Designation: C 871 – 08a

Standard Test Methods for

Chemical Analysis of Thermal Insulation Materials for
Leachable Chloride, Fluoride, Silicate, and Sodium Ions1
This standard is issued under the fixed designation C 871; 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 (´) indicates an editorial change since the last revision or reapproval.

1. Scope and Water-Formed Deposits by Flame Photometry3

1.1 These test methods cover laboratory procedures for the 2.2 AWWA Standards:
determination of water-leachable chloride, fluoride, silicate, 4500-Si D Molybdosilicate Method for Silica4
and sodium ions in thermal insulation materials in the parts per 4500-Si E Heteropoly Blue Method for Silica4
million range. 3. Terminology
1.2 Selection of one of the test methods listed for each of the
ionic determinations required shall be made on the basis of 3.1 Definitions—Refer to Terminology C 168 for definitions
laboratory capability and availability of the required equipment relating to insulation.
and appropriateness to the concentration of the ion in the 4. Summary of Test Methods
extraction solution.
1.3 The values stated in inch-pound units are to be regarded 4.1 Insulation specimens are leached for 30 min in boiling
as standard. The values given in parentheses are mathematical water. Tests to determine quantitatively chloride, fluoride,
conversions to SI units that are provided for information only silicate, and sodium ions are performed on aliquots of the
and are not considered standard. filtered leachate solution.
1.4 This standard does not purport to address all of the 4.2 Analysis for Chloride:
safety concerns, if any, associated with its use. It is the 4.2.1 Amperometric-coulometric titration test method.
responsibility of the user of this standard to establish appro- 4.2.2 Titrimetric test method. This method is no longer
priate safety and health practices and determine the applica- recommended as requested by ASTM International due to use
bility of regulatory limitations prior to use. of a specific hazardous substance.
4.2.3 Specific ion electrode test method.
2. Referenced Documents 4.3 Analysis for Fluoride:
2.1 ASTM Standards:2 4.3.1 Specific ion electrode test method.
C 168 Terminology Relating to Thermal Insulation 4.3.2 SPADNS colorimetric test method.
C 692 Test Method for Evaluating the Influence of Thermal 4.4 Analysis for Silicate:
Insulations on External Stress Corrosion Cracking Ten- 4.4.1 Atomic absorption spectrophotometry test method.
dency of Austenitic Stainless Steel 4.4.2 Colorimetric test methods—AWWA Methods 4500-Si
C 795 Specification for Thermal Insulation for Use in Con- D and 4500-Si E.
tact with Austenitic Stainless Steel 4.5 Analysis for Sodium:
C 871 Test Methods for Chemical Analysis of Thermal 4.5.1 Flame photometric test method
Insulation Materials for Leachable Chloride, Fluoride, Test Methods D 1428.
Silicate, and Sodium Ions 4.5.2 Atomic absorption spectrophotometry test method.
D 1428 Test Method for Sodium and Potassium in Water 4.5.3 Sodium Ion-Selective electrode.
5. Significance and Use
1
These test methods are under the jurisdiction of ASTM Committee C16 on
5.1 Research has demonstrated that in addition to the halide
Thermal Insulation and are the direct responsibility of Subcommittee C16.31 on ion chloride; fluoride ions, when deposited and concentrated on
Chemical and Physical Properties. the surface of austenitic stainless steel, can contribute to
Current edition approved Dec. 1, 2008. Published January 2009. Originally
approved in 1977. Last previous edition approved in 2008 as C 871 – 08.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM Withdrawn.
4
Standards volume information, refer to the standard’s Document Summary page on Standard Methods for the Examination of Water and Wastewater , 17th Edition,
the ASTM website. American Public Health Association, Washington, DC, 1989.

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 C 871 – 08a
external stress corrosion cracking (ESCC) in the absence of 8. Test Specimen
inhibiting ions.5 Two widely used insulation specifications that 8.1 Apparatus and tools used for special preparation and
are specific to ESCC allow the use of the same Test Methods leaching shall be clean and free of chlorides, fluorides, sili-
C 692 and C 871 for evaluation of insulation materials. Both cates, sodium, and acidic or alkaline materials that might affect
specifications require fluoride ions to be included with chloride the chemical test. Distilled water must be used in all tests
ions when evaluating the extractable ions. unless deionized water has been shown to be adequate.
5.2 Chlorides (and fluorides) can be constituents of the 8.1.1 For molded insulation, use a band saw or equivalent,
insulating material or of the environment, or both. Moisture in making several cuts through the entire cross section of each
the insulation or from the environment can cause chlorides piece of insulation to be tested. Each specimen shall be
(and fluorides) to migrate through the insulation and concen- representative of the entire cross section of the piece, except
trate at the hot stainless steel surface. that metal screen, or expanded metal used as a supportive
5.3 The presence of sodium and silicate ions in the insula- facing shall not be included. It is recommended that thin wafers
tion has been found to inhibit external stress corrosion cracking of material be cut between 1⁄16 and 1⁄8 in. (1.6 and 3.2 mm)
caused by chloride (and fluoride) ions, whether such ions come thick. Cut enough material for two 20-g samples.
from the insulation itself or from external sources. Further- 8.1.2 Blanket fibrous materials are cut into strips across the
more, if the ratio of sodium and silicate ions to chloride (and entire width of the blanket using clean, dry scissors.
fluoride) ions is in a certain proportion in the insulation, 8.1.3 Samples containing moisture are placed in a suitable
external stress corrosion cracking as a result of the presence of container, protected from contamination, and oven dried at 230
chloride (and fluoride) in the insulation will be prevented or at 6 10°F (1006 5°C) ( or manufacturers recommended tem-
least mitigated (see also Specification C 795). perature) to a constant weight (60.1 g) or overnight.

6. Reagents 9. Extraction Technique

6.1 Purity of Reagents—Reagent grade chemicals shall be 9.1 Apparatus:
used in all tests. Unless otherwise indicated, it is intended that 9.1.1 Electronic Balance, capable of weighing to 2000 g
all reagents shall conform to the specifications of the Commit- with readability to the nearest 0.1 g.
tee on Analytical Reagents of the American Chemical Society, 9.1.2 Blender, with jar-top thread preferred.
where such specifications are available.6 Use other grades only 9.1.3 Beaker, 1-L stainless or borosilicate.
if is first ascertained that the reagent is of sufficiently high
9.1.4 Filter, Buchner with suitable filter paper.
purity to permit its use without lessening the accuracy of the
determination. 9.2 Using a closed-top blender, such as a 1-qt Mason jar
with blender blades, blend exactly 20.0 g of sample (or other
6.2 Purity of Water— Distilled or deionized water (DI), weight if necessary) in approximately 400 mL of DI or distilled
having maximum conductivity of 2.5 µS/cm and containing water for 30 s. While most materials blend to a homogeneous
less than 0.1 ppm of chloride ions shall be used in all tests. mixture in 30 s, some very hard materials require 60 s or more.
9.3 Quantitatively transfer the mixture to a tared 1-L stain-
7. Sampling
less steel or borosilicate beaker, rinsing with distilled or DI
7.1 With low-chloride insulating materials, wear clean poly- water.
ethylene gloves while taking and handling the sample to avoid 9.4 Bring to boiling and maintain at the boiling point for 30
chloride contamination from perspiration. Do not use gloves 6 5 min.
made from chloride-containing compounds such as neoprene 9.5 Remove from heat, and cool in a cold water bath to
or saran, or materials with metallic chlorides in their formula- ambient temperature.
tions. Prior to use, rinse gloves twice, drain, and air-dry in a 9.6 Remove water from the outside of the beaker and place
clean, halide-free environment. Store clean gloves in a closed on a balance. Add DI (or distilled) water to bring amount of
container or envelope. water up to exactly 500.0 mL (g) (or other weight if necessary).
7.2 It is suitable to handle materials with more than 25 ppm 9.7 Stir mixture until it is uniform and filter through filter
chloride with clean, dry hands with no significant contamina- paper to get a clear filtrate. If not clear after the first filtration,
tion. refilter through a finer filter paper. The first small portion of
filtrate is used to rinse the receiving flask and Solution A bottle.
Complete this filtration by putting this filtrate in the bottle
5
Whorlow, Kenneth M., Woolridge, Edward and Hutto, Francis B., Jr., “Effect of
labeled Solution A. Since the relationship between solids and
Halogens and Inhibitors on the External Stress Corrosion Cracking of Type 304 liquid has been established, it is not necessary to filter all of the
Austenitic Stainless Steel”; STP 1320 Insulation Materials: Testing and Applica- extract. DO NOT WASH THE FILTER CAKE!
tions, Third Volume, Ronald S. Graves and Robert R. Zarr, editors , ASTM West
Conshohocken, PA, 1997 page 485
9.8 Calculate the Gravimetric Conversion Factor (GCF) by
6
Reagent Chemicals, American Chemical Society Specifications , American dividing the weight of the water by the weight of the sample.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not In the ideal case, this is 500/20 = 25. If weights are not exactly
listed by the American Chemical Society, see Analar Standards for Laboratory as prescribed, a correct GCF must be calculated and used.
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary , U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, 9.9 With calcium silicate insulation it has been shown that it
MD. is not necessary to pulverize the thin chips called for in 8.1.1.

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 C 871 – 08a
Equivalent results are obtained, and a lengthy filtration step is in which fluoride ions are mobile. When the membrane is in
avoided, by extracting the unpulverized chips. contact with a fluoride solution, an electrode potential develops
across the membrane. This potential, which depends on the
10. Test Procedures level of free fluoride ions in solution, is measured against an
10.1 Chloride Determination—One of the following test external constant reference potential with a digital pH/mV
methods shall be used on a fresh aliquot from Solution A. The meter or specific ion meter. Operation and use should follow
precision of the test equipment is often improved through the manufacturer’s recommended procedures, especially noting
use of analytical techniques involving known addition (or any corrections for interferences to determinations.
sample and standard spiking) when the ion concentrations are 10.2.2 SPADNS Colorimetric Test Method—This colorimet-
very low. It is recommended for chloride ion concentrations ric test method is based on the reaction between fluoride and a
less than 20 ppm. zirconium-dye lake. The fluoride reacts with the dye lake,
10.1.1 Amperometric-Coulometric Titration Test Method— dissociating a portion of it into a colorless complex anion (ZrF6
Use an apparatus7 in which direct current between a pair of 2−) and the dye. As the amount of fluoride is increased, the
silver electrodes causes electrochemical oxidation of the anode color produced becomes progressively lighter or different in
and produces silver ions at a constant rate. When all of the hue, depending on the reagent used.
chloride ions have combined with silver ions, the appearance 10.2.3 Ion Chromatography— It is suitable to use and ion
of free silver ions causes an abrupt increase in current between chromatograph, following the manufactures directions and
a pair of indicator electrodes. Because silver ions are generated appropriate techniques for the concentration of the ion in the
at a constant rate, the amount used to precipitate the chloride extraction solution.
ions is proportional to the elapsed time. Hence, the chloride 10.3 Silicate Determination—One of the following test
content of the titration solution can be determined. Since the methods shall be used on a fresh aliquot from Solution A. If
coulometric titrator would not discriminate between chloride, Solution A is cloudy, it shall be refiltered through a 0.45-µm
bromide, and iodide—all would test as chloride—in some millipore filter or centrifuged until clear before use.
cases it is practical to differentiate between the halides to show
10.3.1 Atomic Absorption Spectrophotometry Test
chloride only, since the others have not been shown to cause
Method—Atomize an aliquot from Solution A by means of a
stress corrosion cracking in austenitic stainless steel. A
nitrous oxide-acetylene flame. The absorption by the silicon
chloride-sensitive electrode detects chloride only.
atoms of radiation being emitted by a silicon hollow cathode
10.1.2 Titrimetric Test Method8—This method is no longer
lamp source provides a measure of the amount of silicon
recommended as requested by ASTM International due to use
present in the solution, using an atomic absorption spectropho-
of specific hazardous substance.
tometer.
10.1.3 Specific Ion Electrode Test Method—The chloride-
sensitive electrode consists of silver halide/silver sulfide mem- 10.3.2 Colorimetric Test Method—This test method covers
branes bonded into the tip of an epoxy electrode body. When the determination of soluble silica (SiO 2) by the molybdosili-
the membrane is in contact with a chloride solution, silver ions cate colorimetric procedure. In this test method, ammonium
dissolve from the membrane surface and the electrode develops molybdate at low pH reacts with soluble silicate or phosphate
a potential due to the silver ion concentration. This concentra- to produce heteropoly acids. Oxalic acid is used to destroy the
tion is in turn determined by the sample chloride ion concen- molybdophosphoric acid but not the molybdosilicic acid. The
tration. This potential is measured against a constant reference intensity of the yellow molybdosilicate complex follows Beers
potential with a digital pH/mV meter or specific ion meter. law. This test method is an adaption of AWWA
Operation and use should follow manufacturer’s recommended Methods 4500-Si D and 4500-Si E. If phosphates are not
procedures, especially noting any corrections for interferences present as contaminants, the oxalic acid may be omitted to
to determinations. The chloride-sensitive electrode is not obtain a more stable molybdosilicate complex.
reliable for chloride levels below 2 ppm in Solution A. 10.3.2.1 Reagents:
10.1.4 Ion Chromatography—It is suitable to use an ion (1) 10 % Ammonium Molybdate—Dissolve 10.0 g of
chromatograph, following the manufacturers directions and (NH4)6Mo7O24·4H 2O in distilled water, bringing final volume
appropriate techniques for the concentration of the ion in the to 100.0 mL.
extraction solution. (2) Hydrochloric Acid—Dilute 125 mL of concentrated
10.2 Fluoride Determination—One of the following test HCl to 500 mL to make 1:3.
methods shall be used on a fresh aliquot from Solution A: (3) Oxalic Acid—Dissolve 7.5 g of H 2C2O4·2H2O in
10.2.1 Specific Ion Electrode Test Method for Fluoride— distilled water to make 100.0 mL.
The fluoride-sensitive electrode consists of a single-crystal (4) Silica—Prepare a standard silica solution from pure
lanthanum fluoride membrane, and an internal reference, sodium metasilicate or equivalent concentrate to a stock
bonded into an epoxy body. The crystal is an ionic conductor concentration of 1000 mg/L (µg/mL) on SiO2 basis.
10.3.2.2 Apparatus:
7
Bowman, R. L., Cotlove, E., Trantham, H. V., “An Instrument and Method for (1) Spectrophotometer, with a 1-cm cell or tube.
Automatic, Rapid, Accurate, and Sensitive Titration of Chloride in Biologic (2) Volumetric Flasks, 50 mL, for solution and sample
Samples,” Journal of Laboratory and Clinical MedicineVol 51,1958 , pp. 461–468.
8
Clarke, F. E., “Determination of Chloride in Water Improved Colorimetric and
preparation.
Titrimetric Methods,” Analytical Chemistry, Vol 22, 1950, pp. 553–555. (3) Pipettes, miscellaneous.

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 C 871 – 08a
10.3.2.3 Calibration Procedure—Turn on the spectropho- 10.4.3 Ion-Selective Electrode—Use the Sodium Ion-
tometer and set to 410 nm. Prepare 100-µg/mL standard by Selective electrode according to the manufacturer’s directions,
diluting 100 mL of the 1000-µg/mL stock to 1000 mL. Pipette calibrating with standards to bracket the range of the unknown.
1, 2, and 4 mL of the 100-µg/mL standard into each of the three 10.4.4 Ion Chromatography—It is suitable to use an ion
50-mL volumetric flasks. Set out one more 50-mL flask for chromatograph, following the manufactures directions and
reagent blank use. Pipette 2.0 mL of ammonium molybdate appropriate techniques for the concentration of the ion in the
solution into each volumetric flask. Pipette 2.0 mL of 1:3 extraction solution.
hydrochloric acid into each flask, then bring volumes to exactly 10.5 pH, when required—Determine the pH8 of an aliquot
50.0 mL, and mix well (see Note 1). Start the timer. Zero the from Solution A. Discard the aliquot after the determination.
spectrophotometer with the reagent blank. Read all three The pH shall be run as quickly as possible after the extraction
standards versus the reagent zero between 10 and 30 min of the because solutions sometimes change pH on standing.
time when the reagents were added. Plot the optical density
versus millilitres of 100-µg/mL standard added (µg/mL in test 11. Calculation
solution). 11.1 Procedure—The gravimetric conversion factor (GCF)
is calculated using Eq 1:
NOTE 1—When it has been determined that phosphates are present, 2.0
mL of oxalic acid must be added after the other two reagents. When oxalic GCF 5 $Volume liquid ~g!%/$Sample weight ~g!% (1)
acid is used, the timing is much more important, because the yellow color
begins to fade after 15 min. 11.2 Chloride content of insulation is calculated using Eq 2:
10.3.2.4 Determination of the Unknown—Test as soon as Cl2 ~µg/g! 5 concentration observed
possible after cooling Solution A, preferably on the same day, in Solution A ~µg/mL! 3 GCF (2)
overnight at worst. In a 50-mL volumetric flask, add 1.0 mL of
Solution A (see Note 2), 2.0 mL of ammonium molybdate 11.3 Fluoride content of insulation is calculated using Eq 3:
reagent, and 2.0 mL of 1:3 hydrochloric acid, (and 2 mL oxalic
F2 ~µg/g! 5 concentration observed
acid solution when necessary), followed by swirling to dissolve in Solution A ~µg/mL! 3 GCF (3)
any precipitated material. Add distilled (or DI) water to bring
volumes to exactly 50.0 mL. Mix well and start the timer.
11.4 Silicate content of insulation is calculated using Eq 4:
Between 10 and 30 min, read the sample versus the reagent
zero. Consult the calibration curve to find equivalent millilitres S iO3 5 ~µg/g! 5 concentration of SiO 2 observed
of 100-µg/mL standard. in Solution A ~µg/mL! 3 76/60 3 GCF (4)

NOTE 2—This test method was designed for determining soluble NOTE 5—The factor 76/60 converts observed SiO2 to SiO3 = as
silicate in materials containing 1000 to 10 000 ppm of soluble silicate as required by Specification C 795 and other specifications relating to
determined by this test method. For materials out of this range, more or austenitic stainless steel corrosion.
less of Solution A must be used with appropriate adjustments being made
to the calculation procedure. 11.5 Sodium content of insulation is calculated using Eq 5:
10.4 Sodium Determination—One of the following test N a1 ~µg/g! 5 concentration observed
in Solution A ~µg/mL! 3 GCF (5)
methods shall be used on Solution A. The precision of the test
equipment is often improved through the use of analytical
techniques involving known addition (or sample and standard 12. Report
spiking) when the ion concentrations are very low. It is
recommended for sodium ion concentrations less than 500 12.1 Include in the report of the results of each test the
ppm. following information:
12.1.1 Any pertinent information concerning the identifica-
10.4.1 Flame Photometric Test Method—Atomize the fil-
tion of the material.
tered aliquot in a flame and determine the concentration of
12.1.2 The test methods used for determination of chloride,
sodium by photometry in accordance with Test Methods fluoride, sodium, and silicate.
D 1428 or equivalent. 12.1.3 The numerical results of the tests expressed in µg/g
NOTE 3—Corrections must be made if high concentrations of calcium, (ppm) of chloride, fluoride, sodium, and silicate calculated on
potassium, or magnesium are present. the basis of weight of each dry insulation specimen.
10.4.2 Atomic Absorption Spectrophotometry Test 13. Precision and Bias
Method—Atomize the filtered aliquot by means of an air-
13.1 A round robin was conducted utilizing three different
acetylene flame. The absorption by the sodium atoms of
types of insulation and two prepared extracts. Samples were
radiation being emitted by a sodium hollow cathode lamp
supplied to ten laboratories. Seven reported results on all of the
source provides a measure of the amount of sodium present in
samples, and one reported partial results.
the solution, using an atomic absorption spectrophotometer.
13.1.1 Of the 236 data points supplied, 39 were thrown out
NOTE 4—Corrections must be made if high concentrations of calcium, as outliers because they were either double or one half of the
potassium, or magnesium are present. average of the other comparative data points. Twenty-six of the

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 C 871 – 08a
TABLE 1 Round-Robin Mean Values and Standard Deviations
Sample Type Calsil Perlite Fiber Glass Solution Solution
Chloride mean 121 40.3 116 129 54.2
Standard deviation 13.4 8.9 22.5 16.3 12.6
sd/mean 3 100 11.1 22.1 19.3 12.6 23.2

Fluoride mean 55.6 17.5 1.9 44.0 13.2

Standard deviation 7.4 3.7 0.8 2.9 2.8
sd/mean 3 100 13.3 21.1 42.1 6.6 21.2

Sodium mean 5845 23 950 732 5243 1692

Standard deviation 1472 3531 194 595 523
sd/mean 3 100 25.1 14.7 26.5 11.3 30.9

Silicate mean 5926 45 860 498 4275 1358

Standard deviation 1609 5190 206 831 295
sd/mean 3 100 27.2 11.3 41.3 19.4 21.7

outliers were from three laboratories that were using the ion ing interlaboratory and within-laboratory precision data. The
chromatograph. Of these 26, 6 and an additional 4 were from results of these tests are for the chemical analysis only and do
a laboratory that used an unapproved extraction method. not include the extraction step, which was covered by the
13.1.2 For each determination, a mean value and a standard previous precision and bias testing.
deviation were calculated. Table 1 shows the results. 13.2.1 The interlaboratory reproducibility standard devia-
13.1.3 There was no estimation of bias, since the true values tion as a percentage of the mean value obtained by all of the
for the samples were unknown. labs (SD/Mean x 100) was higher at the low ion concentrations
13.1.4 Since the material samples were run in duplicate by and therefore the data is summarized with ranges:
all of the participating laboratories but one, a within laboratory Silicate <1000ppm = 12.1%; >1000ppm = 7.5%
value could have been calculated but was not. Suffice it to say Sodium <600ppm = 21.7%; >600ppm = 9.0%
that the within laboratory variability should have been some- Chloride <20ppm = 23.6%; >20ppm = 10.0%
what less than the between laboratory variability. Fluoride <5ppm = 34.1%; >5<10ppm = 13.4%; >10ppm = 5.7%
13.1.5 A full report of the data is on file with ASTM as a
13.2.2 The within-laboratory repeatability standard devia-
research report.9
tion as a percentage of the mean value obtained within the lab
13.2 An interlaboratory round-robin10 was performed by
(SD/Mean x 100) is summarized as follows:
five laboratories on samples taken from large batches of
Silicate <1000ppm = 5.4%; >1000ppm = 2.6%
prepared extraction solutions from six different kinds of
Sodium <600ppm = 5.7%; >600ppm = 1.8%
thermal insulation containing a wide range of extractable ions Chloride <20ppm = 9.6%; >20ppm = 7.4%
concentrations. Each lab ran the test series three times provid- Fluoride <5ppm = 4.0%; >5<10ppm = 2.5%; >10ppm = 3.0%

9
Supporting data have been filed at ASTM International Headquarters and may
14. Keywords
be obtained by requesting Research Report RR: C16–1015. 14.1 chemical analysis; chloride; fluoride; silicate; sodium;
10
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR: C16–1029. thermal insulation

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