃取剂种类和用量、超声时间、流动相的组成等条件。在优化条件下,19种磺胺类药物在0.1～40.0μg/L范围内线性良好且相关系数均大于0.999 0,方法检出限为0.02～0.80ng/L,平均回收率为73.5%～92.8%,相对标准偏差为1.2%～8.7%。该方法操作简单、灵敏度高、所需样品及有机溶剂少,适用于实际的分析检验工作。     

反向流动注射分析法(rFIA)多组分同时测定的研究——氧化物和硫化物的分析

本文研究了分別使用吡啶/巴比妥酸和Fe(Ⅲ)/邻菲啰啉体系同时测定CN~-和S~(2-)的反向流动注射分析法。酸化后的样品溶液流经PTFE微孔膜时CN~-透过膜溶入吸收液中,而S~(2-)仍留存在原溶液中,而后分别和相应的显色试剂反应测定。方法适用于电镀厂废水的检测。每小时可分析30个样品。     

环境污染与防治网络版论文摘要

正离子色谱法测定入境废塑料浸出液中阴离子含量杨丽飞王晶胡德新(天津出入境检验检疫局化矿金属材料检测中心,天津300456)建立了离子色谱法同时测定废塑料中F-、Cl-、Br-、NO-3、SO2-4含量的方法。将废塑料破碎后浸提,浸提液经0.22μm微孔滤膜后,用NaOH溶液作淋洗液,利用AS-19型阴离子分离柱和ASRS-3004mm连续自动再生化学抑制器分离阴离子并采集数据。方法的线性相关性好(r0.999),被测离子的检出限(信噪比(S/N)=3)均低于20μg/L,样品的平均加标回收率为95%~107%。关键词废塑料离子色谱法阴离子     

钍试剂分光光度法测定固定源烟气中SO3

以80%(体积分数)异丙醇为吸收液采集SO3后,用过量的Ba(ClO4)2与吸收液中SO42-反应,剩余Ba2 与钍试剂生成钍-钡络合物,测定该络合物在530 nm处的吸光度,由此间接计算出固定源烟气中SO3的浓度.钍试剂分光光度法对溶液SO42-测定范围为2.00～60.00 μg/mL,检出限为1.17 μg/mL.不同浓度样品的重复性实验和回收率检验结果证明了该法具有很好的精确度和准确度.样品中含有少量的Ca2 、Na 、K 、CO2-3、Cl-等,对测定结果无显著影响.     

工业废水中有机氟的测定

一、引 言 上海高校协作组承担了黄浦江水质污染的监测与治理任务。在对黄浦江上游吴泾工业区水质的监测中提出了工业废水中有机氟的分析课题。关于氟污染的分析,国内外多是进行植物中含氟量,人体中血氟、尿氟、骨氟和水质、土壤、空气中氟离子的测定,而对工业废水中有机氟的测定未见报道。本文对工业废水中有机氟的测定作了初步探索,即用液-液萃取法或大孔树脂吸附法对废水中的有机氟进行富集,再用氧瓶法分解,最后用离子选择电极法测定。本方法对模拟水样、实验室废水及工业废水中的有机     

气相色谱测定蔬菜上百菌清残留量的方法研究

本文主要介绍百菌清在八种蔬菜中的残留分析方法。该法前处理简便、准确,平均回收率为97.8％,平均变异系数为3.53％。一、方法提要用丙酮溶剂振荡提取,经石油醚液—液分配净化,浓缩,定容后用气相色谱法电子捕获检测器(ECD)测定百菌清的残留量。仪器的最低检出量为2.2×10~(-11)g,样品的最低检出浓度为10ppb。     

气相色谱法测定空气中的1，2-二氯乙烷

建立了一种用气相色谱法测定空气中1，2-二氯乙烷的方法。空气中1，2-二氯乙烷用活性炭吸附，二硫化碳解析，直接进样分析。其回收率为97．6％～100．8％，最低检出浓度为0．005mg／m^3，相对标准偏差为0．7％-2．4％；该方法具有前处理简单、速度快、干扰少、灵敏度高等特点，可用于空气中1，2-二氯乙烷的测定。     

电热蚊香片益多克含量的气相色谱测定

叙述了采用气相色谱法,以ＦＩＤ检测器和内标法定量测定电热蚊香片中益多克的含量。方法的变异系数为１．１％,回收率达到９８．７％,线性相关系数为．９９９１。该方法适用电热蚊香片中益多克的含量测定。     

浊度仪法快速测定水体中硫酸盐含量

为了适应野外水质快速测定的要求,根据硫酸钡比浊法的方法原理,采用浊度仪测定浊度的方法,建立了水体中硫酸盐含量的快速测定方法。实验考察了浊度、氯化钡加入形态、摇动时间,静置时间等影响因素。结果表明,浊度在5～25 NTU时,其对硫酸盐的测定几乎没有影响。在实验最佳条件下,氯化钡的加入量为0.2 g,中速手摇40 s,静置时间5min,所建立方法的线性范围为5～90 mg/L,相关系数R2=0.9998,方法的检出限为0.25 mg/L。加标回收率为94.00%～105.25%,相对标准偏差(RSD)为0.19%～1.75%(n=5),方法便携、简单,适用于野外与浊度同步测定。     

ASE提取GPC净化双塔双柱气相色谱法测定土壤中有机氯农药

对土壤中8种有机氯农药(α-HCH、β-HCH、γ-HCH、δ-HCH、p,p’-DDE、p,p’-DDD、o,p’-DDT、p,p’-DDT)进行了分析,使用加速溶剂萃取(ASE)仪对土壤样品中的目标组分进行萃取、凝胶渗透色谱(GPC)仪对萃取液净化、双塔双柱同时进样分析,采用双电子捕获检测器(ECD)同时定性定量测定。结果表明,该方法检测效果较好,8种有机氯农药的回收率在81.3%～88.6%,相对标准偏差为3.9%～5.7%,检出限为0.18～0.37μg/kg。与传统的方法相比,该方法操作简便、重复性好,定性定量更准确。     

Quantitative analysis of acetamiprid and imidacloprid residues in tomato fruits under greenhouse conditions

Abstract

A selective liquid chromatographic analytical method was studied for determination of two neonicotinoids, acetamiprid and imidacloprid, in tomato fruits under greenhouse conditions in Egypt. The fruits were extracted and cleaned up by QuEChERS method followed by HPLC determination. The method showed a good linearity with a determination coefficient (R²) of higher than 0.99 for the 0.0125–0.15 µg/mL concentration range. The method was validated using a blank tomato spiked at 5, 25 and 50 mg/kg and the recovery percentages were 83.71, 94.52 and 97.49% for acetamiprid and 88.59, 89.63 and 90.18% for imidacloprid, respectively. The rates of dissipation of both pesticides were studied and the preharvest intervals (PHIs) were calculated. Imidacloprid dissipated faster than acetamiprid and half-life periods were 1.30 and 2.07 days, respectively. Acetamiprid and imidacloprid residues were below the already established European maximum residue limits (EU MRLs) (0.5 mg/kg) 3 and 5 days after application, respectively.     

Determination of toxaphenes in fish and marine mammals

An analytical method for the determination of toxaphene in biological materials using gas chromatography with an electron capture detector (GC-ECD) has been established and validated for three single congeners (chlorinated bornanes (CHB) 26, 50 and 62). The analytical method was based on a method for determination of PCB, DDT and other chlorinated pesticides. To include toxaphene congeners an extra step, adsorption chromatography on silica columns, was introduced to separate the pesticides from PCB. The recovery of CHB-26, 50 and 62 were 97+/-11%, 94+/-10% and 99+/-12%, respectively. Samples from cod, ringed seal and polar bear from the Norwegian arctic environment have been analysed. The levels of CHB-26 and 50 found were 13-55 ng/g fat in cod, 1.3-7.7 ng/g fat in ringed seal and 0.4-119 ng/g fat in polar bear. The levels of CHB-62 were 2.0-13, 0.8-3.4, 0.2-11 ng/g fat in cod, ringed seal and polar bear, respectively.     

固相微萃取-气相色谱-质谱法测定地毯中总挥发性有机化合物

建立了一种固相微萃取与气相色谱质谱联用测定地毯中总挥发性有机化合物的方法,该方法简便快速,重现性好,分析结果同小型环境平衡舱法测定的结果比较吻合。     

基于三波长透射率的水体色度检测标准

为了推动有关分光光度法测量水体色度的国家标准的建立，对美国和台湾地区的水体色度标准检测方法进行了研究，提出了新的基于三波长透射率测量水体色度的方法。根据现行国家标准中的色度学相关数据，选择在595、555和445 nm 3个波长处的光谱透射率计算水样的三刺激值，依照国标推荐的色差公式建立了测量水样色度的标准检量线。利用所提出的新的水体色度测量方法对5个水样的色度值进行了实际测量，结果表明，新的测量方法所得到的水体色度值与铂钴比色法一致。     

AA3流动注射仪快速测定地表水中的总氰化物

在反复实验的基础上建立了运用Bran+Luebbe AutoAnalyzer 3流动注射分析仪快速测定地表水中总氰化物的分析方法。结果表明,该方法与传统的分光光度法相比,具有自动进样、分析速度快、测定成本低等优点。与经典的分析方法相对照,结果无显著性差异,能够满足大批量地表水监测的要求。在测试系统中引入了恒温槽,进一步提高了测试的精密度和准确度。     

Novel method for determining pyrene biodegradation using synchronous fluorimetry

To study the biodegradation rate of pyrene dissolved in liquid medium supplemented with mineral salts, a synchronous fluorimetry (SF) method was established. The limit of detection for pyrene dissolved in mineral salts medium (MSM) was determined as 0.19 ng/ml with a relative standard deviation of less than 1.3% (n = 9). The pyrene degrading rates of four bacterial strains were investigated using this method under the same experimental conditions. The degradation rates of the three active strains ranged from 76% to 87% after a 14-h incubation. The results were confirmed by the gas chromatography with a flame ionized detector (GC/FID) method. This implies that pyrene degradation can be directly monitored by the SF method without the solvent extraction of samples. The advantages of SF are that it is less laborious, faster, and less expensive than the GC/FID determination method with solvent extraction. The SF method provides a new tool for studying the degradation of polynuclear aromatic hydrocarbons (PAHs) in the natural environment and under experimental conditions.     

A rapid and efficient determination of natural estrogens in soils by pressurised liquid extraction and gas chromatography-mass spectrometry

We present a new analytical procedure for the extraction and determination of natural estrogens in soils based on pressurised liquid extraction and GC-MS determination. After testing twelve solvents, acetone proved to be the most efficient extractant. The optimum extraction temperature is 60 degrees C. Soil extracts have to be purified and concentrated by C-18 solid phase extraction. The dried extracts are derivatised by N-methyl-N-(trimethylsilyl)trifluoro-acetamide before measurement by GC-MS. Recoveries of 79-103% with relative standard deviations 相似文献