Organic acids and inorganic anions in Bayer liquors by ion chromatography after solid-phase extraction

A method for the simultaneous separation and determination of organic acids and inorganic anions in Bayer liquors was developed by gradient ion chromatography with suppressed conductivity detection. Formate, acetate, propionate, oxalate, succinate, glutarate, fluoride, chloride and sulfate were separated and determined in 33 min. The samples were pretreated with solid-phase extraction, which has high selectivity for removing a large number of metallic ions in the Bayer liquors, and filtered with a 0.45 μm filter membrane before being injected into the ion chromatographic system. The separation of six organic acids and three inorganic anions was achieved on an IonPac AS11-HC column with KOH as the eluent, and the detection was performed by a conductivity detection mode. No interference is found in the presence of fluorate, chlorate and sulphate when organic acids are determined. The calibration graphs of peak area for all the analytes are linear over a wide range. The relative standard derivation of the peak area of analytes is less than 2.14%. Under optimum conditions the detection ranges from 0.2 to 100.0 mg/L. The average recoveries of the added standards are between 94.3% and 102.8%.

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. Satisfactory linear range, limits of detection and good repeatability were obtained. The procedure was applied to analyze inorganic anions in two commercial ethyl acetate samples.

Determination of Inorganic Anions and Melamine in Fertilizers by Ion Chromatography

A chromatographic analysis method for determining inorganic anions and melamine in fertilizers was established using ion chromatography(IC).The fertilizer samples were extracted by ultrasonic method with 7 g/L trichloroacetic acid solution and centrifuged.The supernatant is purified by a solid phase extraction column.Then,the anions in the solution were purified using SH-AP-1(250 mm×4.0 mm)as a separation column,and measured by a suppressed conductivity detector;the melamine in the solution was separated using SH-CC-4(200 mm×4.0 mm)as a separation column and detected by a UV detector.The results show that the mass concentration of anions had a linear relationship with its peak area within a certain range,the linear correlation coefficient r of the standard curve was greater than 0.999,the recovery rate of spiked samples was 93.4%-104.4%,and the relative standard deviation(RSD)of the measured value(n=6)was less than 4%.Thus,this method is widely suitable for detection of anions and cations in a variety of fertilizer samples.

Separation of Inorganic Anions Using Methacrylate-Based Monolithic Column Modified with Trimethylamine in Ion Chromatography Capillary System

Methacrylate-based monolithic column was prepared in fused-silica capillary (80 ′ 0.32 mm i.d.) by in situ polymerizetion reaction using glycidyl methacrylate as monomer;ethylene dimethacrylate as crosslinker;1-propanol, 1,4-butanediol, and water as porogenic solvents. The monolith matrix was modified with trimethylamine to create strong anion exchanger via ring opening reaction of epoxy groups. The morphology of the monolithic column was studied by using Scanning Electron Microscope (SEM). This column had good mechanical stability and permeability. The effects of various mobile phases for separation of inorganic anions were investigated. Iodate, bromate, nitrite, bromide, and nitrate were separated within 11 min using100 mMpotassium chloride as mobile phase and detected at 210 nm. This method showed good precision of retention time, acceptable linearity and good sensitivity. Under the optimum condition, the RSD of the retention time was in the range of 1.09%-1.75% (n = 6). The calibration curve showed linear relationships between the peak area and the concentration. The limits of detection (LOD) and the limits of quantitation (LOQ) were between 0.08-0.18 mM and 0.26-0.61 mM, respectively. This method was applied to the determination of inorganic anions in tap water and ground water samples.

Effect of Methanol in the Wash-Solvent Bottle and the OnGuard Cartridges on the Determination of Different Anions Using Ion Chromatography

The effect of using methanol in the flush-solvent bottle of the auto-sampler of Ion Chromatograph on the determination of sulfate ions was studied using AS11-HC 2 mm analytical column. The use of 50% methanol in the flush solvent bottle results in overestimation of sulfate concentration by 18%. However, the use of 10% methanol instead of 50% did not show such error in the determination of sulfate using the same column. Furthermore, the effect of using OnGuard-RP and OnGuard-P cartridges for sample pretreatment on the determination of different anions was also studies using AS14-HC 2 mm analytical column. The results indicate that using OnGuard-RP cartridge caused the concentration of fluoride, bromide, nitrate, phosphate and sulfate ions to be underestimated, whereas the concentration of chloride ions to be overestimated. The error in the determination of fluoride, bromide, nitrate, phosphate sulfate, and chloride was found to be 40.0%, 26.0%, 22.8%, 26.8%, 18.0%, and 25.0% of the certified standard concentration, respectively. It was also found that the use of OnGuard-P cartridge resulted in underestimation of fluoride, chloride, bromide, nitrate, phosphate, and sulfate by 60.0%, 40.0%, 82.0%, 87.2%, 45.2%, and 39.0% of the certified standard concentration, respectively. These findings point out to careful corrections that should be considered in any application of ion chromatography utilizing such sample pretreatment.

Trace analysis of anions in organic matrices by ion chromatography coupled with a novel reversed-phase column for on-line sample pretreatment

An ion chromatography（IC） system coupled with on-line column-switching technique was used to determine anions ofμg/g levels in organic chemicals of analytical reagent grade.A novel polystyrene-divinylbenzene-carbon nanotube（PS-DVB-CNT） stationary phase was utilized for matrix elimination.A calibration study was conducted by preparing and analyzing eight concentrations（between 10 and 5000μg/L） of eight standards in deionized water.The linearity was between 0.9978 and 1.And the detection limits ranged from 1.54μg/L to 10.02μg/L.A spiking study was performed on two representative organic chemicals.The recoveries were between 84.3%and 119.6%.

Science Letters:Simultaneous determination of fluoride, chloride, sulfate, phosphate, monofluorophosphate, glycerophosphate, sorbate, and saccharin in gargles by ion chromatography

Simple, reliable and sensitive analytical methods to determine anticariogenic agents, preservatives, and artificial sweeteners contained in commercial gargles are necessary for evaluating their effectiveness, safety, and quality. An ion chroma-tography (IC) method has been described to analyze simultaneously eight anions including fluoride, chloride, sulfate, phosphate, monofluorophosphate, glycerophosphate (anticariogenic agents), sorbate (a preservative), and saccharin (an artificial sweetener) in gargles. In this IC system, we applied a mobile phased gradient elution with KOH, separation by IonPac AS18 columns, and suppressed conductivity detection. Optimized analytical conditions were further evaluated for accuracy. The relative standard deviations (RSDs) of the inter-day's retention time and peak area of all species were less than 0.938% and 8.731%, respectively, while RSDs of 5-day retention time and peak area were less than 1.265% and 8.934%, respectively. The correlation coefficients for targeted analytes ranged from 0.999 7 to 1.000 0. The spiked recoveries for the anions were 90%~102.5%. We concluded that the method can be applied for comprehensive evaluation of commercial gargles.

Determination of common anions in oxalate by ion chromatography coupled with UV photolysis pretreatment

A new and simple method was developed to determine anions in oxalate of analytical reagent grade. After UV photolysis with optimal 1% H2O2 in 10,000 mg/L oxalate in the fabricated photoreactor, sample was directly injected into IC system. Satisfactory linearity, detections limits, good repeatability and spiked recovery were obtained. The method was successfully applied to determine anions in two commercial oxalate samples.

Analysis of trace elements in air particulate matters by non-suppressed ion chromatography

The application of non-suppressed ion chromatography for monitoring of trace elements in air particulate matter was studied in the present investigation. The results indicate that the use of microwave acid digestion method is superior in comparison with the conventional thermal acid digestion method as it leads to higher recovery, better reproducibility, lower volatility loss, better protection against environmental contamination and much less digestion time (5 minutes vs. 24 hours). The use of eluent as extractant is shown to reduce the water dip problem in the chro-matogram. The addition of chelating agent in the eluent coupled with UV detection is shown to provide satisfactory chromatographic separation and good sensitivity for the analysis of transition metals present in the air particulate matter. Using the U.S. National Bureau of Standards Reference Material 1648 Urban Particulate Matter as standard for checking, the analytical procedure is shown to give good recovery and reproducibility for the detection of the following cations and anions in air particulate matter: Fe2 Cu, Mn, Pb, Zn, Mg, Na, HN4+, Cl-, NO3- and SO42-. Field test was also performed to check the applicability of the method and the results obtained were discussed in the present paper.

Trace Analysis of Anions in Perfluorodecalin by Green Liquid-Liquid Extraction Combined with Ion Chromatography

Perfluoronaphthenes,with inert chemical and biological properties and ability to dissolve large amounts of oxygen,have received the most attention in medical applications.However,the excessive anion contained may cause some side effects.Herein,liquid-liquid extraction technique with shaking and ultrasonic extraction was used for the trace analysis of five anions(F^(-),Cl^(-),NO_(3)^(-),PO_(4)^(3-),SO_(4)^(2-))in perfluorodecalin using water as green extractant.The optimum pretreatment technology and ion chromatography detection conditions were established.Good linearity was observed in each concentration range,and the linear correlation coefficient(R^(2))was better than 0.997.The limits of detection(S/N=3)of five anions from perfluorodecalin were 3.2,5.5,14.2,23.2 and 29.5μg/L,respectively.The established method with high sensitivity and accuracy has been successfully appliedfor the determination of five anions in three perfluorodecalin products,which provides a basis for further development of green detection and quality standard formulation in perfluorodecalin and other fluorocarbon solvents.

A novel composite stationary phase composed of polystyrene/divinybenzene beads and quaternized nanodiamond for anion exchange chromatography

An approach for preparation of a novel composite anion exchanger composed of polystyrene/divinylbenzene (PS/DVB) beads and quaternized nanodiamods (QND) were proposed. Oxidized nanodiamonds (OND) were quaternized by the condensation polymerization between methylamine (MA) and 1,4-butanediol diglycidyl ether (BDDE), which were characterized by Fourier transform infrared (FTIR) spectra, X-ray phtoelectron spectroscopy (XPS), thermogravimetric analysis (TGA). QND with layers of cationic polyelectrolyte was attached onto the surface of sulfonated PS/DVB beads electrostatically. Subsequently, hyperbranched reaction of QND agglomerated on the PS/DVB bead surface was performed by the alternate reaction between MA and BDDE to increase the exchange capacity. The composite anion exchanger showed good stability in organic solvent and a wide pH range.The surface of these microspheres was characterized by scanning electron microscopy. In addition, ion exchange selectivity and separation efficiency of the anion exchangers were assessed using the mixtures of anions (F,Cl,NO_2,Br,NO_3,HPO_4~2 and SO_4~2) with carbonate/bicarbonate as eluent, and the anion exchanger with high exchange capacity could be used to analyze chloride in aqueous solution with high concentration of fluoride. This work explores the potential of nanodiamods as an agglomerated material for ion chromatography stationary phases for the separation of inorganic anions.

INVESTIGATION ON SEPARATION OF INORGANIC ANIONS BY REVERSED-PHASE ION-PAIR LIQUID CHROMATOGRAPHY

Ⅰ. INTRODUCTIONReversed-phase ion-pair liquid chromatography is widely used in the separation of ionized organic compounds. In recent years, the separation of inorganic ions by the reversedphase ion-pair liquid chromatography with indirect UV detection or conductivity

离子色谱测定水中无机阴离子的方法应用能力验证研究

文章依据国家标准方法HJ 84-2016和HJ 168-2020,对离子色谱法测定水中F^(-)、Cl^(-)、Br^(-)、NO_(3)^(-)、PO_(4)^(3-)、SO_(4)^(2-)开展了方法应用能力验证,验证的主要内容包括标准曲线、方法检出限、测定下限、准确度和精密度。验证结果表明:六种无机阴离子的标准曲线线性关系、检出限、测定下限、准确度、精密度均满足国家标准方法HJ 84-2016要求,实验室的技术能力能达到该标准方法的要求,通过对离子色谱测定水中无机阴离子进行方法应用能力验证,有利于促进实验室检测能力的持续提高,确保检测结果准确、可靠。

双通道离子色谱法测定陶质文物表面结晶盐中有机酸根和无机阴阳离子

对双通道离子色谱同时测定陶质文物表面结晶盐中的CH_(3)COO^(-)、HCOO^(-)、F^(-)、Cl^(-)、SO_(4)^(2-)、NO_(3)^(-)等9种阴离子和Li^(+)、Na^(+)、K^(+)等6种阳离子的测定方法进行优选。通过优化色谱条件,确定采用Metrosep A Supp7色谱柱为阴离子分析柱,3 mmol/L碳酸钠为阴离子淋洗液,流速为0.7 mL/min;Metrosep C4型色谱柱为阳离子分析柱,0.8 mmol/L吡啶二羧酸-1.6 mmol/L硝酸为阳离子淋洗液,流速为0.7 mL/min。在此方法下,净化后的滤液一次进样,电导检测器检测,各离子峰形好,分离时间适中,分离效果很好。各离子的标准曲线相关系数R>0.999,具有良好的线性关系,检出限在0.005~0.05 mg/L之间,加标回收率在96%~106%之间,相对标准偏差为0.1%~4%(n=5)。结果表明,瓦当表面结晶盐中主要含有Ca^(2+)、Na^(+)、CH_(3)COO^(-)、Cl^(-)、SO_(4)^(2-)、NO_(3)^(-)。该方法简单快速、准确度高,可有效分离文物表面结晶盐中的常见有机酸根离子和无机阴阳离子。

冷凝收集-离子色谱法测定呼出气中的有机酸和阴离子

建立了一种非侵入式冷凝收集-离子色谱方法测定人体呼出气中乳酸、甲酸、乙酸、丙酮酸、Cl^(-)、NO_(2)^(-)、NO_(3)^(-)、SO_(4)^(2-)。搭建自制呼出气冷凝装置,该装置包括吹气口、与吹气口相连的单向阀和流量计、置于半导体冷凝装置中的冷阱以及一次性冷凝收集管。通过呼出气冷凝装置对人体呼出气进行收集,利用离子色谱对冷凝液(EBC)中有机酸和阴离子的含量进行检测。优化采集冷阱温度和采集流量,得到冷阱最佳冷凝温度为-15℃,呼气流量为15 L/min。采用1.5 mmol/L碳酸钠和3 mmol/L碳酸氢钠混合溶液作为流动相,泵流速为0.8 mL/min,分析柱为IC-SA3(250 mm×4.0 mm),柱温为45℃。8种有机酸和阴离子的线性范围均为0.1~10.0 mg/L,相关系数均≥0.9993。在进样量为100μL时,方法的检出限为0.0017~0.0150 mg/L(S/N=3),定量限为0.0057~0.0500 mg/L(S/N=10)。方法的日内和日间精密度均≤7.50%(n=5)。采用该方法对5位健康受试者呼出气中的有机酸和阴离子进行检测,得到8种有机酸和阴离子的含量为0.18~42.3 ng/L。在10 km的长跑运动过程中,除了一位受试者代谢异常,其余受试者呼出气中的有机酸和阴离子含量总体变化趋势为先增加后减小。本方法采样过程简单,精密度好,且没有副作用,受试者不会产生任何明显不适或风险,可为日后人体代谢物的研究提供实验思路和理论依据。

液相色谱-离子色谱联用体系同时测定环境基质中的6种硝基芳烃类化合物和3种阴离子

同时测定环境土壤和水基质中的硝基芳烃类化合物和阴离子对于选择合适的硝基芳烃类化合物降解方法和实现地表水水质监测具有重要意义。本文通过两个六通阀和一根富集柱将高效液相色谱和离子色谱连接,搭建了色谱联用体系。系统操作可分为4个阶段:(A)样品加载到定量环;(B)分离硝基芳烃类化合物和阴离子;(C)阴离子在AG20柱中富集;(D)高效液相色谱和离子色谱分别测定硝基芳烃类化合物和阴离子。通过将液相色谱柱直接连接电导率检测器,确定阴离子流出液相色谱柱的时间,优化六通阀的切换时间,保证方法的准确性。在最优条件下,阴离子的检出限为0.005~0.020 mg/L,硝基芳烃类化合物的检出限为0.043~0.150 mg/L。3组不同加标浓度样品的平均回收率为88.20%~105.38%,相对标准偏差为2.0%~11.5%。该方法被用于检测5份地表水样品和5份土壤样品,硝基芳烃类化合物均未检出,3种阴离子在地表水样品中的检出量为0.41~55.3 mg/L,在土壤样品中的检出量为0.56~30.2 mg/kg。经过方法学验证和实际样品检测,证明该色谱联用体系检测方法自动化程度高,操作简单,重复性好,准确度高,具有广泛的适用性和较高的灵敏度,适用于环境基质中硝基芳烃类有机物和亚硝酸根离子等阴离子含量的快速测定。

离子色谱法测定玉溪北城“涩水”中4种无机阴离子

为了研究玉溪市北城“涩水”中无机阴离子的含量是否符合《生活饮用水卫生标准》中的限值,采用离子色谱法测定了玉溪北城“涩水”中F^(-)、Cl^(-)、NO_(3)^(-)、SO_(4)^(2-)的含量。结果表明,玉溪北城“涩水”中1月、2月、3月和4月的F^(-)、Cl^(-)、NO_(3)^(-)、SO_(4)^(2-)四种无机阴离子含量低于《生活饮用水卫生标准》中的限值。该方法标准曲线相关系数在0.9990以上,样品加标回收率在93.73%~109.20%之间,检出的数据准确可靠。结果为进一步探究“涩水”的水源保护和商用价值开发提供了数据支撑。

离子色谱法测定种植土壤中8种水溶性阴离子

对土壤中水溶性阴离子进行测定,可监测土壤盐渍化的类型和程度,为改良、治理及科学施肥提供参考。土壤样品经风干研磨过0.15 mm筛,以去离子水萃取、0.22μm微孔滤膜过滤,用碳酸钠和碳酸氢钠溶液等度洗脱,离子色谱仪同时测定土壤萃取液中F^(-)、BrO_(3)^(-)、Cl^(-)、NO_(2)^(-)、Br^(-)、NO_(3)^(-)、PO_(4)^(3-)、SO_(4)^(2-)等8种水溶性阴离子含量。结果表明:8种阴离子在0.2~10.0 mg/L曲线线性关系良好,相关系数大于0.999;土壤样品阴离子检出限为0.6~7.0 mg/kg;进行3浓度水平加标实验,回收率为65.6%~120%,相对标准偏差为0~8.9%,表明方法具有较高的精密度和准确度。方法用于蔬菜种植基地、农田、绿化带土壤及养殖塘泥检测,结果显示,样品中检出F^(-)、Cl^(-)、NO_(2)^(-)、Br^(-)、NO_(3)^(-)、PO_(4)^(3-)和SO_(4)^(2-),浓度为5.0~1 090.6 mg/kg,均未检出BrO_(3)^(-)。各类型土壤阴离子浓度差异较大,蔬菜种植基地土壤中含有较高的Cl^(-)、NO_(3)^(-)或SO_(4)^(2-),可能与长期施用特定类型的化肥有关,农田土壤和塘泥长时间处于水中,水溶性阴离子已充分溶解,各阴离子含量较低;绿化带土壤未充分开垦,阴离子浓度接近于该类型土壤本底值。

离子色谱法在湿电子化学品阴离子检测中的应用进展

湿电子化学品中的阴离子可能引发元件污染,导致短路、沉积、缺陷和腐蚀等问题,因此准确测定阴离子至关重要。离子色谱法因其检测灵敏度高,结果准确等特点,适用于湿电子化学品的产品质量检测。简要介绍了常见湿电子化学品及其应用领域和离子色谱仪的结构,综述了离子色谱法在检测湿电子化学品阴离子时的常用样品预处理(在线预浓缩和在线阀切换)技术,以及多种湿电子化学品(超纯水、无机酸/碱类超净高纯试剂、超净高纯有机试剂和光刻胶)中的应用。此外,还探讨了离子色谱法当前技术难点及未来发展方向(引用文献66篇)。

双抑制在线基体去除-离子色谱法测定电池级碳酸锂中痕量阴离子

建立了一种测定电池级碳酸锂中痕量阴离子的方法。用超纯水超声辅助溶解碳酸锂,采用在线基体去除法去除碳酸锂基体,基体去除过程中,样品首先流入到ADRS600(4 mm)抑制器(抑制电流150 mA,抑制器再生液外接水流速2 mL/min)中,在抑制器内通过离子交换膜作用,碳酸锂中的锂离子与氢离子置换,碳酸锂变成碳酸;然后经过CRD 200(4 mm),碳酸以二氧化碳的形式排出离子色谱系统,从而达到去除碳酸锂基体的目的;最后待分析阴离子被自动富集在IonPac UTAC-LP2浓缩柱(35 mm×3 mm)上,通过阀切换技术将阴离子自动转移到色谱分析系统中。在色谱分析系统中,以IonPac AG18(50 mm×2 mm)为保护柱,IonPac AS18(250 mm×2 mm)为分析柱,柱温箱为30℃,KOH溶液为淋洗液进行梯度洗脱,泵流速0.30 mL/min,抑制器为ADRS600(2 mm),抑制电流25 mA,进样体积为250μL,检测器为电导检测器。结果显示:F^(-)、Cl^(-)、NO_(2)^(-)、Br^(-)、NO_(3)^(-)及SO_(4)^(2-)离子在各自的线性范围内具有良好的线性关系(r≥0.999);各离子的检出限和定量限分别为0.05~0.88μg/L和0.15~2.92μg/L;碳酸锂样品连续6针进样各离子峰面积的相对标准偏差(RSD)均≤0.73%;同一碳酸锂样品处理完后分别放置0、2、4、8、12、18、24 h后进样,各离子峰面积的RSD均≤0.96%;在3个添加水平下,各离子加标回收率为93.3%~99.3%,RSD(n=6)为0.97%~3.45%;本方法具有方法定量限低(各离子定量限均为0.5 mg/kg)及多种离子同时分析的优势,适用于电池级碳酸锂中痕量阴离子的检测。