Sample preparation methods Microwave digestion

The ICP was a Perkin-Elmer 3000DV with an AS90 Autosampler, which has an instrument detection limit of about 1 ppb (for most elements) with a linear calibration up to 100 ppm (for most elements). Solid samples were prepared via microwave digestion in concentrated nitric and hydrochloric acids, then diluted to volume. The ICP was calibrated and verified with two independent, certified standard sets. Spikes and dilutions were done for each batch of samples to check for and/or mitigate any matrix effects. The ICP process ran a constant pump rate of 1.5 mL/min for all samples and standards during analysis. A 3 mL/min rinse and initial sample flush were used to switch between each sample and standard. The plasma was run at 1450 W with argon flow. Trace metal-grade (sub-ppb) acids and two independently NIST-certified calibration standard sets were used for calibration and method verification. 

Sample Preparation Using Microwave Acid Digestion Method... 

The concentration of metals that are detrimental to catalysts added can vary between 20.0 ppm for Fe to 100 ppm for Ni and lOOOppm for V. The presence of these metals necessitates the need for analysis of these metals to determine their concentrations prior to the cracking process. The best method to analyse these oil samples needs to be rapid and accurate. Careful selection of the method either from experience or by trial and error may be applied depending on the metal and the concentration. Sample dissolution in a solvent or solvent mixture is considered the easiest but may not be suitable for low limits of detection. Destructive sample preparation methods, i.e. oxygen bomb combustion, microwave acid digestion followed by pre-concentrating may be required for trace analysis and/or with the aid of a hyphenated system, e.g. ultrasonic nebuliser. Samples prepared by destmctive methods are dissolved in aqueous solutions that have very low matrix and spectral interferences. 

SB 8-27. Challenge Problem. Zwanziger and Sarbu conducted a study to validate analytical methods and instruments. The following data are results obtained in the determination of mercury in solid wastes by atomic absorption spectroscopy using two different sample preparation methods a microwave digestion method and a traditional digestion method. 

Mineralisation consists of the destruction of organic matter. Dry (oven) or humid (acid treatment) methods can be used for this purpose. Due to the absence of a universal method applicable to all mineral elements, it is necessary to adapt mineralisation to the sample being analysed. This stage, which is indispensable for the preparation of many types of samples, particularly those analysed by atomic absorption or emission, can be facilitated by the use of microwave digestion. 

Inductively coupled plasma-mass spectrometry (ICP-MS) has been utilized as a bulk technique for the analysis of obsidian, chert and ceramic compositional analyses 12-14). However, due to the high level of spatial variation of ceramic materials, increased sample preparation is necessary with volatile acids coupled with microwave digestion (MD-ICP-MS) to properly represent the variability of ceramic assemblages IS, 16). Due to the increased sample preparation and exposure to volatile chemicals, researchers have continued to utilize neutron activation analysis (INAA) as the preferred method of chemical characterization of archaeological ceramics (77). 

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