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Method Abstract for Post-column Liquid
Chromatography 120
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Bromate is a disinfection
by-product that is formed when Ozone reacts with
naturally occurring Bromide in drinking water.
Bromate is a known animal carcinogen and has also
been listed as a group 2B toxin: probable human
carcinogen. The U.S. EPA Method 300.1 employs
conductivity as the means of detection which works
well for most anions. However, the method is
nonspecific and coeluting interferences cannot be
identified. The more recent U.S. EPA Method 317.0
utilizes a Bromate specific reagent in a
post-column reaction. This allows for a very
specific and sensitive assay for Bromate in
complex matrices.
METHOD
• LC with a binary pump
• UV/VIS
detector
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Pickering Laboratories single reagent PINNACLE PCX
or VECTOR PCX
• Pickering Laboratories anion-exchange column,
4.6 x 150mm (Cat. No. 0785150)
• 9.0 mM Sodium carbonate
• Conc.
Nitric acid (70%)
•
Potassium bromide
• o–Dianisidine
dihydrochloride
• Methanol
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LC COLUMN
TEMPERATURE: |
42°C |
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SAMPLE INJECTION
VOLUME: |
250 µL |
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LC FLOW RATE: |
1.3 mL/min |
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MOBILE PHASE: |
9 mM Na2CO3 |
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POST-COLUMN
SYSTEM: |
Pinnacle PCX |
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REACTOR VOLUME: |
0.5 mL |
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REACTOR TEMPERATURE: |
60°C |
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REAGENT: |
o–Dianisidine dihydrochloride (Add
40 mL of 70% HNO3 to 300mL
deionized water in a 500mL volumetric
flask. Dissolve 2.5g KBr in this solution.
Dissolve 250mg of o–Dianisidine
dihydrochloride in 100mL of Methanol and
add to the Nitric acid/KBr solution and
dilute to volume.) |
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FLOW RATE: |
0.7 mL/min |
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DETECTION: |
UV/VIS detector,
 max=450
nm |
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REFERENCES
1. U.S.EPA
Method 317.0. Determination of inorganic oxyhalide
disinfection by-products in drinking water using
ion chromatography with the addition of a
post-column reagent for trace bromate analysis.
2. H.P.Wagner,
B.V.Pepich, D.P.Hautman and D.J.Munch,
J.Chromatography A, 882 (2000) 309 – 319.
3.
C.R.Warner, D.H.Daniels, F.L.Joe and G.W.Diachenko,
Food Additives and Contaminants, vol. 13, No.6
(1996) 633 – 638.
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