Microwave-Assisted Vapor-Phase Nitric Acid Digestion of Small Biological Samples for Inductively Coupled Plasma Spectrometry

1998 ◽  
Vol 52 (6) ◽  
pp. 900-907 ◽  
Author(s):  
Dula Amarasiriwardena ◽  
Antoaneta Krushevska ◽  
Ramon M. Barnes
Keyword(s):  
Nitric Acid ◽  
Vapor Phase ◽  
Biological Samples ◽  
Inductively Coupled Plasma ◽  
Closed Vessel ◽  
Acid Digestion ◽  
Inductively Coupled ◽  
Microwave Assisted ◽  
Microwave Apparatus ◽  
Nitric Acid Digestion

The applicability of microwave-assisted, vapor-phase nitric acid digestion of small biological samples in closed-vessel microwave systems is examined for the inductively coupled plasma atomic emission spectroscopy (ICP-AES) determination of 10 elements (Al, As, Ca, Cu, Cd, Fe, Mn, Mo, Pb, and Zn). A 1.8 mL quartz sample container geometry was optimized for the successful decomposition of 50 to 90 mg of powdered biological samples. Microwave energy was efficiently coupled by addition of 250 μL of distilled deionized water to the sample. A single microwave-assisted, vapor-phase acid sample digestion was accomplished within 30 min (including cooling time) at ∼1200 psi pressure and 450 W microwave power in a commercial pressurized microwave decomposition (PMD) system. Multiple microwave-assisted, vapor-phase acid digestions were achieved at moderately high pressure (400 to 480 psi) and 230 °C with a second closed-vessel microwave apparatus. The results for 10 elements in biological standard reference materials agree well with the certified values.

Greening microwave-assisted acid digestion of animal feed samples

2019 ◽  
Vol 11 (46) ◽  
pp. 5857-5863 ◽  
Author(s):  
Marianela Savio ◽  
Lucimar L. Fialho ◽  
Joaquim A. Nóbrega
Keyword(s):  
Nitric Acid ◽  
Green Chemistry ◽  
Animal Feed ◽  
Acid Digestion ◽  
Microwave Assisted ◽  
Nitric Acid Digestion ◽  
Recycle And Reuse ◽  
Feed Samples ◽  
Dilute Nitric Acid

The combination of dilute nitric acid digestion followed by recovery of the acid digests, represents steps towards green chemistry approaches: “reduce the use, recycle and reuse”, strictly following the major green chemistry recommendations.

Determination of Trace Elements in Water by Inductively Coupled Plasma–Mass Spectrometry: Collaborative Study

1994 ◽  
Vol 77 (4) ◽  
pp. 1004-1023 ◽  
Author(s):  
J E Longbottom ◽  
T D Martin ◽  
K W Edgell ◽  
S E Long ◽  
M R Plantz ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Trace Elements ◽  
Inductively Coupled Plasma ◽  
Acid Digestion ◽  
Inductively Coupled ◽  
Icp Ms ◽  
Relative Standard ◽  
Nitric Acid Digestion ◽  
Plasma Mass Spectrometry

Abstract A joint U.S. Environmental Protection Agency (U.S. EPA)—AOAC interlaboratory method validation study was conducted on U.S. EPA method 200.8, Determination of Trace Elements in Waters and Wastes by Inductively Coupled Plasma–Mass Spectrometry. The purpose of the study was to determine and compare the mean recovery and precision of the inductively coupled plasma–mass spectrometry (ICP–MS) analyses for 20 trace elements in reagent water, drinking water, and groundwater. The formal study was based on Youden’s nonreplicate plan for collaborative tests of analytical methods. The test waters were spiked with the 20 trace elements at 6 concentration levels in the 0.8–200 μg/L range, prepared as 3 Youden pairs. Thirteen collaborators spiked 100 mL aliquots of the test waters, acidified them with 1 mL concentrated HNO3 and 0.5 mL concentrated HCl, reduced the volume to 20 mL by heating in an open beaker at 85°C, refluxed them for 30 min at 95°C, and diluted them to 50 mL. After centrifuging or settling the samples, a 20 mL portion of the supernatant was diluted to 50 mL and analyzed by ICP–MS. Related experiments evaluated the method performance in wastewater and wastewater digestate at a single concentration pair, and an alternative nitric acid digestion procedure. Mean recoveries for reagent water, drinking water, and groundwater were generally 95–105% with between-laboratory relative standard deviations about 4–8%. The method also worked well with wastewaters and digestate, with between-laboratory relative standard deviations averaging 8% and recoveries averaging 100%. Recoveries of silver, however, were low in all matrixes at concentrations over 100 μg/L. The nitric acid digestion procedure was comparable in accuracy and precision to the mixed-acid digestion in U.S. EPA method 200.8. The method was adopted first action by AOAC INTERNATIONAL.

scholarly journals Determination of Micronutrients in Feed Products by Inductively Coupled Plasma Mass Spectrometry

1998 ◽  
Vol 81 (5) ◽  
pp. 923-930
Author(s):  
James S Mcguire ◽  
Douglas A Hite
Keyword(s):  
Nitric Acid ◽  
High Purity ◽  
Inductively Coupled Plasma ◽  
Element Analysis ◽  
Inductively Coupled ◽  
Ultra High Purity ◽  
Feed Control ◽  
Icp Ms ◽  
Nitric Acid Digestion ◽  
Plasma Mass Spectrometry

Abstract Micronutrients are widely used in feed products and are very important to the health and productivity of farm and domestic animals. It is imperative to have analytical capabilities for rapid and accurate results. By using a simple nitric acid digestion of the feed coupled with inductively coupled plasmamass spectrometry (ICP/MS), rapid and accurate results can be obtained. ICP/MS has many advantages over classical wet chemical methods, atomic absorption methods, and other ICP methods: speed of analysis, reduced standards preparation, reduced waste stream, and qualitative scan capabilities. One gram portions of feed products were placed into 250 mL volumetric flasks and digested with 30 mL concentrated high-purity nitric acid for about 20 min. They were then brought to volume with ultra-high-purity water, shaken, and filtered. Ten milliliter portions were taken, and 0.5 mL internal standards were added. Standards were made up in concentrations to agree with the expected range of the desired element. Analysis of check samples from the Association of American Feed Control Officials shows that this method is comparable with other methods of choice

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