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.

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

PrefaceIntroduction1 BASIC PRINCIPLES Atomic structure Plasmas Emission and absorption of radiation Ionization Dissociation Sources for atomic spectrometry Analytical atomic spectrometry 2 SPECTROMETRIC INSTRUMENTATION Figures of merit of an analytical method Optical spectrometers Mass spectrometers Data acquisition and treatment SAMPLE INTRODUCTION DEVICES Pneumatic nebulization Ultrasonic nebulization Hydride generation Eletrothermal evaporation Direct solids sampling Cathodic sputtering 4 ATOMIC ABSORPTION SPECTROMETRY Principles Atomic absorption spectrometers Flame atomic absorption Electrothermal atomic absorption Hydride generation Background correction techniques Fields of application 5 ATOMIC EMISSION SPECTROMETRY Principles Atomic emission spectrometers Flame emission Arcs and sparks Plasma sources Glow discharges Laser sources Fields of application 6 PLASMA MASS SPECTROMETRY Principles Instrumentation Glow discharge mass spectrometry ICP mass spectrometry Fields of application 7 ATOMIC FLUORESCENCE SPECTROMETRY Principles Figures of merit 8 LASER ENHANCED IONIZATION SPECTROMETRY Principles Figues of merit Analytical Applications9 SAMPLE PREPARATION FOR ATOMIC SPECTROMETRY Sample Preparation in direct compact sample analysisGrinding, sieving and compaction of powdersSample dissolutionWet chemical methodsFusion ProceduresMicrowave-assisted methodsCombustion TechniquesFlow injection analysisLeaching sample preparation methods 10 COMPARISON WITH OTHER METHODS Power of detection Analytical accuracy Economic aspectsLiteratureIndex

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Analytical Atomic Spectrometry with Flames and Plasmas

The operational variables are optimized for chromatographic resolution and detection limits. A comprehensive method for the determination of mono-, di-, tri-, and some tetraalkylated organotin compounds in water and sediments by gas chromatography-atomic emission detection (GC-AED) is developped. The absolute detection limit is about 0,05 pg (as Sn), and the calibration is linear over three decades.

Optimization of comprehensive speciation of organotin compounds in environmental samples by capillary gas chromatography helium microwave-induced plasma emission spectrometry

Atomic Absorption, Atomic Emission, and Flame Emission Spectrometry

Sodium tetra(n-propyl)borate: a novel aqueous in situ derivatization reagent for the simultaneous determination of organomercury, -lead and -tin compounds with capillary gas chromatography–inductively coupled plasma mass spectrometry

Ionic alkyllead compounds are extracted from water samples into pentane by complexation with sodium diethyldithiocarbamate. Inorganic lead is complexed with EDTA. The organic phase is evaporated to dryness by vacuum distillation, after which butylation with n-butyl Grignard reagent is carried out in a microvolume of n-nonane. The analysis is performed by gas chromatography with atomic absorption spectrometric detection. The effects of various parameters on the analytical performance are discussed. With 500 mL of water, detection limits for individual species are situated at the ng.L/sup -1/ level.

Determination of ionic alkyllead compounds in water by gas chromatography/atomic absorption spectrometry.

A reproducible and interference-free method is presented for simultaneous determination of individual tri-, di- and monoalkyltin species present in aqueous systems The ionic methyltin and butyltin compounds are extracted from water into pentane as diethyldithiocarbamate complexes at pH 5 The organic phase is then evaporated to dryness under reduced pressure, after which derivatization withn-pentyl (Pe) Grignard reagent is carried out in a microvolume ofn-octane to form pentylated alkyltin compounds RnSnPe(4-n) (R = Methyl, Me or Butyl, Bu) The quantitation is subsequently performed by gas chromatography with quartz furnace atomic absorption spectrometric detection (GC-AAS) Absolute detection limits range between 016 ng and 040 ng Sn for the various organotin species, allowing speciation in natural water down to the 4-10 ng ⁗ 1−1 level

Speciation of organotin compounds in water by gas chromatography/atomic absorption spectrometry

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Determination of ionic alkyllead compounds in water by gas chromatography/atomic absorption spectrometry.

Speciation of organotin compounds in water by gas chromatography/atomic absorption spectrometry