Micro-quantity tissue digestion for metal measurements by use of a microwave acid-digestion bomb.

1989 ◽  
Vol 35 (3) ◽  
pp. 488-490 ◽  
Author(s):  
J R Nicholson ◽  
M G Savory ◽  
J Savory ◽  
M R Wills

Abstract We describe a simple and convenient method for processing small amounts of tissue samples for trace-metal measurements by atomic absorption spectrometry, by use of a modified Parr microwave digestion bomb. Digestion proceeds rapidly (less than or equal to 90 s) in a sealed Teflon-lined vessel that eliminates contamination or loss from volatilization. Small quantities of tissue (5-100 mg dry weight) are digested in high-purity nitric acid, yielding concentrations of analyte that can be measured directly without further sample manipulation. We analyzed National Institute of Standards and Technology bovine liver Standard Reference Material to verify the accuracy of the technique. We assessed the applicability of the technique to analysis for aluminum in bone by comparison with a dry ashing procedure.

1988 ◽  
Vol 34 (6) ◽  
pp. 1128-1130 ◽  
Author(s):  
D B Van Wyck ◽  
R B Schifman ◽  
J C Stivelman ◽  
J Ruiz ◽  
D Martin

Abstract We developed a rapid acid-digestion method for preparing tissue samples for iron determination. Specimens were digested in nitric acid and hydrogen peroxide under high temperature and pressure in closed Teflon vessels, with microwave energy. Analysis for iron in 25- to 250-mg portions of digested bovine liver powder (National Bureau of Standards Certified Reference Material no. 1577a) showed excellent linearity ([predicted] = 1.007[actual] - 0.166 micrograms per sample) and analytical recovery (98%). Precision (CV) was 5.4% when iron content was 10 micrograms per sample. Assaying split samples of mouse tissues, we found a close correlation between iron concentrations obtained with closed vs open vessels ([closed] = 0.878[open] + 68 micrograms/g, r = 0.994, range 400-4600 micrograms/g dry weight). In contrast to time-consuming conventional procedures for tissue dissolution, closed-vessel digestion with microwave energy dramatically shortens time for tissue preparation, minimizes use of caustic acid, reduces risk of sample loss or contamination, and yields accurate and reproducible results.


2012 ◽  
Vol 40 (1) ◽  
pp. 147-153 ◽  
Author(s):  
Abu Tweb Abu Ahmed ◽  
Suman Mandal ◽  
Didarul Alam Chowdhury ◽  
Abu Rayhan M Tareq ◽  
M Mizanur Rahman

The present study was carried out to determine the level of bioaccumulation of some heavy metals in a freshwater fish Ayre (Sperata aor Hamilton, 1822) collected from Rajfulbaria (23°48?56.36? N and 90°14?54.04? E) of  Dhaleshwari river. Four heavy metals, namely chromium (Cr), copper (Cu), lead (Pb), and cadmium (Cd) were selected for this study. Metal concentrations were   determined by Flame Atomic Absorption Spectrophotometer after nitric acid  digestion of samples. The concentrations of accumulated heavy metals in fish were  also compared with the concentrations of metals in the sediments and waters of  that river. The level of bioaccumulations in different organs of S. aor were determined separately and compared among them. Average bioaccumulation levels  in S. aor were Cr: 1.458 mg/kg, Cu: 31.500 mg/kg, Pb: 18.776 mg/kg and Cd:  0.487 mg/kg of dry weight. The levels of heavy metals in sediments were Cr: 27.393 mg/kg, Cu: 37.450 mg/kg, Pb: 15.797 mg/kg and Cd: 2.083 mg/kg, and in water were Cr: 0.130 ppm, Cu: 0.000 ppm, Pb: 0.201 ppm and Cd: 0.001 ppm.The bioaccumulation of these four heavy metals in fish organs, sediment and  water samples were also compared with FAO approved standard levels and other  related studies, and found that the levels of bioaccumulation in the Dhaleshwari river exceeded all the standard levels. DOI: http://dx.doi.org/10.3329/bjz.v40i1.12904 Bangladesh J. Zool. 40(1):147-153, 2012


1996 ◽  
Vol 79 (3) ◽  
pp. 773-776 ◽  
Author(s):  
Miguel Navarro ◽  
Herminia Lopez ◽  
Maria C Lopez ◽  
Vidal Perez

Abstract A procedure has been developed for determination of total selenium in urine by hydride generation atomic absorption spectrometry. Mineralization was performed with a nitric acid–perchloric acid mixture on a thermostated digestion block. The method was validated by comparison with the method involving mineralization in a microwave acid digestion bomb containing nitric acid and small amounts of vanadium pentoxide. Se(VI) was reduced to Se(IV) by dissolution in 7N HCI. Sample recoveries, precision studies, and analyses of a certified reference material demonstrated the reliability and accuracy of this technique. Urine samples had selenium concentrations ranging from 4.6 to 50.3 μg/L. These values correspond to an average of 54.9 μg per person per day total ingested and bioavailable Se in the daily diet.


2006 ◽  
Vol 60 (4) ◽  
Author(s):  
P. Hornik ◽  
D. Milde ◽  
Z. Trenz ◽  
K. Vysloužil ◽  
V. Stužka

AbstractConcentration of four trace elements (copper, zinc, iron, and selenium) was determined in colon tissue from twenty-three patients with colorectal cancer. The tissue samples were dried and dissolved using microwave-assisted digestion technique. The content of trace elements was determined using atomic absorption spectrometry. No significant differences between Zn levels in normal and cancerous tissues were observed. However, the levels of Cu, Fe, and Se were significantly higher in cancerous tissues than in the control samples.The results obtained sing microwave-assisted technique were compared to those obtained via alkaline digestion with tetramethylammonium hydroxide. Both techniques were used for the digestion of certified reference material of pork liver. Very good agreement with the certified values of Cu, Fe, and Zn in the reference material was achieved using alkaline digestion procedure. This technique seems to be an efficient alternative to decomposition of biological samples.


2020 ◽  
Vol 103 (5) ◽  
pp. 1256-1263 ◽  
Author(s):  
Yasemin Bakircioglu Kurtulus ◽  
Dilek Bakircioglu ◽  
Alper Can Babac ◽  
Selcuk Yurtsever ◽  
Nukte Topraksever

Abstract Background The emulsion induced by emulsion breaking (EIEB) procedure was previously reported for the extraction of copper, iron, manganese, and nickel from liquid oil samples such as vegetable oil. Objective To optimize the EIEB procedure for determination of copper, iron, manganese, and nickel in solid oil (margarine) samples by Graphite Furnace Atomic Absorption Spectrometry (GFAAS). Methods The extraction procedure uses a surfactant in nitric acid to form an emulsion followed by heating to break the emulsion. Optimization included variation of the test portion size, the type and concentration of the surfactant, the concentration of nitric acid in the aqueous solution, the emulsion agitation time, heating temperature, and the time required to break the emulsion. Results Mean element concentrations of 11 margarine samples were in the following ranges: Cu 0.031–0.131 µg/g, Fe 5.7–24.9 µg/g, Mn 0.542–1.11 µg/g, and Ni 0.108–0.134 µg/g. Under the optimized extraction conditions, the detection limits (µg/kg) were 4.8, 13, 1.5, and 23 for Cu, Fe, Mn, and Ni, respectively. The accuracy of the extraction procedure was determined by comparison to commonly used microwave digestion procedure. The EIEB results were not statistically different from the microwave digestion results when analyzed by GFAAS as determined by the statistical tests. Conclusions The EIEB procedure was shown to be equivalent to the commonly used microwave digestion procedure for extraction of analytes from margarine samples. Highlights The optimized EIEB extraction procedure is simple, rapid, low cost, and environmentally friendly. It has improved detection limits and allows calibration with aqueous standards.


2006 ◽  
Vol 89 (5) ◽  
pp. 1410-1416 ◽  
Author(s):  
Tasneem G Kazi ◽  
Hassan I Afridi ◽  
Mohammad K Jamall ◽  
Gul H Kazi ◽  
Mohammad B Arain ◽  
...  

Abstract An ultrasonic-assisted leaching procedure was developed for the determination of heavy elements (As, Cu, Cd, Pb, and Zn) in Certified Reference Material of human hair (CRM 397) provided from the Community Bureau of Reference (BCR) of the Commission of the European Community. Concentrated nitric acid30% hydrogen peroxide (2 + 1) was used for the leaching method. The effects of different factors on acid leaching of elements, such as presonication time (without ultrasonic stirring), sonication or exposure time to ultrasound, and temperature of the ultrasonic bath have been investigated. Optimum values of these parameters were selected for the maximum extraction of heavy metals from CRM BCR 397 and human scalp hair samples of normal healthy males. To check the validity of the proposed method, a wet acid digestion method was used to obtain the total elemental concentration in CRM BCR 397 and scalp hair samples. Cu and Zn in leachate and digests were measured by flame atomic absorption spectrometry using a conventional air/acetylene flame, while As, Cd, and Pd were determined by electrothermal atomic absorption spectrometry. Under optimized conditions, the recovery for Zn, Cd, Pd, As, and Cu was 98, 98.5, 97.5, 98.2, and 95%, respectively, of those obtained with the wet acid digestion method.


2020 ◽  
Vol 993 ◽  
pp. 1502-1510
Author(s):  
Ling Ling Gao ◽  
Ye Chen ◽  
Ning Wang ◽  
Shan Shan Liu ◽  
Yu Hui Wang ◽  
...  

As consumer awareness of heavy metal content in textile increased, it is necessary to develop analytical methods that identify and quantify heavy metals. In order to comprehensively investigate the potential risks of antimony (Sb) in recycled polyester fiber to humans health, this study developed acid digestion method, with the condition that the volume ratio of concentrated sulfuric acid to hydrogen peroxide was 1, and digested at 200°Cfor 1.5h, which produced clear and colorless solutions.Currently, microwave and dry ashing are also common methods for digesting polyethylene terephthalate samples. Three pretreatment methods for determining the content of Sb in recycled polyester fibers was evaluated. Results showed that inductively coupled plasma-optical emission spectrometry (ICP-OES) analysis of acid digested recycled polyester samples resulted in Sb content higher than for the microwave and dry ashing digestion methods which incompletely digest recycled polyester. Moreover, compared with microwave digestion and dry ashing, acid digestion had a low detection limit of 0.0116 ug/mL, a high spike recovery of 82% to 106% and the RSD value less than 2%, which indicates that the data was accurate and reproducible. Therefore, in this study, acid digestion - ICP-OES was an effective method for detecting the content of heavy metal Sb in recycled polyester.


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