Dispersive liquid–liquid microextraction of cadmium(II) for preconcentration prior to flame atomic absorption spectrometric detection in water

A dispersive liquid–liquid microextraction procedure for cadmium(II) as its 2-(5-bromo-2-pyridylazo)-5-diethylamino-phenol chelate is presented. Carbon tetrachloride and methanol were used as extraction and dispersive solvents, respectively. After phase separation, the preconcentrated-separated cadmium(II) is determined by flame atomic absorption spectrometry with a microinjection technique. The factors which affected the extraction efficiency, i.e. the pH of the sample solution and the volumes of reagent and sample were investigated. The effects of some alkali, alkali earth, and transition metal ions, and of some anions on the recovery of cadmium were also studied. A preconcentration factor of 250 was obtained for a sample volume of 50?mL under optimum conditions. The method was validated by analysis of certified reference materials and applied to some water samples from Turkey.     

Comparison of sample digestion procedures for the determination of trace elements in antarctic krill by GF‐AAS

Two independent digestion procedures for Antarctic krill samples were compared. Dry ashing (DA) and microwave (MW) acid‐assisted digestion were tested for decomposing the samples to determine essential (Cu, Fe, Cr) and toxic elements (Cd, Pb) by graphite furnace‐atomic absorption spectrometry (GF‐AAS). A mixture of HNO₃ and H₂O₂ as digesting agent was used in the microwave procedure. For the dry ashing digestion, the organic matter was oxidated at 480°C in an open system. Both digestion methods were compared in terms of accuracy and applied to the analysis of a certified reference material: MURST‐ISS‐A2 (Antarctic krill).

The detection limits for the five elements analysed ranged from 3 to 150 ng g^‐1. Both digestion procedures are suitable for the decomposition of krill samples. However, dry ashing is not recommended to determine Pb and Cd because losses can occur.     

Determination of pesticides in apples,grapes and apple juice from a Kosovo market by gradient liquid chromatography with tandem mass spectrometry

Apple, grape, and apple juice were analyzed for pesticides using a multireaction mode (MRM) method in samples taken from a Kosovo market. With this method it was possible to analyze about 100 pesticides in the ESI mode. In these samples some types of pesticides were found, but most of them did not exceed the maximum tolerance levels. In apple samples, six pesticides were detected but only three of them were in sufficient quantitites. Dimethoat was below the limit, while acephate and imazalil exceeded the limit. In grape and apple juice samples, all of pesticides which were found did not exceed the maximum tolerable limits.     

污染水体中鱼体内三聚氰胺的累积及其在清洁水体中的消除

以吉富罗非鱼（Oreochromis niloticus）为受试动物,在室内用水族箱进行模拟养殖试验,设定污染水体中三聚氰胺初始浓度为0.2 g·L-1,考察罗非鱼在其中饲养1周期间体内三聚氰胺的累积情况。再将鱼转移至不含三聚氰胺的清洁水体中饲养1周,考察鱼体内三聚氰胺在其中的消除情况。结果表明,三聚氰胺能在鱼体内迅速富集,鱼肉及内脏中三聚氰胺的含量均与鱼在污染水体中暴露的时间成正相关。其中,鱼肉中三聚氰胺的浓度几乎成线性增大,拟合所得方程为y=5.598 8x＋12.897,相关系数为0.995 9。内脏对三聚氰胺的富集速率先快后慢,且其中三聚氰胺的浓度为鱼肉的2~3倍。在试验后期,鱼肉及内脏中三聚氰胺的浓度分别高达51.55 mg·kg-1和93.89 mg·kg-1,此时罗非鱼表现出明显的中毒迹象。将罗非鱼转移至清洁水体中养殖后,鱼肉及内脏中三聚氰胺的残留量均迅速下降,尤其是后者的消除速度甚快,一周后两者的浓度分别降至0.13 mg·kg-1和0.21 mg·kg-1。此时,罗非鱼中毒症状逐渐消失,活动趋向正常。     

Simultaneous analysis of five taste and odor compounds in surface water using solid-phase extraction and gas chromatography-mass spectrometry

In this paper, a method using solid-phase extraction (SPE) and gas chromatography-mass spectrometry (GC-MS) was developed to simultaneously analyze five taste and odor compounds in surface water, i.e., 2-methylisoborneol (2-MIB), 2,4,6-trichloroanisole (TCA), 2-isopropyl-3-methoxy pyrazine (IPMP), 2-isobutyl-3-methoxy pyrazine (IBMP), and trans-1,10-dimethyl-trans-9-decalol (geosmin, GSM). The mass spectrometry was operated in selective ion monitoring (SIM) mode. Three kinds of SPE columns and three eluting solvents were compared, the C18 column was chosen as optimum SPE column, and methanol was chosen as the optimum eluting solvent. It was found that the method showed good linearity in the range of 1–200 ng·L^-1 and gave detection limits of 0.5–1.5 ng·L^-1 for individual compounds. Good recoveries (93.5%–108%) and relative standard deviations (1.58%–7.31%) were also obtained. Additionally, concentrations of these taste and odor compounds in Jinan’s surface and drinking water were analyzed by applying this method, and the results showed that GSM and 2-MIB were the dominant taste and odor compounds in Jinan’s raw water.     

硫精砂制酸尾气达标排放及资源化回收利用

硫精砂制酸排出的尾气中SO2含量一般为0.2%~0.5%(体积分数,下同),目前国内普遍采用一转一吸或两转两吸流程来吸收硫酸尾气,使SO2质量浓度达到低于860 mg/m3的国家二级排放标准。但随着国家颁布新的《硫酸工业污染物排放标准》,要求现有硫酸企业SO2排放质量浓度必须于2013年10月1日前全部低于400mg/m3,因此必须对尾气进行进一步的处理。本文结合湖北新洋丰肥业股份有限公司和武汉中东化工有限公司硫酸生产的实际情况,总结了采取三段氨吸法处理硫酸尾气的技术改造和资源化回收利用。     

纳米X型沸石制备及其对含铜废水处理

采用水热合成法以煅烧高岭土为原料合成了纳米级X型沸石分子筛,并采用透射电镜(TEM)和X射线衍射(XRD)进行了表征.研究了影响纳米X型沸石分子筛对Cu(Ⅱ)吸附的因素,包括纳米X型沸石分子筛用量、pH值、接触时间和温度.结果表明:投加0.4 g纳米X沸石分子筛,在pH为5.0、温度为25 C、吸附时间为10 min情况下,去除率达到99.65%,最大吸附量可达101.4 mg/g.采用0.5 mol/L的Na2EDTA能较完全洗脱纳米级X型沸石分子筛所吸附的Cu(Ⅱ),表明纳米级X型沸石分子筛能循环使用,可应用于含铜废水的处理.     

红外光度法测定水中微量石油类问题探讨

对用红外光度法测定水中石油类影响检出限的诸多因素进行了探讨。结果表明,采用适当的方法,可使检出限提高到μg/L级。     

标准加入法在原子吸收光度法中的应用

介绍了原子吸收光度法中的光谱干扰和非光谱干扰，指出标准加入法和分析校准曲线法是消除和减少某些干扰最简单、快速的校准方法。在标准加入法中，当分析曲线呈线性时，表明分析结果可信，当分析曲线不呈线性，表明方法灵敏度随质量浓度变化而变化，分析结果的准确性有问题。以改变基体的质量浓度和在同一质量浓度的基体溶液中加入不同量的标准两个实验可以验证标准加入法在原子吸收光度法中的适用性。     

2-氯-5-三氯甲基吡啶的波谱学数据与结构分析

2-氯-5-三氯甲基吡啶是重要的农药中间体.以3-甲基吡啶为原料通过光氯化反应合成2-氯-5-三氯甲基吡啶,经分离后得到纯度为99.5%的产品.利用红外(IR)、紫外(UV)、质谱(MS)、核磁共振(NMR)等实验技术研究了其波谱学特征,详细讨论了该化合物的1HNMR、13CNMR谱,并对所有1HNMR、13CNMR谱的信号进行了归属.讨论了红外吸收特征峰对应官能团的振动形式,样品的官能团与目标化合物一致.该方法为此类化合物的结构解析提供了有益的分析依据.