Microwave Digestion and Ultrasonic Nebulization for Determination of Boron in Animal Tissues by Inductively Coupled Plasma Atomic Emission Spectrometry With Internal Standardization and Addition of Mannitol

Abstract A microwave digestion procedure was developed for determining aluminum and boron and 13 other elements in plant tissues by inductively coupled plasma atomic emission spectrometry (ICP-AES). The sample (0.5 g) was digested in a closed Teflon vessel with 10 mL concentrated nitric acid and 3 mL hydrofluoric acid, and further digested in an open Teflon vessel with 5 mL hydrogen peroxide. Excess hydrofluoric acid was eliminated by adding 0.2 g silicon (IV) oxide. Four National Institute of Standards and Technology standard reference materials (apple leaves, peach leaves, tomato leaves, and pine needles) were analyzed to test the reliability of the method. The excellent recoveries indicate that the proposed procedure is simple and effective for determination of Al, B, Ba, Ca, Cr, Cu, Fe, K, Mg, Mn, Na, P, S, Sr, and Zn in plants.

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Determination of Alloy and Impurity Elements in the WC-Co Based Cemented Carbide by Microwave Digestion - Inductively Coupled Plasma Atomic Emission Spectrometry

Applied Mechanics and Materials ◽

10.4028/www.scientific.net/amm.271-272.222 ◽

2012 ◽

Vol 271-272 ◽

pp. 222-226

Author(s):

Yong Cheng

Keyword(s):

Inductively Coupled Plasma ◽

Microwave Digestion ◽

Atomic Emission ◽

Atomic Emission Spectrometry ◽

Emission Spectrometry ◽

Control Parameters ◽

Plasma Atomic Emission ◽

Plasma Atomic Emission Spectrometry ◽

Inductively Coupled

Using high-pressure sealed microwave heating method, the WC-Co based cemented carbide samples were digested completely by nitric acid and phosphoric acid (VHNO3: VH3PO4 = 5:1). Then the digestion solution was diluted with water to a constant volume, and directly using inductively coupled plasma atomic emission spectrometry (ICP-OES) determination of the content of 0.005 to 10% Co and 0.005 ~ 1% of Fe, Nb, Ta, V, Cr, Mo and Ni. This paper examine the best digestion conditions, including reagent composition, ratio, and microwave control parameters, etc., then establish a set of microwave digestion and by complex reactions with inorganic reagents to stabilize the high tungsten matrix digestion method, in order to quickly and completely digest the tungsten-cobalt-based samples and avoid the generation of tungsten acid precipitation resulting in the loss of some of the analyte and impact of organic complex agents on the spectral determination. The results showed that: the control parameters of using 5 min to heat the sample to 130 °C and keep for 5 min, then heated to 190 °C in 5 min and keep for 15 min is better to maintain the digestion. By optimizing elemental analysis line, ICP measurement parameters and matrix matching and synchronization of background correction method, the high tungsten matrix effects and spectral interference are eliminated; ensure the detection performance of the method. Background equivalent concentration of 5μg/L (Nb) ~ 18μg/L (Fe), elements of the detection limit of 4μg/L (Nb) ~ 13μg/L (Fe), which used for the determination of impurities in the alloy or elements with the results is RSD <3%, recovery 97.0% ~ 103.5% corresponding with the national standard examination method.

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On-Line Complexation/Preconcentration System for the Determination of Lead in Wine by Inductively Coupled Plasma–Atomic Emission Spectrometry with Ultrasonic Nebulization

Journal of AOAC International ◽

10.1093/jaoac/84.5.1555 ◽

2001 ◽

Vol 84 (5) ◽

pp. 1555-1560 ◽

Cited By ~ 6

Author(s):

Rodolfo G Wuilloud ◽

Alfredo H González ◽

Eduardo J Marchevsky ◽

Roberto A Olsina ◽

Luis D Martinez

Keyword(s):

Inductively Coupled Plasma ◽

Atomic Emission ◽

Atomic Emission Spectrometry ◽

Emission Spectrometry ◽

Plasma Atomic Emission ◽

Plasma Atomic Emission Spectrometry ◽

Ultrasonic Nebulization ◽

Inductively Coupled ◽

On Line

Abstract An on-line lead preconcentration and determination system implemented with inductively coupled plasma–atomic emission spectrometry (ICP–AES) with ultrasonic nebulization (USN) in association with flow injection was studied. For the preconcentration of lead, a Pb–quinolin–8–ol complex was formed on-line at pH 6.8 and retained on Amberlite XAD–16 resin. The lead was removed from the microcolumn by countercurrent elution with nitric acid. A total enhancement factor of 225 was obtained with respect to ICP–AES with pneumatic nebulization (15.0 for USN and 15.0 for the column). The detection limit for Pb for the preconcentration of a 10 mL wine sample was 0.15 μg/L. The precision for 10 replicate determinations at a Pb level of 25 μg/L was a relative standard deviation of 2.5%, calculated from the peak heights obtained. The calibration graph obtained by using the preconcentration system for lead was linear with a correlation coefficient of 0.9995 for levels near the detection limit up to ≥ 1000 μg/L. The method was successfully applied to the determination of lead in wine samples.

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