磷酸钕共沉淀选择性分离富集-原子吸收测定环境水样中痕量铅

研究提出了用磷酸钕(NdPO4)作为共沉淀捕集剂分离富集环境水样中的痕量Pb2 ,用火焰原子吸收光谱(FAAS)测定的方法.共沉淀受pH、NdCl3和H3PO4溶液用量的影响.结果显示,在溶液pH为3.2时,20 mL水样中加入5 mg/L NdCl3 2 mL、0.5 mol/L H3PO4 3 mL条件下,铅的加标回收率为96.6%～104.2%,方法的检测限为5.7×10-3 mg/L,水体中常见碱金属、碱土金属离子及阴离子在一定范围内不影响测定.     

正交实验设计的电浮选方法净化含Cr(Ⅲ)污水的研究

选定电流密度i(A),浮选时间t(B),液位高度H(C),溶液pH(D),溶液电导率k(E)和表面活性剂SDS浓度CSDS(F)6个影响电浮选效率的因素,按照L27(313)正交表,用电浮选方法对处理含Cr(Ⅲ)污水进行了研究。得到最佳的实验室浮选条件为i=125 A/m2,t=30 min,H=0.73 m,pH=9.0,CSDS=1×10-4mol/L,在此条件下,出水含Cr(Ⅲ)浓度低于0.5 mg/L。实验结果方差分析表明,i和t是影响浮选效率的高度显著因素,且两者之间有显著的交互作用,表面活性剂SDS对浮选效率也表现出一定的影响。     

固相萃取分离富集分光光度法测定水环境中的二价铁

提出了应用固相萃取分离富集分光光度法测定水环境中痕量Fe2 的新方法.水样中的Fe2 首先与1,10-邻二氮菲(1,10-phen)络合剂作用生成有色阳离子络合物, 然后通过Sep-Pak C18柱预富集分离,以乙醇和盐酸混合溶液为洗提液,在509 nm测定痕量Fe2 .同时,以人工海水为对象详细讨论了盐含量对分析测定的影响.该方法灵敏度高, 选择性好,方法的最低检测限2.9 μg/L,相对标准偏差0.93%,可用于测定淡水和海水水样中痕量Fe2 , 回收率为92%～102%.     

全固态硝酸根离子选择电极

研究了一种以玻碳电极为基底电极,以聚吡咯为中间体,以聚氯乙烯(PVC)为敏感基膜的全固态硝酸根离子选择电极。结果表明,电极在1×10-5~1×10-1mol/L的硝酸钠溶液中呈现近能斯特响应,响应斜率为(-54±1.0)m V/dec,检测下限为3.16×10-6mol/L。该电极的响应时间短,稳定性及重复性较好,对硝酸根具有很好的选择性。用于实验室水样中硝酸根的回收率测定,结果令人满意。该电极制作简单,机械强度高,使用寿命超过3个月,对用于水中硝酸根的在线分析与测定有重要意义。     

聚L-组氨酸修饰电极方波溶出伏安法同时测定痕量铅和镉

在pH=3.0的NaAc-HAc缓冲液中,用循环伏安法制备聚L-组氨酸修饰玻碳电极,研究Pb2+和Cd2+在修饰电极上的方波阳极溶出伏安特性,建立了方波阳极溶出伏安法测定Pb2+和Cd2+的新方法。在最佳实验条件下,Pb2+和Cd2+的摩尔浓度为5.00×10-8~7.50×10-4 mol/L时与峰电流呈良好的线性关系,Pb2+和Cd2+检出限分别为5.0×10-9、1.0×10-9 mol/L。     

邻菲啰啉活化催化褪色光度法测定环境水体中痕量铜(Ⅱ)

根据邻菲啰啉活化痕量铜(Ⅱ)催化溴酸钾氧化甲基紫褪色反应,建立了催化褪色光度法测定痕量铜(Ⅱ)的新方法.讨论了介质、试剂用量、反应温度、反应时间、活化剂和共存离子的影响,确定了最佳试验条件.结果表明,在25 mL溶液中,72 ℃恒温反应15 min,加铜(Ⅱ)和不加铜(Ⅱ)的吸光度差值与铜(Ⅱ)质量浓度间的关系在铜(Ⅱ)质量浓度为2.40×10-3～5.12×10-2 mg/L时呈线性关系,符合比尔定律;该新方法的测定波长为578 nm,铜(Ⅱ)检出限为2.40×10-3 mg/L,用于环境水体中痕量铜(Ⅱ)的测定,最大相对标准偏差为3.14%,加标回收率为96.0%～105.0%,对比<水质铜的测定二乙基二硫代氨基甲酸钠分光光度法> (GB/T 7474-1987) 相对误差低于6.00%.     

流动注射-火焰原子吸收法快速测定水样化学需氧量

采用流动注射-火焰原子吸收法(FI-FAAS)测定水样化学需氧量.以KMnO4作氧化剂、葡萄糖作基准物质,在95 ℃反应,生成的Mn(Ⅱ)在线分离吸附于阳离子交换树脂微型柱上,用3 mol/L HCl洗脱后,送至火焰原子吸收检测器检测.在反应盘管长500 cm、反应时间30 s的条件下,测定化学需氧量的线性范围为8.00～200.00 mg/L,检出限为2.30 mg/L;采样频率为24次/h,Cl-质量浓度至100 mg/L无干扰,Mg2 质量浓度至1 000 mg/L无干扰;对50.00 mg/L的化学需氧量标样重复测定7次,相对标准偏差为3.37%.用该法测定河水、池塘水和轻度污染工业废水的化学需氧量,获得了与重铬酸盐法(标准方法)基本一致的测定结果.     

反相高效液相色谱法测定污水中壬基酚聚氧乙烯醚总量

建立了固相萃取一反相液相色谱一荧光检测法分析污水中壬基酚聚氧乙烯醚总量的方法.固相萃取采用Wa-ters Oasis HLB固相萃取柱(30 μg×60 mg×3 mL),6 mL二氯甲烷/甲醇(90/10,V/V)混合溶剂洗脱,洗脱液用氮吹仪浓缩至1 mL,回收率为99.68%.采用ZORBAX Eclipse XDBC-18(4.6 mm×150 mm,5 μm)反相色谱柱,甲醇/水为流动相,流速1.0 mL/min,以每分钟增加2.5%的梯度陡度进行洗脱,流动相中甲醇比例由70%增加到100%,柱温23℃,进样量15μL.荧光检测器的激发波长230 nm,发射波长313 nm.采用外标法定量.该方法的空白加标和污水样品加标回收率均在90%以上,标准偏差小于10%,定量下限为0.97～1.90 μg/L.利用该方法分别对污水处理厂进水水样、二级处理出水水样、再生水水样进行了测定,测定结果的准确度和精密度满足痕量分析的要求.     

臭氧化降解结晶紫溶液的机理

采用臭氧化法对模拟废水中难生物降解的结晶紫染料进行降解实验研究,藉助紫外光谱、红外光谱、气相色谱、化学需氧量和总有机碳的检测结果对反应机理进行了初步探讨。实验结果表明,当溶液初始质量浓度0.88 mmol/L,臭氧投加量9.06×10-5mol/min,调节初始溶液pH为10.0,控制反应温度298 K,反应120 min后,结晶紫溶液COD去除率达到97.0%。分析表明,结晶紫染料降解的中间产物主要是对氨基苯酚、丁烯二酸、乙酸等有机小分子物质,最终产物为水和二氧化碳。     

吹扫捕集-GC-MS测定废水中的硝基氯苯

建立了吹扫捕集-GC-MS测定水样中硝基氯苯类化合物的方法.考察了吹扫温度、吹扫时间等对吹扫捕集效率和方法检出限的影响.在室温下,当吹扫时间为30 min时,该方法的最低检出限可达0.002 mg/L,工作曲线的线性范围为2×10 -3 ～2 mg/L,相对标准偏差在2%～6%,加标回收率在97.0%～110.0%.与国家标准方法相比,该法具有操作简便、灵敏度高、线性范围宽且无须使用有毒有机溶剂等优点,可满足工业废水和地表水中硝基氯苯的测定要求.     

Rapid PCDD/PCDF screening method for fly ash with ion trap MS/MS

A rapid screening method for the polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/PCDF) in fly ash has been developed. The screening is done in two steps: (a) the extraction by the accelerated solvent extraction and (b) the quantitative measurement by ion trap tandem mass spectrometer (MS/MS). Anhydrous sodium sulfate was added to the fly ash containing activated carbon in order to increase the extraction efficiency. The selectivity of the ion trap MS/MS was confirmed with 13C-labelled internal standard. Then the results of the screening method were compared with those obtained by the conventional analytical method using high-resolution mass spectrometer (HRMS).     

硫化沉淀法处理矿山酸性废水研究

对沉淀浮选机理进行了分析 ,讨论了选择性沉淀 浮选技术 ,论述了硫化沉淀浮选法不仅能处理矿山含重金属离子废水 ,同时还能回收其中的有用金属     

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   

An improved extraction method to determine the initial emittable concentration and the partition coefficient of VOCs in dry building materials

Based on the extraction method presented by Smith et al. (2008), this paper proposes an improved method, the multi-emission/flush regression method, to simultaneously determine the initial emittable concentration and the partition coefficient. Compared to the extraction method, the proposed method has the following advantages: (1) it is unnecessary for the target volatile organic compounds (VOCs) to emit completely from the material, thus greatly reducing experimental time; (2) it provides a simpler way to obtain the partition coefficients of VOCs for tested materials and can avoid the measurement uncertainties at low VOC concentrations which often occur during the last few cycles of the extraction method; (3) it does not require grinding the building material into powders thus making this method more convenient to use. Comparisons were made between the initial emittable VOC concentrations determined by the original extraction method and the proposed method. Results show good agreements between these two methods. To further validate the proposed method, the type of static chamber developed by Wang et al. (2006) was used to conduct the experiment for a type of medium density board, and formaldehyde was selected as the target compound. Based on the initial emittable concentration and partition coefficient obtained using the proposed method, and the diffusion coefficient obtained by the mercury intruding porosimetry, the chamber formaldehyde concentration was predicted and compared with the experimental measurements. Results show that the predicted chamber VOC concentration using the measured parameters agree well with the experimental data.     

Relevance study of bare and coated zero valent iron nanoparticles for lindane degradation from its by-product monitorization

Zero-valent iron nanoparticles (NZVI) as well as polymer–stabilized nanoparticles were synthesized and used for lindane (γ-hexachlorocyclohexane) degradation in aqueous solution. To study the effectiveness of the different coated nanoparticles, simple and rapid analytical methods have been developed to measure and to detect lindane and its by-products. For the monitorization of lindane degradation solid-phase extraction (SPE) was used, while volatile by-products formation measurement was carried out by headspace-solid phase microextraction (HS–SPME) followed by GC/MS. The SPE–GC/MS method provides low detection limits (0.2 μg L⁻¹), high recovery (above 95%) and it is a valuable tool for kinetic studies of the degradation process for each polymer used, while HS–SPME–GC/MS has proved to be an effective tool for the extraction and evaluation of volatile degradation by-products.     

移动式絮凝-气浮集成系统研制及其在城市污染河湖治理中的应用

针对北京城市河湖的污染状况,论述了传统絮凝-气浮工艺在污染治理中的应用研究及以该工艺为基础的集成系统的开发.结果表明,该系统对TP、COD去除率分别达81%和75%.该系统的研制成功为城市河湖的污染治理开辟了新途径.     

移动式絮凝-气浮集成系统研制及其在城市污染河湖治理中的应用

针对北京城市河湖的污染状况，论述了传统絮凝一气浮工艺在污染治理中的应用研究及以该工艺为基础的集成系统的开发。结果表明，该系统对TP、COD去除率分别达81％和75％。该系统的研制成功为城市河湖的污染治理开辟了新途径。     

Multivariate optimization of solid-phase extraction applied to iron determination in finished waters

In this work, Amberlite XAD-4 resin functionalized with salicylic acid was synthetized, characterized and applied as a new packing material for an on-line system to iron determination in aqueous samples. The detection method is based on the sorption of Fe(III) ions in a minicolumn containing the synthesized resin, followed by a desorption step using an acid solution and measurement of iron by vis-spectrophotometry (CAS method). The optimization of the solid-phase extraction system was performed using factorial design and Doehlert matrix considering six variables: sample percolation rate (0.5-9 ml min(-1)), sample metal concentration (20-200 microg l(-1)), flow-through sample volume (0-5 ml) (all three directly linked to the extraction step), elution flow-rate (0.5-9 ml min(-1)), concentration and volume of eluent (HCl 0.1-0.5M) (all three directly linked to the elution step). The aim of this study was to obtain a set of operating ranges for the six variables tested in order to obtain--by means of a mathematical function allowing maximisation of each response (desirability function)--at least 90% of iron recovery rates. Using the experimental conditions defined in the optimization, the method allowed iron determination with achieved detection limit of 2.3 microgl(-1) and precision (assessed as the relative standard deviation) of 9.3-2.8% for iron solutions of 10.0-150 microgl(-1). Real samples (coming from a water treatment unit) were used successfully when evaluating potentialities of the developed SPE procedure coupled to a spectrophotometric determination.     

A comparative evaluation of accelerated solvent extraction and Polytron extraction for quantification of lipids and extractable organochlorine in fish

Optimal conditions for extraction methods using an accelerated solvent extractor (ASE) and a Polytron homogenizer were established for quantification of (crude) lipids and extractable organochlorine (EOCl) in fish. The two methods, an ASE consecutive extraction at 55 and 100 degrees C for ground, freeze-dried filets, and a Polytron extraction at room temperature with four repetitions for ground, wet filets and with two repetitions for wet fish livers were evaluated in terms of reproducibility and comparability. With respect to lipid measurement, the two methods have comparable reproducibility and the experimental errors are relatively small compared to natural variations of fish to fish within a sampling site. For EOCl measurement, the relative standard deviation tends to increase with decreasing levels of EOCl in specimens. An important factor for the relative standard deviation of measurements of analytes present at trace levels in fish matrices is sampling error in taking aliquots. Statistical analysis using a paired comparison design showed that measurement values (crude lipids or EOCl) obtained from these two extraction methods are, in general, not equivalent. There is a good correlation between the two methods for lipid measurement; whereas for EOCl measurements, high degrees of correlation exist within the exposed fish group, but not in the reference group.     

海水中挥发酚的检测与质量控制

为提高挥发酚测定的精密度和准确度，用4-氨基安替比林光度法测定海水中挥发酚含量，该法符合质量要求。