An automated hydride generation-cryogenic trapping-ICP-MS system for measuring inorganic and methlylated GE, Sb and As species in marine and fresh waters

Michael Ellwood, William Maher

    Research output: Contribution to journalArticle

    Abstract

    In this paper we describe a hydride generation system for measuring the inorganic and methylated species of three metalloids, Ge, Sb and As, in marine and freshwater samples. The system utilises the principles of both flow injection and batch hydride generation and couples it to an automated cryogenic trapping unit with detection by ICP-MS. The Teflon cryogenic trap was packed with 10 cm of SE-30 5% Chromosorb W-HP 80–100 mesh and wound with 1.2 m of resistance wire. A motorised cryofocusing unit was designed and built to lower and raise the hydride trap into and out of a liquid nitrogen dewar and to control the heating of the hydride trap. The compromise conditions for hydride generation and cryogenic trapping of inorganic and methylated species were final solution concentrations of 0.06 M hydrochloric acid, 0.5% w/v sodium tetrahydroborate and 0.5% w/v cysteine. For measurement of AsIII and SbIII cysteine was omitted. Samples were purged and trapped with helium at a flow rate of 80 ml min−1. One run took 8.75 min for a 1 ml sample. Detection limits were 1-5 pM for Ge species, 0.001–0.004 nM for Sb species and 0.002–0.069 nM for As species. The analytical precision for inorganic and methylated species was 2–8% for all but two of the species (TMSb, 20% and DMSb, 11%) at concentrations typically found in the environment. Results for a range of natural waters are presented to illustrate the use of the system
    Original languageEnglish
    Pages (from-to)197-203
    Number of pages7
    JournalJournal of Analytical Atomic Spectrometry
    Volume17
    Issue number3
    Publication statusPublished - 2002

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    Hydrides
    Cryogenics
    Water
    Cysteine
    Metalloids
    Dewars
    Silicone Elastomers
    Helium
    Hydrochloric Acid
    Polytetrafluoroethylene
    Liquid nitrogen
    Flow rate
    Wire
    Heating

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    title = "An automated hydride generation-cryogenic trapping-ICP-MS system for measuring inorganic and methlylated GE, Sb and As species in marine and fresh waters",
    abstract = "In this paper we describe a hydride generation system for measuring the inorganic and methylated species of three metalloids, Ge, Sb and As, in marine and freshwater samples. The system utilises the principles of both flow injection and batch hydride generation and couples it to an automated cryogenic trapping unit with detection by ICP-MS. The Teflon cryogenic trap was packed with 10 cm of SE-30 5{\%} Chromosorb W-HP 80–100 mesh and wound with 1.2 m of resistance wire. A motorised cryofocusing unit was designed and built to lower and raise the hydride trap into and out of a liquid nitrogen dewar and to control the heating of the hydride trap. The compromise conditions for hydride generation and cryogenic trapping of inorganic and methylated species were final solution concentrations of 0.06 M hydrochloric acid, 0.5{\%} w/v sodium tetrahydroborate and 0.5{\%} w/v cysteine. For measurement of AsIII and SbIII cysteine was omitted. Samples were purged and trapped with helium at a flow rate of 80 ml min−1. One run took 8.75 min for a 1 ml sample. Detection limits were 1-5 pM for Ge species, 0.001–0.004 nM for Sb species and 0.002–0.069 nM for As species. The analytical precision for inorganic and methylated species was 2–8{\%} for all but two of the species (TMSb, 20{\%} and DMSb, 11{\%}) at concentrations typically found in the environment. Results for a range of natural waters are presented to illustrate the use of the system",
    author = "Michael Ellwood and William Maher",
    year = "2002",
    language = "English",
    volume = "17",
    pages = "197--203",
    journal = "Annual Reports on Analytical Atomic Spectroscopy",
    issn = "0267-9477",
    publisher = "Royal Society of Chemistry",
    number = "3",

    }

    TY - JOUR

    T1 - An automated hydride generation-cryogenic trapping-ICP-MS system for measuring inorganic and methlylated GE, Sb and As species in marine and fresh waters

    AU - Ellwood, Michael

    AU - Maher, William

    PY - 2002

    Y1 - 2002

    N2 - In this paper we describe a hydride generation system for measuring the inorganic and methylated species of three metalloids, Ge, Sb and As, in marine and freshwater samples. The system utilises the principles of both flow injection and batch hydride generation and couples it to an automated cryogenic trapping unit with detection by ICP-MS. The Teflon cryogenic trap was packed with 10 cm of SE-30 5% Chromosorb W-HP 80–100 mesh and wound with 1.2 m of resistance wire. A motorised cryofocusing unit was designed and built to lower and raise the hydride trap into and out of a liquid nitrogen dewar and to control the heating of the hydride trap. The compromise conditions for hydride generation and cryogenic trapping of inorganic and methylated species were final solution concentrations of 0.06 M hydrochloric acid, 0.5% w/v sodium tetrahydroborate and 0.5% w/v cysteine. For measurement of AsIII and SbIII cysteine was omitted. Samples were purged and trapped with helium at a flow rate of 80 ml min−1. One run took 8.75 min for a 1 ml sample. Detection limits were 1-5 pM for Ge species, 0.001–0.004 nM for Sb species and 0.002–0.069 nM for As species. The analytical precision for inorganic and methylated species was 2–8% for all but two of the species (TMSb, 20% and DMSb, 11%) at concentrations typically found in the environment. Results for a range of natural waters are presented to illustrate the use of the system

    AB - In this paper we describe a hydride generation system for measuring the inorganic and methylated species of three metalloids, Ge, Sb and As, in marine and freshwater samples. The system utilises the principles of both flow injection and batch hydride generation and couples it to an automated cryogenic trapping unit with detection by ICP-MS. The Teflon cryogenic trap was packed with 10 cm of SE-30 5% Chromosorb W-HP 80–100 mesh and wound with 1.2 m of resistance wire. A motorised cryofocusing unit was designed and built to lower and raise the hydride trap into and out of a liquid nitrogen dewar and to control the heating of the hydride trap. The compromise conditions for hydride generation and cryogenic trapping of inorganic and methylated species were final solution concentrations of 0.06 M hydrochloric acid, 0.5% w/v sodium tetrahydroborate and 0.5% w/v cysteine. For measurement of AsIII and SbIII cysteine was omitted. Samples were purged and trapped with helium at a flow rate of 80 ml min−1. One run took 8.75 min for a 1 ml sample. Detection limits were 1-5 pM for Ge species, 0.001–0.004 nM for Sb species and 0.002–0.069 nM for As species. The analytical precision for inorganic and methylated species was 2–8% for all but two of the species (TMSb, 20% and DMSb, 11%) at concentrations typically found in the environment. Results for a range of natural waters are presented to illustrate the use of the system

    M3 - Article

    VL - 17

    SP - 197

    EP - 203

    JO - Annual Reports on Analytical Atomic Spectroscopy

    JF - Annual Reports on Analytical Atomic Spectroscopy

    SN - 0267-9477

    IS - 3

    ER -