火焰原子吸收光谱法测定赣南脐橙中6种微量元素含量

将赣南脐橙经硝酸和高氯酸消化后，在样品中加入氯化镧作为释放剂以消除共存离子的干扰，采用火焰原子吸收光谱法测定了Ca、Mn、Zn、Fe、Cu和Pb元素的含量。结果表明，标准加入法的回收率为．96．58％～104．31％，10次平行测定结果的相对标准偏差RSD均小于2％。该法灵敏度高、操作简便快速，结果准确，重现性好。可见赣南脐橙中各元素含量差异显著，其中ca的含量比较丰富，Mn、Fe和zn的含量中等，含有人体必需的微量元素，而对身体有害的元素如P11含量却相当低，这说明赣南脐橙具有一定的药用和经济价值，为进一步探讨赣南脐橙开发利用提供实际依据。     

Investigation of artifacts caused by deuterium background correction in the determination of phosphorus by electrothermal atomization using high-resolution continuum source atomic absorption spectrometry

The artifacts created in the measurement of phosphorus at the 213.6-nm non-resonance line by electrothermal atomic absorption spectrometry using line source atomic absorption spectrometry (LS AAS) and deuterium lamp background correction (D₂ BC) have been investigated using high-resolution continuum source atomic absorption spectrometry (HR-CS AAS). The absorbance signals and the analytical curves obtained by LS AAS without and with D₂ BC, and with HR-CS AAS without and with automatic correction for continuous background absorption, and also with least-squares background correction for molecular absorption with rotational fine structure were compared. The molecular absorption due to the suboxide PO that exhibits pronounced fine structure could not be corrected by the D₂ BC system, causing significant overcorrection. Among the investigated chemical modifiers, NaF, La, Pd and Pd + Ca, the Pd modifier resulted in the best agreement of the results obtained with LS AAS and HR-CS AAS. However, a 15% to 100% higher sensitivity, expressed as slope of the analytical curve, was obtained for LS AAS compared to HR-CS AAS, depending on the modifier. Although no final proof could be found, the most likely explanation is that this artifact is caused by a yet unidentified phosphorus species that causes a spectrally continuous absorption, which is corrected without problems by HR-CS AAS, but which is not recognized and corrected by the D₂ BC system of LS AAS.     

Determination of minor, trace and toxic elements in chewing tobacco products by instrumental neutron activation analysis and identification of glutamic acid

Tobacco smoking/chewing has been a cause of concern because of it being related with oral cancer. It causes stimulation and ill physiological effects. Ten different brands of spit tobacco, eight gutkaas and five paan masalas have been analyzed for seven minor (Al, Na, K, Ca, Cl, Mg, and P) and 17 trace (As, Ba, Br, Co, Cr, Cs, Cu, Eu, Fe, Hg, La, Mn, Rb, Sb, Sc, Th, and Zn) elements by instrumental neutron activation analysis. Also Ni and Pb were determined by atomic absorption spectrophotometry. Concentration of Cd was below detection limit (<10?mg?kg^?1) in the tobacco samples. Mg, generally added as MgCO₃ to prevent caking, is present as minor constituent in spit tobacco and gutkaas but is below detection limit (<1?g?kg^?1) in paan masalas. Most elemental concentrations vary in a wide range depending on the nature of chewing tobacco. Spit tobacco has been found to be more enriched in essential elements (Ca, K, Na, P, Mn, and Rb), whereas gutkaas contain higher concentrations of Fe, Cr, Cu, and Zn. Paan masalas contain lower contents of other elements but higher content of Hg. Gutkaas also contain higher amounts of As and Pb. Further glutamic acid has been separated from tobacco leaves and characterized as it might bind with some elements.     

电感耦合等离子体原子发射光谱法测定黄铜中主、次量元素

提出了电感耦合等离子体原子发射光谱法同时测定黄铜中铜和锌等主量元素,镍、铅、铝、锡、铁、锰、磷和钴等次量元素的分析方法。选择了各元素的分析谱线,运用干扰元素系数法校正光谱干扰,用内标校正和同步背景校正消除基体影响。各元素的质量分数均在一定的范围内与其信号强度呈线性关系。方法用于分析两个铜合金样品,测定结果与光电直读光谱法、化学法的测定值一致;用于分析3种铜合金标准样品,测定值与标准值相一致。     

Submicro Determination of Copper and Zinc in Needle Biopsy-Sized Cardiac and Skeletal Muscles by Atomic Absorption Spectroscopy Using Stoichiometric Air-Acetylene Flame

Abstract

A highly sensitive and rapid procedure is described for submicro quantitation of copper and zinc contents from the nitric acid extract of fat free-dry-tissue (FFDT) by a double beam atomic absorption spectrophotometer using stoichiometric air-acetylene flame. Simultaneous background correction was afforded with a deuterium lamp for Zn analysis to eliminate interferences from non-atomic absorption at 213.9 nm. Cu and Zn standards, as well as the muscle extracts, were prepared in an aqueous medium containing 0.75 M Ultrex quality HNO₃ for spectral analysis which did not quench or enhance the relevant absorbance signals. Inherent mineral constituents of muscle such as Ca, Mg, Na, K, and P, when added upto ～10-60 fold greater than the physiological concentration, did not cause either analytical or chemical interferences. Muscle specimens weighing between 0.8-12.0 mg FFDT were extracted in 5 ml of 0.75 M HNO₃ and directly aspirated into the flame. Muscle Cu and Zn contents were expressed in mg/kg FFDT. The smallest sample size confidently analyzed using this technique was ～0.4 mg FFDT which corresponds to 2.0 mg of fresh tissue and can be safely obtained from a patient by muscle needle biopsy. Recovery studies from the inherent muscle matrix revealed 100.01 ± 0.399 and 99.64 ± 0.13% precisions for Cu and Zn respectively.     

The determination of trace metals in mineral waters : Part I. Atomic Absorption Spectrometric Determination of Cd,Co, Cr,Cu, Ni and Pb by Electrothermal Atomization After Concentration by Co-precipitation

Procedures based on flameless atomic absorption spectrometry are described for the determination of Cd, Co, Cr, Cu, Ni and Pb in mineral waters. Because of matrix effects and the inadequate detection limits for direct determinations, the metals are separated from the macrocomponents by precipitation of their tetramethylenedithiocarbamates with iron(III) as collector, or by co-precipitation on Fe(OH)₃. The detection limits are 0.005, 0.3, 0.08. 0.10, 2 and 0.10 μg l^- for Cd, Co, Cr, Cu, Ni and Pb, respectively, and are satisfactory for the determination of these elements in mineral waters. The precision is 2–7%.     

Background correction in frequency modulated simultaneous atomic absorption spectrometry

Summary For a long time simultaneous multielement determination by AAS has been a subject of intensive research. In this work a simultaneous multielement atomic absorption spectrometry method is described in a special new arrangement, called frequency modulated simultaneous AAS (FremsAAS), using fiberoptics, interference filters and frequency modulation and demodulation by lock-in amplifiers as main devices. Purpose of this work was to equip the FremsAAS with a D₂-background correction and to test it with certified reference materials. Mn, Cd, Pb, Cu, Ni, Cr and Zn had been determined simultaneously (three at a time) in sewage sludge (BCR/CRM 146), estuarine sediment (BCR/CRM 277) and phosphate rock (BCR/CRM 32) with good feasibility. Frequency modulated simultaneous AAS with background correction (FremsAASUK) represents an interesting alternative to known instruments.Dedicated to Prof. Dr. V. Krivan on the occasion of his 60th birthday     

Analysis of standard reference materials after microwave-oven digestion in open vessels using graphite furnace atomic absorption spectrophotometry and Zeeman-effect background correction

Summary Heating-covered teflon digestion vials located inside a reheatable container in the presence of different acid mixtures with microwave oven dissolve the metals from biological and environmental certified reference materials. Pb, Cd, Cu, Mn and Fe from the dissolved samples are determined by graphite furnace atomic absorption spectrophotometry and Zeeman-effect background correction. The method allows the treatment of about 100 samples per operation.     

Comparison of the Results of Atomic Absorption and X-ray Fluorescence Analysis of Metals in Atmospheric Aerosols

Factors responsible for the systematic discrepancies between the results of atomic absorption (standard procedure) and X-ray fluorescence determination of metals in atmospheric aerosols preconcentrated on a filter were studied. Patterns describing the errors in the results of determining Fe, Cu, Pb, Zn, Mn, and Cr by the proposed procedures depending on the type of the metal compound and the concentration of SiO₂ in aerosol particles were found. It was shown that the underestimation of the results of atomic absorption analysis in comparison to those obtained by X-ray fluorescence is due to the incomplete decomposition of some analyte compounds and the adsorption of Fe, Cu, and Pb on the precipitated SiO₂.     

原子吸收光谱法测定水中重金属镍的干扰研究进展

讨论了影响原子吸收光谱法测定水中镍元素的干扰因素及消除或抑制的方法,并展望了光谱干扰中背景校正技术和原子吸收仪器的发展前景.     

An integrated approach to the complete chemical analysis of magnesium or sodium diuranate (yellow cake) sample

A procedure for the complete chemical analysis of magnesium or sodium diuranate (yellow cake) sample is reported. Uranium is determined gravimetrically after peroxide precipitation. Optimum parameters, such as pH, quantity of hydrogen peroxide, volume of sample, temperature and complexing agent for quantitave precipitation of uranium, and effective separation of other elements were studied. Aluminum, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, and Zn were determined by flame atomic absorption spectrometer and B, Mo, SO₄, REEs and Y by inductively coupled plasma atomic emission spectrometer in the filtrates of hydroxide and peroxide precipitation separation. The proposed method is accurate and the precision is characterized by an RSD of ~0.2% for U; 2 to 6% for Mg, Na, K, Ca, Fe, SiO₂, Al, Cd, Co, Cr, Fe, Mn, Ni, Pb, and Zn and 3 to7% for REEs, Y, Mo and B     

Investigation of the influence of interfering elements on the determination of palladium in copper ores by graphite furnace atomic absorption spectrometry

Palladium contents in copper ores and copper ore concentrates at the part per billion (ppb) concentration levels have been determined after separation by extraction with dimethylglyoxime into chloroform. The influence of elements present in the extracts (Cu, Fe, Pb) on palladium absorbance signals when using a THGA graphite furnace with Zeeman background correction has been examined. It has been found that with the recommended temperature programme (T_pyr=1100°C, T_at=2200°C) Pb and Fe together influence the readings of Pd 247.642 nm through background overcorrection due to the Pb 247.638-nm line. This interference can be eliminated by increasing the pyrolysis temperature to 1200°C thus removing all Pb before the atomization step. In the presence of Cu (2.5–40 mg l⁻¹) and Fe (5–1000 mg l⁻¹) in the analysed solution no influence on the determination of palladium has been observed.     

Polarized Zeeman effect atomic absorption spectrophotometry using a flame atomizer

A static magnetic field at 10 kG$\text{\$}\text{?}$was applied to a 10cm laminar flame produced by a premix type burner, and absorptions were observed for the polarized components of the radiation from a hollow cathode lamp. The dynamic range of the measurement was 10⁴–10⁵ for typical elements.The results showed that (1) the optimal conditions for double beam measurement and accurate correction of background absorption are achieved at the same time, (2) even if the flame conditions and the light intensity are changed, the baseline is not shifted, (3) the flame fluctuation noise and the lamp flicker noise are reduced, and (4) background absorption is corrected exactly at the same wavelength as the atomic absorption line.We thus concluded that the feasibility of flame atomic absorption spectrophotometry is much improved with this technique.     

Particle Size Determination of Trace Elements in Urban Air

Abstract

Airborne urban particulate matter was collected and fractionated according to size by cascade impactors. The elements zinc, cadmium, copper and lead on each size fraction were analyzed by anodic stripping voltammetry. The elements aluminum, iron, manganese, calcium and magnesium were analyzed by atomic absorption spectrophotometry. The data showed three different classes of particle size distribution for these nine elements. Lead and cadmium belonged to the first class with more than 70 % of the total collected element associated with particles having aerodynamic diameters below 0.5 micron. The calculated average mass median equivalent diameter (MMD) of cadmium and lead was approx. 0.1 micron. In the second class about 60% of the elements Zn, Cu, Mg and Fe was associated with particles smaller than 0.5 micron. The average MMD's for these elements were between 0.3 and 0.4 micron. For the elements Al, Ca and Mn about 50% of the metal was associated with particles smaller than 0.5 micron and the MMD's were between 0.5 and 0.6 micron. Examination of elemental ratios (using Al as a reference element) showed that Pb and Cd were about 1000 times more concentrated in atmospheric particulate matter than in average crustal material and that in general the Pb/Al and Cd/Al ratios are inversely proportional to particle size. The Zn/Al and Cu/Al ratios of atmospheric partides were age or less independent of particle size and approx. 20 times higher than these same ratios in average crustal material. The ratios Fe/Al, Mn/AI, Ca/M and Mg/AI in all sizes of particulate matter were essentially identical to the same ratios in average crustal material.     

Spectral interferences in the determination of trace elements in environmental materials by inductively coupled plasma atomic emission spectrometry

This paper deals with spectral interferences in inductively coupled plasma atomic emission spectrometry (ICP-AES) encountered with environmental materials. These samples normally contain high concentrations of aluminium, calcium, magnesium, iron, titanium, potassium and sodium. The investigations cover: (a) spectral data for Al, Ca, Mg, Fe, Ti, K and Na as interferents for 200 pm wide windows centred (±100 pm) around the prominent lines of As, B, Ba, Be, Cd, Cr, Cu, Hg, Mn, P, Pb, Sb, Se, Sn, Tl, U and Zn; (b) a data base of Q-values for line interference [Q_Ij(λ_a)] and Q-values for wing background interference [Q_Wj(Δλ_a)] for two values of the excitation temperature 6200 K and 7200 K. The lines free or negligibly influenced by line interference were selected for analyte determination. Q-values were used for calculation of correction factors under a spectral line without the measurement of a reference blank at the wavelength of the prominent analysis lines. The accuracy of ICP-AES with the Q-concept as a basic methodology is checked by the analysis of a certified reference material IAEA/Sediment SD-N-1/2/. The precision of the method is characterised by an RSD of 0.6–1.7%. Extraction of trace elements soluble in aqua regia was used as a decomposition method. This article is an electronic publication in Spectrochimica Acta Electronica (SAE), a section of Spectrochimica Acta, Part B (SAB). The hardcopy text is accompanied by an electronic archive, stored on the SAE homepage at http://www.elsevier.nl/locate/sabe. The archive contains the tabular material of this article in electronic form.     

Chelating resins for the concentration of trace elements from sea water and their analytical use in conjunction with atomic absorption spectrophotometry

An investigation has been made of the uptake of trace elements from both distilled water and sea water by the chelating ion-exchange resins Chelex-100 and Permutit S1005. The resins retained the following elements with an efficiency of ca. 100%: Ag, Bi, Cd, Cu, In, Pb, Mo, Ni, rare earths, Re (90% only), Sc, Th, W, V, Y and Zn. Manganese was retained quantitatively only by the Chelex resin. The following elements are removed with 100% efficiency by means of₂N mineral acids: Bi, Cd, Co, Cu, In, Ni, Pb, rare earths, Sc, Th, Y and Zn. Ammonia (4 N) completely removes molybdenum, tungsten, vanadium and rhenium. The resins have been used in conjunction with atomic absorption spectrophotometry for the simultaneous determination of zinc, cadmium, copper, nickel and cobalt in sea waters.     

藏药材铁棒锤的微量元素含量分析

目的研究藏药材铁棒锤的微量元素含量。方法使用电感耦合等离子体质谱仪(ICPMS)测定藏药材铁棒锤药材中As、Hg、Pb、Cd含量,使用原子吸收光谱仪(火焰法、石墨炉法)测定药材中Zn、Mn、Cr、Fe、Ca、K、Cu元素的含量并进行分析。结果铁棒锤中有害元素As、Hg、Pb、Cd含量较低,Cu、Fe等有益元素含量较高。结论藏药材铁棒锤有丰富的微量元素,具有较高的开发利用价值。     

新型原子吸收背景校正装置的研制

本文研制了一种新的原子吸收背景校正装置,将自吸效应校正背景吸收的光源和产生自吸分为两个部分,自吸在一个被称为自吸管的装置内发生,文章讨论了这种分离式自吸效应校正原子吸收背景的可行性及可能存在的优点,研制成的自吸管对铜、锌、铁、铬、镍空心阴极灯光源的自吸收达到一定的深度。     

The Determination of Trace Transition Elements in Biological Tissues Using Flameless Atom Reservoir Atomic Absorption

Abstract

The development of an analytical technique generally applicable to the determination of Ag, Cd, Co, Cu, Fe, Mn, Ni, Pb, V, and Zn in all biological tissues is described. All of these elements may readily be determined in tissue samples of less than 0.5 g using flameless atom reservoir atomic absorption with a Perkin-Elmer heated graphite atomizer. Some of the operational characteristics of this atomizer system are discussed. The utility of the method is illustrated by analyses of selected marine biota and of NBS standard orchard leaves.     

Direct Atomic Absorption Analysis of Powdered Whole-Coal Slurries

Abstract

A procedure has been developed which permits the direct analysis of powdered whole-coal samples by atomic absorption or atomic emission methods using conventional instrumentation, thereby eliminating time-consuming ashing and sample-digestion procedures. Linear plots of the absorption signal intensity versus the elemental concentration of analyzed whole-coal samples were obtained for several elements. Preliminary results indicate this method is applicable for the estimation of both minor-level (eg., Fe and Ca) and trace-level (eg., Pb and Zn) constituents.