General aspects of trace analytical methods-VI. Acid pressure decomposition in trace element analysis

Jackwerth, E.; Gomišček, S.

doi:10.1351/pac198456040479

Cited by 68 publications

(17 citation statements)

References 6 publications

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“…The autoclave system, also known as digestion bomb using polytetrafluoroethylene (PTFE) interior reinforced with steel has been widely used in digestion procedures after 1960. 14 The autoclave system was often convectively heated which enabled the digestion of large number of samples, for example in laboratory drying oven. The digestion of inorganic matrices was extensively studied 15,16 but, however, the research related to digestion of plastics was limited until the development of commercial high pressure asher (HPA) and microwave-assisted (MW-AD) digestion systems.…”

Section: Introductionmentioning

confidence: 99%

Determination of metal concentrations in certified plastic reference materials after small-size autoclave and microwave-assisted digestion followed with inductively coupled plasma optical emission spectrometry

Lehtimäki

Väisänen

2017

Spectrochimica Acta Part B: Atomic Spectroscopy

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The digestion methods for the determination of As, Cd, Cr, Pb, Sb, Sn and Zn concentrations in plastic samples using microwave-assisted digestion (MW-AD) and small-size autoclave digestion was developed. The certified polyethylene, polypropylene, polyvinyl chloride and acrylonitrile butadiene styrene certified reference materials were used in order to find digestion method working properly for several sample matrices. Efficiency of the digestion methods was evaluated by analyzing the residual carbon in digests by TOC analyzer. MW-AD using a mixture of 7 mL of HNO 3 and 3 ml of H 2 O 2 as a digestion solution resulted in excellent recoveries for As, Cd, Pb, Sb and Zn, and were in the range of 92-107 % for all the analytes except Pb in polyethylene material. Autoclave digestion using 5 mL of concentrated HNO 3 as a digestion solution resulted in similar recoveries with the exception of a higher As recovery (98 %). Tin recovery resulted in low level after both MW-AD and autoclave digestion. Autoclave digestion was further developed resulting in a partially open two-step digestion process especially for the determination of Sn and Cr. The method resulted in higher recoveries of Sn and Cr (87 and 76 %) but with the lower concentration of easily volatile As, Cd and Sb.

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Section: Introductionmentioning

confidence: 99%

Determination of metal concentrations in certified plastic reference materials after small-size autoclave and microwave-assisted digestion followed with inductively coupled plasma optical emission spectrometry

Lehtimäki

Väisänen

2017

Spectrochimica Acta Part B: Atomic Spectroscopy

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“…Allen et al (1974) used open vessels, enabling HF acid to be fumigated along with silicon, reducing matrix interferences in the subsequent analysis. More commonly sealed acid pressure vessels are used which ensure more complete dissolution (Jackwerth and Gomiscek 1984;Garçon et al 2012), but which then requires greater care in the management of matrix effects. Boric acid (H 3 BO 3 ) is added to make the solution safe.…”

Section: Extraction Methodsmentioning

confidence: 99%

Lacustrine Archives of Metals from Mining and Other Industrial Activities—A Geochemical Approach

Boyle

Chiverrell

Schillereff

2015

Environmental Contaminants

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Since the first studies reporting recent stratigraphic changes of metal concentration in lake sediments, many hundreds of studies have been published in the peer-reviewed literature. It is an impossible task to do justice to all of these works here; instead we: (1) examine recent methodological advances and place these in the context of the historical development of the discipline; and (2) explore the various purposes to which such methods have been applied. Such a historical emphasis may appear in conflict with the needs of a review of new approaches; however, this is not in fact the case for two main reasons. First, most new advances supplement rather than replace traditional methods, such that a thorough understanding of the practical and theoretical issues impacting these is still essential for reliable interpretation of palaeolimnological data. Second, while many of the new methods purport to circumvent problems, they achieve this only under favourable conditions, not dissimilar to the conditions that influence the earlier methods, so the same lesson must be learned anyway. Consequently, we use this historical narrative to address the fundamentals of the discipline.The chapter comprises two main parts; methodology and applications. The methodological section has three subsections: (1) Introduction to processes controlling natural variations in metal fluxes and concentrations in lake sediments; (2) Measurement of metal concentrations in sediments; (3) Calculation of enrichment or fluxes from sediment metal concentration data.There are four main applications subsections focusing on the value of lake sediment records of metals derived from mining or industry. They are: (1) Geochronological markers in sediments providing chronology for other research goals; (2) Lake sediment heavy metal records to quantify pollution loading histories, or to

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“…The total metal content of the calcined samples and residues was measured after complete dissolution using a pressure decomposition system [13] as follows. A powdered sample, either the calcined sample (1/10 of the total weight) or the solid residue, was added to 12 M HCl (10 mL) in a PTFE inner vessel.…”

Section: Characterizationmentioning

confidence: 99%

Dissolution Process of Palladium in Hydrochloric Acid: A Route via Alkali Metal Palladates

Kasuya

Miki

Morikawa

et al. 2015

Metall Mater Trans B

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To improve the safety of the Pd recovery processes that use toxic oxidizers, dissolution of Pd in hydrochloric acid with alkali metal palladates was investigated. Alkali metal palladates were prepared by calcining a mixture of Pd black and alkali metal (Li, Na, and K) carbonates in air. Almost the entire amount of Pd was converted into Li 2 PdO 2 after calcination at 1073 K (800°C) using Li 2 CO 3 . In contrast, PdO was obtained by calcination at 1073 K (800°C) using Na and K carbonates. Our results indicated that Li 2 CO 3 is the most active reagent among the examined alkali metal carbonates for the formation of palladates. In addition, dissolution of the resulting Li 2 PdO 2 in HCl solutions was evaluated under various conditions. In particular, Li 2 PdO 2 rapidly dissolved in diluted (0.1 M) HCl at ambient temperature. Solubility of Pd of Li 2 PdO 2 was found to be 99 pct or larger after dissolution treatment at 353 K (80°C) for 5 minutes; in contrast, PdO hardly dissolved in 0.1 M HCl. The dissolution mechanism of Li 2 PdO 2 in HCl was also elucidated by analysis of crystal structures and particulate properties. Since our process is completely free from toxic oxidizers, the dissolution process via alkali metal palladates is much safer than currently employed methods.

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General aspects of trace analytical methods-VI. Acid pressure decomposition in trace element analysis

Abstract: Abstract

Cited by 68 publications

References 6 publications

Determination of metal concentrations in certified plastic reference materials after small-size autoclave and microwave-assisted digestion followed with inductively coupled plasma optical emission spectrometry

Determination of metal concentrations in certified plastic reference materials after small-size autoclave and microwave-assisted digestion followed with inductively coupled plasma optical emission spectrometry

Lacustrine Archives of Metals from Mining and Other Industrial Activities—A Geochemical Approach

Dissolution Process of Palladium in Hydrochloric Acid: A Route via Alkali Metal Palladates

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