PMID- 18329794 OWN - NLM STAT- MEDLINE DCOM- 20090107 LR - 20131121 IS - 0304-3894 (Print) IS - 0304-3894 (Linking) VI - 157 IP - 2-3 DP - 2008 Sep 15 TI - Determination of Cd, Co, Ni and Pb in biological samples by microcolumn packed with black stone (Pierre noire) online coupled with ICP-OES. PG - 410-7 LID - 10.1016/j.jhazmat.2008.01.014 [doi] AB - A simple and sensitive method using microcolumn (20-mm length x 2.0-mm i.d.) packed with black stone (Pierre noire) for the separation/preconcentration of Cd, Co, Ni and Pb in biological samples prior to their online determination by inductively coupled plasma optical emission spectrometry (ICP-OES) has been developed. Optimal experimental conditions including pH, eluent concentration and volume, sample volume and sample flow rate were investigated and established. The adsorption capacity of black stone for Cd, Co, Ni and Pb were found to be 23.4, 21.2, 18.1 and 22.2 mg g(-1), respectively. With a preconcentration time of 72 s and an elution time of 4s, an enrichment factor of 20 and a sampling frequency of 25 h(-1) were obtained. The detection limits corresponding to three times the standard deviations of the blank for Cd, Co, Ni and Pb were found to be 0.3, 0.4, 0.4 and 1.1 ng mL(-1). The precision for seven replicate determinations of Cd, Co, Ni and Pb gave relative standard deviations (RSDs) of 5.9, 4.8, 2.7 and 1.1%, respectively (n=7, C=10 ng mL(-1)). The method was validated with certified reference material GBW09103 human urine and the results obtained were in good agreement with the certified values. The method was also applied to the determination of the target analytes in biological samples with satisfactory results. FAU - Suleiman, Jibrin Sabo AU - Suleiman JS AD - Department of Chemistry, Wuhan University, Wuhan, China. FAU - Hu, Bin AU - Hu B FAU - Huang, Chaozhang AU - Huang C FAU - Zhang, Nan AU - Zhang N LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20080112 PL - Netherlands TA - J Hazard Mater JT - Journal of hazardous materials JID - 9422688 RN - 00BH33GNGH (Cadmium) RN - 2P299V784P (Lead) RN - 3G0H8C9362 (Cobalt) RN - 7OV03QG267 (Nickel) SB - IM MH - Adsorption MH - Cadmium/*analysis MH - Cobalt/*analysis MH - Geologic Sediments/*chemistry MH - Hydrogen-Ion Concentration MH - Lead/*analysis MH - Nickel/*analysis MH - Spectrophotometry, Atomic EDAT- 2008/03/11 09:00 MHDA- 2009/01/08 09:00 CRDT- 2008/03/11 09:00 PHST- 2007/09/06 00:00 [received] PHST- 2008/01/03 00:00 [revised] PHST- 2008/01/03 00:00 [accepted] PHST- 2008/03/11 09:00 [pubmed] PHST- 2009/01/08 09:00 [medline] PHST- 2008/03/11 09:00 [entrez] AID - S0304-3894(08)00042-3 [pii] AID - 10.1016/j.jhazmat.2008.01.014 [doi] PST - ppublish SO - J Hazard Mater. 2008 Sep 15;157(2-3):410-7. doi: 10.1016/j.jhazmat.2008.01.014. Epub 2008 Jan 12.