超声雾化-ICP-AES测定植物样品中的微量元素

研究了超声雾化-ICP-AES测定植物样品中As、Pb、Se、Bi、Ge、Mo的方法。对样品的测定条件进行了优化。在选定的仪器工作参数下,加标回收率达到95.5%~103%,RSD均小于3%。     

微波消解-超声雾化-ICP-AES测定发样中微量元素

研究了微波消解-超声雾化-ICP-AES测定人发样品中12种常量、微量元素的方法。对样品的测定条件进行了优化，并对20例女性拉祜族长寿老人发样进行了测定。与普通老人比较，女性拉祜族长寿老人发样中Mn、Mo、Ge的含量均明显高于普通老人发样中含量，存在显著性差异。     

Comparison of sample digestion procedures for the determination of arsenic in certified marine samples using the FI-HG-AAS-technique

 High-pressure digestion and a closed-vessel microwave heated system, both employing a mixture of nitric acid and hydrogen peroxide as digesting agent, were tested for decomposing the certified samples of BCR 278 mussel tissue (Mytilus edulis) and of BCR 422 cod muscle to determine arsenic by use of FI-HG-AAS. While the microwave system is insufficient to mineralize arsenic in marine samples (arsenic recoveries of 13±10% in BCR 278, 2±1% in BCR 422; n=4), high-pressure ashing at 300 °C results in recovery percentages of 56±15% (n=4) in mussel tissue (BCR 278) and of 25±10% (n=4) in cod muscle (BCR 422). A dry ashing procedure is given as a reference digestion, yielding complete recoveries of arsenic for both materials. The nitrite interference arising during measurement can be entirely overcome by using an amino sulfuric acid concentration of about 350 mmol/L in the solutions for measurement. Received: 30 April 1996/Revised: 12 July 1996/Accepted: 16 July 1996     

微波消解-端视ICP-AES测定茶叶中微量重金属元素

采用微波消解-端视等离子体原子发射光谱(ICP-AES)测定茶叶中微量重金属元素Pb、As、Cd、Cu、Fe,并对ICP-AES工作参数及条件进行了优化和选择。Pb、As、Cd、Cu、Fe的检出限分别为2.9×10-3μg/mL、5.2×10-3μg/mL、0.056×10-3μg/mL、0.55×10-3μg/mL、0.59×10-3μg/mL,线性范围为0~10000μg/L,相对标准偏差为1.7%~8.5%;回收率为90%~104%。该方法与国标法比较,结果无显著性差异。本法能用于茶叶测定。     

Comparison of digestion methods for ICP-MS determination of trace elements in fish tissues

A comparison is presented of six methods involving nitric acid in conjunction with other reagents to digest three certified marine biological samples (DOLT-3, DORM-3, IAEA-407) and a fish bone homogenate (prepared from Merluccius australis). An inductively coupled plasma-mass spectrometer with an octopole collision cell was used to determine up to 40 elements (Li, B, Na, Mg, Al, K, Ca, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sr, Y, Ag, Cd, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Ho, Er, Tm, Yb, Lu, Pb, Th, U) in the digests. These results were assessed in terms of their accuracy and precision, and a flow chart was developed to aid the selection of the optimal digestion method. Although none of the methods was found to give accurate determinations for all elements in the different reference materials, a relatively simple method involving nitric acid and hydrogen peroxide heated in a domestic microwave oven gave the most acceptable results.     

Comparison of microwave-assisted digestion procedures for total trace element content determination in calcareous soils

The aim of the study was to determine total trace (Cd, Co, Cr, Cu, Mn, Pb and Zn) and major (Al and Fe) element concentrations in calcareous soils using microwave-assisted digestion procedures. The literature showing lack of consensus regarding digestion procedures and unsatisfying recoveries for calcareous materials, four procedures using various acid combinations (HCl, HNO₃, H₂O₂, HF) and volumes were tested using a certified reference material (CRM 141R) and natural calcareous soil samples. Digests were analysed by inductively coupled plasma-atomic emission spectrometry (ICP-AES). Repeatability (R.S.D. <5%) and recoveries (82-116%) showed that the procedures were precise and accurate for most elements. Five calcareous soil samples from a Champagne vineyard plot were, then, subjected to these procedures. In calcareous materials, the presence of HF resulted in Al being severely underestimated (recovery <5%) and Co overestimated (recovery >124%) due to complex formation or spectrochemical interferences, respectively. As digestion was not significantly influenced by the addition of H₂O₂, the procedure corresponding to Aqua regia (HCl-HNO₃) appeared as the best compromise and was selected for further multielemental environmental studies on calcareous materials, even if the absence of HF could lead to incomplete digestion of accessory silicate minerals. Results for a vineyard plot showed that the soils were contaminated (3.65 mg kg⁻¹ Cd, 67 mg kg⁻¹ Cr, 278 mg kg⁻¹ Cu, 143 mg kg⁻¹ Pb and 400 mg kg⁻¹ Zn) as a consequence of urban waste and copper-treatment applications.     

Sample digestion procedures for trace element determination

A survey is given of both dry and wet procedures for matrix dissolution for the purpose of trace element determination in all kinds of materials. Various methods are compared and evaluated. With wet digestion methods special attention is paid to mixtures of strong acids and oxidants. Emphasis is laid on the completeness of these digestions, for which the use of HF is a prerequisite.     

Comparison of digestion procedures for the determination of mercury in soils by cold-vapour atomic absorption spectrometry

Five digestion procedures were investigated for the determination of mercury in soils by cold-vapour atomic absorption spectrometry. These methods included three acid leaching procedures in open systems and two acid digestion procedures in closed decomposition vessels. The closed vessels were heated in a conventional laboratory oven or a laboratory microwave oven. In the open systems, digestion with concentrated acids at elevated temperatures led to considerable losses of (organo) mercury compounds, while digestion at ambient temperature gave incomplete oxidation of the sample matrix. To prevent any losses of mercury and to obtain complete oxidation, the use of a closed decomposition system at elevated temperatures appeared to be necessary. The results obtained with these closed systems were in good agreement with those obtained by neutron activation analysis. Heating in a microwave oven appeared to be a considerable improvement over conventional thermal heating.     

Determination of major and trace elements in six herbal drugs for relieving heat and toxicity by ICP-AES with microwave digestion

ObjectiveTo establish a method to simultaneously determine major and trace element contents of Na, K, Cu, Fe, Zn, Mn, Ca, Mg, Cr, Ni, Pb, Se, As and Cd in six herbal drugs.MethodsMicrowave digestion procedure was applied under optimized conditions for digesting medicinal herbs. Concentrations of elements were determined by ICP-AES.ResultsThe results indicated that the herbal drugs were abundant in major and trace element contents which are healthy for human body. After optimizing the microwave digestion technology, the recovery of the element was 96.79–103.47% and the RSD < 5.0%.ConclusionICP-AES combined with the microwave digestion technology has a lot of merits in terms of saving time and effort, reducing environmental pollution, fast and accurate determination of results in determining major and trace elements.     

自动消解仪—ICP法测定水系沉积物中6种重金属元素

建立了自动消解仪-电感耦合等离子体发射光谱法(ICP-OES)同时测定水系沉积物中Cu、Zn、Ni、Cr、Pb、Co六种元素含量的方法。该方法的相关系数好、检出限低。方法经国家标准物质(GBW07361)验证,准确度和精密度均能达到环境监测分析的要求,为水系沉积物中重金属元素含量的测定提供了简单可靠的分析方法。     

Comparison of four microwave digestion methods for the determination of selenium in fish tissue by using hydride generation atomic absorption spectrometry

Four microwave digestion methods of fish tissue for selenium determination by hydride generation atomic absorption spectrometry were compared, in which potassium hexacyanoferrate(III) was chosen as a masking agent for eliminating matrix interferences. The results showed that the methods employing HNO(3)/H(2)O(2), HNO(3)/K(2)S(2)O(8)/H(2)O(2) and HNO(3)/H(3)PO(4)/H(2)O(2) digestion media were unreliable. However, the decomposition using the digestion media of HNO(3)/H(2)SO(4)/H(2)O(2) enabled adequate digestion of fish tissue and retention of selenium in a state amenable for determination. Therefore, the digestion procedures with HNO(3)/H(2)SO(4)/H(2)O(2) media are proposed for the determination of selenium in fish tissue by hydride generation atomic absorption spectrometry. The recoveries of the spiked samples investigated ranged from 90 to 102%. The result obtained from analyzing the NIES CRM No. 6 mussel was in good agreement with the reference value (reference value: 1.5 mug/g; found: 1.45 +/- 0.05 mug/g). The limit of detection for selenium was 0.03 mug/g dry mass for a 100 mg sample. The contents of selenium in local fish species investigated ranged from 0.49 to 2.90 mug/g, and the relative standard deviation for the determination of selenium was less than 8%.     

Multielement determination of major elements in polymer additives by microwave induced plasma atomic emission spectrometry after microwave digestion

A method for multielement determination of major elements in polymer additives by microwave induced plasma atomic emission spectrometry (MIP-AES) has been elaborated. Microwave digestion with nitric acid was selected for sample preparation because of its speed and versatility. Sodium nitrate was added to the digestion mixture in order to reduce phosphorus losses. The precision obtained varied between 2 and 4.5% depending on the element determined. The accuracy of the method was studied by analyzing the Spex 5-element oil standard. The method was applied to a variety of commercial and in-house prepared compositions.     

Efficiency of decomposition procedures for the determination of some elements in soils by atomic spectroscopic methods

Nine decomposition procedures for soil samples, such as via acid mixtures and fusion in open systems and microwave and autoclave dissolution (in closed systems under elevated temperature and pressure) were assessed using certified soil reference materials. The determination of various elements in solutions was performed by FAAS and ICP-OES and the results were compared with certified values and with direct current arc OES analysis.     

Efficiency of decomposition procedures for the determination of some elements in soils by atomic spectroscopic methods

Nine decomposition procedures for soil samples, such as via acid mixtures and fusion in open systems and microwave and autoclave dissolution (in closed systems under elevated temperature and pressure) were assessed using certified soil reference materials. The determination of various elements in solutions was performed by FAAS and ICP-OES and the results were compared with certified values and with direct current arc OES analysis. Received: 3 March 1997 / Revised: 30 May 1997 / Accepted: 3 June 1997     

Comparison of ten digestion procedures for the determination of arsenic in soils by hydride-generation atomic absorption spectrometry

Ten different digestion methods were investigated for the determination of arsenic in soils by hydride-generation atomic absorption spectrometry. These methods included a dry ashing/digestion, several acid-leaching procedures, and digestions in a pressure decomposition vessel or a Kjeldahl apparatus. A certified reference sample was analysed and the results obtained for five other soil samples were compared with the data obtained by spectrophotometry. A nitric/sulphuric acid digestion was the most suitable. A brief interference study is reported.     

Comparison of two digestion procedures for the determination of lead in lichens by electrothermal atomic absorption spectrometry

The efficiency of two procedures for the digestion of lichen was investigated using a heating block and a microwave oven. In the open vessels, concentrated nitric acid was added to the samples, left for 1 h, and the addition of 30% (v / v) hydrogen peroxide completed the digestion. In the closed system, the complete digestion was performed using concentrated nitric acid and hydrogen peroxide, reducing the amount of chemicals, time and contamination risk. Both digestion methods gave comparable results, and recoveries were statistically not different. For a lichen sample spiked with 10 μg Pb, the recovery was 111% and 110% using microwave and heating block digestion, respectively, while it was 100% and 103% for a 100 μg Pb spike. For the determination by electrothermal atomic absorption spectrometry samples were diluted 20 times with water and a volume of 20 μL was injected into the graphite furnace without chemical modifier. Pyrolysis and atomization temperatures of 700 °C and 1500 °C, respectively, were used. The characteristic mass was 8.4 ± 0.6 pg for aqueous calibration solutions and 8.9 ± 0.8 pg for samples. Calibration was against matrix matched standards. The recovery test showed some contamination problem with the lowest concentrations in both procedures. The detection limits were 4.4 μg L^− 1 with microwave oven and 5.4 μg L^− 1 with the heating block in the undiluted blank.     

微波消解-电感耦合等离子体质谱法测定人面果树中的重金属元素

建立了微波消解-电感耦合等离子体质谱(ICP-MS)法测定人面果树中As,Cr,Cd,Pb,Ni,Se,Hg 7种重金属元素含量的方法。样品采用HNO3-H2O2消解体系,避免了赶酸的操作,经微波消解后,用电感耦合等离子体质谱(ICP-MS)测定样品中As,Cr,Cd,Pb,Ni,Se,Hg 7种重金属元素的含量。方法对7种元素的校准曲线的相关系数r>0.9997,检出限在0.0098～0.0874μg/L之间,回收率在93%～115%之间,RSD在0.41%～4.9%。     

On the microwave digestion of soils and sediments for determination of lanthanides and some toxic and essential elements by inductively coupled plasma source mass spectrometry

Four digestion procedures for microwave dissolution of soils and sediments are investigated. Accurate results (accuracy better than 10%) for lanthanides, Be, Bi, Te, Th, U and Y are obtained only after an overnight stay with a mixture of 2 ml 48% HF and 2 ml 65% HNO(3) and afterwards stepwise microwave digestion with 1 ml 48% HF and 10 ml 5% H(3)BO(3). Only As is not be to be determined by this procedure due to significant interferences from Eu, Nd and Sm. For all other elements, accurate results are obtained by all four procedures.     

ICP-AES法同时测定高纯碘化铯中杂质元素

研究了用ICP-AES法同时测定高纯铯盐中Mn、Mg、Sr、Ca、Ba的方法。在选定的仪器工作参数下，加标回收率达到96％～104％，对合成样品10次重复测定的相对标准偏差〈0．5％，方法简便快捷。     

Comparison of sample preparation methods for the ICP-AES determination of minor and major elements in clarified apple juices

Inductively coupled plasma atomic emission spectrometry (ICP-AES) was used for the determination of minor and major elements present in apple juices. Prior to ICP-AES measurement, samples were diluted with nitric acid or digested in a microwave assisted digestion system. The differences in the measured element concentrations after application of different types of sample preparation procedures are discussed. The direct measurement compared to closed microwave dissolution was found to be the best sample preparation procedure. Prior to the measurements the ICP-AES method was validated and optimized for the determination of elements in apple juices. For diluted apple juice samples the lowest limits of detection (LOD) were obtained for Ba and Cd (< 20 μg L^{− 1}), moderate ones for Cu, Mn, Ni, Fe, Ag, Ca, Cr, Zn, Mg, and Sr (20–100 μg L^{− 1}), and the highest LODs for K, Pb, Na, and Al (> 110 μg L^{− 1}). The results obtained for the repeatability (< 0.9%), the intermediate precision (< 4.5%), the day-to-day reproducibility (< 5.2%), and the overall uncertainty of measurement (approx. 4–7%) for all elements analyzed demonstrated the good applicability of the proposed method. Differences in major element content in fresh and commercial apple juice are discussed.