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International comparison (CCQM-3) on the determination of organic compounds using isotope dilution mass spectrometry: (pp'-dichlorodiphenyl) dichloroethylene (pp'-DDE) in solution

K S Webb, D Carter and V J Barwick

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A comparison (CCQM-3) of the concentration of the compound (pp'-dichlorodiphenyl) dichloroethylene (pp'-DDE) in 2,2,4-trimethyl pentane solvent by national laboratories using isotope dilution mass spectrometry has been completed. Two levels of sample solution were provided within the range 0.05 µg g-1 to 5 µg g-1. A discussion on the choice of compound for this comparison is given. The purity of the pp-DDE material used was determined using gas chromatography, differential scanning calorimetry and high-performance liquid chromatography. Details of the preparation of the comparison solutions are given, including choice of containers and septum seals to prevent solvent evaporation. Full results of the comparison are given. Good agreement was obtained between laboratories at both concentration levels, with a majority of participants achieving a result within 1% of the reference values. There was a lack of consistency in the calculation of the overall uncertainty, therefore a typical example of a measurement uncertainty estimation for this comparison is given. Brief details of calibration procedures in IDMS are also given.


PACS

82.80.Ms Mass spectrometry (including SIMS, multiphoton ionization and resonance ionization mass spectrometry, MALDI)

06.20.Dk Measurement and error theory

06.20.F- Units and standards

82.80.Bg Chromatography

Subjects

Instrumentation and measurement

Chemical physics and physical chemistry

Dates

Issue 2 (April 1999)



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