Assessment of Dissolution of Silicate Rock Reference Materials with Ammonium Bifluoride and Nitric Acid in a Microwave Oven

2018 ◽  
Vol 43 (1) ◽  
pp. 189-208 ◽  
Author(s):  
Thais T. Magaldi ◽  
Margareth S. Navarro ◽  
Jacinta Enzweiler
2017 ◽  
Vol 105 (8) ◽  
Author(s):  
Nicholas T. Hubley ◽  
John D. Brockman ◽  
J. David Robertson

AbstractDissolution of geological reference materials by fusion with ammonium bifluoride, NH


2020 ◽  
Vol 100 (4) ◽  
pp. 393-407
Author(s):  
Muhammad Babar Javed ◽  
Iain Grant-Weaver ◽  
William Shotyk

A robust and reliable analytical procedure for the determination of trace (mg∙kg−1) and ultra-trace elements (μg∙kg−1) in soil and sediments by inductively coupled plasma quadrupole mass spectrometry (ICP-QMS) was optimized. Aliquots of ∼200 mg of two certified reference materials (IAEA Soil-7, soil and IAEA SL-1, lake sediments) were digested in nitric acid (HNO3) purified twice by sub-boiling distillation using a microwave-heated high-pressure autoclave. Incremental addition of tetrafluoroboric acid (HBF4, 0.1–2 mL) to HNO3 was evaluated for yield. The selection of appropriate proportions of digestion acids was crucial to obtain accurate results. Digested samples were analyzed for a range of trace elements including those that are potentially toxic (Ag, Cd, Pb, Sb, and Tl), plant micronutrients (Cu, Fe, Mn, and Zn), those enriched in bitumen (Mo, Ni, and V), and lithophile elements (Al, Ba, Co, Cr, Rb, Sr, Th, Ti, Y, and Zr). Nitric acid alone proved to be sufficient to completely liberate Cd, Co, Cr, Fe, Mn, Ni, Pb, V, and Zn in both soil and sediments (87%–120% recovery). For almost all the other elements, addition of HBF4 was needed for improved recovery. A combination of 3 mL of HNO3 and 1.5 mL of HBF4 was optimal to fully liberate an extended list of elements including Ba, Sb, and Sr from both the reference materials. Conservative lithophile elements (Th, Ti, Y, and Zr) could not be completely recovered with the proposed method, requiring hydrofluoric acid for complete dissolution of recalcitrant minerals.


1985 ◽  
Vol 68 (4) ◽  
pp. 766-769
Author(s):  
Thomas R White ◽  
Garnett E Douthit

Abstract A sample preparation method has been developed that provides a nitric acid-hydrogen peroxide digestion of plant tissue when it is heated internally by the oscillating electromagnetic field generated in a microwave oven. The total elemental concentration for barium, calcium, magnesium, manganese, phosphorus, potassium, sodium, sulfur, and zinc can be determined by inductively coupled argon plasma emission spectroscopy after sample preparation in a microwave oven. The method is rapid and provides quantitative results that agree with certified values for 4 National Bureau of Standards Standard Reference Materials: 1570 Spinach, 1572 Citrus Leaves, 1573 Tomato Leaves, and 1575 Pine Needles.


2017 ◽  
Vol 105 (12) ◽  
Author(s):  
Christian A. Mason ◽  
Nicholas T. Hubley ◽  
J. David Robertson ◽  
Dana L. Wegge ◽  
John D. Brockman

AbstractThere is significant interest in reducing the timeline for post detonation nuclear debris examination. A critical need is rapid dissolution of refractory nuclear debris to facilitate measurement of key radioisotopes and isotope ratios. Field deployable, rapid dissolution and analysis methods could significantly shorten the attribution analysis timeline. The current practice uses HF in combination with other acids to attack silicates and other refractory minerals expected in debris samples. However, techniques requiring HF are not amenable to use in the field. The fluorinating agent ammonium bifluoride (ABF) is a potential field deployable substitute for HF. In this work we report on the use of in-direct sonication with ABF as a means to improve low-temperature acid digestion of seven USGS and NIST geological reference materials. Using this method, elemental recoveries for USGS reference materials DNC-1a Dolerite, QLO-1a Quartz Latite, SDC-1 Mica Schist, and BHVO-2 Hawaiian Basalt were quantitative while the recovery of elements in USGS AGV-2 Andesite and NIST SRM 278 Obsidian and 1413 High Alumina Sand were low.


2019 ◽  
Vol 70 (9) ◽  
pp. 3225-3227
Author(s):  
Adina Magdalena Bunget ◽  
Michael Schenker ◽  
Alin Dragos Demetrian ◽  
Aurel Gherghina ◽  
Lucretiu Radu ◽  
...  

The purpose of this study was to perform a comparative study of cations in the vegetative organs of Sambucus ebulus by applying three different methods of digestion before atomic absorption spectrometry. Of the tested methods, the most effective was method 3 (mineralisation with nitric acid in a microwave oven), the other methods of sample digestion leading to incomplete mineralization of the samples and implicitly to the incomplete transfer of the analytes into solution, reflecting the slightly different contents in metal cations we obtained.


The Analyst ◽  
1991 ◽  
Vol 116 (9) ◽  
pp. 957 ◽  
Author(s):  
Suei Y. LamLeung ◽  
Vincent K. W. Cheng ◽  
Yuet W. Lam

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