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。     

原子吸收法测定降水中的钾、钠、钙、镁的改进

对标准分析方法中的K、Na、Ca、Mg分开测定改进为混合测定。改进法与标准法的校准曲线、精密度与准确度均较为一致。改进法简化了操作程序，提高了工作效率。     

钼锑抗分光光度法测定总磷问题的讨论

钼锑抗分光光度法测定总磷，方法相对成熟，但是实验过程中干扰因素多，因此需通过大量的对比实验，来探讨测定水中总磷的最佳条件。     

分光光度法测定降水中微量过氧化氢

研究了一种测定降水中微量过氧化氢的方法。在0.4～1.5mol／L磷酸介质中，过氧化氢与钒（V）及2－（3，5-二溴-2-吡啶偶氮）－5-二乙氨基苯酚（3,5-diBr-PADAP）反应形成一种组成比为1：1：1的蓝色三元配合物，其最大吸收波长为598nm，表现摩尔吸光系数为5.6×104L·mol-1·cm-1。过氧化氮量在2×10-7～1．3×10－5mol／L时服从比耳定律。方法简便，选择性较高，用于降水中微量过氧化氢的直接测定，结果令人满意。     

石油类测定方法的改进

使用F2000型红外光度测油仪，以四氯化碳作为参比溶液，测定水体中石油类，由于以未经过与水样相同的步骤萃取的四氯化碳作为参比溶液，以及F2000型红外光度测油仪是直接显示水样中石油类的浓度，因此，所得的水样浓度并未扣除水样萃取过程中可能存在的干扰。笔者认为，采用经活性炭吸附处理过的超纯水，通过与水样相同的操作步骤所得的萃取液，来作为测定水样时的参比溶液，测定的结果会更加贴近实际，能够更好的反映水体受石油类污染的情况。     

紫外分光光度法测定对硝基苯酚的适宜条件的探讨

对对硝基苯酚的浓度,溶液的ｐＨ,温度以及波长对测定结果的影响进行了初步实验,找出用紫外分光光度法测定对硝基苯酚的适宜条件。     

多元线性回归分光光度法同时测定污水中的苯酚,苯胺

苯酚、苯胺与４－ＡＡＰ络合后所形成的吸收光谱出现严重重桑。采用多元线性，建立了计算分光光度法可测定污水苯酚、苯胺含量。其加标回收率分别在９５－１０５％，９８－１０３．３％之间，方法较好地解决了采用分光光度法测定污水中苯酚、苯胺时的相互干扰。     

邻菲啰啉分光光度法测定水中总铁的改进

对邻菲啰啉分光光度法测定水中总铁的方法进行了改进：采用50mL比色管水浴还原水样——分光光度计比色测定水中总铁。测试结果表明，改进法精密度和准确度均优于标准方法，是测定水中总铁较为理想的方法。     

流动注射分光光度法快速测定废水中的钼

钼（VI）与显色试剂在酸性介质中反应，形成稳定的橙红色络合物，在460nm下测定钼的含量，显色试剂由一定浓度的硫氰酸钾、硫脲、硫酸铜组成。将流动注射分析技术应用于该反应体系，可快速、重现、准确地测定废水样品的钼。方法检出限为0．05mg／L，线性范围为1～20mg／L，相对标准偏差（n=11）〈3％，分析速度可达60次／h。     

分光光度法测定废水中CNS^—离子

应用分光光度法测定废水中CNS~-离子,文献已经指出Cr~(6+)、还原剂、有机物对测定结果有明显影响。经过我们的观察与实验发现还有其它因素,如使用液浓度、反应时间、Cl~-离子干扰。这些对CNS~-离子测定也起着重要影响。     

The Fate of Endosulfan in Water

Although the use of endosulfan to control cotton pests has declined, this insecticide still has widespread application in agriculture and can contaminate riverine systems as runoff from soil or by aerial deposition. The degradation of endosulfan in pure water at different pH values of 5, 7 and 9 and in river water from the Namoi and the Hawkesbury rivers of New South Wales (NSW), Australia, was studied in the laboratory. Endosulfan transformation into endosulfan sulfate in river water using artificial mesocosms was also investigated. The results show endosulfan is stable at pH 5, with increasing rates of disappearance at pH 7 and pH 9 by chemical hydrolysis. Incubation of endosulfan with river water at pH 8.3 resulted in the disappearance of endosulfan and the formation of endosulfan diol due to the alkaline pH as well as formation of endosulfan sulfate. Although the degradation of endosulfan by Anabaena, a blue-green alga, did not result in the transformation of endosulfan to endosulfan sulfate, we conclude that other microorganisms catalyzed the formation of the sulfate. Significant conversions of endosulfan into endosulfan sulfate were also reported from associated field studies using artificial mesocoms containing irrigation water from rivers inhabitated by micro-macro fauna. From these results, we conclude that the presence of endosulfan sulfate in river water cannot be used to distinguish contamination by runoff from soil from contamination by aerial drift or redeposition.     

连云港市天然山泉水和井水调查

于2018年六五环境日期间开展便民服务,监测山泉水或井水。监测项目主要有:酸碱度、溶解性总固体、总硬度、氟化物、氯化物、硫酸盐、硝酸盐、亚硝酸盐、重金属等。参照《生活饮用水标准检验法》(GB/T5750-2006)和《生活饮用水卫生标准》(GB5749-2006)对居民送样水监测分析后评价,80%的水样存在某一项或几项指标超标,其中一半水样硝酸盐超标,需予以重视,建议提高安全用水意识,不要作为饮用水使用。     

Remediation of DDT-Contaminated Water and Soil by Using Pretreated Iron Byproducts from the Automotive Industry

The objective of this study was to quantify the effectiveness of different pretreated iron byproducts from the automotive industry to degrade DDT [(1,1,1-trichloro-2,2-bis(4-chlorophenyl) ethane] in aqueous solutions and soil slurry. Iron byproducts from automotive manufacturing were pretreated by three different methods (heating, solvent and 0.5N HCl acid washing) prior to experimentation. All pretreated irons were used at 5% (wt v^{? 1}) to treat 0.014 mM (5 mgL^{? 1}) of DDT in aqueous solution. Among the pretreated irons, acid pretreated iron results in the fastest destruction rates, with a pseudo first-order degradation rate of 0.364 d^{? 1}. By lowering the pH of the DDT aqueous solution from 9 to 3, destruction kinetic rates increase more than 20%. In addition, when DDT-contaminated soil slurry (3.54 mg kg^{? 1}) was incubated with 5% (wt v^{? 1}) acid-pretreated iron, more than 90% destruction of DDT was observed within 8 weeks. Moreover, DDT destruction kinetics were enhanced when Fe(II), Fe(III) or Al(III) sulfate salts were added to the soil slurry, with the following order of destruction kinetics: Al(III) sulfate > Fe(III) sulfate > Fe(II) sulfate. These results provide proof-of concept that inexpensive iron byproducts of the automotive industry can be used to remediate DDT-contaminated water and soil.     

K-Ca-Mg-Cl-H_2O体系中硫酸钙结晶介稳区的研究

对K-Ca-Mg-Cl-H2O体系中硫酸钙结晶介稳区进行了研究。以一定浓度氯化钙溶液与硫酸镁溶液反应结晶的方式,采用激光散射法测定了不同浓度复合盐溶液和温度下硫酸钙过饱和度与结晶之间的关系,并测定了与之平衡的溶解度,从而确定该体系中硫酸钙结晶介稳区宽度,探讨了影响结晶介稳区的因素,以及硫酸钙结晶和结晶相与复合盐溶液浓度、温度、结晶介稳区之间的关系。     

A Rapid Titrimetric Method for Sulfate in Lead Dioxide Exposed to Atmospheric Sulfur Pollution

A titrimetric method is described for the analysis of sulfate in lead dioxide candles which have been exposed to atmospheric sulfur pollution. The time taken to analyse one sample is 3 hr. Sixty milliliters of 8% ammonium carbonate solution is used to convert the lead sulfate present on the candle to ammonium sulfate. The solution is filtered lc remove lead dioxide, and an aliquot of the filtrate is heated to remove ammonium carbonate. The solution of ammonium sulfate remaining is titrated directly for sulfate with 0.02 M barium perchlorate, using Thoron as indicator. The accuracy of the method is ±10 and ±6 % of theoretical, for 10 mg, and 40 mg or greater amounts of sulfate, respectively. For 2 mg of sulfate, results are about 20% high. Good agreement has been obtained between results for duplicate field candles, analyzed by the standard sodium carbonate gravimetric method, and the method presented, over a five-month period.     

Parameterization of wet deposition of sulfate by precipitation rate

A method for the estimation of wet deposition of sulfate is developed using routinely available meteorological data and the observed airborne sulfate concentration. This approach takes into account different mechanisms of precipitation formation that determine sulfate concentration in precipitation water. Four different precipitating cloud types, including cold cloud, warm cloud, stratified layered cloud and convective cloud, according to their precipitation formations are incorporated differently to estimate sulfate concentration in precipitation water. This method is implemented to estimate wet deposition of sulfate in Seoul for the days when the airborne sulfate concentration is available. The estimated wet deposition of sulfate shows that the model slightly overestimates the wet deposition of sulfate especially for the warm cloud case while it does underestimate sulfate deposition for the Bergeron process in developing precipitation particularly when the input airborne sulfate concentration is small. The precipitation amount weighted mean wet deposition of sulfate obtained from the model, overestimates that observed by a factor of 1.6 for this case study. This discrepancy might be associated with non-steady revolutional features of precipitating clouds and the resolvable scaling difference between the model and observation.     

IV. Recovery of Flue Gas Sulfur as Ammonium Phosphate

The present development in industry has greatly increased the consumption of fossil fuel all over the world. The sulfur present in these fuels on combustion impairs the atmosphere and has to be removed before or after combustion. Direct desulfurization is still in its initial stage of commercial application and is thought to be rather expensive. Most projects today are concerned with flue gas desulfurization and a few people have been successful in the pilot plant scale. Flue gas sulfur is usually recovered as sulfuric acid or ammonium sulfate. The Kiyoura-T.I.T. process employs a completely dry method to recover this sulfur as ammonium sulfate. However, the present trends in fertilizers show that there is a marked drop in the consumption of this type of fertilizer except for China and other Asian countries.

Experiments were carried out to produce a high grade phosphatic fertilizer with a larger field of application. The authors were successful in rendering the phosphate in phosphate rock water soluble by reacting it with the sulfate radical of the ammonium sulfate. Ammonium acid sulfate was used in the experiments and the phosphate radical was determined by a colorimeter utilizing the ammonium molybdate method.

The results showed a conversion and an extractability of 98%, when the molecular ratio of ammonium acid sulfate to the CaO in phosphate rock was in the vicinity of 1:1.4-1.5. The reaction time was 120-180 minutes.

The extracted liquid was crystallized and put through X ray diffractometer experiments which showed that most of the crystals were ammonium phosphate containing about 15% N and 39% P₂O₅ on a dry basis. Thus, it is evident that this could be effectively applied in a commercial scale plant, recovering the flue gas sulfur as ammonium phosphate. The Kiyoura-T.I.T. process can be utilized to recover the flue gas sulfur either as the sulfate or as the phosphate.     

Determination of sulfur oxides formed during the S(IV) oxidation in the presence of iron

The reaction products (i.e., sulfate (SO4(2-)) and dithionate (S2O6(2-))) of S(IV) oxidation in the presence of iron(III) under different experimental conditions were investigated. Ion-interaction chromatography was used for the separation of sulfate and dithionate using tetrabutylammonium hydroxide (TBAOH) as an ion-pair reagent. The chromatographic method was optimized by varying the composition of the mobile phase (i.e., concentration of TBAOH, acetonitrile and Na2CO3) and by varying the flow rate of the mobile phase. The method was successfully applied to the determination of dithionate formed during the S(IV) oxidation in the presence of Fe(III). In air-saturated solutions sulfate was observed as the only product, while in N2-saturated solutions dithionate was also determined, but it is the minor reaction product and represents about 4% of the total amount of oxidized HSO3- under the studied conditions.     

Adsorptive micellar flocculation as an efficient method for processing soil extracts containing both surfactant and polychlorinated biphenyls: practical demonstration.

The main purpose of the paper is to share the results and experience from processing soil extracts containing a high concentration of both anionic surfactant and polychlorinated biphenyls (PCBs) by use of method the called adsorptive micellar flocculation. The method is similar to coagulation, but the mechanism is more complicated. The flocculants examined in the laboratory section involved ferric chloride, aluminium chloride, ferric sulfate, and aluminum sulfate. It was observed that ferric chloride provides the best PCB removal efficiency from the extract. Subsequently, two extracts obtained from the pilot-scale demonstration of the PCBs leaching from the soils by the surfactant solution were processed by this method. The volume of the extracts processed was several hundred liters. The method proved it can remove PCBs from all extracts with a very high efficiency (greater than 99.99%). The residual PCB concentrations in solution were less than 1 microg/L.     

发光细菌法在水质综合毒性在线检测中的应用

以海洋发光细菌费氏弧菌（Vibriofischeri）作为检测生物，采用冻干菌粉快速复苏技术，研究费氏弧菌在水质检测中的最佳测试温度和有效性测试条件，并对硫酸锌等多种毒物和几种实际水样进行发光抑制作用分析。研究表明，费氏弧菌冻干粉复苏菌液保存在2～5℃条件下能有效测试7d，最佳测试温度为15℃，最佳测试时间为15min。氯化汞、硫酸锌、硫酸镉等重金属和苯胺、多菌灵、甲醛等有机毒物对费氏弧菌均具有较强的光抑制作用，也即费氏弧菌对以上毒物较为敏感，并能够连续7d保持对同一浓度硫酸锌的敏感性较为一致。对几种实际水样的测试和分析表明，以费氏弧菌为指示生物的发光细菌法能够应用于水质环境安全的综合毒性在线监测预警中。