This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what

changes have been made to the previous version. Because

it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.

Designation: F 2013 – 001

Standard Test Method for

Determination of Residual Acetaldehyde in Polyethylene
Terephthalate Bottle Polymer Using an Automated Static
Head-Space Sampling Device and a Capillary GC with a
Flame Ionization Detector1
This standard is issued under the fixed designation F 2013; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

1. Scope
1.1 This test method covers a gas chromatographic procedure for the determination of the ppm residual acetaldehyde (AA)
present in poly(ethylene terephthalate) (PET) homo-polymers and co-polymers which are used in the manufacture of beverage
bottles. This includes sample types of both amorphous and solid-stated pellet and preform samples.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D 4509 Test Method for Determining the 24-Hour Gas (Air) Space Acetaldehyde Content of Freshly Blown PET Bottles2

1
This test method is under the jurisdiction of ASTM Committee F02 on Flexible Barrier Materials and is the direct responsibility of Subcommittee F02.30 on Test Methods.
Current edition approved April 10, 2000. 2001. Published A June 2001. Originally published as F 2013 – 00. Last previous edition F 2013 – 00.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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 F 2013 – 001
E 691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method3

3. Terminology
3.1 The terms employed in this test method are commonly used in normal laboratory practice and require no special comment.

4. Summary of Test Method

4.1 A specified size (800 to 1000 µm) of granulated sample is weighed into a 20-mL head-space vial, sealed, and then heated
at 150°C for 60 min. After heating, the gas above the sealed sample of PET polymer is injected onto a capillary GC column. The
acetaldehyde is separated, and the ppm of acetaldehyde is calculated.

5. Significance and Use

5.1 This test method is of particular use as a quality control tool for a molding or synthesis operation. Acetaldehyde is a volatile
degradation product generated during melt processing of PET. Thus, it becomes trapped in the sidewalls of a molded article and
desorbs slowly into the contents packaged therein. In some foods and beverages AA can impart an off-taste that is undesirable, thus,
it is important to know its concentration in PET articles that are to be used in food contact applications.
5.2 The desorption conditions of 150 C for 60 min are such that no measurable AA is generated by the sample during the
desorption process.

6. Sources of Error
6.1 A bias is known to exist if the ratio of sample mass (mg) to head-space vial volume (mL) exceeds a value of ten.
6.2 Acetaldehyde is very volatile and must be handled carefully to avoid sample loss during the calibration procedure. Storing
the standard vials in a refrigerator is a must to minimize the error due to volatility.
6.3 Failure to achieve a tight seal on the head-space vial will result in the loss of acetaldehyde during storage and desorption,
producing a false low value.
6.4 Failure to grind the sample to the appropriate particle size may lead to a false low value for residual AA due to the increased
path length for desorption.
6.5 Samples submitted for 8residual AA measurement’ should be stored in a freezer until they are tested. Failure to do so can
result in lower than expected results.
6.6 Excessive grinding of samples can cause residual AA contained therein to be desorbed. Extensive excessive grinding can
lead to actual melting of the polymer and AA generation. Samples which have been chilled in liquid nitrogen properly should only
be in the grinder for ;30 s or less.

7. Apparatus
7.1 Gas Chromatograph, Hewlett-Packard 6890 series4
7.2 Integrator, Hewlett-Packard Model 6890 series, H-P ChemStation, H-P LAN.4
7.3 Head-Space Sampler, Hewlett-Packard 7694.4
7.4 Column, 30-m by 0.53-mm i.d. inside diameter (megabore capillary column).5
7.5 Vials, 20-mL, head-space, with 20-mm septa, 20-mm aluminum caps, and crimper for 20-mm caps
7.5.1 Vials:
Perkin-Elmer Part Numer 0105–0129, or Kimble Glass Inc. Part Number 60827A-23756, or Kimble Glass Inc. Part Number
60827A-23757, or Hewlett-Packard Part Number 5182–08374.
7.5.2 Septa:
Pierce Part Number 12720, or Hewlett-Packard Part Number 9301–0807.4
7.5.3 Caps:

2
Annual Book of ASTM Standards, Vol 08.03.
3
Hewlett-Packard apparatus, website: hewlett-packard.com, was used in the development
3
Annual Book of this standard. If you are aware of alternative suppliers, please provide this information to ASTM headquarters. Your comments will receive careful
consideration at a meeting of the responsible technical committee, which you may attend. Standards, Vol 14.02.
4
J & W Scientific GS-Q (Catalogue Number 115–3435), available from 91 Blue Ravine Rd., Folsom, CA,
4
Hewlett-Packard apparatus, website: JWscientific.com, hewlett-packard.com, was used in the development of this standard. If you are aware of alternative suppliers,
please provide this information to ASTM headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may
attend.
5
AJ & W Scientific GS-Q (Catalogue Number 115–3435), available from Perkin-Elmer, 91 Blue Ravine Rd., Folsom, CA, website: JWscientific.com, was used in the
developmerknt of this stan-dard. If you are aware of alternative suppliers, please provide this information to ASTM headquarters. Your comments will receive careful
consideration at a meeting of the responsible technical committee, which you may attend.
6
Available from Kimbel/Kontes, Vineland, NJ, e-mail: cs@kimble-kontes.com. Perkin-Elmer, website: perkin-elmer.com.
7
Wheaton Part Number 224303, available
7
Available from 1501 North 10th St., Millville, NJ 08332, website: algroupwheaton.com, was used in the development of this standard. If you are aware of alternative
suppliers, please provide this information to ASTM headquarters. Your comments will receive careful consideration at a meeting of the responsible technical commitee, which
you may attend. Kimbel/Kontes, Vineland, NJ, e-mail: cs@kimble-kontes.com.

2
 F 2013 – 001
Pierce Part Number 13214, or Hewlett-Packard Part Number 9301–0721.4
7.6 Crimper, 20-mm, Wheaton Part Number 224303.8
7.7 Decrimper, 20-mm, Kimble Part Number 69903–20.7
7.8 Wiley Mill, equipped with an 800 to 1000-µm screen, or equivalent
7.9 Syringe, calibrated, with certificate of calibration.9
7.10 Small Vacuum Cleaner, with host attachment for cleaning.
7.11 Analytical Balance, capable of accurately weighing to at least 60.0001 g.
7.12 Hammer.

8. Reagents and Materials

8.1 Acetaldehyde (AA), 500 ppm AA in water (or 1000 ppm), purchased certified standard.10
8.2 Liquid Nitrogen, plant grade (R-3, S-3).

9. Calibration and Standardization

NOTE 1—The following procedure should be performed and recorded once every three months.
9.1 Break open a certified AA standard ampule. (Aampules must be stored in a refrigerator) or prepare AA standard by the
attached supplemental procedure. (See Appendix X5.)
9.2 Using the syringe, fill it by placing the tip in the liquid standard and quickly moving the plunger up and down several time
to evacuate any bubbles, then pull the plunger back past the 2.000-µL mark to 2.200 to 2.250 µL.
9.3 Wipe the syringe needle with a tissue.
9.4 Depress the plunger until the digital readout is 2.000 µL.
9.5 Smear the excess liquid that is on the syringe tip on the OUTSIDE of the headspace vial.
9.6 Place the syringe inside of the vial so that the tip just touches the bottom of the vial.
9.7 Quickly inject the liquid standard into the vial and swirl the syringe tip around the inside of the vial to smear all liquid on
the vial walls.
9.8 Remove the syringe and IMMEDIATELY cap the vial.
9.9 Calculate the weight of AA based on the standard’s certified value and a 2.000-µL injection volume.
NOTE 2—Acetaldehyde is very volatile. The AA ampules must be stored in a refrigerator, and the standards prepared immediately after breaking open
an ampule.
9.10 Analyze the working standard by the procedure described in Section 11, starting with 11.2.11.
9.11 Calculate an AA response factor for the standard using the following equation:
response factor of AA 5 Wt of AA in µg/area of AA (1)
NOTE 3—Due to the error associated with the certified standard, 9.1-9.11 should be performed five times using five different standard ampules.
9.12 Average the five response factors obtained, and use this value for the sample analyses.
9.13 Manually enter the calculated response factor in the calibration list of the Hewlett-Packard 68904 integrator or data system.
NOTE 4—During a series of sample analyses, a periodic check of instrument performance is recommended by placing a few liquid standard samples
throughout the sample set. If these values fall out of the acceptable range as specified by the certificate of analysis, recalibration (9.1-9.12) should be
performed.

10. Sample Preparation

10.1 Parisons or Preforms or Plaques—May be cryogenically ground whole, or can be broken into small pieces with a hammer
(using liquid nitrogen) and then ground with the aid of grinding mill equipped with a 20-mesh or 850-µm screen. The grind should
be thoroughly homogenized before sampling for AA. If the appropriate size screen is not available on the large grinding mill, then
it is suggested that the sample be ground to 3 to 6 mm on the large mill and the sample thoroughly homogenized. A portion can
then be taken to a smaller mill equipped with the 20-mesh or 850-µm screen and cryogenically ground again before analysis. Again
the final sample should be thoroughly homogenized.

8
Hamilton Digital with 2–µL capacity, Model
8
Wheaton Part Number 7002KH, 224303, available from 1501 North 10th St., Millville, NJ 08332, website: algroupwheaton.com, was used in the development of this
standard. If you are aware of alternative suppliers, please provide this information to ASTM headquarters. Your comments will recieive careful consideration at a meeting
of the responsible technical committee, which you may attend.
9
Protocol Analytical Supplies, Inc., Middlesex, NJ 08846 (R-3, S-2).
9
Hamilton Digital with 2–µL capacity, Model Number 7002KH, was used in the development of this standard. If you are aware of alternative suppliers, please provide
this information to ASTM H headquarters. Your comments will receieve careful consideration at a meeting of the responsible technical committee, which you may attend.
10
A research report is available from
10
Protocol Analytical Supplies, Inc., Middlesex, NJ 08846 (R-3, S-2). If you are aware of alternative suppliers, please provide this information to ASTM headquarters.
Request RR:F02–1015. Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend.

3
 F 2013 – 001
10.2 Pellets—May be cryogenically ground in a small grinding mill using liquid nitrogen. The final sample should be
thoroughly homogenized before sampling for analysis.
NOTE 5—Samples, either preforms, plaques, or pellets, should be chilled in the liquid nitrogen for several minutes until the liquid nitrogen stops boiling
and then dropped immediately into the grinder. Sample should be sufficiently ground in a few seconds. The grinder should not be allowed to operate more
than 20 to 30 s as in such cases undesirable sample heating can occur.

11. Procedure
NOTE 6—Refer to the general operating manual for the Hewlett-Packard 68904 gas chromatograph, the Hewlett-Packard 76944 head-space sampler,
and the Hewlett-Packard 68904 series integrator for instructions in performing steps in this procedure.
11.1 Adjust the H-P 68904 gas chromatograph to the conditions specified in Appendix X1. Adjust the H-P 76944 head-space
sampler to the conditions in Appendix X2. Set the H-P 68904 series integrator to the conditions in Appendix X3.
11.2 Sample Analysis:
11.2.1 Place 2 to 3 of polymer pellets (or crushed preform) into a small Dewar flask.
11.2.2 Cover the polymer with 20 to 40 mL of liquid nitrogen.
11.2.3 Allow the polymer to chill under the liquid nitrogen for approximately 3 min (or until most of the liquid N2 has
evaporated).
11.2.4 Turn on the Wiley mill equipped with a 800 to 1000-µm screen.
11.2.5 Slowly pour the remaining liquid nitrogen from the Dewar flask through the Wiley mill, followed by the chilled polymer
sample (tapping the sample may be required).
11.2.6 Collect the ground polymer in a small glass jar or small manila envelope.
11.2.7 Turn off the Wiley mill and clean it with a vacuum cleaner.
11.2.8 Allow the ground polymer sample to come to room temperature (approximately 10 min).
11.2.9 Weigh approximately 0.2000 (6 0.0200) g, recorded to the nearest 0.0001 g, into a 20-mL head-space vial.
11.2.10 Place a septum (with Teflon side down towards the inside of the vial) on the vial. Place an aluminum cap on top of the
septum, and crimp the cap with a crimper UNTIL THE CAP CANNOT BE TURNED. Remove the center piece of the aluminum
cap (if it exists).
11.2.11 Place the vial in the appropriate position in the head-space sampler.
11.2.12 Press the “Vial Parameter” key on the H-P 79644 head-space sampler, and enter the starting and stopping vial positions.
11.2.13 Press the “START” button on the H-P 76944 head-space sampler.
11.2.14 The head-space sampler will heat the sample for 60 min at 150°C and then automatically inject the head-space gas and
start the gas chromatograph and integrator.
11.2.15 The final report will appear on the H-P 68904 integrator or the data system when the GC is finished. This report will
give the micrograms of AA.
11.2.16 To determine the concentration in ppm of AA in the polymer sample, divide the micrograms of AA (reported in 11.2.15)
by the sample weight in the vial (recorded in 11.2.9 as grams of polymer).
12. Calculation
12.1 The AA response factor is calculated as described in 9.11 and 9.12. The ppm of AA can be calculated manually by
multiplying the response factor and the area of the AA peak, and then dividing this number by the sample weight in the vial (in
grams).
13. Report
13.1 Report the ppm of AA to two decimal places.
14. Precision and Bias
14.1 To be written
14.1 The following was taken from work done in completed by the International Society of Beverage Technologists (ISBT)
subcommittee concerning standardization of method to determine residual AA in PET.
14.2 The number of laboratories, materials, and determinations in this study meets the minimum requirements for determining
precision in accordance with Practice E 691. A complete report is on file at ASTM Headquarters.11
14.3 This round robin was conducted by having one laboratory mold PET preforms on a 48-cavity injection molding machine
and selecting 6 of those cavities as the sample set. Even though these preforms all came from one PET sample (material), each
cavity has its own unique AA value, and thus, were treated as six different materials. Also, two different types of precision and
bias were calculated, one based on each laboratory using their own calibration standard solution and another when each laboratory
calibrated with a “common” calibration standard.

11
This test method is under the jurisdiction of ASTM Committee F02 on Flexible Barrier Materials and is the direct responsibility of Subcommittee F02.30 on Test
Methods.
Current edition approved April 2001. Published June 2001. Originally published as F 2013 – 00. Last previous edition F 2013 – 00.

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 F 2013 – 001
Practice E 691 Study Minimum
Laboratories: 6 6
Materials: 6 4
Determinations: 3 2

14.4 Precision and Bias With Each Laboratory Using Their Own Calibration Standard—Precision, characterized by
repeatability, Sr and r, and reproducibility, SR and R, has been determined for the materials to be as follows:
Materials Average Sr SR r R
Material A 5.21 0.1812 0.6403 0.5074 1.7928
Material B 6.25 0.4060 0.7464 1.1368 2.0899
Material C 6.37 0.2880 0.6713 0.8066 1.8796
Material D 7.21 0.3285 0.7743 0.9198 2.1680
Material E 7.01 0.4217 0.8350 1.1808 2.3380
Material F 5.88 0.3930 0.7168 1.1003 2.0071

14.4.1 Since the materials used in this study are all from one specific type of material (PET), but have different AA levels
because they are from different cavities, it makes more sense to have one set of precision values rather than one for each cavity.
This will be derived by squaring each Sr and SR, averaging each of Sr2 and SR2 across materials and taking the square root.
Sr SR r R
0.3466 0.7335 0.9705 2.0538

14.4.1.1 Standard Deviation (Sr)—Sr is the square root of the average within laboratory variance.
14.4.1.2 Standard Deviation (SR)—SR is the square root of the sum of the within laboratory variance and between laboratory
variance of the laboratory means.
14.4.1.3 Repeatability—r is the interval representing the largest expected difference between two test results for the same
material, obtained by the same operator using the same equipment on the same day in the same laboratory. A difference larger than
8r’ indicates more variation is present than expected.
14.4.1.4 Reproducibility—R is the interval representing the largest expected difference between two test results for the same
material, obtained by different operators using different equipment in different laboratories, not necessarily on the same day. A
difference larger than 8R’ indicates more variation is present than expected.
14.5 Precision and Bias When Each Laboratory Uses a Common Calibration Standard—Precision, characterized by
repeatability, Sr and r, and reproducibility, SR and R, has been determined for the materials to be as follows:

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 F 2013 – 001
Materials Average Sr SR r R
Material A 5.42 0.1849 0.4128 0.5178 1.1596
Material B 6.47 0.4123 0.6438 1.1545 1.8026
Material C 6.59 0.2703 0.5020 0.7567 1.4057
Material D 7.45 0.3113 0.6333 0.8716 1.7732
Material E 7.26 0.4014 0.5747 1.1240 1.6090
Material F 6.10 0.3854 0.5085 1.0792 1.4237

14.5.1 Since the materials used in this study are all from one specific type of material (PET), but have different AA levels
because they are from different cavities, it makes more sense to have one set of precision values rather than one for each cavity.
This will be derived by squaring each Sr and SR, averaging each of Sr2 and SR2 across materials and taking the square root.
Sr SR r R
0.3376 0.5518 0.9453 1.5450

14.6 Bias—There are no recognized polymer standards by which to estimate bias of this test method. Testing a known liquid
standard with all laboratories using common calibration did not show any laboratory bias between laboratories or between the
average of all laboratories and the known value.
15. Keywords
15.1 acetaldehyde; carbonated soft drink; ground parison AA; PET bottles; 24 hours headspace; AA test; water

APPENDIXES

(Nonmandatory Information)

X1. HEWLETT-PACKARD 689034 SERIES GC CONDITIONS

TABLE X1.1 Hewlett-Packard 689034 Series GC Conditions

Temp 1 Isothermal 90°C
Time 1 8.00 min
Injector Temperature 250°C
Detector Temperature 250°C
Head Pressure 10 psi
Column-Flow 12.2 mL/min Helium
Velocity 85 cm/s
Split Ratio 2.0
Detector Air Flow 300 mL/min
Detector Hydrogen Flow 30 mL/min
Detector Makeup Flow 20 mL/min helium

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 F 2013 – 001

X2. HEWLETT-PACKARD 769434 HEAD-SPACE SAMPLER CONDITIONS

TABLE X2.1 Hewlett-Packard 769434 Head-Space Sampler Conditions

Oven Temp 150°C
Loop Temp 160°C
Transfer Line Temp 170°C
Carrier Pressure 11.5 psi
Vial Pressure 10.5 psi
Vial Eq. Time 60 min
Pressurize Time 0.2 min
Loop Fill Time 0.2 min
Loop Eq. Time 0.1 min
Inject Time 0.2 min
GC Cycle Time 9 min

X3. HEWLETT-PACKARD 6890 SERIES34 INTEGRATOR METHOD FILE

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 F 2013 – 001

FIG. X3.1 Hewlett Packard 6890 Series4 Integrator Method File

8
 F 2013 – 001

FIG. X3.1 Hewlett Packard 6890 Series4 Integrator Method File (continued)

9
 F 2013 – 001

FIG. X3.1 Hewlett Packard 6890 Series4 Integrator Method File (continued)

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 F 2013 – 001

X4. CHROMATOGRAM OF A TYPICAL SAMPLE

FIG. X4.1 Chromatogram of a Typical Sample

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 F 2013 – 001

X5. PREPARATION OF ACETALDEHYDE CALIBRATION STANDARDS

X5.1 Introduction
X5.1.1 The acetaldehyde (AA) calibration standards are used for calibrating gas chromatographs in the determination of AA
present in PET preforms which are used in the food and beverage industry.

X5.2 Materials
X5.2.1 The materials for AA calibration standards are as follows:
X5.2.1.1 Distilled water.
X5.2.1.2 1-L Class A volumetric flask.
X5.2.1.3 Sylon CT.12
X5.2.1.4 Acetaldehyde.
X5.2.1.5 Syringe (1 mL).
X5.2.1.6 Amber caps (4 mL).13
X5.2.1.7 Hole caps14 and TFE-fluorocarbon-faced septa.15
X5.2.1.8 Glass tray.
X5.2.1.9 Balance (capable of 1-mg readings).
X5.2.1.10 Refrigerator, set at 4°C.

X5.3 SetUp
X5.3.1 Use distilled water that is stored in a container other than PET (that is, high-density polyethylene or polyvinyl chloride
bottles)
X5.3.2 If this is the first time a 1-L Class A volumetric flask is being used or the flask has been used for something other than
AA preparation, then proceed to X5.3.3. If the flask has been used previously for AA solution preparation, then proceed to X5.3.4.
X5.3.3 The flask must be deactivated which is done with Sylon CT, or equivalent.12
X5.3.4 Using the distilled water described in X5.3.1, fill the deactivated or previously used 1-L flask to the fill line using the
meniscus.
X5.3.5 Place the flask in a refrigerator and allow it to cool and equilibrate to ;4°C.
X5.3.6 The following items should also be stored in the refrigerator at ;4°C including the acetaldehyde, a 1-mL syringe, a box
of unopened 4-mL amber vials,13 and a glass tray.
X5.3.7 Prepare the caps by placing the TFE-flurocarbon-faced septa15 in the aluminum 8hole-in-cap’ lids14 (Supelco cat.
# 2-712OU, or equivalent). Make sure that the TFE-flurocarbon facing is on the inside so that it is between the rubber septum and
the glass vial. Please note that caps do not have to be refrigerated.

X5.4 Procedure
X5.4.1 Remove the AA, syringe, and 1-L flask and place them beside the balance.
X5.4.2 Fill the syringe with AA, handling the syringe by the top, taking care not to touch the body of the syringe, thereby
causing it to heat up. Place the syringe on the balance and tare it.
X5.4.3 Remove the glass stopper from the 1-L flask, then insert the tip of the syringe into the water and discharge the AA.
Remove the syringe and touch the inside sidewall of the flask to remove any drops. Recap the flask and weight the empty syringe
immediately and record the weight loss.
X5.4.4 Invert the flask and shake at least ten times to ensure proper mixing of the AA.
X5.4.5 Remove the glass tray and the box of vials from the refrigerator. Place no more than 10 vials in the tray. The purpose
of the tray is to catch overfill material.
X5.4.6 Using the 1-L AA solution in the flask, remover the stopper and fill the vials to above the brim, then re-stopper the flask.
X5.4.7 Cap all of the vials with the caps prepared in X5.3.7. It is important to complete X5.4.6 and X5.4.7 as quickly as possible
to prevent AA loss.
X5.4.8 Repeat X5.4.6 and X5.4.7 until the desired amount of vials have been filled, never filling more than 10 at a time.
X5.4.9 For every five vials prepared, prepare one control vial of distilled water. This can be done at room temperature. This
should be done after X5.5.1 and X5.5.3 have been completed as to prevent mislabeling.
X5.4.10 Check all vials to ensure they have no air bubbles (discard vials with air bubbles).

12
Available from Supelco and other suppliers, Catalogue # 3-3065-U. It comes with instructions on deactivating glass.
13
Available from Supelco, Catalogue # 2-7115U, or equivalent.
14
Available from Supelco, Catalogue # 2-712OU, or equivalent.
15
Available from Supelco, Catalogue # 2–7144, or equivalent.

12
 F 2013 – 001
X5.5 Labeling
X5.5.1 Prepare labels containing the concentration listed as XXX milligrams of AA/litre of solution using the value obtained
in X5.4.3 as well as the current date.
X5.5.2 Prepare labels for the control vials saying distilled water.
X5.5.3 Place labels on the appropriate vials.

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 F 2013 – 001

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in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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14