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Technical Note: Using FIMS to determine mercury content in sewage sludge, sediment and soil samples

Journal of Automatic Chemistry
Hindawi Publishing Corporation
Publication Date
DOI: 10.1155/s1463924696000272
  • Research Article
  • Mathematics


Journal of Automatic Chemistry, Vol. 18, No. 6 (November-December 1996) pp. 221-223 Technical Note: Using FIMS to determine mercury content in sewage sludge, sediment and soil samples Tiezheng Guo and J6rn Baasner Bodenseewerk Perkin-Elmer GmbH, berlingen, Germany The Flow Injection Mercury System (FIMS) is an dedicated system that integrates flow injection mercury cold vapour generation with a very sensitive detector. Instrumental detection limits can be as low as 5 ng/1 using a sample volume of 500 tl. The FIMS permits sample dilution, therefore reducing the likelihood of an interference occurring with complex samples. In this study samples were digested with aqua regia using reflux conditions according to DIN method 38414. After proper dilution of the digested sample solution, Hg was measured interference free using SnC12 as the reductant. The recoveries of spiked mercury in sewage sludge samples ranged from 96 to 100%. The method was checked by the analysis of standard reference materials. All results were in agreement with certified values. The RSD for three replicates was approximately 2% at 10 tg/1 Hg levels. The sample solutions were also measured using an FIAS to generate the Hg vapour and the analytical data was collected using an AA spectrometer equipped with a 02 background corrector. The results are in agreement with those obtained with the FIMS, which demonstrates that any background absorption for these determinations was negligible. Carrier solution 3% v/v HC1. 30 ml HC1 was diluted to 11 with deionized water. Stabilizing solution 0"5% m/v K2Cr207 in + HNOa 0"5 g K2Cr207 was dissolved in 50 ml of water, and 50 ml of concentration HNOa was added. Calibration standards Stock standard mercury solution #1, 1000 mg/1, was prepared from Merk Tritisol(R). Stock mercury solutions #2 and #3:10 mg/1 and mg/1 respectively, were pre- pared by further dilution of the stock standard solution #1. Calibration standards at different mercury levels were prepared from stock solutio

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