Facile synthesis of quantum dots metal oxide for photocatalytic degradation of organic hazardous materials and factory effluents

Solar photocatalytic behavior of zinc oxide quantum dots (ZQs) was studied and synthesized using a modified precipitation process and characterized using various spectroscopic techniques. HRTEM was used to demonstrate and verify the purity of the prepared quantum dot material and the calculated crystallite size is 4.4 and 5.3 nm for the ZQ1 and ZQ2 samples, respectively. The optical characteristics and the BET analysis of ZQs samples investigated great value for the bandgap energy and the specific surface for ZQS samples. The photodegradation process of Indigo Carmine dye (IC) (one of the commercial organic hazardous materials used in the dying process) by ZQ1 recorded the highest synthetic levels equal to 17.18 × 10^-3S^-1. Also, the ZQ1 sample with the smallest particle size reaches the maximum fluorescence rate by almost 31 % in coumarin photo-oxidation than the ZQ2 sample with the largest particle size. This study included a report of the mineralization of IC dye, 16 investigated factory effluents samples, and their recovery ability for ten replication cycles as a case study in the presence of ZQs by sunlight for two months. These evaluation processes are by TOC analysis and COD measurements.     

近红外光谱技术用于白砂糖质量的实时监测研究

采用国产近红外在线分析仪,结合漫反射光谱分析技术,对广西某糖厂的白砂糖质量进行了在线应用研究.讨论了影响建模的因素,并提出一些解决问题的方案.采用SupNIR-4000型长波近红外在线分析仪,直接对产品传送带上的白砂糖进行扫描获得光谱数据,运用偏最小二乘法对实验数据进行多元统计分析建立数学模型,并进行了预测.样品色值的预测值和实测值间的相关系数为0.885,标准校正偏差为4.300,色值预测偏差小于糖厂要求的±10;样品浊度预测值和实测值间的相关系数为0.909,标准校正偏差为2.308,浊度预测偏差小于糖厂要求的±4.结果显示,模型预测结果符合糖厂要求,表明在线近红外技术在白砂糖质量监控中具有较好的应用前景.     

Developments in sample preparation and separation techniques for the determination of inorganic ions by ion chromatography and capillary electrophoresis.

A review is presented of sample preparation and separation techniques for the determination of inorganic ions by ion chromatography (IC) and capillary electrophoresis (CE). Emphasis has been placed on those sample treatment methods which are specific to inorganic analysis, and the developments in separation methods which are discussed are those which enhance the capabilities of IC and CE to handle complex sample matrices. Topics discussed include solid-phase extraction for sample clean-up and preconcentration, dialytic methods, combustion methods, matrix-elimination IC, electrostatic IC, electrically polarised ion-exchange resins, electromigration sample preparation in CE, chromatographic sample preparation for CE, use of high-ionic strength background electrolytes, buffering of background electrolytes in CE, use of capillary electrochromatography for inorganic determinations, and methods for the manipulation of separation selectivity in both IC and CE. Finally, some possible future trends are discussed.     

Application of ion chromatography to qualitative and quantitative determination of the main inorganic ionic components of samples from a production process of potassium sulphate

This review presents the possibility to use ion chromatography (IC) to analyse solids and brines deriving from treatment procedures of potassium salts. Qualitative and quantitative determination of ions samples has been used to make their chemical reconstruction. By using conventional calibration methods covering the whole concentration interval, analysis were not suitably accurate. During this process, the analysis is considered acceptable when the difference between the sum of the equivalents of cations and anions (ΔE) is ≤2%. For the process, a calibration method has been used employing four reference curves; each defined by three points corresponding to three standards purposely devised in our laboratory. The composition of the standards matched that expected for the samples from the different stages of the process reaction, after their usual sampling, dissolution and dilution. By comparing the conductivity of the analyte in the real sample to the conductivity of the same analyte in a standard, the effects of other analytes present in the medium are practically cancelled and need not be considered. The IC method results are in good agreement with conventional analysis methods (potentiometric titration, atomic absorption, gravimetric analysis).     

Monolithic stationary phases for fast ion chromatography and capillary electrochromatography of inorganic ions

The focus of this review is on current developments in monolithic stationary phases for the fast analysis of inorganic ions and other small molecules in ion chromatography (IC) and capillary electrochromatography (CEC), concentrating in particular on the properties of organic (polymer) monolithic materials in comparison to inorganic (silica-based) monoliths. The applicability of these materials for fast IC is discussed in the context of recent publications, including the range of synthesis and modification procedures described. While commercial monolithic silica columns already show promising results on current IC instrumentation, polymer-based monolithic stationary phases are currently predominantly used in the capillary format on modified micro-IC systems. However, they are beginning to find application in IC particularly under high pH conditions, with the potential to replace their particle-packed counterparts.     

毛细管离子电泳

Capillary ion electrophoresis (CIE) was reviewed with 72 references. It is firstly compared with ion chromatography(IC). Then detection method, separation and analysis methods of anions and cations were guidelined. Determination of ions in various samples was also reviewed.     

Recent developments in the separation of inorganic and small organic ions by capillary electrophoresis

Which method should I use for ion analysis, ion chromatography (IC) or capillary electrophoresis (CE)? In terms of actual theoretical plates CE has a clear-cut advantage. The separation ability of IC is adequate for many sample types, and many separation scientists feel that IC offers greater reliability and confidence than CE. However, IC is a more mature technique and there has been more time to solve problems such as peak tailing and to improve reproducibility. The two techniques should be viewed as complementary. A number of recent developments in ion analysis by CE are discussed. These include some simple ways to control electroosmotic flow and improve reproducibility, separation of isotopes, improved methods of indirect photometric detection, a new contactless conductivity detector, separation of ions at low pH, and in solutions of high salt content. Progress in a new technique called IC-CE will be described in which a soluble ion-exchange polymer is added to the capillary electrolyte to separate anions based on differences in both electrophoretic mobility and ion-exchange interactions.     

Determination of water-soluble inorganic and organic species in atmospheric fine particulate matter

The use of ion chromatography (IC) in conjunction with ultrasonic extraction is described for the routine analysis of water-soluble major inorganic ions and organic acids in atmospheric fine particles (PM_2.5). Both the extraction method and the IC analysis were validated using NIST SRM 1648 (urban particulate matter). In addition, the reliability of the IC method was established by intercomparison of results obtained with those from suitable alternative analytical techniques (atomic absorption spectrometry (AAS), proton-induced X-ray emission (PIXE) spectrometry, and UV-Visible spectrophotometry). The validated IC method was successfully applied for field monitoring of PM_2.5 particles collected in Singapore over an extended period of time. The IC analysis revealed that the concentrations of individual ions were in the order, SO₄²⁻ > NH₄⁺ > NO₃⁻ > Na⁺ > K⁺ > Cl⁻, respectively. Among the major ionic components, SO₄²⁻ contributed 50% to the measured water-soluble aerosol mass followed by NH₄⁺ (16.5%) and NO₃⁻ (9.0%). The cations Na⁺, K⁺, Mg²⁺, and Ca²⁺ accounted for 24% of the total water-soluble mass. The IC analysis was performed to quantify the organic acids, which typically account for a small fraction of water-soluble organic compounds in PM_2.5. Oxalate was found to be the dominant species among the organic acids measured in this work.     

Membrane-based solvent extraction for selective removal and recovery of metals

A membrane-based solvent extraction process was developed for selective removal and recovery of metals from aqueous solutions. The process utilizes microporous membranes as an interface between an aqueous solution and organic solvents containing liquid ion exchangers. Metal ions are transported from the aqueous solution to the organic phase at the interface created in the pores of membrane. The organic solvent, which is loaded with metal ions in the extraction module, is regenerated in contact with the stripping solution in the stripping module. One important feature of this process is the stability of the membrane system, which results from using an aqueous—organic separator to remove aqueous solution from the organic circulating line. This process was evaluated for enrichment of copper using solvents containing LIX 64N. The process is applicable to selective recovery of metals from ore leachates or metal-containing wastewater.     

Solid-phase extraction for metabolomic analysis of high-salinity samples by capillary electrophoresis-mass spectrometry

Environmental samples such as soil solutions contain inorganic ions such as NH4(+), K(+), Na(+), NO3(-), and PO4(3-) in high concentrations, which must be removed prior to capillary electrophoresis-mass spectrometry analysis to obtain accurate results. However, the separation of these inorganic ions from ionic metabolites, which are the target compounds in capillary electrophoresis-mass spectrometry analysis, is difficult because the physicochemical properties of the inorganic ions are similar to those of the ionic metabolites. In this study, we used various solid-phase extraction (SPE) columns for the purification of the samples containing inorganic ions in high concentrations. We found that cation-exchange SPE columns successfully filtered out the inorganic ions while retaining most of the organic compounds, which were easily collected with high recovery rates. In addition, 17 cationic metabolites in the soil solution were quantified by CE-MS analysis following the SPE purification process. The results suggest that our method can be used to analyze other environmental samples containing inorganic ions in high concentrations.     

离子色谱技术的重要进展和我国近年的发展概况

介绍了离子色谱技术近年的几项重要进展,包括Reagent-Free离子色谱系统,简易阀切换技术,弱电离有机酸的高灵敏分析,快速分析色谱柱,与前处理技术、电感耦合等离子体质谱和氢化物发生-原子荧光光谱联用,在生物医药分析中的应用等;并概述了近年来我国离子色谱在硬件技术研发、仪器检定规范的修改、标准方法和药典修订等方面的进展。     

超声提取-高温燃烧吸收-离子色谱法测定纺织品中可吸附有机卤化物北大核心CSCD

建立了一种对纺织品中可吸附有机卤化物(AOX)的超声提取-高温燃烧吸收-离子色谱定量检测分析新方法。该方法采用超声方式提取纺织品中的AOX,提取液加入活性炭进行振荡吸附,并用酸性硝酸钠溶液对无机卤化物进行去除。采用程序升温的氧化燃烧方式对吸附AOX的活性炭进行裂解、燃烧及气化,其产生的卤化氢等气体随载气进入吸收液并完全转化为无机卤素阴离子,采用离子色谱分离测定,外标法定量。实验优化了超声提取时间、活性炭用量、燃烧气及其流量、燃烧升温程序、吸收液和吸收方式等前处理条件,并对离子色谱的仪器分析条件如色谱柱、柱温及淋洗液流速等进行优化。结果表明,氟、氯、溴、碘4种卤素离子的标准溶液在0.02~10 mg/L范围内呈线性关系,线性相关系数(R^(2))均在0.999以上;AOX测定的方法定量限为0.10~0.50 mg/kg。以棉、毛和涤纶3种不同种类的阴性纺织样品作为样品基质,选取典型的有机卤化物进行加标,在低、中、高3个加标水平下测得AOX的平均回收率为82.3%~98.7%,相对标准偏差(RSD,n=7)为2.0%~5.7%,表明方法具有良好的回收率和精密度。将该方法应用于实际纺织样品的测定,检出了不同含量的AOX,且重复性好。研究建立的方法通过采用活性炭的振荡吸附、程序升温的高温氧化燃烧方式和多孔吸收瓶的二级吸收方法,提高了AOX转化为无机卤素的回收率;同时利用离子色谱仪器选择性好、灵敏度高的特点成功地一次性分离检测4种AOX,且无杂质离子的干扰。该方法简单、准确、可靠,满足国内外法规和标准对纺织品中AOX的限量要求,适用于纺织品中AOX的分析测定。     

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.     

Cationization of organic molecules under pulsed laser induced ion generation

Mass spectra of various involatile organic compounds, obtained by surface analysis with a laser microprobe mass analyser are reported. Metal-cationized quasimolecular ions of adenine, adenosine, 5-adenylic acid and sucrose supported on metal foils were observed. Metal attachment can also be detected from mixtures of metal salts and the organic compounds. Silver-cationized sugar molecules and atomic silver ions solvated by (H₂O)_x and (NH₃)_x (x = 1,2) have been found. The mass spectra are compared with those obtained by secondary ion mass spectrometry and similar techniques, discussing the processes of ion generation involved.     

Determination of 2,4,6-trichloroanisole in wines by headspace solid-phase microextraction and gas chromatography-electron-capture detection

The retention behaviour of alkaline earth cations was studied as a function of changing composition of acidified ethylenediamine eluent. The multiple eluent species retention model developed for separation of calcium, magnesium and strontium ions was utilized for determination of selectivity coefficients for sample and eluent ions. The suggested model accurately describes and predicts retention of analytes under elution conditions [0.5-2.0 mM C2H4(NH2)2 and pH 4-6] which are of practical importance. The results in three-dimensional retention surface with species distribution graphs are demonstrated. Complexometric titrations and ion chromatography (IC) were compared for the analysis of calcium and magnesium ions. Statistical data indicated that there was no evidence for relative differences between the two methods. However, IC gives several advantages over volumetric method.     

Influence of Extruder Temperature and Screw Speed on Pretreatment of Corn Stover while Varying Enzymes and Their Ratios

Pretreatment is being the first and most expensive step, it has pervasive impacts on all other steps in overall conversion process. There are several pretreatment methods using physical, chemical, and biological principles which are under various stages of investigation. Extrusion can be used as one of the physical pretreatment methods towards biofuel production. The objective of this study was to evaluate the effect of barrel temperature and screw speed on sugar recovery from corn stover, to select a suitable enzyme combination and its ratio. Corn stover was pretreated in a single screw extruder with five screw speeds (25, 50, 75, 100, and 125 rpm) and five barrel temperatures (25, 50, 75, 100, and 125 °C). In order to select a suitable enzyme combination and ratio, different levels of cellulase and β-glucosidase, multienzyme complex and β-glucosidase were used during saccharification of pretreated corn stover. From the statistical analysis, it was found that screw speed and temperature had a significant effect on sugar recovery from corn stover. Higher glucose, xylose, and combined sugar recovery of 75, 49, and 61%, respectively, were recorded at 75 rpm and 125 °C. This pretreatment condition resulted in 2.0, 1.7, and 2.0 times higher than the control sample using 1:4 cellulase and β-glucosidase combination.     

Measuring nitrate concentration in wastewaters with high chloride content

The presence of chloride ions in wastewaters in concentrations above 50 mg/L poses interference in several methods used for the measurement of nitrate-nitrogen. The aim of this study was to characterise the reliability and costs of some commonly available methods for the analysis of nitrate concentration in landfill leachate which contains high chloride levels. To investigate the effect of chloride interference, several widely used methods [ion chromatography (IC), continuous flow analysis (CFA), the German standard method (DIN), cuvette test (CUV), standard addition method (SAM) and reflectometric test (REF)] were used to measure the nitrate concentration in synthetic solutions containing varying concentrations of chloride and nitrate-nitrogen. Nitrate recoveries of the various methods were found to decrease in the following rank order: CUV (>95%) > IC (>90%) > CFA (89%) > DIN (88%) > REF (70%) > SAM (<80%). In the second part of the study, the same methods were used to measure nitrate concentrations in samples of biologically nitrified landfill leachate with and without chloride elimination. For leachate samples without chloride elimination, CUV results were well correlated (linear regression) with IC results (slope = 1.02/R² = 0.99) but to lesser extents with results obtained by CFA (0.91/0.86), DIN (0.89/0.97) and REF (0.86/0.77), and not correlated with SAM (0.74/–1.3). The incurred measurement costs per sample (in Euros) for the methods were as follows: CFA (<0.1) < DIN (0.6) < REF (0.7) < SAM (3) < CUV (3.8) < IC (15). Cuvette tests are recommended as the method of choice due to their accuracy and lower cost than IC.     

离子色谱法同时测定化妆品中的铵和6种烷基胺

建立同时测定化妆品中铵和6种烷基胺的离子色谱(IC)分析方法。优化了色谱条件和样品前处理方法,样品经100 mmol/L乙酸-20%(v/v)乙腈溶液浸提,固相萃取(SPE)柱去除阴离子、中和氢离子后进样测定。考察了提取溶液的pH、有机溶剂和共存离子对测定结果的影响。分析方法的线性范围为0.3～15 mg/L,检出限为2.1～7.9 mg/kg,定量限为7～26 mg/kg。采用建立的分析方法测定了清洗、柔肤、祛斑、防晒、烫发、染发和育发类化妆品的加标回收率的范围在80.2%～109.2%之间,相对标准偏差(RSD)的范围为0.5%～3.1%。方法选择性好,灵敏度高,抗干扰强,用于实际样品测定结果准确。     

Rapid and efficient purification of cimetropium bromide and mifentidine drug metabolite mixtures derived from microsomal incubates for analysis by mass spectrometry.

A comparative study of the use of organic solvent extraction versus Sep-Pak C18 cartridges in the recovery and analysis of phase I (unconjugated) drug metabolites using mass spectrometry is presented. Standard mixtures of putative metabolites of the anticholinergic drug cimetropium bromide and the H2-antagonist mifentidine were purified from inactivated liver microsomal preparations using both methods, and subsequently the recovery of each compound was quantitated. In general, the percentage recovery and degree of purification were greater when using Sep-Pak C18 cartridges compared with organic solvent extraction. Even more efficient recovery was achieved when zinc sulphate precipitation of proteins in the liver microsomal mixtures was carried out prior to analysis. Also, the HPLC-grade solvents used in this study contained a variety of ultraviolet-inactive, hydrophobic components. This leads to problems of suppression in fast atom bombardment mass spectrometric analysis. Using Sep-Pak C18 cartridges directly prior to analysis by fast atom bombardment with single or tandem mass spectrometry leads to far superior mass spectral results compared with organic solvent extraction.     

Ligand Sensitized Flourometric Determination of Dysprosium(III) Ion Using Terephthalic Acid

Several trivalent lanthanide ions are known to exhibit excellent luminescence characteristics when they are coordinated with appropriate organic ligands. Various analytical methods have been developed to determine lanthanide ions or organic compounds by taking advantage of these luminescence characteristics. The luminescence enhancement of the lanthanide ions by complexation with organic ligands has been explained on the basis of a ligand to metal energy transfer process.