Trace Elements in Lycium barbarum L. Leaves by Inductively Coupled Plasma Mass Spectrometry after Microwave Assisted Digestion and Multivariate Analysis

The concentrations of 14 elements in Lycium barbarum L. leaves collected from the Qaidam basin (China) were determined by inductively coupled plasma mass spectrometry after microwave assisted digestion. This work presents two goals: (1) to determine 14 elements in L. barbarum leaves; (2) to examine the relationship between elements using correlation analysis, principal component analysis, and cluster analysis. The accuracy and precision were verified against a GBW07605 Tea Leaves certified reference material. The results demonstrated that the method was reliable, reproducible, and suitable for determination of the concentrations of trace elements in L. barbarum leaves. Correlation analysis showed that aluminum–copper, arsenic–zinc, manganese–selenium, and chromium–iron have medium correlation coefficients. Principal component loading for L. barbarum leaves extracted seven components explained about 85% of the total variance. Cluster analysis depicts four clusters: (1) arsenic and titanium; (2) calcium, magnesium, manganese, selenium, and zinc; (3) cobalt, iron, and molybdenum; (4) aluminum, copper, and chromium.     

微波消解-火焰原子吸收光谱法测定下火药材中的微量元素

微波消解样品,火焰原子吸收光谱法测定下火药材中5种微量元素的含量。菊花中钙、镁、铁、锌、锰的含量分别为15.80,31.42,7.68,0.935,0.105g/kg;桑叶中钙、镁、铁、锌、锰的含量分别为195.6,33.69,7.02,0.839,2.21g/kg;夏枯草中钙、镁、铁、锌、锰的含量分别为110.9,38.69,14.75,1.24,0.112g/kg。该方法加标回收率在90.1%—106.3%之间,方法简单、灵敏、准确,可为下火药材的基础研究提供依据。     

汉中元胡中8种金属元素含量的测定

采用微波消解-火焰原子吸收光谱法对汉中元胡中钾、钙、钠、镁、锌、锰、铜、铁8种金属元素的含量进行测试,测得结果分别为K（2033.97mg/kg）、Ca（600.87mg/kg）、Na（1395.55 mg/kg）、Mg（494.88mg/kg）、Zn（220.36mg/kg）、Mn（107.75mg/kg）、Cu（39.68mg/kg）、Fe（2462.79mg/kg）。相对标准偏差的范围为0.0356%—4.4288%,回收率的范围为96.8%—101.2%。微波消解-火焰原子吸收光谱法是一种简便而又灵敏的测定中草药中微量元素的方法。     

ICP-AES测定土壤中钡、铬和锰含量的不确定度评定

电感耦合等离子体-原子发射光谱法(ICP-AES)测定土壤中钡、铬和锰含量的不确定度主要来源于样品称量、样品消解液定容体积和测定样品消解液中各元素的浓度,对这些分量进行了量化计算。土壤中钡、铬和锰的质量分数可分别表示为218.5±17.1,342.5±40.4,1468.9±47.1mg/kg。影响各元素含量测量不确定度的主要因素是测量样品消解液中各元素的浓度引起的不确定度。     

微波消解-火焰原子吸收光谱法测定彝药毒清药中微量元素

建立火焰原子吸收光谱法测定＂毒清药＂中钙、镁、铁、锌、铜、锰元素含量的方法。用浓硝酸微波消解样品,采用校准曲线法测定。结果显示毒清药中含有Ca9.07mg/g,Mg3.56mg/g,Fe2.11mg/g,Zn0.070mg/g,Cu0.022mg/g,Mn0.61mg/g。RSD为3.1%—9.6%,回收率为94%—105%。此方法简单、准确,结果令人满意。     

Anomalous magnetic behaviour of zinc and chromium ferrites without any hyperfine splitting

Two groups of ferrite namely zinc ferrite and chromium ferrite were synthesized by citrate precursor route in the size range of 8 to 35 nm. We have studied the structural and magnetic behaviour of these ferrites using X-ray diffraction (XRD), vibrating sample magnetometer (VSM) and Mössbauer spectroscopic techniques. Our studies show that the nanocrystalline ferrites interact with the hand magnet strongly and give large magnetization in the VSM measurement. The maximum magnetization in the samples sensitively depends on the particle size of synthesized ferrites. We observed as large as 28 Am²/kg of magnetization in the zinc ferrite nanoparticles while that in chromium ferrite is around 11 Am²/kg. In spite of the large magnetization in the zinc ferrite nanoparticles we did not observe any hyperfine splitting even down to 12 K of temperature. Similar behaviour is also observed for chromium ferrite down to 16 K.     

光谱法分析研究新疆瓜果微量元素含量

利用原子吸收法和原子发射法对新疆十一类瓜果八种微量元素进行检测,并与中国生物标准进行比较分析。 结果发现,新疆和田地区苹果含锌66.75 mg·kg-1、含钾819.2 mg·kg-1、含锰4.657 mg·kg-1,大枣含锶8.62 mg·kg-1;新疆库尔勒地区石榴含钾687 mg·kg-1;新疆哈密地区大枣锰、锌、锶、钙、铁、镍和钾七种微量元素含量均高出各相应的中国生物标准;在十一类瓜果中铜元素含量均低于中国生物标准;八种微量元素含量平均值在新疆库尔勒石榴、新疆和田苹果、新疆哈密大枣中表现很高（分别为91.82, 121.5, 275.3 mg·kg-1）;在新疆五家渠种植的西瓜中八种微量元素表现出果皮中平均含量（54.19 mg·kg-1)是瓤中平均含量(48.69 mg·kg-1)的1.11倍。其研究结果对新疆瓜果营养成分研究提供科学的基础数据。     

Effect of Metallic Salts of Malonic Acid on the Formation of β Crystalline Form in Isotactic Polypropylene

The effects of malonic acid and the lithium, sodium, potassium, zinc, magnesium, calcium, strontium, and barium salts of malonic acid on the formation of β crystalline form in isotactic polypropylene at the crystallization temperatures 120 and 130°C have been investigated. It was found that malonic acid and the lithium, sodium, and potassium salts of malonic acid inhibit the formation of β crystalline form in polypropylene. Zinc malonate has a limited positive effect on the formation of β crystalline form, while magnesium, calcium, strontium, and barium salts are β nucleating agents, in descending order. The decreased β nucleation abilities of the alkaline earth metallic salts of malonic acid are attributed to the increasing atomic radii of the combined metals and decreasing crystallization temperatures.     

原子吸收光谱法测定清热解毒类中草药中的11种微量元素

采用灰化法处理样品,HNO₃溶解灰化残渣,用火焰原子吸收光谱法测定了射干、白头翁、山豆根、鱼腥草、连翘、大青叶、车前草、野菊花、金银花、莲子芯、蒲公英、板兰根等20种中草药中的Ca,Mg,Mn,Cu,Fe,Zn,Cd,Pb,Co,Ni和Cr共11种微量元素。结果表明：清热解毒中草药中含有丰富的Ca,Mg,Fe,Zn,Mn和Cu等对人体有益的微量元素;加标回收率90％～110％。     

Online Copper Removal for Selenium Determination by Hydride Generation–Inductively Coupled Plasma Optical Emission Spectrometry

Abstract

Selenium determination in samples with a high copper content by hydride generation–inductively coupled plasma optical emission spectrometry (HG‐ICP‐OES) after online copper removal and selenium (VI) reduction is described. An activated carbon minicolumn was used for the retention of copper and its subsequent separation of Se. Se(VI) was then online reduced by heating into a PTFE coiled reactor with 12 M HCl. The analyte was introduced into a water stream containing sodium tetrahydroborate (NaBH₄) in order to generate selenium hydride (H₂Se). The detection limit (DL) obtained was 0.8 µg L^?1, and the precision, expressed by the relative standard deviation (RSD), was 2.5% (n=10; 10 µg L^?1 selenium level). The current method was applied to the Se determination in two copper reference materials, MBH‐39DK 3601 (with a Se content of 90 mg kg^?1) and MBH‐39 DK 3604 (with a Se content of 15 mg kg^?1).     

Determination of macronutrients,micronutrients, non-essential elements in milk based-infant formulas by atomic absorption and inductively coupled plasma-optical emission spectroscopy after microwave and ultrasound assisted digestion

Microwave and ultrasound procedures for samples preparations were adopted and the elements were determined by validated flame atomic absorption and inductively coupled plasma–optical emission spectrometry. Student’s t-test was established whether there was a difference between the sample preparation methods. Trueness of certified values by all methods was ensured which were not differing significantly at 95% level of confidence interval. The highest intensity ratio of magnesium (II)/magnesium (I) was obtained at 1120 radiofrequency value to achieve accurate and reproducible results by inductively coupled plasma–optical emission spectrometry. The value of corresponding correlation coefficient (r²) were obtained as >0.990 indicating the excellent linearity for concentration range chosen for each element to be determined in commercial samples. Results showed that concentrations of calcium, magnesium, potassium, sodium, chromium, copper, iron, manganese, selenium, and zinc found in commercially available products are in good agreement with label as declared by the manufacturers. Exposure to aluminum, cadmium, and lead from consumption of products under evaluation was estimated and it was in compliance with permissible level suggested by European Commission regulations. Regarding the food safety monitoring, the proposed methods are rapid and met green chemistry approach so that can be implemented in laboratories easily for routine analysis.     

ICP-MS测定章松八味沉香散中的微量元素

采用电感耦合等离子体-质谱法（ICP-MS）分析藏药章松八味沉香散中铬、钴、铜、锰、锌、钼、铁、镍等8种微量元素的含量,其中铁、铜、镍、锰含量较高,其他元素含量较低,藏药章松八味沉香散中元素的分布特点与章松八味沉香散具有消心热、宁心安神、行气降压之功效有关,为现代用药提供了参考数据。     

Rapid analysis on the heavy metal content of spent zinc–manganese batteries by laser-induced breakdown spectroscopy

Laser-induced breakdown spectroscopy (LIBS) technique was used to investigate the applicability for the rapid analysis on the heavy metals in spent Zn–Mn batteries. Besides the major elements carbon and zinc, a number of minor and trace elements, such as iron, manganese, vanadium, chromium, aluminum, silicon, calcium, copper, magnesium and lead were identified in the positive and negative electrode materials, and their concentrations were determined. It was found that the concentrations of heavy metals of vanadium, vanadium, manganese, zinc, iron and copper were high in the mixture of positive electrode material, while zinc and lead had high concentration in the negative electrode material. These heavy metals are of a great harm to the environment and human health.     

Lead-free BFN ceramics doped by chromium,lithium or manganese

The material of the study was lead-free BaFe_0.5Nb_0.5O₃ ceramics subject to modification. The base composition BaFe_0.5Nb_0.5O₃ as well as the chromium, lithium and manganese modified ones were obtained using conventional mixed oxides and carbonates method. Synthesis was performed by the powder calcination method at high temperature 1250 °C for 4 h, while the densification was carried out by free sintering method under conditions 1350 °C/4 h. The paper presents a complex study of admixtures influence on the crystal structure, microstructure and dielectric properties of the BFN type samples. The mentioned dopants chromium, lithium or manganese in the BFN-type ceramics among other caused the reduction of the electric permittivity maximum as well as significant decrease in value of dielectric loss.     

Application of extraction induced by emulsion breaking for trace multi-element determination in jet fuel by inductively coupled plasma-mass spectrometry

ABSTRACT

A novel method, based on extraction induced by emulsion breaking, is proposed for rapid simultaneous determination of iron, manganese, copper, and zinc in jet fuel by inductively coupled plasma-mass spectrometry. Several parameters affecting the extraction efficiency were investigated including the concentrations of nitric acid and emulsifying agents, centrifugal speed, and extraction time. The limits of detection for iron, manganese, copper, and zinc were 0.116, 0.028, 0.06, and 0.085 µg L^?1, respectively. The accuracy of the method was tested by the analysis of spiked samples (recovery percentages between 90% and 107% were observed) and by comparison with a well-established method.     

Determination of Microamounts of Proteins by Resonance Light Scattering with Copper Phthalocyanine Tetrasulfonic Acid

Abstract

Based on the strong enhancement effect of proteins on the resonance light scattering of copper phthalocyanine tetrasulfonic acid, a method for the determination of microamounts of proteins has been developed. Under the experimental conditions (2.0×10^?6 mol/L copper phthalocyanine tetrasulfonic acid, pH 2.60, ionic strength 0.001 mol/L NaCl), the linear range of this assay is 0.06–4.0 µg/mL for bovine serum albumin (BSA), 0.1–2.0 µg/mL for human serum albumin (HSA), 0.0–2.0 µg/mL for human γ‐IgG, and 0.2–6.0 µg/mL for ovalbumin. The detection limits (3δ) are 16.8 ng/mL for BSA, 23.4 ng/mL for HSA, 37.6 ng/mL for human γ‐IgG, and 48.3 ng/mL for ovalbumin, respectively. This method has been applied to the analysis of total proteins in human serum samples collected from the hospital, and the results were in good agreement with those reported by the hospital.     

Sub‐ppm determination of Hg and Cr in water: Cr speciation

A sensitive and alternative analytical procedure for the determination of chromium and mercury content in natural waters by coprecipitation with APDC and determination using an absolute thin layer EDXRF method is described. The use of ¹⁰⁹Cd and ²³⁸Pu annular radioisotope sources, the influence of the chromium oxidation states and the elemental concentration were studied. At pH 4, 100% recovery was found for mercury. The coprecipitation of Cr(VI) was not quantitative (75%) but constant for the selected concentration range (5–100 µg/l). On the other hand, Cr(III) did not precipitate at the same pH. The relative standard deviations (RSD) were lower than 9.0% for mercury (10 µg/l) and 5.0% for chromium (50 µg/l). The detection limits (DLs) for mercury and chromium were 0.4 and 0.6 µg/l when the ²³⁸Pu source was employed. Nevertheless, higher DL values were achieved using ¹⁰⁹Cd (0.6 and 3.3 µg/l). The proposed method was applied to the analysis of surface water samples. An alternative and simple chromium speciation procedure without chemical separation of Cr species is recommended. Copyright © 2007 John Wiley & Sons, Ltd.     

原子吸收光谱法测定抗肿瘤中成药中微量元素

利用原子吸收光谱法测定了复方天仙胶囊、消癌平片、参灵蓝胶囊、至灵胶囊和参莲胶囊5种抗肿瘤中成药中的15种微量元素。详细讨论了消化液(混酸)种类、混酸比例、消化时间及消化液体积对测定结果的影响。结果表明：5种抗癌中成药中,Ca,Mg,K,Na,Fe,Zn,Mn,Co和Ni的含量较为丰富。     

微波消解ICP-MS测定尿样中硒及其他重金属元素

建立微波消解电感耦合等离子体-质谱法(ICP-MS)同时测定尿样中硒及铬、镉、砷、铅、锰、钴、镍、铜、锌10种重金属元素的方法。采用硝酸-过氧化氢消解体系,微波消解法制备样品.以铟、铋为内标物质,直接用ICP-MS测定上述10种元素。所测10种元素的检出限为0.006-0.073μg/L,校准曲线线性关系好(r>0.9999),相对标准偏差(RSD)均小于3%,对尿样标准物质的测定值均在标准参考值范围内。应用微波消解ICP-MS分析尿样,方便快捷,灵敏度高,检出限低,重现性好,是理想的生物样本检删分析方法。     

Determination of Trace Amounts of Zinc in Welding Fumes by Flow‐Injection Flame Atomic Absorption Spectrometry

A flow‐injection flame atomic absorption spectrometric method for the determination of zinc in welding fumes has been developed. The method is based on the continuous ultrasound‐assisted dissolution of the zinc oxide collected on the air filter. Variables such as sonication time, nature and concentration of the acid solution used as dissolving solution, dissolution temperature, flow rate of the continuous manifold, and dissolving solution volume were simultaneously studied by applying a Plackett–Burman design. Results showed that only the concentration of nitric acid solution used as dissolving solution was a statistically significant variable (confidence interval of 95%). Factors such as dissolution temperature and sonication time were finally optimized by using a central composite design. The detection limit was 1.1 µg/m³ and the repeatability of the overall method is 1.6% (n=11) for a zinc concentration of 75.4 µg/m³. The proposed method was applied to the determination of zinc in welders' workplace environments.