Species-Selective Analysis by Microcolumn Multicapillary Gas Chromatography with Inductively Coupled Plasma Mass Spectrometric Detection

Multicapillary gas chromatography has been applied to the speciation of organomercury compounds. Basic investigation of the fundamental properties of multicapillary columns, to evaluate their potential and limitations as a rapid separation unit, are presented. For analysis of methylated and ethylated mercury compounds a complete separation can be performed within 45 s under isothermal conditions. The adaptation of the technique for use with a purge and trap system and with an element-selective plasma-emission detector results in a compact and effective system for mercury speciation. Results from analysis of certified reference materials were in good agreement with certified values within the significance levels.

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“…Coupling of multicapillary GC to ICP-MS as detector for elemental speciation has been demonstrated by Lobinski's group [10].…”

Section: Instrumentationmentioning

confidence: 99%

Rapid separation of elemental species by multicapillary GC

Rosenkranz¹,

Bettmer

2002

Anal Bioanal Chem

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“…In this sense the detection limits achievable by use of GC are much lower than those obtained by HPLC [4], because introduction of the sample to the atomizer is almost 100% efficient. The couplings preferred so far are GC-AAS, GC-MIP-AES, GC-FPD, GC-MS, and, more recently, GC-ICP-MS [5,6,7]. This latest hyphenated technique can furnish detection limits as low as 0.05-0.1 ng mL -1 , as tin [8] -even lower when special preconcentration procedures such as HS-SPME (headspace solid-phase micro extraction) [9] or LVI (largevolume injection) [10] are used.…”

Section: Introductionmentioning

confidence: 99%

Determination of butyltin compounds in environmental samples by isotope-dilution GC–ICP–MS

Alonso¹,

Encinar²,

González³

et al. 2002

Anal Bioanal Chem

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Isotope-dilution analysis in combination with GC-ICP-MS detection has been applied to the determination of butyltin species in environmental samples. Different spikes containing the isotopically labeled butyltin species have been synthesized in the laboratory after optimization of the reaction conditions. The isotopic compositions of the tin species in the different spike solutions were determined by GC-ICP-MS after derivatization by aqueous ethylation with sodium tetraethylborate. Reverse isotope-dilution analysis was used for quantitation of the spike solutions by means of natural MBT, DBT, and TBT standards. The mixed spikes were used for simultaneous analysis of MBT, DBT and TBT in the certified reference materials, PACS-2, CRM 462, and CRM 646, with satisfactory results. The excellent agreement of the different speciation results obtained by use of the different spikes is a good indicator of the precision, accuracy, and reliability which can be achieved by using isotope-dilution analysis for trace metal speciation. Application of a double spike containing (119)Sn-enriched MBT (79.7 At%), (118)Sn-enriched DBT (86.7 At%), and (119)Sn-enriched TBT (83.1 At%) also enabled evaluation of the conditions resulting in quantitative extraction of the species from the solid matrix, in combination with possible alterations depending on the different extraction procedures used (mechanical shaking, ultrasounds, and microwaves). Mathematical equations used for this purpose computed the correct species concentrations directly and, additionally, the decomposition factors (from TBT to DBT and from DBT to MBT) after precise measurement of the (119)Sn/(120)Sn and (118)Sn/(120)Sn ratios for all butyltin species by GC-ICP-MS.

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“…A detailed description of the pre-commercial interface version has been published. 199,200 A different GC-ICP-MS coupling principle, based on the simultaneous introduction of GC effluent and liquid from a standard spray chamber has been commercialised by Thermo Electron Corp. Here, the GC is coupled to the ICP-MS via a flexible line, using a modified torch, where GC and standard liquid sample introduction are connected simultaneously (Figure 7.13).…”

Section: (B) Commercial Gc-icp-ms Systemsmentioning

confidence: 99%

“…Because of the high costs for the enriched isotope starting material, microscale synthesis methods have been developed. The synthesis and purification of 201 MeHg as well as 199 MeHg has been successfully accomplished using methylation via methylcobalamine. 291,292 Ruiz-Encinar 293 described the synthesis of 118 Sn-labelled DBT as well as the synthesis of a mixed spike containing 119 Sn-labelled MBT, DBT and TBT.…”

Section: (A) Synthesis and Characterisation Of Isotopically Labelled mentioning

confidence: 99%