环境水中低含量氟化物的离子色谱分析

建立了离子色谱仪测定环境水中氟离子的方法.优化了试验条件,即淋洗液选1.8 mmol/L Na_2CO_3-1.7mmol/L NaHCO_3,流速0.8 m L/min.试验选择了活性炭作为固体吸附剂,采用固相萃取消除环境水中有可能存在的痕量乙酸对检测F~-的干扰.方法的检出限为0.022 2 mg/L,回收率为97.6%~98.9%,相对标准偏差小于2%.结果表明方法处理简单、准确度高,可用于环境水中低含量氟化物的测定.     

CO_2 residual concentration of potassium-promoted hydrotalcite for deep CO/CO_2 purification in H_2-rich gas

Elevated-temperature pressure swing adsorption is a promising technique for producing high purity hydrogen and controlling greenhouse gas emissions. Thermodynamic analysis indicated that the CO in H_2-rich gas could be controlled to trace levels of below 10 ppm by in situ reduction of the CO_2 concentration to less than 100 ppm via the aforementioned process. The CO_2 adsorption capacity of potassiumpromoted hydrotalcite at elevated temperatures under different adsorption(mole fraction, working pressure) and desorption(flow rate, desorption time, steam effects) conditions was systematically investigated using a fixed bed reactor. It was found that the CO_2 residual concentration before the breakthrough of CO_2 mainly depended on the total amount of purge gas and the CO_2 mole fraction in the inlet syngas.The residual CO_2 concentration and uptake achieved for the inlet gas comprising CO_2(9.7 mL/min) and He(277.6 mL/min) at a working pressure of 3 MPa after 1 h of Ar purging at 300 mL/min were 12.3 ppm and0.341 mmol/g, respectively. Steam purge could greatly improve the cyclic adsorption working capacity, but had no obvious benefit for the recovery of the residual CO_2 concentration compared to purging with an inert gas. The residual CO_2 concentration obtained with the adsorbent could be reduced to 3.2 ppm after 12 h of temperature swing at 450 °C. A new concept based on an adsorption/desorption process, comprising adsorption, steam rinse, depressurization, steam purge, pressurization, and high-temperature steam purge, was proposed for reducing the steam consumption during CO/CO_2 purification.     

镧掺杂二氧化钛/沸石微柱在线预富集-分光光度法测定溶菌酶含量

以镧掺杂二氧化钛/沸石吸附剂微柱为萃取装置,建立了溶菌酶的分光光度检测法.考察了实验条件对萃取效率的影响.以甲醇为洗脱液,流速2.0 mL/min;样品的pH=5.0,流速1.2 mL/min,体积1.2 mL;检测波长280 nm.对蛋清、蜂蜜及葡萄酒中溶菌酶的含量进行了测定,日内与日间精密度分别为2.1%和2.8%...     

Speciation analysis of inorganic Sb(III) and Sb(V) ions by using mini column filled with Amberlite XAD-8 resin

The speciation of inorganic Sb(III) and Sb(V) ions in aqueous solution was studied. The adsorption behavior of Sb(III) and Sb(V) ions were investigated as iodo and ammonium pyrollidine dithiocarbamate (APDC) complexes on a column filled with Amberlite XAD-8 resin. Sb(III) and Sb(V) ions were recovered quantitatively and simultaneously from a solution containing 0.8 M NaI and 0.2 M H₂SO₄ by the XAD-8 column. Sb(III) ions were also adsorbed quantitatively as an APDC complex, but the recovery of the Sb(V)-APDC complex was found to be <10% at pH 5. According to these data, the concentrations of total antimony as Sb(III)+Sb(V) ions and Sb(III) ion were determined with XAD-8/NaI+H₂SO₄ and XAD-8/APDC systems, respectively. The Sb(V) ion concentration was calculated by subtracting the Sb(III) concentration found with XAD-8/APDC system from the total antimony concentration found with XAD-8/NaI+H₂SO₄ system. The developed method was applied to determine Sb(III) and Sb(V) ions in samples of artificial seawater and wastewater.     

New Composite Sorbent for Removal of Sulfate Ions from Simulated and Real Groundwater in the Batch and Continuous Tests

The evaluation of groundwater quality in the Dammam formation, Faddak farm, Karbala Governorate, Iraq proved that the sulfate (SO₄²⁻) concentrations have high values; so, this water is not suitable for livestock, poultry and irrigation purposes. For reclamation of this water, manufacturing of new sorbent for permeable reactive barrier was required through precipitation of Mg and Fe hydroxides nanoparticles on the activated carbon (AC) surface with best Mg/Fe molar ratio of 7.5/2.5. Mixture of 50% coated AC and 50% scrap iron was applied to eliminate SO₄²⁻ from contaminated water with efficiency of 59% and maximum capacity of adsorption equals to 9.5 mg/g for a time period of 1 h, sorbent dosage 40 g/L, and initial pH = 5 at 50 mg/L initial SO₄²⁻ concentration and 200 rpm shaking speed. Characterization analyses certified that the plantation of Mg and Fe nanoparticles onto AC was achieved. Continuous tests showed that the longevity of composite sorbent is increased with thicker bed and lower influent concentration and flow rate. Computer solution (COMSOL) software was well simulated for continuous measurements. The reclamation of real contaminated groundwater was achieved in column set-up with efficiency of 70% when flow rate was 5 mL/min, bed depth was 50 cm and inlet SO₄²⁻ concentration was 2301 mg/L.     

Adsorption of fluoride, phosphate, and arsenate ions on a new type of ion exchange fiber

A new type of ion exchange fiber for the removal of fluoride, phosphate, and arsenate ions has been developed. A batch adsorption technique for investigating adsorption kinetic and equilibrium parameters and determining pH adsorption edges is applied. It is shown that the adsorption properties of the ion exchange fiber for fluoride, phosphate, and arsenate ions depend on the pH value and anion concentration. The adsorption of arsenate on the sorbent reaches a maximum of 97.9% in the pH value range of 3.5 to 7.0. The adsorption percentage of phosphate is more than 99% in the pH range of 3.0 to 5.5. The adsorption of fluoride on the ion exchange fiber is found to be 90.4% at pH 3.0. The Freundlich model can describe the adsorption equilibrium data of fluoride, arsenate, and phosphate anions. The sorption of the three anions on the ion exchange fiber is a rapid process, and the adsorption kinetic data can be simulated very well by the pseudo-second-order rate equation. The column performance is carried out to assess the applicability of the ion exchange fiber for the removal of fluoride, phosphate, and arsenate ions from synthetic wastewaters with satisfactory removal efficiency. The desorption experiment shows that fluoride ion sorbed by the fiber column can be quantitatively desorbed with 5 mL of 0.50 mol/L NaOH at elution rate of 1 mL/min, and 30 mL of NaOH is necessary for the quantitative recovery of phosphate and arsenate ions.     

Successive uranium and thorium adsorption from Egyptian monazite by solvent impregnated foam

The present work deals with uranium and thorium recovery from the Egyptian monazite sulfate leach liquor using the extraction chromatography technique (solvent impregnated material), where tributylamine (TBA) and di-n-octylamine (DOA) solvents were impregnated onto foam uranium and thorium separate recovery. The calculated theoretical capacities of the latter solvents were about 1.4 gU/g foam and 1.6 gTh/g foam, respectively. The attained uranium and thorium adsorption efficiencies (using ion-exchange columnar technique) were about 75 and 70% of its theoretical capacities, respectively. Using 1 M NaCl–0.1 M H₂SO₄ and 2 M H₂SO₄ as eluent solutions for uranium and thorium from the loaded solvents impregnated foam gave 95.8 and 98.7% elution efficiencies, respectively.     

High-Performance Liquid Chromatographic Assay of D-Glucose in Erythrocytes

Abstract

A procedure is presented after several attempts with different modes of chromatography for measuring high concentrations of d-glucose in erythrocytes. The procedure utilizes rapid deproteinization of hemolysate by mixing with acetonitrile. The supernatant is analyzed by strong cation exchange chromatography, using an Organic Analysis Column. Separation conditions are: eluent = 0.01 N H₂SO₄, flow rate = 0.6 ml/min, detection = 195nm at 0.05 AUFS, sample size = 20 μl and temperature = ambient. The coefficients of variation for 5 mg/ml samples were (within-run) 6.7%, and (day-to-day) 7.1%. This study shows the presence of a high concentration (1900 mg/dl) of d-glucose within the erythrocytes as a result of a high external d-glucose concentration (2000 mg/dl) in plasma, and suggests that d-glucose is rapidly transported into the cell.     

Purification of L-Lysine in Simulated Moving Bed and Fixed-Bed Chromatography

 L-Lysine was produced by a microbial process utilizing a Corynebacterium glutamicum (ATCC 21799) strain. L-Lysine was purified from the cultivated medium by fixed-bed and simulated moving bed （SMB） chromatography. The separation conditions including pH, eluent concentration and Lys+ and Lys2+ adsorption isotherms were studied in batch adsorption. The column capacity, eluent flow rate and eluent concentration have been studied in fixed-bed chromatography. Maximum purification rate of lysine was obtained as 0.066 g/(g·h) (per gram resin and per hour) at an eluent flow rate of 10 mL/min in fixed-bed chromatography. The results obtained from SMB were 0.11 g/(g·h) for L-lysine purification rate and 96% for L-lysine recovery.     

Optimization of lead adsorption from lead-acid battery recycling unit wastewater using H2SO4 modified activated carbon

During the recycling of exhausted lead-acid battery, large amount of wastewater is discharged, which contains the toxic Pb(II) ions in high concentration. In this study, the granular activated carbon after modification with sulfuric acid has been used to remove the Pb(II) ions from this wastewater. Adsorbents were characterized using Fourier Transform Infrared, Scanning Electron Microscope, and X-Ray Diffraction analyzer. Taguchi orthogonal L16 array (4^3) was used for batch adsorption study with four levels of three factors initial pH, adsorbent dose, and contact time. Optimum level of parameters was fourty + nd pH 4.5, time 240 min, and dose 0.05 g/50 mL using signal-to-noise ratio (larger-the-better response). Analysis of variance technique was used to signify the adsorption experiment model. The effect of parameters on uptake capacity of adsorbent has been evaluated. Maximum adsorbent capacity for Pb(II) uptake from wastewater of battery recycling unit was found 8.19 mg/g after modification with sulfuric acid. To further understand the mechanism of adsorption, isotherm and kinetic studies were carried out. Experimental data were well fitted with Langmuir isotherm model and pseudo-second-order kinetic model. The study suggested that H₂SO₄ modified granular activated carbon can be potentially used to remove Pb(II) from lead-acid battery recycle wastewater.     

离子排斥色谱法测定黄酒中的13种有机酸

建立了离子排斥色谱法（ion-exclusion chromatography,IEC）测定黄酒中有机酸含量的分析方法。使用Waters离子排斥色谱柱（300 mm×7.8 mm,7 μm）,流动相为H₂SO₄溶液（A）与乙腈（B）的混合溶液（体积比为98：2）,线性梯度程序：0~40 min,流动相A的浓度由0.01 mol/L 上升到0.02 mol/L;40~50 min,流动相A的浓度为0.01 mol/L ;流速为0.5 mL/min,柱温50 ℃,进样量10 μL,检测波长210 nm。结果表明,该方法可在30 min内实现草酸、马来酸、柠檬酸、酒石酸、苹果酸、抗坏血酸、琥珀酸、乳酸、富马酸、乙酸、丙酸、异丁酸和丁酸的完全分离与定量,13种有机酸在0.001~1.000 g/L范围内线性关系良好,回归方程的线性相关系数在0.9997以上。黄酒中13种有机酸的加标回收率为93.4%~103.8%,相对标准偏差为0.1%~1.5%（n=5）。该方法简单快捷、准确、重复性好,可用于黄酒中有机酸的测定。     

Fast analysis of thiocyanate by ion-pair chromatography with direct conductivity detection on a monolithic column

Fast analysis of thiocyanate by ion-pair chromatography using a silica-based monolithic column and direct conductivity detection was carried out. Chromatographic separation was performed on a Chromolith Speed ROD RP-18e using tetrabutylammonium hydroxide （TBA）-phthalic acid-acetonitrile as eluent. The effects of eluent concentration, eluent pH value, column temperature and flow rate on retention time of thiocyanate were investigated. The optimized chromatographic conditions for the determination of thiocyanate were as follows： 0.25 mmol/L TBA-0.18 mmol/L phthalate-7% acetonitrile （pH 5.5） as eluent, column temperature of 30 ℃, and flow rate of 6.0 mL/min. Retention time of thiocyanate was less than 1 min under the conditions. Common anions （Cl^-, NO3 , SO42 and I^- ） did not interfere with the determination of thiocyanate. Detection limit （S/N = 3） of thiocyanate was 0.96 mg/L. Calibration graph between peak area and the concentration of thiocyanate was linear in the range of 2.0- 100.0 mg/L. Relative standard deviation （RSD） of chromatographic peak area was 1.4% （n = 5）. This method has been applied to the determination of thiocyanate in ionic liquids. Recoveries of thiocyanate after spiking were 100.5%.     

Synthesis of rhodanine-bonded silica gel and its application in the preconcentration and separation of noble metals

A silica gel based sorbent containing rhodanine as functional group (RDSG) was prepared. Its adsorption and separation characteristics for Ag(I), Au(III) and Pd(II) were studied by flow-injection (FI) on-line preconcentration. Influence of different experimental parameters such as acidity, eluent, co-existing ions were investigated. Trace amounts of Ag, Au and Pd could be efficiently adsorbed by rhodanine-bonded silica gel from acidic solution and eluted with thiourea solution. Common co-existing ions exhibited virtually no interference to the preconcentration and determination. The adsorption capacity of RDSG was 0.0352, 0.107 and 0.122 mmol/g for Ag, Au and Pd, respectively. Detection limits of 0.004, 0.022 and 0.019 μg/mL for Ag, Au and Pd, respectively, were achieved with a sampling time of 60 s at a flow rate of 5.0 mL/min. The relative standard deviation were 0.5%, 0.9% and 1.7% for 0.040 μg/mL Ag, 0.200 μg/mL Au and 0.300 μg/¶mL Pd. The sorption property did not change after 1000 cycles of sorption-desorption. The contents of Ag and Au in three national certified ore samples and Pd in a secondary nickel alloy, an anode slime and a CoCl₂ electrolytic solution were determined. The results showed good agreement with the certified values.     

Rapid Determination of Trifluoromethanesulfonate and p-Toluenesulfonate by Ion-Pair Chromatography Using a Reversed-Phase Silica-Based Monolithic Column: Application to the Analysis of Ionic Liquids

A method of ion-pair chromatography was developed on a reversed-phase silica-based monolithic column for the fast and simultaneous determination of trifluoromethanesulfonate (CF₃SO₃ ^?) and p-toluenesulfonate (C₇H₇SO₃ ^?). The analysis was performed using a mobile phase of tetrabutylammonium hydroxide?+?citric acid?+?acetonitrile on the Chromolith Speed ROD RP-18e column with direct conductivity detection. The effects of the eluent, column temperature and flow rate on the retention of the anions were investigated. The experimental phenomenon was discussed according to hydrophobic interaction and ion-exchange mechanism in the separation. The optimized chromatographic conditions were selected. The optimized eluent for the separation consisted of 0.2?mmol?L^?1 tetrabutylammonium hydroxide?+?0.10?mmol?L^?1 citric acid?+?9% acetonitrile (pH 5.5). The flow rate was set at 6.0?mL?min^?1. The column temperature was 25???C. Under the optimal conditions, the better separation of CF₃SO₃ ^? and C₇H₇SO₃ ^? was achieved without any interference by other anions (Cl^?, Br^?, I^?, NO₃ ^?, SO₄ ^2?, ClO₃ ^?, BF₄ ^? and PF₆ ^?). The detection limit (S/N?=?3) was 0.28 and 0.71?mg?L^?1 for CF₃SO₃ ^? and C₇H₇SO₃ ^?, respectively. The method has been applied to the determination of CF₃SO₃ ^? and C₇H₇SO₃ ^? in ionic liquids. The spiked recoveries of CF₃SO₃ ^? and C₇H₇SO₃ ^? were 101.1 and 100.2%, respectively.     

Preparation of manganese dioxide loaded activated carbon adsorbents and their desulfurization performance

Manganese dioxide loaded activated carbon adsorbents (MnO₂/AC) were prepared and characterized by N₂ adsorption-desorption, BET method, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectrometry (FT-IR) and scanning electron microscopy (SEM). Effects of preparation conditions and adsorption conditions on desulfurization performance of the adsorbents were studied in a fixed-bed adsorption apparatus. Experimental results show that the surface area and pore volume of MnO₂/AC decreased compared with the unmodified activated carbon, but the adsorption capacity to H₂S was improved greatly. A suitable H₂S removal activity was obtained with manganese dioxide to activated carbon ratio of 1.1: 1 and the calcination temperature of 250°C. At the adsorption temperature of 40°C and gas flow rate of 20 mL/min, the H₂S saturation capacity and H₂S removal rate reached up to 713.25 mg/g and 89.9%, respectively.     

Carbon Nanofibers as Solid‐Phase Extraction Adsorbent for the Preconcentration of Trace Rare Earth Elements and Their Determination by Inductively Coupled Plasma Mass Spectrometry

Abstract

Systematic investigations were carried out into the sorption of rare earth elements (REEs) on carbon nonofibers (CNFs) by inductively coupled plasma mass spectrometry (ICP‐MS). The experimental parameters for preconcentration of REEs, such as pH, sample flow rate and volume, eluent concentration, and interfering ions on preconcentration of REEs have been examined in detail. The studied metal ions can be adsorbed quantitatively on CNFs in a pH range from 2.0 to 5.0, and then eluted completely with 0.5 mol l^?1 HNO₃. Based on the above facts, a novel method using a microcolumn packed with carbon nanofibers as an adsorption material was developed for the separation and preconcentration of REEs prior to their determination by ICP‐MS. The proposed method has been successfully applied to the determination of light (La), medium (Eu and Gd) and heavy (Yb) rare earth elements in real sample with the recovery more than 90%. In order to validate this method, two certified reference materials of tea leaves (GBW 07605) and mussel (GBW 08571) were analyzed, and the determined values are in good agreement with the certified values.     

离子液体中卤素离子杂质的离子色谱-直接电导检测法分析

研究了离子色谱-直接电导检测法分离测定离子液体中的卤素离子(F~-、Cl~-、Br~-)杂质.采用Shim-pack IC-A3阴离子交换色谱柱,考察了淋洗液种类及浓度、流速和色谱柱温度对分离测定的影响.最佳色谱条件为:以1.25 mmol/L邻苯二甲酸氢钾为淋洗液,流速1.5 mL/min,色谱柱温45 ℃.在此条件下可以基线分离卤素离子,且NO~-_3、BF~-_4、SO~(2-)_4不干扰测定.该法测定卤素离子的检出限(S/N=3)为0.02 ～0.11 mg/L,峰面积的相对标准偏差(n=5)不大于0.7%,F~-、Cl~- 和Br~- 的标准曲线的线性范围分别为0.1 ～50、0.1 ～50、0.5 ～100 mg/L.将方法用于烷基咪唑四氟硼酸盐离子液体中卤素离子杂质的测定,加标回收率为98% ～102%.     

测定啤酒和白葡萄酒中有机酸的离子排斥色谱法

研究了离子排斥色谱法分离测定啤酒和白葡萄酒中有机酸；选用常见的盐酸溶液作淋洗液，以四丁基氢氧化铵为再生液，考察了淋洗液浓度、流量等因素对分离和测定的影响，对啤酒和白葡萄酒中常见有机酸在阴离子排斥色谱柱上的保留行为进行了系统的研究；通过试验确定最佳的色谱条件为盐酸浓度1．10mmol/L，流量0．80mL/min；四丁基氢氧化铵浓度5.0mmol/L，流量1.10mL/min；并在该条件下，测定了啤酒和白葡萄酒中的有机酸。     

Synthesis,characterization and batch assessment of groundwater fluoride removal capacity of trimetal Mg/Ce/Mn oxide-modified diatomaceous earth

In this study, trimetal Mg/Ce/Mn oxide-modified diatomaceous earth (DE) was synthesized at optimal conditions. Comparison of the SEM images and the results of EDX analyses of the raw and the modified DE confirmed the surface modification of the raw DE with the trimetal oxide. Groundwater fluoride removal capacity of the sorbent was evaluated by batch method at various defluoridation conditions. At a sorbent dosage of 0.6 g/100 mL (contact time: 60 min, mixing speed of 200 rpm and temperature: 297 K), the fluoride removal was >93% for solutions containing initial fluoride concentration of 10–60 mg/L. Sorbent’s optimum fluoride uptake capacity was 12.63 mg/g at the initial fluoride concentration of 100 mg/L. Fluoride removal was >91% for solutions with initial pH range of ∼4–11 (initial fluoride concentration: 9 mg/L, sorbent dosage: 0.6 g/100 mL). Appraisal of the effect of co-existing anions on fluoride removal showed that CO₃²⁻ would reduce the amount of fluoride removed from solution, while other anions such as PO₄³⁻, NO₃⁻ and SO₄²⁻ had no observable effect. K₂SO₄ solution was found to be most suitable for regeneration of spent Mg/Ce/Mn oxide-modified DE compared to Na₂CO₃ and NaOH. The mechanism of fluoride removal at pH > 5.45 (pHpzc = 5.45) occurred by exchange of hydroxyl groups on surface of sorbent with fluoride ions from solution. Sorption data fitted better to Langmuir isotherm and pseudo-second-order model. External diffusion was observed to be the sorption rate limiting factor.     

Preconcentration of beryllium via octadecyl silica gel microparticles doped with aluminon, and its determination by flame atomic absorption spectrometry

A simple and sensitive method is presented for solid phase extraction (SPE) and preconcentration of trace quantities of beryllium using octadecyl silica gel modifed with aurin tricarboxylic acid (aluminon). Beryllium is then determined by flame atomic absorption spectroscopy. Parameters affecting SPE such as pH, sample solution and eluent flow rate, type, concentration and volume of eluent, interfering ions and breakthrough volume, were investigated. Under optimal conditions, the beryllium ions were retained on the sorbent at pH 6–6.7, while 3.0 mL of 0.05 mol L^?1 HNO₃ is sufficient to elute the ions. The limit of detection (LOD) based on 3σ was 0.8 µg L^?1 for 250 mL sample solution and 5 mL 0.05 mol L^?1 HNO₃ as eluent. The LOD can reach 0.1 µg L^?1 for 1 L sample solution and 3 mL of 0.05 mol L^?1 HNO₃. The accuracy and precision (RSD %) of the method is >90% and <10%, respectively. The method was applied to the determination of beryllium in aqueous samples.