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Inductively Coupled Plasma Mass Spectrometry In The Analysis Of Precious Metals

Posted on:2009-09-06Degree:MasterType:Thesis
Country:ChinaCandidate:S Q LiuFull Text:PDF
GTID:2191360245972001Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
The chapter 1 mainly reviewed the progress in species and quantitative analysis of platinum group element, 71 references were cited.A brief view was given on origin, development and latest progress of inductively coupled plasma mass spectrometry (ICP-MS) in chapter 2. The interference from mass spectra and non mass spectra, ways to eliminate interference (for example, cool plasma, and shield torch, collision and reaction cell) was introduced in details. A method for determination of noble metals in geo-chemical standard reference samples by ICP–MS is established in chapter 3. The effects of different digestion methods for noble metal are compared and a correct equation for determination Pd was established. By using the correct equation, mass spectrum interferences of Pd could be eliminated efficiently. The detection limits of the method were 1.59ng.g-1 for Pt, 0.82ng.g-1 for Pd and0.04ng.g-1 for Rh. The precision (n=12) is between 3.4%~ 13.0% was obtained. The proposed method has offered a reference for the determination of platinum group elements (PGEs) in geo-chemical samples.The chapter 4 studied the method of inductive coupling plasma mass (ICP- MS) for determination of the platinum group elements (PGEs) Pt, Pd, Rh in environment samples. The different digestion methods and digestion systems for PGEs in the environment samples were compared. The microwave digestion is more efficient than the ordinary aqueous method. The limits of determination of Pt, Pd, Rh respectively are 0.02 ng.g-1, 0.05 ng.g-1, 0.002 ng.g-1. The recoveries are between 91.05%-107.0%. The linear range is 0 ~ 2μg/ml, the correlation coefficients all are bigger than 0.9999. The PGEs in the environment samples include the fish sample that from the market and the rivers or lakes of Beijing were determined. The impact of PGEs on environment of Beijing was discussed.The fish samples from Beijing region were pretreated by microwave digestion and two PGEs metals Pd and Rh content were determined by ICP-MS in chapter 5. The results showed that the accumulation of various metals in tissues and organs of fish were significantly different. Rh and Pd occurred mainly in the gills and viscera. In the same organs the level of PGEs is: Rh> Pd. Pt was not found in samples. In Chapter 6, roadside soil samples collected from the Beijing metropolitan area (China) were evaluated to determine the distribution and the concentration of platinum group elements (PGEs). The dust particles that were smaller than 100 mesh size fraction (150 mm) were analyzed after aqua regia digestion. Concentrations of Pt, Pd, and Rh were found to be between 2.46 ng.g-1 -174.5 ng.g-1, 15.11 ng.g-1 -1416 ng.g-1,2.2 ng.g-1 -49.57 ng.g-1, respectively, in the urban areas of Beijing, whereas for the background samples collected from the suburbs of Beijing, the concentration of Pt, Pd, and Rh were very low and ranged from 0.1 to 0.9 ng.g-1, 0.5 to 1.4 ng.g-1, and 0.8 to 2.2 ng.g-1, respectively. The distributions of PGEs in road dust were an accurate reflection of the levels of pollution and were found to match with the local traffic conditions.Chapter 7 investigated the effects of temperature and acidity on the stability of Pt (II) (Na2PtCl6) and Pt (IV) (K2PtCl4). The results indicated that the temperature is evidence influence the stability of Pt (II) and acidic solution (pH 2) can stabilize Pt (II). The stability of Pt (II) at normal temperature is rather poor. The separate condition of Pt (II) and Pt IV) on HPLC and HPLC-MS were discussed.
Keywords/Search Tags:soil, PGE, microwave digestion, ICP- MS, distribution
PDF Full Text Request
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