US EPA

1206540 

Journal Article 

USE OF PACKED-COLUMN SUPERCRITICAL FLUID CHROMATOGRAPHY WITH OZONE-BASED SULFUR CHEMILUMINESCENCE DETECTION 

Howard, AL; Taylor, LT 

1993 

Yes 

Analytical Chemistry
ISSN: 0003-2700
EISSN: 1520-6882 

65 

6 

724-729 

WOS:A1993KR44500013 

The use of the ozone-based sulfur chemiluminescence detector (SCD) coupled with packed column supercritical fluid chromatography (SFC) was evaluated. Optimization studies performed include the quenching effect of the CO2 mobile phase and organic species on the chemiluminescent species (SO2*) and the necessary air and hydrogen flow rates to gain maximum SCD sensitivity. Detectivities of 2 pg S/s and 1 pg S/s (S/N = 3) were obtained when capillary SFC (60-nL injection) and packed column conditions (500-nL injection) were employed, respectively. The results obtained when 60 nL was injected were in agreement with those obtained with open tubular and packed capillary column SFC/SCD by other investigators, indicating that the increased flow of CO2 does not further quench the chemiluminescent species from that occurring in capillary SFC. Detector linearity was 3-4 orders of magnitude. Methanol-modified CO2 was also demonstrated to be compatible with the SCD even with the high mobile phase flow rate. The analyses of polycyclic aromatic sulfur-containing hydrocarbons (PASH), diesel fuel, and sulfonylurea herbicides were explored as possible applications.