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    Total Reduced Sulfur Emissions from Stationary Sources (Impinger Technique) – USEPA Method 16A

USEPA Method 16A is used for the determination of TRS emissions from recovery boilers, lime kilns, and smelt dissolving tanks at kraft pulp mills, reduced sulfur compounds (H
2S, carbonyl sulfide, and carbon disulfide) from sulfur recovery units at onshore natural gas processing facilities, and from other sources when specified in an applicable subpart of the regulations. 
 
An integrated gas sample is extracted from the stack.  SO
2 is removed selectively from the sample using a citrate buffer solution.  TRS compounds are then thermally oxidized to SO2, collected in hydrogen peroxide as sulfate, and analyzed by the USEPA Method 6 barium-thorin titration procedure.  The flue gas must contain at least 1 percent oxygen for complete oxidation of all TRS to SO2.
 
Reduced sulfur compounds other than those regulated by the emission standards, if present, are measured by this method.  Therefore, carbonyl sulfide, which is partially oxidized to SO
2 and may be present in a lime kiln exit stack, is a positive interferant.
 
Particulate matter from the lime kiln stack gas (primarily calcium carbonate) causes a negative bias if it is allowed to enter the citrate scrubber.  The particulate matter will cause the pH to rise and H
2S to be absorbed prior to oxidation.  Furthermore, if the calcium carbonate enters the hydrogen peroxide impingers, the calcium precipitates sulfate ion.  Proper use of the particulate filter described in the method eliminates this interference.
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Last Update: October 25, 2006