IC SI-35 2B, an anion analysis column was used to analyze perchlorate and its related anions. LC/MS analysis of perchlorate ions has gained attention in recent years, which includes a published EPA Method 6850. Perchlorate ions can be detected at m/z 99 and m/z 101, and their peak area ratio corresponds to the isotopic ratio of 35Cl and 37Cl. Fragment ions of perchlorate ions, m/z 83 and m/z 85 are detected. Their m/z are the same as chlorate ion m/z, but since perchlorate ions and chlorate ions have sufficiently different retention times, this allows their differentiation. Additionally, the m/z 99 ion of perchlorate ions may be influenced by H34SO4-, which has the same m/z, but as they also have distinct retention times enabling the differentiation.
After confirming the retention times of each ion using a mixed standard solution (1 μg/mL each), we measured a mixed standard solution containing 50 ng/mL each. Peaks of perchlorate ions were observed at both m/z 99 and m/z 101. The effects of other components on the perchlorate ion peaks can be checked by the peak area ratio of 35ClO4- to 37ClO4-. In this analysis, even at low concentrations of perchlorate ions, peaks derived from 37ClO4- can be determined.
Sample: 5 μL
Mixed standard solution (1 μg/mL each)
- Perclorate, ClO4-
- Hydrogen sulfate, HSO4-
- Chlorate, ClO3-
- Chloride, Cl-
Sample: 5 μL
Mixed standard solution (50 ng/mL each)
- Perclorate, ClO4-
- Column
- :Shodex IC SI-35 2B (2.0 mm I.D. × 50 mm)
- Eluent
- :(A); 100 mM NH4HCO3 aq., (B); CH3CN, (C); H2O
gradient; 30 % (A), 10 % (B), 60 % (C) (0 min) to 80 % (A), 10 % (B), 10 % (C) (10 to 16 min) to 30 % (A), 10 % (B), 60 % (C) (16.5 to 20 min) - Flow rate
- :0.25 mL/min
- Detector
- :ESI-MS (negative, SIM)
- Column temp.
- :45 ℃
Sample Name Index
Operation Manual / Certificate of Analysis
Operation Manuals and Certificate of Analysis / Inspection Certificate for the following products can be downloaded here.
Product Name Index
Applications
- High Sensitive Analysis of Perchloric Acid and Oxyhalides by LC/MS (JJ-50 2D)
- LC/MS/MS Analysis of Sulfamic Acid According to Japanese Testing Methods for Fertilizers (ODP2 HP-2D)
- High Sensitive Analysis of Bromate by LC/MS/MS (JJ-50 2D)
- LC/MS Analysis of Iodide (VT-50 2D)
- Simultaneous LC/MS Analysis of Haloacetic Acids and Anions Including Chlorate and Bromate (JJ-50 2D)
- Analysis of Chlorate and Bromate in Tap Water by LC/MS/MS, According to Japanese Water Supply Act (JJ-50 2D)