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。     

微波消解-氢化物发生原子荧光光度法测定土壤中的汞

建立了微波消解-氢化物发生原子荧光光度法测定土壤中汞的方法。对微波消解条件、样品粒度等进行了优化,用3 mL硝酸和2 mL盐酸的混合酸作消解溶剂,在设定的微波条件下汞提取完全。用3%的盐酸作为反应载流,0.01%硼氢化钾与0.5%氢氧化钠的混合液为还原剂,直接定容后应用HG-AFS测定,通过测定国家标准参考物质和加标回...     

总氮测定中空白吸光值的控制方法

分析了总氮测定过程中影响空白值的一些因素及控制方法。总氮测定过程中,消解温度和时间、蒸馏水纯度、试剂选用和存放时间、器皿洁净度等等均会影响到试验空白吸光值。笔者提出采用消解温度控制在120～124℃、消解时间在45 min、空白样消解后加入蒸馏水、选用分析纯试剂、试剂存放时间小于7 d等措施可以有效地控制试验空白吸光值。     

冷原子吸收法测定土壤和沉积物中总汞的影响因素研究

冷原子吸收法测汞是一种灵敏度高、干扰较少、准确快速的分析方法,虽然目前对冷原子吸收法测汞的报道不少,但对其影响因素的研究至今未见文献系统报道。本文对各种影响因素进行了研究,确定了测汞的最佳条件。同时,本文对土壤和沉积物试样的预处理也进行了探讨,采用HNO_3—HClO_4—HF体系高压密闭消解法进行消解,并与常规的H_2SO_4-HNO_3-KMnO_4常压消解法进行了比较。结果表明前者重现性好,精密度、准确度均令人满意,样品回收率在95％～101％;而后者重现性相对较差,回收率在90％～110％。虽然采用别的体系高压密闭消解法消解底质样品测定汞已有报道,但由于HNO_3-HClO_4-HF介质高压加热消解法在土壤和沉积物中测定Cr、Cu、Mn、Ni、Pb、Zn等重金属已得到了成功的应用,这样在测定汞及其他重金属元素时,预处     

微波消解-自动电位滴定法测定生活垃圾中的氯含量

建立用微波消解技术处理城市生活垃圾样品,以自动电位滴定法测定城市生活垃圾中的氯含量.讨论微波消解条件、自动电位滴定仪工作参数、酸度及干扰情况,并对城市生活垃圾中的氯含量进行测定,相对标准偏差＜2.5%,回收率为97%～102.5%.     

烘箱法测定地表水中的总氮

以烘箱代替高压锅进行消解,采用过硫酸钾氧化-紫外分光光度法测定地表水中的总氮.经实验研究对比,该法可简化消解过程,使温度易于控制,提高了总氮测定方法的稳定性,且易于操作,灵敏度、准确度、精密度、检出限等均令人满意.     

测定城市生活污泥中重金属的酸消解方法研究

采用HNO3-HC1O4-HF、HNO3-HC1O4、王水-HC1O4、HNO3等不同的酸消解方法对城市生活污泥进行消解。通过对这4种消解方法进行实验比较及对Cu、Ni、Zn三种金属元素浓度的测定,发现HNO3-HC1O4是适合城市生活污泥特点的消解方法。     

水和废水中总氮测定的关键问题研究

结合环境监测工作的实际，应用国标经典分析方法——《碱性过硫酸钾氧化-紫外分光光度法》（GB11894—1989），对水和废水中总氮的测定进行了系统的研究。概述了方法的原理，简介了方法的分析步骤，深入探讨了运用该方法进行水和废水中总氮测定的一些关键操作技术问题，指出在标准分析方法的基础上，选用纯度较高的过硫酸钾，提高氧化消解温度至126—127℃，延长过硫酸钾的氧化消解时间至50min，消解后自然冷却2—3h，能确保水样总氮分析的精密度和准确度。     

总磷过硫酸钾—钼锑抗光度法的过滤影响

采用过硫酸钾－钼锑抗法测定太湖水样中的总磷，以高压釜消解法为佳，过滤问题影响不大，若采用常压消解法，则应注意使消解后的溶液保持１０亳升，消解后的样品先过滤后调ｐＨ为宜。     

一种检测水体总氮的多技术协同氧化消解装置

在分析比较前人方法的基础上，研究开发了一套集臭氧、紫外、超声雾化、高压静放电等多技术协同的氧化消解装置，对含氮水样进行连续消解，将水中含氮物质中的N氧化为NO3-，从而测定水中的总氮。通过实验可以确定最佳消解条件，计算出总氮氧化的转化率，并进行精密度、准确度检验。本法具有无需添加化学氧化剂，总氮氧化率高和消解速度快，精密度、准确度高等特点。     

Total and partial digestion of sediments for the evaluation of trace element environmental pollution

Four different sample treatment methods for the determination of trace elements have been compared: a total digestion with HNO3-H2O2-HF using microwave, and three different standardized methods of fractionation: BCR three-steps sequential extraction, USEPA standard 3050B and ISO standard 11466. The four treatment methods were applied to the determination of Cu and Ni in four samples collected in different areas of Cienfuegos Bay (Cuba). The location of samples and the analytes were selected on the basis of results obtained by previous studies. Analyses following total digestion and BCR three-steps procedure were performed by inductively coupled plasma mass spectroscopy whereas analyses following EPA and ISO procedures were performed by flame atomic absorption spectroscopy. The results obtained have been compared with an estimated anthropic fraction evaluated in each sampling point as the difference between the total concentration and an estimated background concentration level. The BCR three-steps provided the best approximation of the estimated anthropic fraction and was therefore applied also in the determination of Pb and Cd for further consideration.     

Comparative study of hotplate wet digestion methods for the determination of mercury in biosolids

The re-use of biosolids is becoming increasingly popular for land applications. However, biosolids may contain elevated levels of metals and metalloids (including mercury) relative to background environmental concentrations. Consequently, reliable mercury analysis is important to allow classification of biosolids and to determine appropriate options for beneficial uses. This paper reports on a comparative study of 12 hotplate wet digestion methods for their suitability for the determination of mercury in biosolids. The methods were applied to mercury biosolids samples from four localities of two different sewage treatment plants in the State of Victoria, Australia. Samples were also spiked with methylmercury chloride and mercury sulphide to evaluate the Hg recovery in each hotplate digestion method. Aqua regia (HCl:HNO(3)=3:1), reverse aqua regia (HCl:HNO(3)=1:3), nitric, hydrochloric, sulphuric acid and their combinations with or without hydrogen peroxide were studied as wet digestion solutions. The method providing the best mercury recoveries was optimized. Under optimal conditions the corresponding analytical procedure consisted of 1h pre-digestion of 0.4 g biosolids sample with 10 ml reverse aqua regia with temperature increasing to 110 degrees C and 3h digestion at this temperature. In the last 10 min of the digestion step, 2 ml hydrogen peroxide were added to ensure complete decomposition of all mercury containing compounds. After filtering and dilution with deionised water (1:10), the concentration of mercury was determined by cold vapour atomic absorption spectrometry. It is expected, that the wet acid digestion method developed in this study will be also applicable to biosolids from other sewage treatment plants and to other types of solid mercury samples with elevated levels of organic matter.     

Distribution of Pb, V, Cr, Ni, Cd, Cu and Fe in particles formed from the combustion of waste oils

The determination of Pb, V, Cr, Ni, Cd, Cu and Fe in particles of different size obtained from the combustion of waste oils has been carried out. The study consists of the separation of several fractions according to the size of particles, the wet digestion and the individual analysis by graphite furnace atomic absorption spectrometry of the mentioned metals. Taking into account the volatilization temperature of different compounds containing the metals and their distribution on the size fractions, the mineral speciation of metals is proposed.     

Determination of Hg and diet identification in otter (Lontra longicaudis) feces

An analytical procedure for the determination of Hg in otter (Lontra longicaudis) feces was developed, to separate fish scales for the identification of the animal diet. Samples were washed with ultra-pure water and the suspension was sampled and transferred for digestion. The solubilization was performed with nitric-perchloric acid mixture, and detection carried out by the atomic fluorescence spectrometry (AFS). The quality of the analytical procedure was assessed by analyzing in-house standard solutions and certified reference materials. Total Hg concentrations were in the range of 7.6-156 ng g(-1) (July 2004), 25.6-277 ng g(-1) (January 2005) and 14.6-744 ng g(-1) (May 2005) that is approximately the same order of magnitude for all samples collected in two reservoirs at the Tiete River, Brazil. Although Hg concentrations varied with sampling periods and diet, high levels were correlated to the percentage of carnivorous fish scales present in the otter feces.     

青岛市餐厨垃圾与菜市场垃圾混合高温厌氧消化研究

在中试规模下,研究青岛市餐厨垃圾与菜市场垃圾混合(质量比1∶1)高温厌氧消化实验,通过监测厌氧消化过程中产气量、气体组成等产气情况和消化液中pH值、SCOD、NH3-H、VFAs含量和组分等化学指标变化,确定混合厌氧消化的最大有机负荷,并分析混合高温厌氧消化技术的可行性,结果表明,(1)青岛市餐厨垃圾与菜市场垃圾混合高温厌氧消化产甲烷具有技术可行性;(2)混合厌氧消化的最大有机负荷可达4.069 kg VS/(m3.d);(3)当系统最大有机负荷时,每天每千克VS最高可产生甲烷量0.346 m3;(4)混合厌氧消化可削减氨氮对餐厨垃圾单独厌氧消化产沼气的影响。     

Change of PCBs and forms of heavy metals in sewage sludge during thermophilic anaerobic digestion

Determination of seven congeners of PCBs was carried out for sewage sludge before, during and after thermophilic digestion. The overall content of heavy metals (Zn, Cu, Ni, Cd, Pb, Cr) in sludge before and after digestion was determined. Moreover the concentration of heavy metals in particular chemical fractions of the sludge was analyzed. After the thermophilic digestion total concentration of seven PCBs was reduced by 47%, which suggests that thermophilic digestion affects PCB reduction positively. On the 10th d of the process, concentration of lower chlorinated PCBs increased, whereas those of higher chlorinated PCBs decreased. The thermophilic digestion process showed no accumulation of the studied heavy metals in the mobile fractions (exchangeable and carbonate) of the stabilized sewage sludge, except for nickel. The highest increase in zinc, copper, cadmium, and chromium concentration was observed in the organic-sulfide fraction, whereas the highest increase in lead was found in the residual fraction of the sludge. In case of nickel both fractions of organic-sulfide and exchangeable-carbonate fractions were enriched.     

餐厨垃圾厌氧产氢综述

针对餐厨垃圾厌氧产氢过程,从工艺、单组分底物厌氧产氢和过程机理研究阐述了国内外进展,并对未来研究发展方向进行了展望.研究成果表明,餐厨垃圾厌氧发酵产氢过程可行,但影响因素多,系统不稳定,大部分研究停留在实验室小试阶段.尚需针对餐厨垃圾厌氧发酵产氢优势菌种选育、生态因子调控、代谢机理、反应器改进和系统控制模拟等方面开展研究,为该技术的大规模应用提供研究基础.