Determination of traces of chloride and fluoride in H2SO4, H3PO4 and H3BO3 by in situ analyte distillation-ion chromatography.
A simple dual vessel in situ analyte distillation (IAD) system has been developed for suppressed ion chromatographic determination of chloride and fluoride ions in complex matrices. In IAD system, water vapours generated from the outer vessel reacts with sulfuric acid generating heat, thus favouring the quantitative distillation of chloride and fluoride within 30 min on water bath temperature (approximately 80 degrees C). The distilled analytes, as their respective acids in water, were directly injected into an ion-chromatograph. This newly developed method has been applied for analysis of trace impurities in H2SO4, H3PO4 and H3BO3. The detection limits for chloride is 8, 80 and 70ppb (w/w) for H2SO4, H3PO4 and H3BO3, respectively. For fluoride the detection limits are 6 and 60 ppb (w/w) for H2SO4 and H3PO4, respectively. The recovery of spikes for both the analytes ranged between 87 and 100%.
Thangavel
S
S
National Centre for Compositional Characterisation of Materials, Bhabha Atomic Research Centre, ECIL P.O., Hyderabad 500062, India
Dash
K
K
Dhavile
S M
SM
Chaurasia
S C
SC
Mukherjee
T
T
D001888:Boric Acids / Q000737:chemistry*; D002712:Chlorides / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods*; D005459:Fluorides / Q000032:analysis*; D010756:Phosphoric Acids / Q000737:chemistry*; D015203:Reproducibility of Results; D013464:Sulfuric Acids / Q000737:chemistry*; D014835:Volatilization
D001888:Boric Acids; D002712:Chlorides; D010756:Phosphoric Acids; D013464:Sulfuric Acids; C030242:phosphoric acid; C033158:sulfuric acid; D005459:Fluorides; C032688:boric acid