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Methods - Ion Chromatograph

Environment and Natural Resources Institute
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Ion Chromatography

Major anion analyses are performed using IonPac As15 (4mm) column, and self regenerating suppressor ASRS Ultra (4mm); sample loop is 25 μL.

Anion analyzed:
Fluoride
retention time (min)    3.8

Chloride      4.5   
Nitrite      6.2   
Sulfate      7.2   

Bromide

Nirate

12.6

15

Phosphate
20

Samples should be filtered through 0.45μm filters immediately after sampling and stored at 4 ºC. The shelf time of some anions is only 48 hours. The analysis is performed using calibration standard at 4 levels adjusted to concentration of the samples. Quality control and blank control is performed every 10th sample. For a full SOP click here.

Perchlorate is separated using IonPac AS16 (2 mm) column and self regenerating suppressor ASRS Ultra II (2mm) with external water mode.

Eluent    KOH

Isocratic
65 mM

Flow rate
0.25 mL/min

Total time
14 minutes

Anion analyzed:
Perchlorate
retention time
12.5 min

Detection is performed with conductivity detector in water matrixes. For complex matrixes (e.g. tissue) the IC is connected to a mass spectrometer (Finnigan AQA) with an electrospray ionization source. The settings of mass spectrometer are:

Negative mode
-ve

AQA mix
5 V

probe temperature
300 C

For further details on our pechlorate analyses see Dodds, et al. (2004), Anal. Bioanal. Chem. 379:881-887.
© 2008 ASET Laboratory

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