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| - Analysis of Perchlorate inGroundwater by ElectrosprayIonization Mass Spectrometry/MassSpectrometry
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| - An electrospray ionization mass spectrometry/massspectrometry (ESI/MS/MS) method was developed tomeasure part-per-billion (μg/L) concentrations of perchloratein groundwater. Selective and sensitive perchloratedetection was achieved by operating the mass spectrometerin the negative ionization mode and by using MS/MS tomonitor the ClO4- to ClO3- transition. The method of standardadditions was used to address the considerable signalsuppression caused by anions that are typically presentin groundwater, such as bicarbonate and sulfate. ESI/MS/MS analysis was rapid, accurate, reproducible, andprovided a detection limit of 0.5 μg/L perchlorate ingroundwater. Accuracy and precision of the ESI/MS/MSmethod were assessed by analyzing performance evaluationsamples in a groundwater matrix (4.5−75 μg/L perchlorate)and by comparing ion chromatography (IC) and ESI/MS/MS results for local groundwater samples (<0.5−35 μg/Lperchlorate). Results for the performance evaluationsamples differed from the certified values by 4−13%, andprecision ranged from 3 to 10% (relative standarddeviation). The IC and ESI/MS/MS results were statisticallyindistinguishable (P> 0.05) for perchlorate concentrationsabove the detection limits of both methods.
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