Mercury speciation in sea food by flow injection cold vapor atomic absorption spectrometry using selective solid phase extraction.
An on-line inorganic and organomercury species separation, preconcentration and determination system consisting of cold vapor atomic absorption spectrometry (CV-AAS or CV-ETAAS) coupled to a flow injection (FI) method was studied. The inorganic mercury species was retained on a column (i.d., 3 mm; length 3 cm) packed to a height of 0.7 cm with a chelating resin aminopropyl-controlled pore glass (550 A) functionalized with [1,5-bis (2 pyridyl)-3-sulphophenyl methylene thiocarbonohydrazyde] placed in the injection valve of a simple flow manifold. Methylmercury is not directly determined. Previous oxidation of the organomercurial species permitted the determination of total mercury. The separation of mercury species was obtained by the selective retention of inorganic mercury on the chelating resin. The difference between total and inorganic mercury determined the organomercury content in the sample. The inorganic mercury was removed on-line from the microcolumn with 6% (m/v) thiourea. The mercury cold vapor generation was performed on-line with 0.2% (m/v) sodium tethrahydroborate and 0.05% (m/v) sodium hydroxide as reducing solution. The determination was performed using CV-AAS and CV-ETAAS, both approaches have been used and compared for the speciation of mercury in sea food. A detection limit of 10 and 6 ng l(-1) was achieved for CV-AAS and CV-ETAAS, respectively. The precision for 10 replicate determinations at the 1 microg l(-1) Hg level was 3.5% relative standard deviation (R.S.D.), calculated from the peak heights obtained. Both approaches were validated with the use of two certified reference materials and by spiking experiments. By analyzing the two biological certified materials, it was evident that the difference between the total mercury and inorganic mercury corresponds to methylmercury. The concentrations obtained by both techniques were in agreement with the certified values or with differences of the certified values for total Hg(2+) and CH(3)Hg(+), according to the t-test for a 95% confidence level. It is amazing how this very simple method is able to provide very important information on mercury speciation.
Vereda Alonso
E
E
Department of Analytical Chemistry, Faculty of Sciences, University of Málaga, E-29071 Málaga, Spain. eivereda@uma.es
Siles Cordero
M T
MT
García de Torres
A
A
Cañada Rudner
P
P
Cano Pavón
J M
JM
D000818:Animals; D003080:Cold Temperature; D017022:Flow Injection Analysis / Q000295:instrumentation* / Q000379:methods*; D008628:Mercury / Q000302:isolation & purification*; D017669:Mercury Compounds / Q000032:analysis; D015394:Molecular Structure; D008974:Mollusca / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000295:instrumentation / Q000379:methods*; D013054:Spectrophotometry, Atomic / Q000295:instrumentation* / Q000379:methods*; D014835:Volatilization
D017669:Mercury Compounds; D008628:Mercury