University of North Florida
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Stuart Chalk, Ph.D.
Department of Chemistry
University of North Florida
Phone: 1-904-620-1938
Fax: 1-904-620-3535
Website: @unf

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Classification: Reference Material -> NRCC -> PACS-1 -> Harbour sediment

Citations 4

"Determination Of Mercury Traces In Products Of TiO2 Manufacturing"
Analusis 1999 Volume 27, Issue 5 Pages 472-475
N. Mikac, S. Gressier and M. Wartel

Abstract: A simple method far the determination of mercury traces in co-products and final products of titanium (IV) oxide manufacturing was developed. It was shown that different procedures recommended for the total digestion of such materials (using mixtures of HF HNO3, HCl and HClO4) could be efficiently replaced by an unique partial digestion method based on mercury leaching from sample by HNO3. Partial digestion method was much quicker and more sensitive than total digestion methods. Mercury was detected with cold vapor atomic fluorescence spectroscopy and a detection limit of 10 pgHg/g was achieved. The method was validated using certified reference materials PACS-1 (NRCC) and maroccan phosphate rock (BCR). Regarding mercury content in analyzed samples from the point of view of the ecological risk, only residual material after first digestion of raw material with H2SO4 were found to contain mercury concentrations higher than accepted background value for sediment and soils (0.1 µgHg/g). All other cc-products as well as the final product titanium (TV) oxide were almost free of mercury (<0.01 -30 ngHg/g).

"Determination Of Cadmium In Environmental Samples By Hydride Generation With In Situ Concentration And Atomic Absorption Detection"
Analyst 1997 Volume 122, Issue 4 Pages 331-336
Henryk Matusiewicz, Mariusz Kopras and Ralph E. Sturgeon

Abstract: A continuous-flow AAS system for Cd determination is described. A Cd solution acidified with HCl was mixed with 1 µg/ml Co and 0.5% thiourea (and also with 0.01 M didodecyldimethyl-ammonium bromide for reaction with KBH4) and diluted to 1 mL with water. The resulting solution was aspirated at a flow rate of 1 ml/min into a continuous-flow system and merged with a stream of either 2% NaBH4 or 4% KBH4 at a flow rate of 1 ml/min. The mixture was passed through a reaction cell/gas-liquid separator maintained at 50°C and the volatile Cd species evolved were carried by an Ar stream on to the inner wall of a GF for in situ pre-concentration at 200°C. Cd analysis was by ET AAS with atomization at 1800°C for 3 s; detection was at at 228.8 nm. The detection limit was 10 ng/l Cd with KBH4 as reagent. RSD were 10^-14% (n = 10). The method was applied to several environmental and biological CRM. The results obtained agreed with the certified values.
Cadmium Spectrophotometry Heated reaction Volatile generation Reference material Phase separator Preconcentration Volatile generation

"Determination Of Total Mercury In Sediments By Microwave-assisted Digestion - Flow Injection Inductively Coupled Plasma Mass Spectrometry"
J. Anal. At. Spectrom. 1997 Volume 12, Issue 1 Pages 53-56

Abstract: Dry sediment (0.25 g) was digested in an open vessel with 8 mL of HNO3 and again after cooling for 5 min and addition of 2 mL of 30% H2O2, in both instances at 20 W for 5 min. The digest was then diluted with water to the required concentration range of Hg; 5 mL portions of the analytical solution contained 0.1% of Triton X-100, 0.1% of EDTA, 0.1% (v/v) of aqueous NH3, 20 ng/ml of Tl (internal standard), and standard additions of 0-40 ng of Hg. The analysis was based on the ICP-MS detection of 202Hg, while 200Hg was detected for confirmation. The detection limit was 1 ng/g. Recoveries were 95-105%, and results for the reference materials PACS-1, IAEA-356 and S19 agreed well with the certified values.
Mercury Mass spectrometry Sample preparation Reference material Triton X Standard additions calibration Surfactant

"Ion-spray Mass Spectrometry - Mass Spectrometry: Quantitation Of Tributyltin In A Sediment Reference Material For Trace Metals"
Anal. Chem. 1989 Volume 61, Issue 20 Pages 2320-2322
K. W. Michael Siu, G. J. Gardner, and S. S. Berman

Abstract: The reference material, viz, PACS-1, was sonicated with methanol - 10 M HCl (2:1) and extracted with 2,2,4-trimethylpentane, and the extract was diluted with methanolic 1 mM ammonium acetate. Alternatively, the sample was sonicated with butan-1-ol and the extract was likewise diluted. The solution were delivered to the ion-spray source by flow injection. Detection was by selected-ion monitoring of the daughter - parent pair at m/z 179/291. The result of 1.29 ppm with a standard deviation (n = 5) of 0.07 ppm was in close agreement with the certified value.
Tributyltin Sample preparation Mass spectrometry Extraction Dilution Reference material