EPA Method 101

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EPA Method 101:
DETERMINATION OF PARTICULATE AND GASEOUS MERCURY EMISSIONS FROM CHLOR-ALKALI PLANTS (AIR STREAMS)

Summary:
Particulate and gaseous Hg emissions are withdrawn isokinetically from the source and collected in acidic iodine monochloride (ICl) solution. The Hg collected (in the mercuric form) is reduced to elemental Hg, which is then aerated from the solution into an optical cell and measured by atomic absorption spectrophotometry.

Scope:
This method is applicable for the determination of Hg emissions, including both particulate and gaseous Hg, from chlor-alkali plants and other sources (as specified in the regulations) where the carrier-gas stream in the duct or stack is principally air.

Citation:
The official copy of this method is available at 40 Code of Federal Regulations (CFR) 61, Appendix B. The CFR can be accessed on-line at http://www.gpoaccess.gov/cfr/index.html

Interferences:
(A) Sample Collection. Sulfur dioxide (SO2) reduces ICl and causes premature depletion of the ICl solution.(B) Sample Analysis. ICl concentrations greater than 10-4 molar inhibit the reduction of the Hg (II) ion in the aeration cell. Also, condensation of water vapor on the optical cell windows causes a positive interference.

QC Requirements:
(A)Sampling equipment leak-checks and calibration -- This is done to ensure the accuracy and precision of sampling measurements.(B) Spectrophotometer calibration -- This is done to ensure linearity of spectrophotometer response to standards.(C) Check for matrix effects -- This is done to help identify and eliminate matrix effects.

Media:
AIR

Subcategory:
Inorganic

Concentration:
0.5 to 120 ug Hg/ml

Precision:
The estimates are based on collaborative tests, wherein 13 laboratories performed duplicate analyses on two Hg-containing samples from a chlor-alkali plant and on one laboratory-prepared sample of known Hg concentration. The sample concentrations ranged from 2 to 65 ug Hg/ml. The estimated intra-laboratory and inter-laboratory standard deviations are 1.6 and 1.8 ug Hg/ml, respectively. The participating laboratories that analyzed a 64.3 ug Hg/ml (in 0.1 M ICl) standard obtained a mean of 63.7 ug Hg/ml.

Detection:
Detection level taken from the low end of the stated range.

Revision Number:
2000