EPA OAR/OAQPS/EMAEMC: OAQPS-101: Mercury in Air Emissions by Atomic Absorption

Summary
Analytes
Revision
Data and Sites

Official Method Name

Method 101 - Determination of Particulate and Gaseous Mercury Emissions from Chlor-alkali Plants (Air Streams)

Current Revision

2000

Media

AIR

Instrumentation

Cold Vapor Atomic Absorption

Method Subcategory

Inorganic

Method Source

EPA OAR/OAQPS/EMAEMC

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

Brief Method 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Particulate and gaseous Hg emissions are withdrawn isokinetically from the source and collected in acidic iodine monochloride (ICl) solution.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 and Application

This method is applicable to the determination of Hg in air emissions from stationary sources, 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.

Applicable Concentration Range

0.5 to 120 ug Hg/ml

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.

Quality Control 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.

Sample Handling

Elaborate sampling procedures, including sampling train diagrams, are provided in the method.

Maximum Holding Time

Relative Cost

Unknown

Sample Preparation Methods

This method has 1 analyte associated with it.

Analyte	Detection Level	Bias	Precision	Pct False Positive	Pct False Negative	Spiking Level
Mercury(7439-97-6) Hg Hydrargyrum Liquid silver Mercury Mercury (inorganic) Quicksilver	0.500 ug/mL	99% Rec (ML)	1.80 SD (ML)

Precision Descriptor Notes:	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 Level Note:	Detection level taken from the low end of the stated range.

Precision Descriptor Notes:

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 Level Note:

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

Revision	PDF/Link
2000

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EPA OAR/OAQPS/EMAEMC: OAQPS-101: Mercury in Air Emissions by Atomic Absorption

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