二维离子色谱法同时测定4种无机阴离子和葡萄糖酸根离子

建立了一种新的二维离子色谱分析模式,应用阀切换技术并联抑制电导和脉冲安培双检测体系,同时测定Cl^-、NO₂^-、SO₄^2-、NO₃^-和葡萄糖酸根离子。第一维色谱采用Ionpac AG18+Ionpac AS18阴离子分析柱,分别以5和20 mmol/L的NaOH溶液等度淋洗,流速为1.0 mL/min,进样量为25 μL,抑制电导检测Cl^-、NO₂^-、SO₄^2-和NO₃^-。第二维色谱采用CarboPac PA1+CarboPac PA20两保护柱串联,以90 mmol/L NaOH溶液、0.8 mL/min的流速洗脱,由AG15柱分离富集葡萄糖酸根,脉冲安培检测器检测。结果表明:无机阴离子在0.1~5.0 mg/L、葡萄糖酸根在0.0856~4.2825 mg/L范围内有良好的线性关系,RSD在1.05%~1.94%之间,相关系数(R²)在0.9945以上;无机阴离子的方法检出限为0.615~2.17 μg/L,葡萄糖酸根的方法检出限为24.24 μg/L;回收率在90.3%~102.8%之间。该方法并联两种检测模式,有良好的准确度和精密度,适用于复杂样品的分离分析。     

Determination of inorganic anions in ethyl acetate by ion chromatography with an electromembrane extraction method

In this work, the determination of inorganic anions in slightly water-soluble organic solvents (ethyl acetate) was realized by ion chromatography (IC) with a novel-efficient electromembrane extraction method. From an 8 mL ethyl acetate sample, three inorganic anions migrated through the pores of a polypropylene hollow fiber membrane, and into deionized water inside the lumen of the hollow fiber by the application of 600 V. The transport was forced by an electrical potential difference sustained over the liquid membrane, resulting in electrokinetic migration of inorganic anions from the donor compartment to the acceptor solution. After the electromembrane extraction, the acceptor solution was analyzed by IC with a sodium carbonate-sodium bicarbonate eluent. The applied voltage, stirring speed, and extraction time for controlling the extraction efficiency were optimized. Within 10 min of operation at 600 V, chloride, bromide, and sulfate were extracted with recoveries in the range 76-110%, which corresponded to a linear range of 0.01-1 mg/L. The procedure was applied to the analysis of inorganic anions in a real ethyl acetate sample and expands onto other slightly water-soluble organic solvents.     

Determination of inorganic anions in ethyl acetate by in-line hollow fiber membrane extraction with ion chromatography

In this work,a novel hollow fiber membrane extractor was set up to extract inorganic anions from ethyl acetate using deionized water.Inorganic anions in slightly soluble organic solvents can be determined by the in-line hollow fiber membrane extractor coupled with ion chromatography at first time.Different aspects of the extraction procedure such as magnetic stirring speed, extraction flow rate and extraction time were optimized to achieve high extraction efficiency and good separation results. Satisfact...     

Determination of inorganic anions in mushrooms by ion chromatography with potentiometric detection

A simple method for determination of common inorganic anions in mushroom samples has been developed by using suppressed ion chromatography with a pH detection unit. The detection unit which was constructed in such a way that practically no additional dispersion occurred consisted of a flow-through quinhydrone pH sensor and a small reference electrode. Chromatographic separation was performed in the order F⁻, Cl⁻, NO₂⁻, Br⁻, PO₄³⁻, ClO₃⁻, NO₃⁻, and SO₄²⁻, at room temperature by using Ion Pac AS 9-HC anion exchange column. Anion extracts from dried mushroom samples at room temperature were homogenized and filtered before injection. Under optimized analytical conditions, the detection limits of the method were between 2 × 10⁻⁶ and 3 × 10⁻⁴ M, depending on the anion studied. The results showed that the concentrations of fluoride and bromide in all mushroom samples were below their limit of detection. Nitrite was found to be the lowest abundant ion, while the most abundant ion was sulfate in all the mushroom samples studied.     

Separation of inorganic anions by unsuppresed ion chromatography

The elution behaviour of 11 inorganic anions is investigated by unsuppressed ion chromatography with PRP-X100 a macroporous poly(styrene-divinylbenzene) strong-base anion-exchanger. Weak acids (cyanide and sulfide) can be separated and detected at pH 9 with sodium p-hydroxybenzoate as the eluent.     

离子色谱法测定乙二醇中微量有机酸和无机阴离子

建立了以YSA-8阴离子交换柱的离子色谱法分析乙二醇中微量有机酸和无机阴离子的方法,比较了进样乙二醇浓度对F-及有机酸测定结果的影响,进样乙二醇质量分数低于8.5%时,能够得到较准确的数据.用本法对所测的有机酸和无机阴离子检出限均在8.9 μg/L以下,线性相关系数r在0.996～0.999范围内,标准样中各物质的离子峰面积的相对标准偏差(RSD)在4.2%以下(n＝11),对乙二醇质量分数约为8.5%的样品中F-及有机酸的加标回收率在91.6%～100.0%之间,乙二醇含水料直接测定无机阴离子的加标回收率在91.8%～104.8%之间.     

Determination of trace inorganic anions in anionic surfactants by single-pump column-switching ion chromatography

An ion chromatography method has been proposed for the determination of three common inorganic anions(chloride,nitrate and sulfate) in anionic surfactants using a single pump system.The new system consists of an ion exclusion column,a concentrator column,and an anion exchange column connected in series via two 6-ports valves in a Dionex ICS-2000 ion chromatograph.The valves were switched several times for removing surfactants,concentrating and separating the three anions.The chromatographic conditions were optimized.Detection limits(S/N = 3) were in the range of 0.10-0.68μg/L.The relative standard deviations(RSDs) of peak area were less than 4.6%.The recoveries were in the range of 84.1-112.6%.     

Determination of common inorganic anions and cations by non-suppressed ion chromatography with column switching

An ion chromatography (IC) method has been proposed for the determination of seven common inorganic anions (F(-), H(2)PO(4)(-), NO(2)(-), Cl(-), Br(-), NO(3)(-), and SO(4)(2-)) and/or five common inorganic cations (Na(+), NH(4)(+), K(+), Mg(2+), and Ca(2+)) using a single pump, a single eluent and a single detector. The present system used cation-exchange and anion-exchange columns connected in series via a single 10-port switching valve. The 10-port valve was switched for the separation of either cations or anions in a single chromatographic run. When 1.0mM trimellitic acid (pH 2.94) was used as the eluent, the seven anions and the five cations could be separated on the anion-exchange column and the cation-exchange column, respectively. The elution order was found to be F(-)相似文献   

Advances in the determination of inorganic anions by ion chromatography

The time period covered for this review includes articles published from 1997 to 1999, with the addition of a few classic references. The purpose of the review is to include the most relevant works from each topic area of the determination of inorganic anions by ion chromatography, including new sample pretreatments, new separation methods, new detection systems and the latest applications in the field of environmental, water, foods, etc. samples. Experimental conditions such as stationary phase, eluent, detection mode, as well as matrix are summarized in a table.     

正交试验优化土壤萃取法及常见无机阴离子的离子色谱分析

实验采用超声提取离子色谱法测定土壤中常见无机阴离子的含量,以正交试验优化土壤中阴离子的提取条件。研究土壤粒径、料液比、提取功率、提取时间对土壤中阴离子提取量的影响。结果表明:土壤中阴离子提取的最佳条件为A1B2C3D3。即超纯水为提取液,土壤粒径为180μm,料液比为1:30,超声波作用时间为40 min,提取功率为320W,提取次数为一次。该方法可用于土壤中常见可溶性无机阴离子含量的提取测定。     

Determination of inorganic and organic anions in one run by ion chromatography with column switching

A method for the simultaneous determination of low-molecular-mass organic and inorganic anions in aqueous solutions was developed using isocratic ion chromatography (IC) with suppressed conductimetric detection and column switching. Owing to the large differences in distribution coefficients between sulphate, nitrate and phosphate and the other species, these ions are separated in the first stage on a medium-capacity anion exchanger, whereas the other anions are led through a second column packed with a high-capacity anion-exchange resin via a column-switching valve. After optimization of the switching procedure a spiked drinking water sample was analysed. Fluoride, acetate, butyrate, formate, nitrate, nitrite and phosphate could be determined in addition to the main anions (chloride and sulphate). The time for a complete analysis is less than 20 min and the method can easily be automated. The precision and detection limit are as usual in IC with background suppression.     

Determination of inorganic anions in natural water by microcolumn ion chromatography with on-column enrichment.

An on-column enrichment method was developed for the rapid determination of inorganic anions in natural water. The system was assembled from a syringe pump, a six-port switching valve with a sample-enrichment loop, a separation column and a UV detector. The enrichment efficiency of the system was tested by using inorganic anions as samples. The limits of detection were between 0.6 and 7.7 microg/L. The system was applied to the determination of anions in river and pond-water samples.     

Determination of trace inorganic anions in seawater samples by ion chromatography using silica columns modified with cetyltrimethylammonium ion

Conventional silica columns dynamically modified with cetyltrimethylammonium ions were evaluated for the determination of UV-absorbing bromide, nitrate, and nitrite in seawater samples. Cetyltrimethylammonium, which is a quaternary ammonium ion, was dynamically introduced onto silica surfaces. The first layer of the modifier was introduced by electrostatic interaction, whereas the second layer was introduced by hydrophobic interaction. The latter layer worked as the anion-exchange sites. The modified conventional silica columns could be used for separation of inorganic anions. Separation of authentic mixture of five anions was achieved within 17 min. The addition of 0.1 mM cetyltrimethylammonium ion to the eluent improved the repeatability of the retention time. Seawater samples could be directly injected onto the prepared conventional silica columns, and bromide, nitrate, and nitrite levels were determined to be 69, 0.13, and 0.016 ppm, respectively.     

固相萃取-离子色谱法测定甘蔗糖蜜及糖蜜酒精废液中的非氮有机酸和无机阴离子

建立了固相萃取-离子色谱测定甘蔗糖蜜及糖蜜酒精废液中乙酸、乳酸、琥珀酸、苹果酸、酒石酸、草酸、富马酸、柠檬酸、乌头酸等非氮有机酸和盐酸根、硫酸根、磷酸根等3种无机阴离子的方法。样品稀释液经强阴离子(SAX)固相萃取小柱净化除去糖类和色素等干扰基质,再用稀KOH溶液洗脱,经0.45 μm水膜过滤后,用IonPac AS15阴离子分离柱、KOH溶液梯度淋洗-抑制电导检测分离分析。考察了固相萃取小柱对待测离子的保留和洗脱条件。实验结果表明,除乙酸和乳酸的分离不完全、苹果酸与琥珀酸的组分重叠外,其余组分可达到完全分离,被测组分的浓度与其峰高在一定的范围呈良好的线性关系,检出限均低于0.20 mg/L,相对标准偏差(RSD)小于6.7%。测定了2种甘蔗糖蜜和1种糖蜜酒精废液中有机酸及无机阴离子,结果满足检测的要求,样品中各组分的加标回收率为94%～109%。     

Determination of anions in landfill leachates by ion chromatography

Ion chromatography has been used to determine inorganic and organic anions within landfill leachates. Two procedures are operated on split samples which have multiple dilutions and vary in sample treatment: gradient ion-exchange chromatography for inorganic anions and isocratic ion-exclusion chromatography for organic anions. Interference between carbonate and organic acid anions using ion-exclusion chromatography is avoided by treatment with octanesulphonic acid eluent. Using ion-exchange chromatography, the presence of valerate, hexanoate and heptanoate is checked (but not quantified) for a subsample which has been treated to remove chloride; these species are then determined by ion-exclusion chromatography. Analysis of certified standards (10 mg/1 certified VFA standard; Supelco, Bellefonte, PA, USA; 20–150 mg/l inorganic anions, ICMIX1-100, Glen Spectra Reference Materials, Middlesex, UK) gives good agreement (within 5% for organic anions except formate, and within 1% for inorganic anions), with R.S.D. values for all anionic species varying from 0.44–2.23.     

Determination of anions in high-purity water by ion chromatography

Summary The determination of the concentration of some different anions in high-purity water (g/l-level) using ion chromatography after concentration on pre-columns is described. The detection ist made by a conductivity cell after passing an anion fiber-suppressor (AFS). Two different separator columns (AS-5 and AS-4) and some different separator systems were tested. In all cases linearity is given for the determined anions.The concentration of the anions was determined not directly but by addition of a standard solution and subsequent graphic extrapolation of the calibration diagram. The determination levels are below 1 g/l. The AS-5 column gives better results than the AS-4 column.

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Ionen-chromatographische Bestimmung von Anionen in Reinstwasser

Zusammenfassung Die Bestimmung der Konzentration verschiedener Anionen in Reinstwasser (g/l-Bereich) mittels der Ionen-Chromatographie nach Anreicherung auf Konzentriersäulen wird beschrieben. Die Detektion erfolgt über eine Leitfähigkeitsmeßzelle mit vorgeschaltetem Anionen-Hohlfasermembransuppressor (AFS). Es wurden zwei verschiedene Trennsäulen (AS-4 und AS-5) und mehrere Trennsysteme getestet und optimiert. In allen Fällen ergab sich Linearität für die untersuchten Anionen. Die Bestimmung der Anionenkonzentrationen in Reinstwasser erfolgte nicht direkt, sondern durch Aufstocken mit Standardlösung und anschlie\ender graphischer Extrapolation der erstellten Eichgraden. Die Nachweisgrenzen liegen unter 1 g/l. Die AS-5-Säule erwies sich für die beschriebene Methode als geeigneter.

     

Determination of monovalent inorganic anions in high-ionic-strength samples by electrostatic ion chromatography with suppressed conductometric detection

A new ion chromatographic (IC) system has been established by using micelles of 3-(N,N-dimethylmyristylammonio)propanesulfonate (Zwittergent 3-14) loaded onto a reversed-phase packed column as the separation column with an electronic rotary switching valve packed-bed suppressor for conductometric detection of inorganic anions. An aqueous H3BO3-Na2B4O7 solution has been demonstrated to be the most desirable eluent for this IC system. The relationship between retention time and the concentration of the borate eluent was determined for a series of model anionic analytes and this relationship was found to be opposite to that exhibited in a conventional anion-exchange IC system. The rapid elution and complete separation of monovalent inorganic anions were obtained by initially using a high-concentration borate solution as the eluent for a short-period, and then switching to a lower-concentration borate eluent to complete the separation. Detection limits for nitrite, bromide, nitrate, and chlorate were 0.85, 0.88, 0.95 and 4.8 microM, respectively, when a 7.0 mM Na2B4O7 eluent was used. Moreover, the ability to directly detect these monovalent anions in samples containing high concentrations of sulfate and/or chloride ions provided a major advantage of this approach.     

Determination of low-molecular-mass aliphatic carboxylic acids and inorganic anions from kraft black liquors by ion chromatography

An ion chromatographic (IC) method with suppressed conductivity detection (CD) was developed and validated for the quantitative determination of several low-molecular-mass aliphatic mono- and dicarboxylic acids as their carboxylate anions together with some inorganic anions (chloride, sulfate, and thiosulfate) from kraft black liquors. To confirm the identification of some carboxylate anions which lack commercial model substances, a qualitative IC method with suppressed electrospray ionization mass spectrometry (ESI-MS) was also developed. The separations were performed on an IonPac AS 11-HC anion-exchange column operated at 25 degrees C within 25 min by a gradient elution with aqueous potassium hydroxide (suppressed CD in the AutoRegen mode) or sodium hydroxide (suppressed ESI-MS in the pressurized bottle mode). In the validation process a mixture of carboxylic acids and inorganic anions in aqueous media and in seven different types of wood and non-wood black liquor samples were quantitatively analyzed by IC-CD. As a result, calibration lines with correlation coefficients of 1.00 for all analytes were achieved at a concentration range from 0.05 to 105 mg L(-1). In black liquor samples intra-day (n=6) precision values ranged from 0.9 to 5%. Day-to-day (n1=3) and intermediate precision values were less than 5% for all other compounds except sulfate and thiosulfate. The variability in the thiosulfate and sulfate results is due in large part to the oxidation of sulfide and thiosulfate, respectively. Recoveries were close to 100% with standard deviations less than 8%. Depending of the analyte, the limits of detection and quantification were, respectively, between 1 and 8 microg L(-1) and between 3 and 27 microg L(-1) for standard compounds in aqueous media and between 6 and 106 microg L(-1) and between 14 and 148 microg L(-1) for black liquor samples. These validation results clearly indicated that with respect to selectivity, linearity, limits of detection and quantification, precision, and accuracy, the IC-CD method showed good applicability in the determinations described above.     

Determination of organic acids in the presence of inorganic anions by ion chromatography with suppressed conductivity detection

Simultaneous separation of 19 organic acids and 10 inorganic anions has been demonstrated using ion chromatography with a high capacity anion exchange column and the suppressed conductivity detector under an auto-suppression external sulfuric acid mode. Quantitative merits of this method were examined for analysis of nine organic acids of potential significance in cell culture broth. External calibration curves for these analytes were linear with correlation coefficients exceeding 0.999, and the relative standard derivations of observed analyte concentrations were less than 3.0% in both inter- and intra-day evaluations of aqueous standards. Developed methodology was subsequently applied to obtain organic acid profiles of Luria-Bertani liquid media, yeast extract, peptone, and the culture broth of a mutant Escherichia coli strain. Analytes recoveries observed for triplicate analysis of LB media spiked at two concentration levels ranged from 88% to 105% with less than 7% RSD. These data demonstrate quantitative accuracy for LB media and suggest that the report method may also be applicable to complex samples such as fermentation mixture and lignocellulose hydrolysate.     

Separation and determination of organic acids and inorganic anions in Bayer liquors by ion chromatography after solid-phase extraction

An ion chromatographic (IC) method for the determination of six organic acids and three inorganic anions in Bayer liquors was proposed. Formic, acetic, propionic, oxalic, succinic, glutaric acid, F⁻, Cl⁻, and SO ₄ ²⁻ were separated and determined within 33 min. For the first time, repeatability, reproducibility, and recoveries for the determination of these acids in Bayer liquors were estimated. The analytes were removed from a Bayer liquor by using an ion-exchange resin column. The chromatographic separation was achieved with only one IonPac AS11-HC column thermostated at 30°C. Organic acids and inorganic anions were detected with a suppressed conductance detector. The precision results showed that the relative standard deviations of the repeatability and reproducibility were <2.94 and <1.37%, respectively. The accuracy of the method was confirmed with an average recovery ranging between 86.3 and 105.6%. Under optimum conditions the detection limits ranged from 0.008 to 0.053 mg/L. The text was submitted by the authors in English.