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Office of Ground Water and Drinking Water

Date 02/01/2011

MEMORANDUM

SUBJECT: Basis for Expedited Approval of ASTM and Standard Method Revisions

FROM: Glynda Smith, Chemist, Technical Support Center

TO: The Record

This memo documents the reviews conducted on new versions of methods issued by the voluntary 

consensus standard bodies, Standard Methods and ASTM International. It provides the background 

information behind why EPA is approving these methods using the expedited methods approval process. 

Each method is discussed individually below:

Standard Methods 3114 B-09 published on-line at http://www.standardmethods.org

This revision was compared to the approved version, SM 3114 B-97 which is cited at 40 CFR 141.23(k)(1) 

for atomic absorption determination of arsenic and selenium. The revision is nearly identical to the 

approved version with the following modifications:

• The approved version identifies argon as an alternative gas for nitrogen; however, the method 

neglects to mention argon anywhere in the text. The revised version corrects this oversight.

• The approved version specifies six calibration concentration levels. The revised version specifies 

preparation of a minimum of three calibration standards that encompass the linear range of the 

instrument (approx. 1.0 to 20 μg/L As (III) and Se (IV). The EPA Manual for the Certification of 

Laboratories Analyzing Drinking Water, 5th Edition, Chapter IV, Section 7.2.3 states “...a 

calibration curve covering the sample concentration range and all target analytes should be 

generated...the curve should be composed of three or more points.” In addition, EPA Method 

200.9 (Determination of Trace Elements by Stabilized Temperature Graphite Furnace Atomic 

Absorption), also approved for arsenic and selenium determination, states in Section 11.4.4 

“...calibration standards (Section 7.9) prepared at three or more concentrations within the 

usable linear dynamic range of the analyte.”

Since the change in the number of calibration concentration levels described in SM 3114 B-09 is 

consistent with those required in the laboratory certification manual and one of the approved EPA 

atomic absorption methods, SM 3114 B-09 is considered to be equally as effective as the 

promulgated version, SM 3114 B-97.

Standard Methods 3113 B-04 published on-line at http://www.standardmethods.org

The online revision was compared to the approved version, SM 3113 B which was published in the 19th

edition of Standard Methods for the Examination of Water and Wastewater for the analysis of antimony, 

arsenic, barium, beryllium, cadmium, chromium, copper, lead, nickel, and selenium (as cited at 40 CFR 

141.23(k)(1)) as well as aluminum, iron, manganese, and silver (as cited at 40 CFR 143.4(b)) using 

electrothermal atomic absorption spectroscopy. The online revision contains the following changes 

relative to the approved method:

• The revision corrects an error in the preparation of palladium nitrate (Pd(NO3)2•H2O) stock 

solution. Palladium nitrate is used as an optional matrix modifier. The method describes

preparation of a 4000 mg/L palladium nitrate stock solution; however, the actual concentration
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obtained using the amount specified in the approved method is 3800 mg/L. The revised version 

corrects this error, yielding a palladium nitrate stock concentration of 4000 mg/L.

• One additional difference between the revised version and the approved version in the 19th

edition of Standard Methods for the Examination of Water and Wastewater involves the 

frequency of preparation of fresh calibration standard solutions. The 19th edition indicates that 

standard solutions for calibration should be prepared fresh daily. The revised version states that 

standard solutions should be prepared every two weeks, or more often as needed, if instrument 

response indicates degradation of the standards. This is a less wasteful protocol and identical to 

the frequency of preparation of fresh calibration solutions described in another approved 

atomic absorption method, EPA Method 200.9 (Determination of Trace Elements by Stabilized 

Temperature Graphite Furnace Atomic Absorption). 

As a result of the method comparison and error correction, SM 3113 B-04 is considered to be equally as 

effective as the promulgated version described in the 19th edition.

Standard Method 6651 B published in the 21st edition of Standard Methods for the Examination of 

Water and Wastewater and Standard Method 6651 B-00 published on-line at 

http://www.standardmethods.org

Standard Method 6651 B was promulgated for the determination of the regulated herbicide, glyphosate. 

The versions published in the 21st edition of Standard Methods and the on-line version are both identical 

to the promulgated version published in the 20th edition and cited at 40 CFR 141.24(e)(1). Therefore, 

the version in the 21st edition and the on-line version, SM 6651 B-00, are considered equally as effective 

as the promulgated version described in the 20th edition.

Standard Method 6640 B published in the 21st edition of Standard Methods for the Examination of 

Water and Wastewater and Standard Method 6640 B-01 published on-line at 

http://www.standardmethods.org

EPA Method 515.4, Revision 1.0 was used as the basis for comparison because it is currently cited in the 

drinking water regulations at 40 CFR 141.24(e)(1) for determination of 2,4-D, 2,4,5-TP (Silvex), Dinoseb, 

Pentachlorophenol, and Picloram. Standard Method 6640 B was developed directly from EPA Method 

515.4, Revision 1.0 and thus describes the identical sample collection/handling protocols, sample 

preparation and derivatization steps, chromatographic conditions (specifically, the use of a secondary 

confirmation column), and electron capture detection. Standard Method 6640 B and EPA Method 

515.4, Revision 1.0 specify the same quality control requirements and the method performance data 

(detection levels, accuracy and precision) are identical. Therefore, Standard Method 6640 B is equally as 

effective as EPA Method 515.4, Revision 1.0 in determining the concentrations of 2,4-D, 2,4,5-TP 

(Silvex), Dinoseb, Pentachlorophenol, and Picloram in drinking water.

The on-line version, Standard Method 6640 B-01, is identical to the version published in the 21st edition 

and thus is also equally as effective as EPA Method 515.4, Revision 1.0 in determining the 

concentrations of 2,4-D, 2,4,5-TP (Silvex), Dinoseb, Pentachlorophenol, and Picloram in drinking water.

ASTM International D 1067-06 B

ASTM International Method D 1067-02 B was used as the basis for comparison because it is currently 

promulgated in the drinking water regulations at 40 CFR 141.23(k)(1) for determining alkalinity in water

using titrimetry. The following changes were made in the newer version:

• In the Reagents Section of the method, Note 5 has been added to point out that the indicators 

are available commercially in prepared form

• Re-worded the QC sub-section 34.1.2.3
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Other than the minor editorial changes, the two methods are identical with respect to sample 

collection/handling protocols, sample preparation, analytical procedures, and calculation of alkalinity, in 

milliequivalents per liter, in drinking water. The experimental precision and bias are unchanged. 

Therefore, ASTM Method D 1067-06 B is equally as effective as the approved method, ASTM Method D 

1067-02 B, for determining alkalinity in water.

ASTM International D 6919-09 

ASTM International Method D 6919-03 was used as the basis for comparison because it is currently 

promulgated in the drinking water regulations at 40 CFR 141.23(k)(1) for determining sodium, 

magnesium, and calcium in water using ion chromatography. Two very minor editorial changes were 

made:

• Section 1.3 added in order to note that SI units are used for all values in the method

• Section 16.5 updates reference method ASTM D 2777-98 to ASTM D 2777-06

Otherwise, the two methods are identical with respect to sample collection/handling protocols, sample 

preparation, analytical procedures, and calculation of sodium, magnesium, and calcium concentrations, 

in milligrams per liter, in drinking water.

ASTM International Method D 3972-09

ASTM International Method D 3972-02 was used as the basis for comparison because it is currently 

approved in the National Primary Drinking Water Regulations at 40 CFR 141.25(a) for the determination 

of isotopic uranium in water using alpha spectrometry. The following changes have been made to 

Method D 3972-09 relative to the approved version, Method D 3972-02:

• Added Section 1.2 in order to note that SI units are used for all values in the method

• Added ASTM International Practice C 1163 (Practice for Mounting Actinides for Alpha 

Spectrometry Using Neodymium Fluoride) and Practice D 7282 (Practice for Set-up, Calibration, 

and Quality Control of Instruments Used for Radioactivity Measurements)

• Interference Section 6.1 added discussion regarding potential interference of man-made 

Neptunium-237.

• Precautions Section 9.1 added palliative recommendation (calcium gluconate gel) in the event of 

skin contact with hydrofluoric acid.

• Section 12.4 – Electrodeposition. Added footnote discussing alternate sample mounting for 

alpha spectrometry.

• Section 12.5.1 added reference to ASTM Practice D 7282 for guidance on the setup and 

calibration of the instrument, and additional quality assurance measures.

• Section 13.1 modified the concentration calculation terms; the calculation, however, remains 

exactly the same:

o C = net count rate has been changed to Rn

o Aa,i has been changed to ACi (activity concentration of uranium isotope in water, Bq/L)

o At has been changed to ACt (activity concentration of 232U tracer, Bq/L)

• The detector efficiency calculation in Section 13.2 has equation terms modified to those below; 

the calculation, however, remains exactly the same:

o ε = Rn,s/ACs

o Rn,s = net counting rate of a standard source in the energy region of the calibrated alphaparticle emitter, cps, and

o ACs = absolute alpha-particle emission rate of the calibrated alpha-particle emitter, α/s
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• In Section 13.3 calculate the fractional uranium recovery instead of the percent recovery. The 

calculation terms have been modified as discussed in the prior two bullets; however, the 

calculation remains the same.

• A discussion about minimum detectable activity has been edited out of the revised version of 

the method (Sect. 13.5 in ASTM Method D 3972-02). 

• Sections 13.4 and 13.5 incorporate expanded counting uncertainty and total combined 

propagated uncertainty calculations. These calculations are consistent with the U.S. Nuclear 

Regulatory Commission, Multi-Agency Radiological Laboratory Analytical Protocols Manual, 

NUREG-1576 EPA 402-B-04-001A, July 2004, (MARLAP).

• Section 13.6 was added to calculate the critical level concentration (Lc). This is consistent with 

MARLAP

• In Section 13.7, calculation of the a priori minimum detectable concentration (MDC) was 

modified to be consistent with MARLAP

• In Section 5.2.2 the permissible uncertainty of the yield has been lowered from 10% to 5%

• Section 15.5 has been added to specify that the level of analytes found in the method blank 

should be less than the critical level concentration (Lc)

• Section 15.7.1 has been added to specify calculation of the Duplicate Error Ratio (DER) as a 

measure of the statistical agreement between duplicate results to ensure they agree within a 

99.7% confidence level.

The methods are identical with respect to drinking water sample collection/handling protocols and 

sample preparation. ASTM Method D3972-09 and the approved version, D 3972-02, are analytically 

equivalent. The calculation of isotopic uranium concentrations has been updated to capture the 

uncertainty determinations outlined in MARLAP; precision and bias are unchanged. As a result, Method 

D3972-09 is considered to be equally as effective as D 3972-02 for determining isotopic uranium 

concentrations in drinking water.