北京水环境中主要阴离子污染物的监测

针对北京水环境的特点，选定了适宜的色谱条件，用离子色谱法对水环境中常见的阴离子污染物F^-、Cl^-、NO3^-－N和SO4^2-，进行了定量监测，并确定了主要的定量分析掺数。该方法用于实际样品的分析，取得了满意的结果。     

NaAc介质对离子色谱法测定微量阴离子的影响

离子色谱法自1975年问世以来发展很快，已在环境监测、电力、半导体工业、食品、石油化工、医疗卫生和生化等领域得到广泛应用，并有数十项获有关国家批准的标准方法。美国国家环保总局规定水中的无机离子F^-、Cl^-、Br^-、NO2^-、NO3^-、PO4^3-、SO4^2-可用离子色谱法检测。我国生活饮用水标准检测方法也考虑将离子色谱法作为国家标准方法加以应用，由于环境样品常伴随有机弱酸的出现，但未见NaAc介质中微量F^-、NO3^-、SO4^2-、CO3^2-、Cl^-等阴离子测定方法的报道。因此笔者探讨了NaAc介质中Ac^-对测定F^-、Cl^-、CO3^2-、NO3^-、SO4^2-等阴离子的干扰情况及消除干扰的方法。     

葡萄保鲜过程中SO2的离子色谱法测定

研究了离子色谱法（IC）检测葡萄保鲜过程中SO2的方法，并用于SO2释放量及葡萄中SO2残留量的检测。SO2被水吸收或提取后，由H2O2氧化成稳定的SO4^2-。用离子色谱仪测定SO4^2-的含量，与碘量法、盐酸付玫瑰苯胺比色法作对比，结果很好地吻合。结果表明，IC法是一种测定葡萄保鲜过程中SO2及SO2残留量的准确、方便、快速的方法，可用于SO2使用效果的评价。     

新型二氧化硫气体电化学传感器的研究

SO2 是大气的主要污染物 ,并能与环境中的 NOx,O3等协同作用 ,产生更严重的污染 .因此 ,SO2的测定在环境保护、职业健康、工业排放控制等方面起着非常重要的作用 .SO2 的测定方法包括气相色谱法 [1]、离子色谱法 [2 ]、电导测定 [3]和电解电导率 [4]、光纤传感器 [5 ,6 ]等 ,但这些方法所需仪器昂贵、操作繁琐、灵敏度较低、难以实时连续测定 .一些研究者致力于 SO2 电化学传感器的开发 [7～ 8] ,但存在着灵敏度低、需在高温下使用、稳定性差等缺点 .我们成功地研制了一种微型 SO2 气体电化学传感器 ,该传感器稳定性好、灵敏度高、价…     

丙烯中微量硫的测定

本文采用燃烧方法将不同形式的可燃性硫转化为SO2，在硝酸介质中用H2O2将SO2氧化为SO4^2-，并用离子色谱法测定。结果表明，该法样品处理简单，干扰离子少，灵敏度高，能较准确测定出丙烯中的微量硫。     

燃烧氧化偶联离子色谱法检测甲醇、碳黑中氯和硫

提出采用燃烧氧化偶联离子色谱法测定甲醇、碳黑中的氯和硫的含量。方法通过在管式炉中燃烧将甲醇、碳黑中的氯及硫转化为Cl2、HCl,SO2,SO3等气态物质。选用I-/I3-溶液作为燃烧产物的吸收剂。I-/I3-溶液既作氧化剂又作还原剂,将Cl2、HCl转化为Cl-,将SO2、SO3转化为SO42-。用离子色谱法测量吸收剂中Cl-和SO42-的含量进而推算甲醇、碳黑中氯和硫的含量。实验结果表明,该方法简单、准确、灵敏。氯和硫的检出限分别为9.71μg/g和1.64μg/g。     

离子色谱法测定铬酸酐中的微量F-、SO2-4、Cl-

建立了离子色谱法测定铬酸酐中微量F^-,SO4^2-和Cl^-的方法，以水合联氨作还原剂，将铬酸酐溶液中的CrO4^2-还原为Cr^3 ，以沉淀的方式除去，采用离子色谱法测定溶液中的微量F^-,SO4^2-和Cl^-，其测量不确定度分别为6％，6％和5％，方法简便，测量结果准确，可靠。     

离子色谱仪流动注射电导法测定过氧化氢

以H2S03与H2O2反应生成H2SO4产生的电导变化与H202的量呈线性关系为理论依据，根据流动注射原理将现有离子色谱仪进行改装成流动注射仪测定过氧化氢。此方法有很好的重现性，8次进样所得相对标准偏差小于2．6％，所得结果稳定，其检测下限为0．5mg/L，标准曲线的相关系数达0．9995。本实验对某些分析条件，诸如H2SO3的浓度和流速、样品用量及反应管长度等因素进行了探讨。由于实际样品中存在不同离子而具有不同背景电导，因而在测定实际样品时采用经过过氧化氢酶处理的样品作空白，以此消除背景电导的干扰。     

离子色谱法测定油田灌注污水中的CI^—、NO3^—、SO4^2—

采用二氯甲烷萃取、活性炭吸附、Na2CO3/NaHCO3淋洗液储备液沉淀等预处理方法,有效地除去了油田灌注污水样中的有机物质和可能存在的高含量的钙镁离子,进而用离子色谱法同时测定了CI^-、NO3^-、SO4^2-三种离子,相对标准偏差分别为0．06、4．6、2．2,NO3^-、SO4^2-离子的加标回收率分别为97．9％和97．1％。     

氧化银沉淀-离子色谱法测定海水中的痕量亚硝酸根和硝酸根

海水中痕量亚硝酸根、硝酸根的含量是评价海水的富营养化的重要指标,采用离子色谱法可对它们进行同时测定。但海水中大量的Cl^-和SO4^2-会干扰海水中微量NO2^-和NO3^-的测定。目前,在用离子色谱法分析阴离子时排除Cl^-干扰的有效方法是银柱法,但银柱价格较贵,成本较高,使得银柱法的使用在国内受到限制。本实验以固体Ag2O和Ba（OH）,为沉淀剂,采用氧化银沉淀法排除Cl^-和SO4^2-的干扰。用此方法对海水处理后,再用离子色谱法检测NO2^-和NO3^-,不仅结果令人满意,检测费用也大大低于银柱法。     

离子色谱法测定气体中痕量二氧化硫

建立了测定气体中痕量二氧化硫的离子色谱法。采用氢氧化钠–过氧化氢溶液为吸收液,将气体样品中痕量二氧化硫转化为硫酸根离子,以离子色谱法测定硫酸根离子,从而得到气体中二氧化硫含量。二氧化硫气体含量在1~100μL/L范围内与色谱峰面积线性关系良好,相关系数为0.999 9。二氧化硫的检出限为0.1μg/L,测量结果的重复性小于2%(n=6),测定标准样品的回收率在98.1%~99.6%之间,准确度优于对照方法。     

SO2在多组分悬浮液中的吸收反应特性

The emission of sulfur dioxide in flue gases is an important problem in industry involving combustion of coal. The wet scrubbing process using lime/limestone slurry as the scrubbing medium is currently the dominant technology for the flue gas desulfurization. Due to the presence of numerous ionic and neutral species in the slurry, the chemical reactions involved in the slurry upon absorption of sulfur dioxide are complex. In this paper, a method of measuring the sulfur dioxide absorption in multi-component suspensions was developed and the characteristics of sulfur dioxide absorption were investigated. The results show that different additives chosed in the experiment can improve the ability of SO2 absorption. As to the same additive, the improvement effect is differ with different concentration. For the magnesium hydroxide additive, its optimum concentration is 1×10-4 mol/L. Experiment results suggested that dissolved sulfur dioxide reacts mainly with the magnesium sulfite ion pair which is responsible for the increased absorption rate of SO2. However, when CO2-3 or SO24- anions are present in the solution, the catalytic effect of magnesium hydroxide precipitate on sulfur dioxide absorption reduces. According to the experiments, absorbents with better performance can be optimized to be applied in semi-dry or wet FGD process to raise SO2 removal efficiency.     

Evaluation of Gas Phase and Particulate Components Relevant to Polar Tropospheric Processes

Abstract

The measurement of atmospheric trace components relevant to atmospheric chemistry, in gas phase and particulate matter, was carried out in the Antarctica troposphere during the Antarctic summer 1990–91. The determinations were carried out by sampling air through a diffusion denuder/filter pack sampling system, followed by extraction and analysis by ion chromatography. Through the analysis of the mass distribution of anions, an accurate and sensitive method for the measurement of several important species was provided. Results show that sulfur dioxide, nitric acid, sulfates, nitrates and other significant compounds might be well characterized, even at concentration levels as low as a few parts per trillions, thus providing a highly significant and consistent data set for the study of polar atmospheric chemistry.     

The sampling of sulfur dioxide in air with impregnated filter paper

A method is suggested for the sampling of sulfur dioxide in air with impregnated filter paper instead of bubblers. The best aqueous impregnating solution contained potassium hydroxide with glycerol or triethanolamine. The possibilities and limitations of the method are discussed. High collection efficiencies (over 95%) were obtained at relative humidities above 25%. Collected sulfur dioxide was stable for at least several weeks when the filters were kept dry after the sampling. The method is especially suited for short-time measurements and for automatic sampling with smoke samplers.     

三维多孔氮化钛用于高效限硫载体

通过简便、高效、可规模化的一步高温氮化法,利用高温烧结使二氧化钛(TiO₂)粉末在转化成氮化钛(TiN)的同时形成连续的三维多孔网络,具有良好的导电性和高孔隙率。作为高效限硫载体,连续的三维多孔TiN网络不仅能有效增加电子传输路径、增强电子转移、促进离子迁移,而且能够从物理限域和化学吸附两方面对多硫化锂的穿梭效应进行强有力的限制,同时有效提高了硫的负载量。制备的高导电性、高硫负载硫正极展现出较高的放电容量和优异的循环稳定性能。     

三维多孔氮化钛用于高效限硫载体

通过简便、高效、可规模化的一步高温氮化法,利用高温烧结使二氧化钛(TiO₂)粉末在转化成氮化钛(TiN)的同时形成连续的三维多孔网络,具有良好的导电性和高孔隙率。作为高效限硫载体,连续的三维多孔TiN网络不仅能有效增加电子传输路径、增强电子转移、促进离子迁移,而且能够从物理限域和化学吸附两方面对多硫化锂的穿梭效应进行强有力的限制,同时有效提高了硫的负载量。制备的高导电性、高硫负载硫正极展现出较高的放电容量和优异的循环稳定性能。     

Total Sulfur Dioxide Determination in Red Wine by Suppressed Ion Chromatography with In-Sample Oxidation and SPE

Suppressed ion chromatography (IC) based on in-sample oxidation and SPE is described for total sulfur dioxide determination in red wines. In this method, sulfur dioxide was converted to stable sulfate ion through a simple H₂O₂ oxidation step and then the impurities were removed with C-18 micro-column SPE pretreatment. Finally, the sulfate was determined by suppressed ion chromatography coupled with conductivity detection and the content of total sulfur dioxide could be obtained through sulfate content by blank deduction method. By using a mixture of NaHCO₃ and Na₂CO₃ as mobile phase, the analysis of one sample with nine anions could be completed within 25 min. For sulfate detection, a linear calibration curve with correlation coefficient of 0.9993 was obtained from the peak area with low detection limit (0.45 mg L^?1, 3σ) and excellent repeatability (RSD?=?1.12%, n?=?6). This method was applied to sulfur dioxide determination in real wine samples and compared with conventional iodometry.     

Laboratory and field measurements of a badge type passive sampler for the determination of ambient sulfur dioxide concentrations

The performance of a badge type passive sampler for the determination of sulfur dioxide is described. The trapping agent is triethanolamine. Analysis is performed by ion chromatography. Thus, the method allows the simultaneous detection of sulfur dioxide and nitrogen dioxide. The sampler was tested in the laboratory and in the field. The intercomparison with independent methods in the field showed very good agreement against two active sampling methods. Regression analyses (the results of the passive sampler always represent the y-axes) gave r² = 0.81 and k = 1.07 ± 0.01 for the intercomparison with an annular denuder technique and r² = 0.92 and k = 0.96 ± 0.01 for the intercomparison with a commercial fluorescence sulfur dioxide analyzer. The average reproducibility in the field was 7% (RSD). The detection limit was 0.18 μg SO₂/m³ for an exposure time of two weeks. Received: 9 February 1998 / Revised: 22 June 1998 / Accepted: 26 June 1998     

Laboratory and field measurements of a badge type passive sampler for the determination of ambient sulfur dioxide concentrations

The performance of a badge type passive sampler for the determination of sulfur dioxide is described. The trapping agent is triethanolamine. Analysis is performed by ion chromatography. Thus, the method allows the simultaneous detection of sulfur dioxide and nitrogen dioxide. The sampler was tested in the laboratory and in the field. The intercomparison with independent methods in the field showed very good agreement against two active sampling methods. Regression analyses (the results of the passive sampler always represent the y-axes) gave r² = 0.81 and k = 1.07 ± 0.01 for the intercomparison with an annular denuder technique and r² = 0.92 and k = 0.96 ± 0.01 for the intercomparison with a commercial fluorescence sulfur dioxide analyzer. The average reproducibility in the field was 7% (RSD). The detection limit was 0.18 μg SO₂/m³ for an exposure time of two weeks. Received: 9 February 1998 / Revised: 22 June 1998 / Accepted: 26 June 1998     

烟气中二氧化硫及三氧化硫测定方法的研究

本文采用过氧化氢-氯化钡-钍试剂法以及80%异丙醇-氯化钡-钍试剂法分别测定了烟气中的二氧化硫及三氧化硫质量浓度,并对该方法的灵敏度、准确度以及各种影响因素进行了研究分析.本方法简单、快速、准确、便于现场监测控制.