电感耦合等离子原子发射光谱法测定食品添加剂亮蓝中的杂质元素

采用硝酸和双氧水消解体系,使用电感耦合等离子体原子发射光谱仪（IcP-AEs）检测食品添加剂亮蓝中Ph、Mn、cr的含量。结果表明,方法的检出限为0．005～0．015p∥mL,回收率为95．30％～103．9％,RSD小于3．05％。该方法简便、快速、准确,适用于检测食品添加剂亮蓝中的杂质元素。     

Molecular absorption spectrophotometric method for the determination of phosphorus in biodiesel

A molecular absorption method is proposed for the determination of phosphorus in biodiesel. The samples are mineralized using an ashing procedure at 550 °C followed by dissolution of the residue. The analytical procedure is based on the formation of a blue molybdenum complex. 1-amino-2-naphthol-4-sulfonic acid is used as reducing agent. The method was applied to biodiesel samples prepared from soy, canola and sunflower oils and from bovine fat. The limit of detection is 0.57 mg P kg⁻¹ and the limit of quantification is 1.7 mg P kg⁻¹. The observed mean relative standard deviation is about 5%. The simplicity of the procedure added to its precision, accuracy and low cost suggest that it is an excellent option for the determination of phosphorus in biodiesel.     

电感耦合等离子发射光谱（ICP-AES）和原子吸收光谱（AAS）测定涂料中多种元素的比较研究

研究了电感耦合等离子发射光谱（ICP-AES）和原子吸收光谱（AAS）法测定涂料中多种元素的方法,对比了2种方法的检出限、精密度和准确度。试验表明,ICP-AES具有多元素快速测定,操作方便快捷、检出限低、精密度高和准确度好的特点。     

ICP-AES法测定手工奶皮中微量元素的含量

采用ICP-AES法同时测定手工奶皮中的微量元素,实验结果表明手工奶皮中人体必需的Zn、Mg、Mn、Fe、Ca等微量元素含量较高。测定方法简便、快速、省时、稳定性好,加标回收率在98.8～102.2%之间,相对标准偏差RSD〈0.99%,检出限≤0.009μg.L-1,准确度和精密度都很好。     

Entwicklung eines automatisierten Spuren–Matrix-Trennverfahrens für die Bestimmung von Spurenmetallen in hochreinem Titan und Titandioxid

Development of an Automated Trace-Matrix Separation Technique for the Determination of Trace Metals in Pure Titanium and Titaniumdioxide The determination of metal traces in pure titanium with ICP-AES or ICP-MS requires an effective trace-matrix separation technique to eliminate interferences. After digestion in HF and HNO₃ the traces can be separated from the matrix using a cation exchanger column. A computer controlled pumping system is used for the automatic control of the procedure of preconcentration, elution and determination. The method requires a minimum of chemical manipulation and reduces the risk of contamination by using only subboiled acids. Recovery rates of more than 90% and high precision are obtained for 16 analytes. For most of the elements detection limits in the range of 1 to 10 ng/g titanium can be achieved.     

Selective Ion Flotation Separation and Concentration of Ultra Trace Amounts of Bismuth Using Arsenazo III and Its Determination by Inductively Coupled Plasma-Atomic Emission Spectrometry

A rapid, selective, and highly sensitive froth flotation method for the separation and enrichment of ultra trace amounts of bismuth is developed. The bismuth-Arsenazo III complex is concentrated from 1000 mL of aqueous solution into the scum in the presence of cetyltrimethylammonium bromide (CTAB) as a cationic surfactant. The proposed procedure of pre-concentration is applied prior to the determination of bismuth using inductively coupled plasma–atomic emission spectrometry (ICP-AES). Effects of Arsenazo III concentration, pH, CTAB concentration, and foreign ions have been studied. The proposed method possesses a pre-concentration factor of 500 and a detection limit of 0.28 ng mL^?1.     

等离子体原子发射光谱法在金属矿石样品分析中的应用

随着国家对地质科学的重视,由分析矿物的组份来了解成矿规律、指导寻找有用矿床已成为地质科研课题的一个重要方向。因此,对矿物的分析测试方法提出了更高的要求,电感耦合等离子体原子发射光谱法因其具有操作简单、线性范围宽、检出限低、灵敏度高、精密度高、准确度好、基体干扰小、可同时测定多个元素等优点,广泛的应用于分析金属矿石样品中的元素。本文对ICP-AES法进行了概述,并对其在几种常见金属矿石样品分析中的应用进行了综述。     

A novel method for the determination of acid value of vegetable oils

The voltammetric behavior of naphthoquinone in the presence of free fatty acids (FFA) at the polypyrrole (PPy)‐modified electrode was investigated in an ethanol/1,2‐dichloroethane (3 : 1) solution containing 0.1 M LiClO₄. A well‐defined new reduction peak appeared at a more positive potential and was higher than that obtained at the bare Pt electrode. Based on the fact that the new reduction peak current showed a good correlation with the concentration of fatty acids, an electroanalytical method for the acid value (AV) of vegetable oils was developed using the PPy‐modified electrode in linear potential sweep voltammetry. The experimental parameters were optimized to obtain a sensitive voltammetric response in this work. A linear calibration graph was obtained in the concentration range of 5.0×10^–6–6×10^–3 M for FFA (R = 0.993), with a sensitivity of 2.41×10^–2 A L/mol and a detection limit of 1.2×10^–6 M (S/N = 3). Each assay of vegetable oil sample took about 80 s. The developed method is applied to the AV determination of six commercial vegetable oils. The results well agreed with those obtained by the titration method. Compared to the conventional titration method, the proposed method is superior in sensitivity and accuracy and requires a small amount of vegetable oil sample, with no pretreatment.     

ICP-AES法和AAS法测定涂料中多种元素的比较研究

研究了电感耦合等离子发射光谱(ICP-AES)法和原子吸收光谱(AAS)法测定涂料中多种元素,对比了两种方法的检出限、精密度和准确度。试验表明,ICP-AES具有多元素快速测定、操作方便快捷、检出限低、精密度高和准确度好的优点。     

ICP—AES法测定鱼油胶丸中的八种微量元素

用ICP－AES法测定鱼油胶丸中P、Ca、Fe、Zn、Pb、Cd、Mg、As等得量元素,考察了谱线干扰情况,在的分析条件下,各元素的加标回收率均在95％以上。     

微波消解-等离子体发射光谱法测定蒙药敖西根-18和哈日-嘎布日-10中的多种元素含量

采用HNO3∶H2O2(体积比2∶3)为溶样试剂,以微波消解和电感耦合等离子体原子发射光谱法(ICP-AES)联用,同时测定了蒙药敖西根-18和哈日-嘎布日-10中的铝、钛、汞、铜、铅、锌、镉、砷、钡、铁、磷、锡和钙元素的含量。结果表明,在最佳实验条件下,在0.3 g蒙药中各元素的回收率为97.5%～104.2%,RSD<2.1%,检出限介于0.015～10.2μg/L,该方法简便、迅速、准确度和精密度高,适用于蒙成药中这13种元素的同时测定。     

Voltammetric studies of a cobalt(II)-4-methylsalophen modified carbon-paste electrode and its application for the simultaneous determination of cysteine and ascorbic acid

A carbon-paste electrode (CPE) chemically modified with the cobalt(II)-4-methylsalophen (CoMSal) as a Schiff base complex was used as a highly sensitive and fairly selective electrochemical sensor for simultaneous determination of minor mounts of ascorbic acid (AA) and cysteine. This modified electrode shows very efficient electrocatalytic activity for anodic oxidation of both AA and cysteine via substantially decreasing of anodic overpotentials for both compounds. The mechanism of electrochemical oxidation of both AA and cysteine using CoMSal-modified electrode was thoroughly investigated by cyclic voltammetry and polarization studies. Results of cyclic voltammetry (CV) and differential pulse voltammetry (DPV) using this modified electrode show two well-resolved anodic waves for the oxidation of AA and cysteine, which makes it possible for simultaneous determination of both compounds. A linear range of 1 × 10⁻⁴ to 5 × 10⁻⁷ M for cysteine in a constant concentration of 1 × 10⁻⁴ M AA in buffered solution (as a background electrolyte) was obtained from DPV measurements using this electrode. The linear range, which is obtained for AA in the presence of 1 × 10⁻⁴ M cysteine, was in the range of 1 × 10⁻⁴ to 1 × 10⁻⁶ M. The modified electrode has good reproducibility (RSD ≤ 2.5%), low detection limit (sub-micromolar) and high sensitivity for the detection of both AA and cysteine with a very high stability in its voltammetric response. Differential pulse voltammetry using the modified electrode exhibited a reasonable recovery for a relatively wide concentration range of cysteine spiked to a synthetic human serum sample.     

Determination of partially hydrogenated terphenyls-based thermal heating fluid in vegetable oils by HPLC with fluorescence detection

An HPLC method for the determination of partially hydrogenated terphenyls-based thermal heating fluid, Therminol 66^™, in various vegetable oils is described. Direct analysis of palm olein showed that the 3- and 4-cyclohexylbiphenyl peaks of the Therminol 66^™ used in quantitative analysis co-eluted with other fluorescent peaks present naturally in the oil. However, those interfering peaks were readily removed after saponification of palm olein. The concentrations of the 3- and 4-cyclohexylbiphenyls of Therminol 66^™ were monitored by fluorescence detection at 257 (excitation) and 320 nm (emission). The calibration graph obtained by using the peak areas of the 3- and 4-cyclohexylbiphenyls against the concentrations of Therminol 66^™ was linear, with a correlation coefficient of 0.994. The limit of quantitation, using spiked palm olein, was as low as 0.2 μg/g. The coefficients of variation obtained from the intra- and interday studies obtained by using three spiked concentrations (0.2, 0.5, and 1.0 μg/g) were 1.76–6.43 and 3.77–10.4%, respectively. The mean recovery value obtained from sunflower, soybean, and canola oils was more than 88.7%.     

Automated cold vapour flow-injection analysis of mercury at high concentrations

Continuous-flow cold vapour- atomic fluorescence spectrometry is shown to be an extremely sensitive technique for the determination of mercury with detection limits typically below 0.01 μg l^-1. Linear calibration ranges were found to be at least four orders of magnitude (i.e. up to 0.1 mg l^-1). Samples with concentrations exceeding the linear range are susceptible to self-absorption, and may, in severe cases, cause carry-over problems between samples. The flow-injection approach has been utilized to extend the upper limit of the linear calibration range allowing determinations up to 10 mg l^-1 of mercury. A range of certified reference materials and zinc battery anodes have been successfully analysed with a minimal number of sample dilutions.     

Separation and direct detection of heavy lanthanides using new ion-exchange chromatography: fast Fourier transform continuous cyclic voltammetry system

In this study, possibilities of heavy lanthanides (Ho³⁺, Er³⁺, Tm³⁺, Yb³⁺, and Lu³⁺) separation on Nucleosil 100-5-SA, an ion-exchange column, was investigated. Separation of lanthanides was carried out using an isocratic program of α-hydroxyisobutyric acid (HIBA) eluent. Fast Fourier transform continuous cyclic voltammetry (FFT-CCV) at a gold microelectrode was used as the detection method. Simplicity, high precision and accuracy, time efficiency, and being economic are advantages of the developed technique in comparison with the previous reported ones. In addition, removal of oxygen from the test solution is not required, the detection limit is suitable and the technique is fast enough for determination of compounds in a wide variety of chromatographic methods. The waveform potential was continuously applied on an Au disk microelectrode (12.5 μm in radius). The influence of HIBA concentration as well as pH of eluent was optimized. The best performance of the method was obtained at pH of 4.0, scan rate of 30 V s⁻¹, accumulation potential of −300 mV, and accumulation time of 0.3 s. The proposed method displays a linear dynamic range of 140 and 18,000 μg L⁻¹ and a detection limit of 50 μg L⁻¹. Precision, inter-day precision, and accuracy of the assay were reported too. A comparative evaluation of heavy lanthanides distributed in a sophisticated monazite and xenotime minerals solutions was carried out using both FFT-CCV, and inductively coupled plasma-atomic emission spectrometry (ICP-AES).     

ICP-AES测定塑料中的锑铍钴钒

采用微波消解法对样品进行处理后,用ICP-AES法对锑铍钴钒进行测定。通过检出限的确定,精密度试验,回收率试验,验证了该方法具有快速、简便、准确的优点,适合用于塑料中锑铍钴钒的测定。     

微波消解-ICP-AES/ICP-MS测定南果梨中微量元素

采用HNO3和H2O2的混合溶剂作为消解液微波消解南果梨样品,电感耦合等离子体发射光谱法(ICP-AES)和电感耦合等离子体质谱法(ICP-MS)测定了南果梨中14种有益、有害微量元素Ca、Fe、K、Mg、P、Cu、B、Mn、Zn、Mo、Cr、Pb、Cd、As的含量.各元素标准曲线相关系数均大于0.999 3,标准偏差...     

ICP-AES法测定合金钢中Si

建立了一种简捷、实用的合金钢中硅的电感耦合等离子体原子发射光谱（ICP—AES）测定方法。对元素分析谱线、背景干扰校对溶液酸度等因素进行了研究,确定了最佳实验条件。精密度、回收率、检出限、标准样品分析对照均取得了满意的结果。     

Application of crosslinked chitosan in the analysis of ultratrace Mo(VI)

In this work, the adsorption properties of crosslinked chitosan for Mo(VI) were studied. The adsorption rate of Mo(VI) by CCTS was 97% at pH 3.0. Adsorption balance time, elution conditions, the effect of coexisting elements, and the adsorption mechanism were investigated. A novel method of ultratrace Mo(VI) preconcentration with CCTS and determination by graphite furnace atomic absorption spectrometry was found. The detection limit (3σ, n = 10) of the method was 0.040 μg L^?1, and the relative standard deviation was 2.98% at 1.00 μg L^?1. The method has been applied to the determination of Mo(VI) in environmental water samples, with satisfactory results. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 432–435, 2006     

ICP-AES光谱法测定钼产品中微量硅和铝

建立了一种简捷、实用的钼产品中硅和铝的电感耦合等离子体原子发射光谱（ICP-AES）测定方法。精密度、回收率、检出限、标准样品分析对照均取得了满意的结果。方法的检出限为DL=0.000 1%（质量分数）,Si和Al的回收率分别为98.5%~100.5%和99.5%~101.0%。