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1.
悬浮体进样/氟化电热蒸发(ETV)/ICP-AES直接测定二氧化钛粉末中痕量钇 总被引:1,自引:0,他引:1
以聚四氟乙烯(PTFE)悬浮体为氟化剂,悬浮体制样/氟化辅助电热蒸发(ETV)/ICP-AES直接测定TiO2陶瓷粉末中痕量杂质钇;考察了影响基体和待测元素的蒸发过程的各种因素;对比研究了待测元素和基体的氟化蒸发行为;实现了基体和待测元素的预分离,显着降低了基体效应。本法的检出限为0.26μg/L,相对偏差为3.8%(n=5,c=0.5mg/L). 相似文献
2.
Shizhong Chen Feng Li Zhenhuan Liao Tianyou Peng Z. Jiang 《Fresenius' Journal of Analytical Chemistry》1999,364(6):556-559
A method has been described for the direct determination of Ti, Cu, Mn, Cr and Cd in solid biological samples without any
chemical pretreatment by fluorination assisted electrothermal vaporization inductively coupled plasma atomic emission spectrometry
(ETV-ICP-AES) with slurry sampling. A polytetrafluorethylene (PTFE) emulsion was used as a fluorinating reagent to promote
the vaporization of the analytes from the graphite furnace. The interface between furnace device and ICP torch and the main
factors affecting the analytical signal were investigated systematically. The detection limits for the determination of Ti,
Cu, Mn, Cr and Cd are 6.3, 4.7, 10, 13 and 278 ng/mL, respectively; the relative standard deviations are in the range of 1.5
(Mn) ∼4.0% (Cd) after optimization of the operating conditions. The recommended approach has been applied to directly determine
the trace elements of interest in the Chinese traditional medicine Loulu and in the solid biological standard reference material
(peach leaves, GBW 08501) with satisfactory results.
Received: 28 December 1998 / Revised: 9 February 1999 / Accepted: 12 February 1999 相似文献
3.
Shizhong Chen Feng Li Zhenhuan Liao Tianyou Peng Z. Jiang 《Analytical and bioanalytical chemistry》1999,364(6):556-559
A method has been described for the direct determination of Ti, Cu, Mn, Cr and Cd in solid biological samples without any
chemical pretreatment by fluorination assisted electrothermal vaporization inductively coupled plasma atomic emission spectrometry
(ETV-ICP-AES) with slurry sampling. A polytetrafluorethylene (PTFE) emulsion was used as a fluorinating reagent to promote
the vaporization of the analytes from the graphite furnace. The interface between furnace device and ICP torch and the main
factors affecting the analytical signal were investigated systematically. The detection limits for the determination of Ti,
Cu, Mn, Cr and Cd are 6.3, 4.7, 10, 13 and 278 ng/mL, respectively; the relative standard deviations are in the range of 1.5
(Mn) ∼4.0% (Cd) after optimization of the operating conditions. The recommended approach has been applied to directly determine
the trace elements of interest in the Chinese traditional medicine Loulu and in the solid biological standard reference material
(peach leaves, GBW 08501) with satisfactory results.
Received: 28 December 1998 / Revised: 9 February 1999 / Accepted: 12 February 1999 相似文献
4.
A slurry fluorination electrothermal vaporization (ETV)-ICP-AES method for the determination of Cu and Cr in SiO2 powders has been developed. A polytetrafluoroethylene (PTFE) emulsion is used as fluorinating reagent; the matrix (Si) is
partially separated from the sample by selecting the ashing temperature and time to reduce the interference. Moreover, the
vaporization behaviour has been investigated in detail. The detection limits are 1.1 ng/mL with 3.8% of RSD (Cu) and 1.6 ng/mL
with 3.2% of RSD (Cr). The method is applied to analyze the SiO2 powders with satisfactory results.
Received: 6 January 1997 / Revised: 13 March 1997 / Accepted: 28 March 1997 相似文献
5.
氟化电热蒸发/等离子体原子发射光谱直接测定植物试样中硼的研究 总被引:1,自引:0,他引:1
本文提出了用聚四氟乙烯悬浮体制样电热蒸发-ICP-AES直接测定植物试样中新方法,研究了上述元素在该技术中的粒度效应,基效应和存在下的蒸发行为,在优化的实验条件下,本法测定B的检出限为1.2ng/ml,RSD为4.2%,该法有简便,灵敏和分析前试样无需进行化学处理的优点,已应用于生物试样的直接测定,分析结果与参考值吻合。 相似文献
6.
《Spectrochimica Acta Part B: Atomic Spectroscopy》2005,60(4):537-541
A novel method for the determination of trace rare earth impurities in ZrO2 powder has been developed based on electrothermal vaporization inductively coupled plasma atomic emission spectrometry. A polytetrafluoroethylene slurry was used as a fluorinating reagent to convert both the matrix (Zr) and the analytes (rare earth elements) into fluorides with different volatilities at a high temperature in a graphite furnace. The more volatile ZrF4 was removed in-situ by selective vaporization prior to the determination of the analytes, removing matrix spectral interferences. Under optimum operating conditions, the absolute detection limits of the analytes varied from 0.04 ng (Yb) to 0.50 ng (Pr) with relative standard deviations less than 5%. The recommended approach has been successfully applied to the determination of trace rare earth impurities (La, Pr, Eu, Gd, Ho and Yb) in ZrO2 powder and the results were in good agreement with those obtained by pneumatic nebulization inductively coupled plasma atomic emission spectrometry after the separation of the matrix using a solvent extraction procedure. 相似文献
7.
氟化电热蒸发/ICP—AES直接测定SiO2中痕量Fe 总被引:1,自引:0,他引:1
对氟化电热蒸发(FETV)/ICP-AES技术中元素的氟化蒸发行为,基体效应和粒度效应进行了考察,确定了杂质(Fe)与基体(Si)分离的最佳实验条件,本法用于SiO2中痕量Fe的直接测定,有灵敏,简便,试样消耗少和不需化学处理等优点。 相似文献
8.
S. Chen 《Journal of Analytical Chemistry》2005,60(3):254-258
Slurry sampling followed by electrothermal vaporization (ETV) was used as sample introduction technique in inductively coupled plasma atomic emission spectrometry (ICP-AES) for the direct determination of trace elements in food samples. A polytetrafluoroethylene (PTFE) emulsion was used as a fluorinating reagent to promote vaporization and the transportation of analytes. The main factors affecting the analytical signals were investigated in detail. Under optimum operating conditions, the detection limits (DL) for this method varied from 1.8 (Cu) to 215 ng/mL (Zn), while the relative standard deviations (RSD) were in the range 2.6% (Cu)-7.2% (Zn). The proposed method was successfully applied to the direct determination of trace amounts of V, Cu, Cr, Fe, Zn, and La in rice without any chemical pretreatment. The precision was evaluated by analyzing a standard reference material (tea leaves, GBW 07605) and comparing the results from this method with results obtained by pneumatic nebulization (PN) ICP-AES after the wet-chemical decomposition of the same sample.From Zhurnal Analiticheskoi Khimii, Vol. 60, No. 3, 2005, pp. 286–290.Original English Text Copyright © 2005 by Chen.This article was submitted by the author in English. 相似文献
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A novel method has been developed for the direct determination of traces of chromium, cobalt, and nickel in TiO2 powder; it entails slurry sampling and electrothermal atomic-absorption spectrometry (ETAAS) with a polytetrafluoroethylene (PTFE) slurry (6% m/v) as fluorinating reagent. The factors which could affect the vaporization of the matrix and analytes were studied in detail; the fluorinating vaporization behavior of the analyte both in the slurry and in solution were also investigated. Owing to the in-situ separation of the matrix, the matrix influences were reduced significantly. The proposed method has been applied to the direct determination of traces of chromium, cobalt, and nickel in high-purity TiO2 powder without chemical pretreatment. Under the optimum experimental conditions the detection limits of the analytes (Cr, Co, and Ni) were 1.9 ng g(-1), 2.4 ng g(-1) and 5.4 ng g(-1), respectively, the relative standard deviations (RSD) were 3.4% (n=6, c=7.0 ng mL(-1)), 2.9% (n=6, c=0.70 ng mL(-1)), and 7.6% (n=6, c=4.0 ng mL(-1)), again respectively, and the characteristic masses for Cr, Co, and Ni were 8.4 pg/ 0.0044A, 9.3 pg/0.0044A, and 40.0 pg/0.0044A, respectively. 相似文献
12.
A new method for the determination of trace amounts of 14 rare earth elements in high purity Y2O3 using fluorination assisted electrothermal vaporization inductively coupled plasma atomic emission spectrometry with slurry sampling was developed. A polytetrafluoroethylene (PTFE) emulsion was used as a fluorinating reagent to promote the vaporization of the analytes from graphite furnace. The main factors affecting analytical signals were investigated systematically. The interference of matrix could be minimized in the presence of PTFE. Under optimum conditions, the detection limits for rare earth elements were 0.032 ng~2.52 ng and the relative standard deviations were in the range of 1.4% to 4.3%. The proposed method was applied to the direct analysis of high purity Y2O3 powder with satisfactory results. 相似文献
13.
Platform and wall vaporization for electrothermal vaporization (ETV)-inductively coupled plasma mass spectrometry (ICP-MS) determination of some refractory elements (Ti, V, Cr, Mo, La and Zr) and Pb were comparatively studied with the use of poly (tetrafluoroethylene) (PTFE) as fluorinating reagent. The factors affecting the vaporization behaviors of the target analytes in the platform and tube wall vaporization including vaporization temperature and time, pyrolytic temperature and time were studied in detail, and the flow rates of carrier gas/auxiliary carrier gas, were carefully optimized. Under the optimal conditions, the signal profiles, signal intensity, interferences of coexisting ions and analytical reproducibility for wall and platform vaporization ETV-ICP-MS were compared. It was found that both wall and platform vaporization could give very similar detection limits, but the platform vaporization provided higher signal intensity and better precision for some refractory elements and Pb than the wall vaporization. Especially for La, the signal intensity obtained by platform vaporization was 3 times higher than that obtained by wall vaporization. For platform vaporization ETV-ICP-MS, the limits of detection (LODs) of 0.001 μg L−1 (La) ~ 0.09 μg L− 1 (Ti) with the relative standard deviations (RSDs) of 1.5% (Pb) ~ 15.5% (Zr) were obtained. While for wall vaporization ETV-ICP-MS, LODs of 0.005 μg L− 1 (La) ~ 0.4 μg L− 1 (Pb) with RSDs of 3.2% (Mo) ~ 12.8% (Zr) were obtained. Both platform and tube wall vaporization techniques have been used for slurry sampling fluorination assisted ETV-ICP-MS direct determination of Ti, V, Cr, Mo, La, Zr and Pb in certified reference materials of NIES No. 8 vehicle exhaust particulates and GBW07401 soil, and the analytical results obtained are in good agreement with the certified values. 相似文献
14.
《Spectrochimica Acta Part B: Atomic Spectroscopy》2005,60(9-10):1342-1348
A method for the direct determination of trace rare earth elements in ancient porcelain samples by slurry sampling fluorinating electrothermal vaporization inductively coupled plasma mass spectrometry was developed with the use of polytetrafluoroethylene as fluorinating reagent. It was found that Si, as a main matrix element in ancient porcelain sample, could be mostly removed at the ashing temperature of 1200 °C without considerable losses of the analytes. However, the chemical composition of ancient porcelain sample is very complicated, which makes the influences resulting from other matrix elements not be ignored. Therefore, the matrix effect of ancient porcelain sample was also investigated, and it was found that the matrix effect is obvious when the matrix concentration was larger than 0.8 g l− 1. The study results of particle size effect indicated that when the sample particle size was less than 0.057 mm, the particle size effect is negligible. Under the optimized operation conditions, the detection limits for rare earth elements by fluorinating electrothermal vaporization inductively coupled plasma mass spectrometry were 0.7 ng g− 1 (Eu)–33.3 ng g− 1(Nd) with the precisions of 4.1% (Yb)–10% (La) (c = 1 μg l− 1, n = 9). The proposed method was used to directly determine the trace rare earth elements in ancient porcelain samples produced in different dynasty (Sui, Ming and Qing), and the analytical results are satisfactory. 相似文献
15.
A new method for the determination of trace amounts of 14 rare earth elements in high purity Y2O3 using fluorination assisted electrothermal vaporization inductively coupled plasma atomic emission spectrometry with slurry
sampling was developed. A polytetrafluoroethylene (PTFE) emulsion was used as a fluorinating reagent to promote the vaporization
of the analytes from graphite furnace. The main factors affecting analytical signals were investigated systematically. The
interference of matrix could be minimized in the presence of PTFE. Under optimum conditions, the detection limits for rare
earth elements were 0.032 ng∼2.52 ng and the relative standard deviations were in the range of 1.4% to 4.3%. The proposed
method was applied to the direct analysis of high purity Y2O3 powder with satisfactory results.
Received: 19 June 1999 / Revised: 10 December 1999 / Accepted: 16 December 1999 相似文献
16.
电热蒸发进样—等离子体原子发射光谱中钒和钛的蒸发机理研究 总被引:1,自引:0,他引:1
自1974年Nixon报道钽丝电热蒸发作为ICP-AES进样技术以来,这一技术已引起了人们的极大兴趣,受到越来越广泛的重视。电热蒸发(ETV)-ICP-AES是一种将蒸发和激发分步进行的联用技术。石墨是目前普遍使用的蒸发器材料。然而,在高温下某些元素和石墨材料可以发生碳化反应,形成热稳定的碳化物,使分析物蒸发不完全或根本不蒸发,从而影响分析结果的灵敏度和准确性。为了解决这一问题,我们曾提出了以聚四氟乙烯(PTFE)悬浮体为氟化剂,氟化辅助ETV-ICP-AES直接测定粉煤标样中钒和钛的新方法,其检出限 相似文献
17.
Tianyou Peng Zucheng Jiang Bin Hu Zhenghuan Liao 《Analytical and bioanalytical chemistry》1999,364(6):551-555
A method has been developed for the determination of trace impurities in silicon nitride (Si3N4) powders by fluorination assisted electrothermal vaporization (ETV) /ICP-AES using the slurry sampling technique. Polytetrafluoroethylene (PTFE) emulsion as a fluorinating reagent not only effectively destroys the skeleton of Si3N4, but also carries out selective volatilization between the impurity elements (Cu, Cr) and the matrix (Si). The experimental parameters influencing fluorination reactions were optimized. The detection limits for Cu and Cr are 1.05 ng/mL ( Cu) and 1.58 ng/mL (Cr), the RSDs are in the range of 1.9–4.2%. The proposed method has been applied to the determination of Cu and Cr in Si3N4 ceramic powders. The analytical results were compared with those obtained by independent methods. 相似文献
18.
A method for in-situ removal of matrix is proposed for direct determination of trace refractory elements in human serum by ETV–ICP–MS with the use of poly(tetrafluoroethylene) (PTFE) as fluorinating reagent. Attention has been paid to investigating the vaporization behavior both of refractory elements of interest and of matrix elements (Na, K, Ca, Mg, Cl, S, and P) in a graphite furnace with the PTFE modifier present or not. It was shown that potential interferences from the organic and inorganic matrices in the serum sample could be eliminated or reduced to a negligible level by appropriate dilution of the serum and deliberate optimization of the ETV temperature program. The proposed method has been applied to the direct simultaneous determination of V, Cr, Mo, Ba, La, Ce, and W in human serum. The limits of detection for fivefold diluted serum were 0.18 (V), 0.229 (Cr), 0.050 (Mo), 0.328 (Ba), 0.031 (La), 0.038 (Ce), and 0.019 ng mL–1 (W), respectively, and the relative standard deviations of the method were in the range 4–15% (2 ng mL–1 in serum, n=3). 相似文献
19.
火焰原子吸收光谱法间接测定植物叶片中的硫 总被引:1,自引:0,他引:1
将植物叶片中的有机硫和无机硫用酸消化使植物体中的各种硫转化成硫酸盐,利用硫酸盐与铬酸钡悬浊液反应释放出铬酸根,以火焰原子吸收光谱法测定溶液中游离的铬酸根,间接测定消化液中的硫酸盐。研究了试验条件对测定灵敏度的影响,确定了最佳试验条件,该法用于植物叶片中硫含量的分析,回收率在92.5%~96.3%之间。 相似文献
20.
Two new color reactions with boron are reported. Sensitive methods have been developed for their use. A new method for the decomposition of fruit tree leaves and alfalfa, and the subsequent separation of the boron is described.The reagents are 5-benzamido-6'-chloro-1, 1 '-bis (anthraquinonyl) amine(I) and 5-p-toluidino-1,1'-bis (anthraquinonyl) amine(II). Concentrated (96%) sulfuric acid is used as the solvent. The formation of the boron complex of the reagents was found to be dependent on the following variables: time of heating, temperature, sulfuric acid content and the presence of diverse ions.Solutions of the two complexes follow Beer's law over the boron range indicated: Compound I, 0 to 0.5 γ at wavelength of 635 mμ and Compound II, 0 to 0.4 γ at wavelength 720 mμ. The sensitivities are 1 : 300,000,000 and 1 : 200,000,000, respectively. The standard deviation was calculated for the determination of boron with each compound. Results showed 0.002 absorbance unit, i.e., 0.001 γ of boron for Compound I and 0.005 absorbance unit, i.e., 0.002 γ of boron for Compound II.The method of decomposing the leaves and alfalfa samples is based upon destroying all the organic matter with a mixture of 96% sulfuric acid and 30% hydrogen peroxide within, the distilling flask. Boron is then distilled off as the volatile trimethyl ester. The standard deviation of the method is 0.58%. 相似文献