Speciation of lead and methyllead ions in water by chromatography/atomic absorption spectrometry after ethylation with sodium tetraethylborate

A novel method for speciation and determination of Me/sub 3/Pb/sup +/ and Me/sub 2/Pb/sup 2 +/ is described. The procedure includes in situ ethylation by sodium tetraethylborate (NaBEt/sub 4/) in water, purging and trapping of alkyllead molecules, and thermal desorption in an electrically heated quartz AAS furnace. The absolute detection limits of Pb for 50 cm/sup 3/ are ca. 8.7 pg for Me/sub 3/Pb/sup +/ (0.18 pg/cm/sup 3/) and ca. 10.5 pg for Me/sub 2/Pb/sup 2 +/ (0.21 pg/cm/sup 3/). Major advantages for the technique are avoidance of solvent extraction and ample transfers because ethylation to Me/sub 3/EtPb and Me/sub 2/Et/sub 2/Pb takes place in a closed system. Reaction conditions and apparatus operating parameters were optimized by a Simplex algorithm. 24 refs., 3 figs., 1 tab.

[1]  D. J. Hodges,et al.  Determination of ionic alkyl lead species in marine fauna , 1981 .

[2]  D. Chakraborti,et al.  Determination of ionic alkyllead compounds in water by gas chromatography/atomic absorption spectrometry. , 1984, Analytical chemistry.

[3]  R. Pretorius,et al.  The isotopic analysis of boron by the coincident measurement of complementary particles , 1975 .

[4]  P. Bievre,et al.  Boron isotopic measurements by thermal ionization mass spectrometry using the negative BO2− ion , 1983 .

[5]  Julian B. Honeycutt,et al.  Preparation and Reactions of Sodium Tetraethylboron and Related Compounds1 , 1961 .

[6]  M. Stoeppler,et al.  Evidence for the absence of biological methylation of lead in the environment , 1981, Nature.

[7]  M. Caprais,et al.  Degradation of tel in seawater , 1982 .

[8]  R. Harrison,et al.  Determination of tetraalkyl and ionic alkyllead compounds in environmental samples by butylation and gas chromatography‐atomic absorption , 1985 .

[9]  H. Craig.  Isotopic standards for carbon and oxygen and correction factors for mass-spectrometric analysis of carbon dioxide , 1957 .

[10]  John A. Nelder,et al.  A Simplex Method for Function Minimization , 1965, Comput. J..

[11]  M. Nomura,et al.  Fundamental studies on the ion-exchange separation of boron isotopes. , 1977 .

[12]  W. D. Marshall,et al.  Determination of alkyllead salts in water and whole eggs by capillary column gas chromatography with electron capture detection. , 1983, Analytical chemistry.

[13]  T. B. Pierce,et al.  An investigation into the use of the nuclear microprobe for examining distributions of boron isotopes , 1976 .

[14]  O. Donard,et al.  Behavior of methyltin compounds under simulated estuarine conditions. , 1985, Environmental science & technology.

[15]  J. W. Robinson,et al.  Speciation of Organo Lead Compounds by T.L.C. and High Performance Liquid Chromatorgraphy-Atomic Absorption Spectroscopy Decomposition of TEL in Sea Water , 1984 .

[16]  H. R. Potter,et al.  Decomposition of organolead compounds in aqueous systems. , 1981, Environmental research.

[17]  S. Rapsomanikis,et al.  Methylation of tin and lead in the environment: oxidative methyl transfer as a model for environmental reactions. , 1985, Environmental science & technology.

[18]  P. Wong,et al.  Methylation of lead in the environment , 1975, Nature.

[19]  S. Rapsomanikis,et al.  Methylation of lead(II) and methyllead(IV) compounds in water by a trans-dimethylcobalt(III) complex , 1984 .

[20]  P. Wong,et al.  The determination of dialkyllead, trialkyllead, tetraalkyllead and lead(II) ions in water by chelation/ extraction and gas chromatography/atomic absorption spectrometry , 1983 .

[21]  H. Thode,et al.  Natural variations in the isotopic content of boron and its chemical atomic weight. , 1948, Journal of the American Chemical Society.

[22]  H. Yamauchi,et al.  Determination of triethyllead, diethyllead and inorganic lead ions in urine by hydride generation flameless atomic absorption spectrometry. , 1981, Industrial health.

[23]  P. Wong,et al.  Determination of dialkyllead, trialkyllead, tetraalkyllead, and lead(II) compounds in sediment and biological samples. , 1984, Analytical chemistry.

[24]  A. Whitmore,et al.  Lead biomethylation, an elusive goal , 1983 .

[25]  L. J. Snyder,et al.  Rapid Spectrophotometric Determination of Triethyllead, Diethyllead, and Inorganic Lead Ions and Application to the Determination of Tetraorganolead Compounds , 1961 .