Off-campus UMass Amherst users: To download dissertations, please use the following link to log into our proxy server with your UMass Amherst user name and password.

Non-UMass Amherst users, please click the view more button below to purchase a copy of this dissertation from Proquest.

(Some titles may also be available free of charge in our Open Access Dissertation Collection, so please check there first.)

Determination and speciation of arsenic in environmental and biological samples

Tiffany Berg, University of Massachusetts Amherst

Abstract

A method was developed for the determination of total arsenic in rice grain by microwave-assisted digestion inductively coupled plasma mass spectrometry. Standard calibration solutions were matrix-matched with respect to acid concentration and carbon content post-digest. The importance of eliminating the drying step during sample preparation procedures was investigated. The method was validated with spikes containing standard arsenate solutions into the rice matrix, and with certified reference material SRM1568a (rice flour) from NIST. The method was successfully applied to a commercially available rice sample. ^ Four arsenic species [arsenate (As(V)), arsenite (As(III)), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA)] were extracted from rice grains by microwave-assisted extraction and separated with high performance liquid chromatography inductively coupled plasma mass spectrometry. The method includes a novel sample clean-up step involving a dialysis procedure to decrease the amount of large starch molecules in the injection solution, in order to minimize poor resolution of chromatographic peaks and maximize column life. The method was validated with spikes of standard arsenic solutions, added to the rice matrix before the extraction procedure. Literature reference values for arsenic species quantification in SRM1568a (rice flour) were also compared. This method was successfully applied to a commercially available rice sample. ^ A study into improvements in reverse phase-HPLC separations of arsenic species was conducted. For the first time, a Sunfire C8 column from Waters (Milford, CT) was employed for the separation of arsenic species in rice extracts. This column was compared to a Symmetry C8 column with respect to total elution time, detection limits, interference effects, and column life, and evaluated with respect to peak resolution, shifts in retention times, and peak symmetry. ^

Subject Area

Analytical chemistry

Recommended Citation

Berg, Tiffany, "Determination and speciation of arsenic in environmental and biological samples" (2012). Doctoral Dissertations Available from Proquest. AAI3545903.
http://scholarworks.umass.edu/dissertations/AAI3545903

Share

COinS