微波消解-火焰原子吸收法测定豌豆中微量元素锰、锌、铜、铁的含量

探讨了采用微波消解法处理样品,以FAAS法在同一体系中测定豌豆中微量元素锰、锌、铜、铁的方法,包括硝酸、过氧化氢的用量以及消化时间长短对实验的不同影响和在同一体系中锰、锌、铜、铁的彼此干扰情况。在选定的条件下,测得豌豆中锰、锌、铜、铁的含量分别为:锰10.05 mg/g、锌9.48 mg/g、铜3.06 mg/g、铁18.30 mg/g,回收率96.8%~98.9%。     

The Determination of Cadmium,Chromium, Copper,Nickel and Zinc in City Waste Incinerator Ash Using Inductively Coupled Plasma - Atomic Emission Spectrometry

Abstract

This study describes the determination of Cd, Cr, Cu, Ni and Zn in a sample of city waste incinerator ash distributed in 1983 by the European Community Bureau for Reference Materials (sample BCR No. 176) for certification. The sample treatment and the analysis procedure are discussed. The results obtained are evaluated and compared with the values which were later certified.     

Determination of Cadmium, Cobalt, Manganese, Copper, Nickel, and Chromium in Concentrated Solutions of Calcium Chloride by Electrothermal Atomic Absorption Spectrometry

A procedure is developed for the direct determination of Cd, Co, Cr, Cu, Mn, and Ni in concentrated solutions of calcium chloride by electrothermal atomic absorption spectrometry. Ascorbic and oxalic acids and magnesium nitrate were examined as chemical modifiers. Oxalic acid was found to be the best modifier. Although an atomic absorption spectrometer with a background correction system of relatively low efficiency (deuterium lamp) was used, the elements under study can be reliably determined in the presence of oxalic acid at concentrations of calcium chloride in the solution up to 6%. Because cadmium is evaporated before the major part of the given matrix, it can be determined without a modifier.     

Determination of Phytic Acid in Urine by ICP Atomic Emission Spectrometry.

Abstract

A method to determine phytic acid within urine in the range 0.15–2 mg/l is reported. The method is based on the ICP atomic emission spectrometric determination of phosphorus, after previous separation and concentration of phytic acid using the anionic resin AG1-X8. The method has been applied successfully to determine phytic acid in synthetic urine and human urine.     

电感耦合等离子体原子发射光谱同时测定不锈钢食用器皿铬、镍、镉溶出量

用4%醋酸溶液浸泡取自不锈钢食用器皿钢片样品,在室温条件下浸泡24h,将浸泡液按6:1浓缩.通过优化试验确定实验条件,用电感耦合等离子体发射光谱仪准确测定浸泡液中Cr、Ni、Cd的浓度.实验过程操作简单,多种元素同时测定节约试验时间.精密度试验和回收率试验说明该方法检测结果准确可靠.     

电感耦合等离子体发射光谱法测定镍钴锰氢氧化物中硫酸根含量的不确定度评定

采用电感耦合等离子体发射光谱法(ICP-OES)测定镍钴锰氢氧化物(三元正极材料NCM前驱体)中硫酸根含量.确定了适宜的测试条件,依据不确定度评定的方法,分析了不确定度来源、量化不确定度分量、计算检测结果的合成标准不确定度和扩展不确定度.结果表明,NCM前驱体中硫酸根的质量分数为2 709±88 mg/kg,样品加标回收率为97.5%～99.7%,相对标准偏差(RSD)为2.02%.方法简单、快速.     

Determination of Cesium and Selenium in Cultivated Mushrooms Using Radionuclide X-Ray Fluorescence Technique

Cesium and selenium intake of cultivated mushrooms (Agaricus bisporus), with these elements previously added to the culture medium, has been examined from the viewpoint of health- and environmental protection. The process of measuring has been carried out by the radionuclide X-ray fluorescence technique. Treattments of the elementary substance with Se salt appears to influence the Se content of the mushrooms to a significant extent. Cs intake is of considerable importance, as this element is accumulated by mushrooms.     

火焰原子吸收光谱法测定镍基高温合金中的镉

采用火焰原子吸收光谱法测定镍基高温合金中的镉,样品以硝酸-氢氟酸-水混合溶液(1+1+1)前处理,选择Cd 228.8nm为分析线进行测定,并通过标准加入法校正基体效应。考察了消解酸的选择,仪器工作参数的调整,基体和共存离子对镉测定的影响。结果表明,镍基高温合金中镉的检出限为0.088μg/g。加标回收率为94.1%～109%,结果的相对标准偏差(RSD,n=8)在0.54%～1.6%。方法操作简便、分析速度快、准确度好,适用于镉含量在0.0001%～0.001%的镍基高温合金中的测定。     

Determination of Manganese in Sludge,Alloy, and Soil by Tungsten Coil Atomic Emission Spectrometry

A tungsten coil atomic emission spectrometer (WCAES) was developed and evaluated for the determination of manganese in industrial sludge, alloy, and soil. The system employed a coil extracted from a 150 watts/15 volts commercial slide projector light bulb and a simple power supply that provided a constant current to the coil. The analytical signals were resolved and detected using a Czerny-Turner spectrometer and a charge coupled device. Three manganese emission lines were detected simultaneously. Using different emission lines, limits of detection for manganese varied from 0.54 to 0.65 milligram per liter, and relative standard deviations for manganese at 5 milligrams per liter varied from 5.9 to 8.5 percent (n = 10). Summation of the Mn signals improved the detection limit to 0.17 milligram per liter and decreased the relative standard deviation to 1.7 percent. Spectral interferences were observed in the presence of Al, Ca, K, and Na. The accuracy was determined using two certified reference materials, and the results obtained by WCAES were in agreement with those obtained by inductively coupled plasma-optical emission spectrometry at the 95 percent confidence level.     

火焰原子吸收光谱法测定芦荟中锰、铁、铜、锌、镍、钴

１　　引　　　　言芦荟作为药用和保健品越来越引起人们的重视。近年来人们将它作为良好的防癌、抗癌药品而食用。芦荟的主要成分为淡黄色结晶性甙,为芦荟大黄素甙,水解产生ｄ－阿拉伯胶糖、芦荟大黄素等。它有良好的抑菌作用,对表皮癣菌、星形奴卡氏菌等皮肤真菌均有不同的抑制作用。主治烧烫伤、肝经实热等症。还能治疗糖尿病、痔疾、中耳炎、减肥等多种疾病。是人们理想的保健品和药品。芦荟中的金属元素的分析,作者未见文献报道。本文用原子吸收光度法测定了３种芦荟中锰、锌、铜、铁、镍、钴的含量,得到了满意的结果。２　　实验…     

坩埚灰化-电感耦合等离子体原子发射光谱法测定催化油浆中微量钙、钠、铝、铁、镍、硅

目前,有不良商家为了追求经济效益,在减压渣油中掺入了一定比例的催化油浆,催化油浆中含有大量的铝、硅元素,容易造成装置炉管内及其余部位结焦,不利于装置长周期的运行。为了延长设备的使用寿命,需要建立方法来有效监测催化油浆中硅及铝等金属的含量。目前,油品中的微量元素常用的测定方法有原子吸收光谱法[1-3]、原子荧光光谱法[4]、紫外-可见分光光谱法[5-7]等。其中,电感耦合等离子体原子发射光谱法(ICP-AES)因具有多元素同时测定、线性范围宽、灵敏度高、基体效应小、精密度高、快速准确等特点在油品分析中得到广泛的应用[8-11]。本工作采用坩埚灰化-电感耦合等离子体原子发射光谱法同时测定催化油浆中6种非金属和金属元素含量,可为建立高效灵敏的日常生产检测方法提供依据。     

Investigation of Matrix Effects for Direct Determination of Trace Metals in Seawater Using Direct Sample Insertion -Inductively Coupled Plasma Atomic Emission Spectrometry

Direct sample insertion (DSI) technique is an alternative sample introduction method for inductively coupled plasma atomic emission spectrometry (ICP-AES). Sample introduction efficiency of the DSI technique is 100% versus 3-5% for pneumatic nebulization and 30-40% for ultrasonic nebulization. DSI also has the ability to handle small volume (μL) of solution and small quantity (mg) of solids with little or no sample pre-treatment.     

Trace Enrichment and Atomic Absorption Spectrometric Determination of Lead,Copper, Cadmium and Nickel in Drinking Water Samples by Use of an Activated Carbon Column

Abstract

A simple method for atomic absorption spectrometric determination of lead, copper, cadmium and nickel in drinking water samples after preconcentration by sorbing 1-(2-pyridylazo) 2-naphthol (PAN) complex of these metals on an activated carbon column has been established. The metal/PAN complexes were quantitatively retained on the activated carbon in the pH range 6-8. Metals retained on the activated carbon column were completely eluted with 2M HCl in acetone. This method was applied to the determination of lead, copper, cadmium and nickel in drinking water samples and good results were obtained (Recoveries >95%, relative standard deviations <7%, relative error <3%).     

以铁灯作光源-火焰原子吸收法测定饮用水中微量锰

探讨了以铁空心阴极灯作光源,火焰原子吸收法测定饮用水中微量锰。结果表明,本法相对标准偏差为4．12％,加标回收率为96．0％-99．7％,用本法对质控样进行测定和对比试验,结果令人满意,同时实现了一灯多用。     

以结晶紫与亚硝基R盐吸光光度法测定镍

在氨性（ＰＨ９－９．５）条件下，镍（Ⅱ）与结晶紫及亚硝基Ｒ盐反应形成紫色络合物，表观摩尔吸光系数ε５３６＝２．２９×１０＾５Ｌ，ｍｏｌ＾－１，镍浓度在０．０１２０ｍｇ／Ｌ范围内遵守比耳定律，组成摩尔比为Ｎｉ：ＣＶ：Ｒ＝１：２：１，本法快速，为光度测定微量镍的高灵敏方法之一，用于土壤、人发等试样中镍的测定、结果满意。     

On-Line Preconcentration and Determination of Cadmium, Cobalt and Nickel in Food Samples by Flame Atomic Absorption Spectrometry Using a New Functionalized Resin

A new chelating sorbent has been developed using Amberlite XAD-2 resin anchored with pyrocatechol through the –CH₂– group. This sorbent, characterised by elemental analysis and infrared (IR) spectra, was used as a packing material for a minicolumn in an on-line preconcentration system for cadmium, cobalt and nickel determination. Metal ions were sorbed in the minicolumn, from which it could be eluted directly to the nebulizer-burner system of the flame atomic absorption spectrometer (FAAS). Metals can be eluted from the minicolumn with 0.50 mol L⁻¹ HCl or HNO₃. The enrichment factors were 22 (Cd), 23 (Co) and 25 (Ni), for 60 s preconcentration time, and 44 (Cd), 40 (Co) and 48 (Ni), if 180 s preconcentration time was used. Under the optimum conditions, the procedure allowed the determination of cadmium, cobalt and nickel with detection limits of 0.27, 0.59 and 1.29 μg L⁻¹, respectively, when preconcentration periods of 180 s were used. The accuracy of the procedure was sufficient and evaluated by analysing certified reference materials. The method was applied to the analysis of food samples (black tea and rice flour).     

Determination of Trace Elements in Biological Fluids by Arc Atomic Emission Spectrometry

Journal of Analytical Chemistry - Determination of macro- and trace elements in various biological fluids, including saliva and blood serum, is widely used for medical diagnostics and assessment of...     

用N2O-C2H2火焰原子吸收光谱法测定羰基镍粉中钼含量

运用了N₂O-C₂H₂火焰原子吸收光谱法进行羰基镍粉钼含量的测定。介绍了钼最佳测定条件及呈良好线性范围的浓度.同时对样品消化处理条件及在测定中样品的干扰因素进行了综合考虑.该方法的相对标准偏差均小于1.0%(n=6),回收率均在97.0%～102.0%(n=6)之间.达到了实验室分析质量控制的要求.     

电感耦合等离子体原子发射光谱法测定钨铁中硅、锰、铜和磷的含量

钨铁常用作高温合金和各种工具钢、高速钢、热锻磨具钢等。钨元素是炼钢工艺中的添加剂,可以提高钢的蠕变强度,又是钢中碳化物的强促进剂。钨能增加钢的回火稳定性、红硬性、热强性以及形成特殊的碳化物而增加钢的耐磨性.     

同时萃取-火焰原子吸收光度法测定锂盐及某些盐中锰、铬、铜、锌、镉、铁、钴、镍和铅

本文系用二乙基二硫代氨基甲酸二乙铵(DEDTC)/甲基异丁基甲酮(MIBK)pH5.7萃取体系,预浓缩以后,用原子吸收法在RbCl、 CsCl、 Sr(NO_3)_2、H_3BO_3、NH_4NO_3、NaBr、KI、Li_2CO_3、NaCl、KCl、CaCl_2、MgO、BaCl_2、KH_2pO_4、KNaC_4H_4O_6、C_6H_6O_7等盐类中测定痕量的锰、铬、铜、锌、镉、铁、钴、镍、铅等九个元素,其中应用于前面七个样品是我们提出的。检出限为1×10~(-4)％,九个元素的回收率在93～106％之间,相对标准偏差(n=7)为2.7％。