On-line monitoring of wastewater using ion chromatography

Ion Chromatography (IC) has been used for the on-line determination of anions and cations in a variety of process streams. On-line monitoring of process and wastewater streams optimizes the control of treatment methods by providing early indications of problems that could increase discharges of hazardous compounds to the environment. It is important for the immediate detection and remediation of process upsets in critical streams. The waste flow to the Radioactive Liquid Waste Treatment Facility at the Los Alamos National Laboratory (LANL) is processed before discharge and requires monitoring. Process chromatography is used to monitor the trends of contaminants in real time. The purpose of this study is to develop an automated on-line IC procedure for the simultaneous determination of anions in LANL wastewater.     

阀切换离子色谱法测定电厂烟气异丙醇吸收液中三氧化硫的含量

建立了一种阀切换离子色谱法检测烟气中SO_3的方法,通过检测异丙醇(80%)前处理过的样品中SO_4~(2-)含量来实现对SO_3含量的检测。采用异丙醇(80%)吸收液将样品中的SO_3转化为SO_4~(2-),利用阀切换的在线预处理方法除去高浓度异丙醇对SO_4~(2-)测定所造成的影响。结果表明,在0.5～10.0mg/L线性范围内,其相关系数R~2=0.999 3,相对标准偏差为2.7%(n=6),检出限为0.7×10~(-2) mg/L,所得样品的加标回收率为95.0%～105%。方法可用于燃煤电厂烟气中SO_3含量的检测。     

The economic viability of a thermal power plant: a case study

Journal of Thermal Analysis and Calorimetry - The present paper deals with the economic viability of a coal-fired power plant (CFPP) situated in the northern part of India. The plant with a...     

Mineral speciation of copper and zinc in flying ash from a thermal power plant

Summary We studied the mineral speciation of Cu, Zn and Hg in fly ash from a large thermal plant burning lignite. By applying various treatments carried out under different conditions and taking into account the solubility and physical properties (boiling and melting point, etc.) and the behaviour towards combustion of the different possible compounds, we concluded that the ash assayed contained 109.6, 114.4 and 14.30 g/g of zinc silicate, zinc oxide and/or zinc sulphide and metal zinc, respectively, as well as 24.5 g/g of copper silicate and 31.2 g/g of a mixture of copper oxide, sulphide and metal. The formation of these compounds in the combustion of lignite is discussed.     

Developments in the application of counter-current chromatography to plant analysis

Counter-current chromatography is a very versatile separation technique which does not require a solid stationary phase. It relies simply on the partition of a sample between the two phases of an immiscible solvent system. Some of the more recent applications of the method to the separation of plant-derived natural products are described here. Crude plant extracts and semi-pure fractions can be chromatographed, with sample loads ranging from milligrams to grams. Aqueous and non-aqueous solvent systems are used and the separation of compounds with a wide range of polarities is possible. The technique is complementary to other chromatographic methods and is compatible with gradient systems. The possibilities for solvent selection are almost limitless but some guidelines for the choice of successful systems are presented.     

Adsorption characteristics of carbon on ion exchange resin in nuclear power plant

The adsorption characteristics of carbon on a strong base anion and cation exchange mixed resin, Amberlite IRN-150 in OH⁺ and H⁻ (1∶1) used in nuclear power plant, were investigated at 6, 30 and 50 °C at a concentration of carbon up to 0.02M. The expression for the adsorption of carbon was well fitted to the Freundlich equation and the constants,k andn in the equation were deduced. Furthermore, we could explain that the adsorption capacity on the mixed resin increases with temperature.     

The application of thermal and mass chromatography to thermal oxidative degradation of polymers

A modification of a relatively new technique (thermal and mass chromatography) is used to study the volatile products evolved in the thermal oxidative degradation of isotactic poly(1-pentene) at 115° C under 100% oxygen. This new technique allows certain data to be obtained much more easily and more reliably than before.     

Flow-through calcium-selective electrode: application in flow-injection analysis and ion chromatography

The use of solid contact flow-through calcium-selective electrodes as potentiometric detectors in flow-injection analysis and non-suppressed ion chromatography is discussed. Owing to the high selectivity of the membrane electrode based on tetratolyl-m-xylylenediphosphine dioxide, it can be used to monitor trace amounts of calcium ions in the presence of a 100-fold excess of alkali metal, ammonium and magnesium ions. The detection limit is about 1 × 10^?6 M. The composition and thickncss of the calcium selective membrane influence both the detection limit and selectivity of the electrode. The sensitivity of this potentiometric detector in ion chromatography relative to alkaline earth and heavy metals is significantly higher than that of a commercial conductivity detector.     

On-line pH modification of carbonate eluents using an electrolytic potassium hydroxide generator for ion chromatography

Classical gradient elution, based on the application of a gradient pump used for mixing two or more prepared eluent components in pre-determined concentrations, was replaced by a chromatography system equipped with an isocratic pump and an electrolytic KOH generator. The isocratic pump delivered a constant concentration eluent composed of pure hydrogencarbonate solution. Carbonate ions, the main component of carbonate/hydrogencarbonate-based eluents, were formed by titration of hydrogencarbonate with KOH formed on-line in the electrolytic KOH generator. By changing the concentration of electrolytically-generated KOH, the eluent composition could be changed from pure hydrogencarbonate to a carbonate/hydrogencarbonate buffer, and finally to a carbonate/hydroxide-based eluent. The described system was tested to achieve pH-based changes of retention behavior of phosphate under constant inflow eluent composition conditions.     

Polymer-coated cation exchangers in high-performance ion chromatography: preparation and application

Low-capacity cation-exchange stationary phases for ion chromatography were prepared by coating a vinyl-modified silica gel with polystyrene or poly(glycidyl methacrylate). Strong acid ion-exchange groups were formed by sulphonation with concentrated sulphuric acid or by ring opening of the polymer-coated silica gels with sulphite solution. Carbon-sulphur elemental analyses of the polymer-coated cation exchangers (PCCEs) were applied to determine the average polymer film thickness. The pH stability depended on the polymer film thickness. The PCCEs were stable in the pH range 0.5–9. The low-capacity PCCEs (capacities 18–91 μmol/g) were applied to determine alkali and alkaline earth metal ions in tap and mineral waters.     

双功能聚合物基质阳离子交换固定相的制备及其在离子色谱中的应用

离子色谱是分离分析阳离子型化合物的重要手段之一。高效阳离子交换固定相的制备研究对离子色谱技术的发展具有重要的意义。该文以丙烯酸和顺丁烯二酸酐为单体,2-巯基乙基磺酸钠为巯基改性剂,提出了聚合物基质微球巯基改性自由基聚合修饰方法,用以制备新型双功能的阳离子交换固定相。该固定相以羧基和磺酸基为功能基,仅用简单的强酸淋洗液便可以实现常规阳离子的基线分离。利用色谱学模型,对金属离子和有机胺的保留行为进行了研究。采用梯度淋洗模式,可在24 min内实现10种阳离子的分离,表明固定相具有优异的色谱性能。"巯基-烯"修饰方法简单、高效。此外,通过调节巯基改性剂的比例能够实现对固定相交换能力的调控。     

Suppressed ion chromatography for monitoring chemical impurities in steam for geothermal power plants

A suppressed ion chromatography (IC) technique has been evaluated as a chemical monitoring tool for detecting major anions (F-, Cl-, NO3- and SO4(2-)) of condensed steam in geothermal power plants. It is shown that the suppressed IC technique provides a suitable means for preventing possible damage to generating equipment in the geothermal industry. An electrical conductivity detector (0.1 microS sensitivity) with an anion-exchange column (IonPac AS4A-SC), a micro-membrane suppressor (AMMS II), and an isocratic high-pressure pump system were successfully used for detecting low concentrations of inorganic anions. Method detection limits for the anions of interest were <0.184 mg/L. Details of the IC methodology as well as some experimental results obtained during its application for the chemical monitoring of geothermal steam pipes are also described.     

Separation of inorganic anions on a triazole-functionalized ion exchanger in ion chromatography

The retention behavior of inorganic anions on a triazole-based stationary phase was first examined in ion chromatography. It was initially designed for hydrophilic interaction liquid chromatography and was simply prepared by introducing the triazole groups onto the surface of silica gel via click chemistry. Effective separation of common inorganic anions, including iodate, chloride, bromide, nitrate and iodide, was achieved with Na(2)SO(4) eluent. The logarithm of the retention factor of analytes was observed to be linear with the logarithm of the eluent concentration, and the slopes of the plots were almost the same as those of the ideal theoretical value. The eluent pH value in the range of 3.4-7.0 had little effect on the separation. The utility of the column was demonstrated for the determination of UV-absorbing anions in saliva and tap water.     

Determination of mepiquatchloride in animal and plant matrices by ion chromatography with conductivity detection

Summary A new residue method, based on ion chromatography, for the determination of trace amounts of the ionic plant growth regulator mepiquatchloride is described. The method is adapted to plant and animal matrices and does not require any derivatization steps. This new technique provides higher recoveries of the analyte, better reproducibility and increased speed than the previous method. The limit of determination is 0.05 mg/kg.     

On-line coupling of ion chromatography and atomic spectrometry for ultra trace analysis in high purity molybdenum- and tungsten-silicide

The well-established technique of on-line coupling ion chromatography and atomic spectrometry for ultra trace analysis in high purity molybdenum and tungsten is extended to include the silicides MoSi(x) and WSi(x). An additionally included matrix elimination step allows an almost interference-free trace analysis in the silicide matrices. Reproducibility and accuracy of the on-line method were checked by comparison with several other methods, such as isotope dilution, radiochemical neutron activation analysis, direct determination by atomic absorption analysis and not at least with glow discharge mass spectrometry. The results show the high potential of the on-line method for reaching detection limits in the pg g(-1) range, but they show also remaining problems with contamination and system calibration.     

On-line separation of Pu(III) and Am(III) using extraction and ion chromatography

An on-line method developed for separating plutonium and americium was developed. The method is based on the use of HPLC pump with three analytical chromatographic columns. Plutonium is reduced throughout the procedure to trivalent oxidation state, and is recovered in the various separation steps together with americium. Light lanthanides and trivalent actinides are separated with TEVA resin in thiocyanate/formic acid media. Trivalent plutonium and americium are pre-concentrated in a TCC-II cation-exchange column, after which the separation is performed in CS5A ion chromatography column by using two different eluents. Pu(III) is eluted with a dipicolinic acid eluent, and Am(III) with oxalic acid eluent. Radiochemical and chemical purity of the eluted plutonium and americium fractions were ensured with alpha-spectrometry.     

固相萃取-离子交换色谱法测定植物提取物中三聚氰胺

建立了固相萃取-离子交换色谱法测定5种植物提取物中三聚氰胺。植物提取物样品经1%三氯乙酸水溶液提取,OASISMCX固相萃取柱净化。分析时用LC-SCX离子交换色谱柱（25 cm&#215;4.6 mmi.d.,5μm）分离,V（0.05 mol/LKH2PO4）∶V（乙腈）=75∶25溶液为流动相,流速1.0 mL/min,在紫外波长240 nm下检测。三聚氰胺在0.5-100.0 mg/L的范围内,质量浓度与色谱峰面积呈良好的线性关系（r=0.9999）,检出限为1.0 mg/kg,加标回收率在82.8%-103.2%范围内,相对标准偏差小于5.5%。     

Experimental study on optimized composition of mixed carbonate for phase change thermal storage in solar thermal power plant

36 kinds of mixed carbonate molten salts were prepared by mixing potassium carbonate, lithium carbonate, sodium carbonate in accordance with different proportions. The data of melting point and latent heat are measured by the analysis of DSC curves of 36 kinds of salts, which show that the majority of ternary carbonate’s melting points are close at around 400 °C. 24 kinds of eutectic molten salts were selected among 36 kinds of molten salts. With high latent heat, ternary carbonate salt has the potential to be employed for phase change thermal storage. The costs for phase change thermal storage of 24 kinds of carbonate salts are calculated. Finally, 13 kinds of ternary carbonate salts with lower cost for phase change thermal storage are recommended, where there are 6 kinds of mixed carbonates have the considerably larger latent heat of melting.     

On-line solid-phase extraction-thermal desorption-gas chromatography with ion trap detection tandem mass spectrometry for the analysis of microcontaminants in water

An improved set-up for solid-phase extraction with thermal desorption coupled on-line to gas chromatography (SPETD-GC) is presented. It includes a newly designed liner for a programmable temperature vaporizer (PTV) and an improved water elimination system. The SPETD procedure now includes a washing step with HPLC-grade water to prevent degradation of analytes due to interaction with remaining sample constituents. The system was used to analyze surface and tap water samples over a 4-month period. No decrease of chromatographic or trace-enrichment performance was observed, and a liner packed with Tenax GR could be used for at least 150 analyses. The SPETD module was coupled to GC with ion-trap detection for mass spectrometric (MS) and MS/MS detection. The linearity and repeatability of the procedure for several pesticides which were tested in the 0.5–10 μg/1 range were fully satisfactory (1 μg/1, RSD range 5–11%; n = 5). When using sample volumes of 0.1 ml only, detection limits were as low as 0. 1-0.2 μg/1. As an example, the confirmation and quantification of a suspected pesticide in a real-life sample using electron impact and positive chemical ionization in both the MS and MS/MS mode is shown.