SIMPLE MICROWAVE DIGESTION TECHNIQUE FOR ELEMENTAL ANALYSIS OF MINERAL SOIL SAMPLES

1990 ◽  
Vol 70 (4) ◽  
pp. 617-620 ◽  
Author(s):  
C. J. WARREN ◽  
B. XING ◽  
M. J. DUDAS

A new, rapid, and inexpensive method is described for digestion and dissolution of mineral soil and clay samples for determination of total elemental abundance. Standard soil samples were dissolved using HF and HNO3 in 60 mL Teflon bombs. Dissolution was complete after 7 min using a household microwave oven operating at 350 W. Addition of H3BO3 stabilized the digests against loss of silicon. Precise and accurate results were obtained for digests analyzed by inductively coupled plasma atomic emission spectrometry for total content of Si, Al, Fe, Mg, Ca, Na, K, and Mn. Key words: Elemental composition, standard soils, soil analysis

Author(s):  
Trajče Stafilov ◽  
Robert Šajn ◽  
Ivana Mickovska

The aim of this study was to investigate the distribution of chemical elements in topsoil and subsoil, focusing on the identification of natural and anthropogenic element sources in the area of the Crn Drim River Basin, Republic of Macedonia. For that purpose, by using sampling network of 5 × 5 km, 124 soil samples from 62 locations (topsoil and bottom soil) were collected. In total 60 elements were analysed, from which 18 elements (Ag, Al, B, Ba, Ca, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, P, Pb, V и Zn) were analysed by inductively coupled plasma - atomic emission spectrometry (ICP-AES) and an additional 42 elements were analysed by ICP - mass spectrometry (ICP-MS). Multivariate statistical analysis was applied to the obtained data. Factor analysis applied to the ICP-AES results produced four geogenic fac-tors: F1 (Ba and K); F2 (Ag, Cd, Cu, Ni, Pb and Zn), F3 (Cr, Fe, Na, Ni and V) and F4 (Al, Ca, Mg and Mn). Data ob-tained from the distribution maps and data analysis on soil samples, indicate the natural occurrence of the analysed ele-ments as well as low concentrations of heavy metals in the studied area.


1997 ◽  
Vol 80 (3) ◽  
pp. 647-650 ◽  
Author(s):  
Da-Hai Sun ◽  
James K Waters ◽  
Thomas P Mawhtnney

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.


2020 ◽  
Vol 2020 ◽  
pp. 1-7
Author(s):  
Li Yang ◽  
Qinghua Yan ◽  
Huixuan Zhang ◽  
Jianwei Zhang

Objective. To establish a method for analysis of microelements in five kinds of traditional Chinese medicine in high blood pressure medicinal food, mainly including manganese, cobalt, selenium, iron, magnesium, and other 15 elements. Methods. The samples were digested using a microwave digestion instrument through NHO3-H2O2 solution, and then, the elements were synthesized by inductively coupled plasma atomic emission spectrometry (ICP-AES). Results. The content of cobalt, manganese, zinc, copper, and nickel in the high blood pressure diet foods is higher, the RSD is between 0.005% and 4.82%, and the recovery rate ranges from 93.40% to 106.5%. The precision and recovery of the detection method are higher. Conclusion. The experiment result is better. Medicinal foods curing high blood pressure contain a number of micronutrients that are beneficial to the human body. This experiment provides some meaningful basis for the prevention and treatment of cardiovascular diseases such as hypertension.


2012 ◽  
Vol 271-272 ◽  
pp. 222-226
Author(s):  
Yong Cheng

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.


1989 ◽  
Vol 19 (8) ◽  
pp. 981-985 ◽  
Author(s):  
Y. P. Kalra ◽  
D. G. Maynard ◽  
F. G. Radford

A microwave digestion procedure was developed for multi-element determinations in tree foliage by inductively coupled plasma–atomic emission spectrometry. The procedure involved the sequential digestion of 0.500 g of plant material with HNO3 (10 mL), H2O2 (1 mL), and HCl (2 mL) at 90% power for 30 min, 90% power for 15 min, and 30% power for 10 min, respectively. The proposed method gave Ca, Mg, K, Na, Mn, P, and S results in good agreement with the National Institute of Standards and Technology plant reference materials. Iron and aluminum concentrations were 20 to 30% lower than the certified National Institute of Standards and Technology values. Recovery of standard additions of the elements tested (including iron and aluminum) ranged from 93 to 105%. The proposed digestion method provides accurate and precise results for multi-element analysis on one solution. In addition, HClO4, an extreme laboratory hazard, has been replaced in the digestion procedure by H2O2. The microwave digestion method has been used successfully in our laboratory for over 1 year for routine analysis and for a quality assurance program using a variety of plant materials. With this method 36 to 48 samples per person per day can be prepared for inductively coupled plasma–atomic emission spectrometry analysis.


2014 ◽  
Vol 2014 ◽  
pp. 1-8 ◽  
Author(s):  
Anetta Zioła-Frankowska ◽  
Marcin Frankowski ◽  
Karel Novotny ◽  
Viktor Kanicky

The determination of boron by inductively coupled plasma-atomic emission spectrometry has been carried in water-soluble and acid soluble (total content) fractions of 36 samples of traditional black tea and fruit brew. The estimation of the impact of the type of tea on the concentration of boron in water-soluble and acid extracts and potential human health risk from the daily intake of boron was carried out in this study. The levels of boron differed significantly in black and fruit tea types. The mean total content of boron ranged from 8.31 to 18.40 mg/kg in black teas, from 12.85 to 15.13 mg/kg in black tea with fruit flavor, and from 12.09 to 22.77 mg/kg in fruit brews. The degree of extraction of boron in black tea ranged from 8% to 27% and for fruit tea from 17% to 69%. In addition, the values below 25% were of black teas with fruit flavors. The daily intake of B from tea infusions (three cups/day) is still within the average daily intake except for some of the fruit brews which exceed acceptable regulations of the daily intake of total boron by humans. Hence, it may not produce any health risks for human consumption, if other sources of metal contaminated food are not taken at the same time.


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