A S T M DI339 A4 lls%l 0759530 0023500 4 ___ -~

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4CrI~ Designation: D 1339 - 84
NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

Standard Test Methods for

SULFITE ION IN WATER'
This standard is issued under the h e d designation D 1339; the number immediately foUowingthedesignationindicates 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 mppraval.
These methods have been approvedfor tise by agencies of the Department of Defense andfir listing in the DoD Index of Specifcations
and Standards.

1. Scope 3. Definitions
1.1 These test methods cover the volumetric 3.1 For definitions of terms used in these
determination of sulfite ion in water. The follow- methods refer to Definitions D 1129.
ing three methods are included:
4. Significance and Use
Range Section
Method A 0.1 to 6 mg/L 7 to 14 4.1 The determination of sulfite is usually
Na2S03 made on process waters, boiler waters, and other
Method B 6 mg/L Na2S03 15 to 22 waters that have been treated with sodium sulfite.
or higher Generally, in boiler applications, a cataIyzed so-
Method C 3 mg/L Na2S03 23 to 29
or higher lution of sodium sulfite is injected continuously
into the feedwater system for the purpose of
1.2 Method B may be used for samples con- removing dissolvedoxygen to prevent pitting and
taining less than 6 mg/L Na2S03with some loss excessive oxidation of metal components. In
of precision; in such applications the end point most boiler operations, the sulfite concentration
may be determined with starch indicator. is maintained above 20 mg/L in the boiler water.
1.3 This standard may involve hazardoiis ma- Sulfite injection is restricted to Iower-pressure
terials, operations, and equipment. This standard boilers (<lo00 psi, 6900 kPa) because of the
does not purport to address all of the safety prob- tendency for decomposition at higher tempera-
lems associated with its tise. It is the responsibil- tures. When exposed to the environment, dis-
ity of whoever uses this standard to constilt and charges containing sulfites wilI react with the
esrablish appropriate safety and health practices oxygen to form sulfates. Generally speaking, sul-
and determine the applicabilityof regulatorylimi- fites are not found in natural waters.
tations prior to use.
5. Purity of Reagents
5.1 Purity of Reagents-Reagent grade chem-
2. Applicable Documents icals shall be used in all tests. Unless otherwise
2.1 ASTM Standards: . indicated, it is intended that all reagents shall
D 1129 Definitions of Terms Relating to conform to the specifications of the Committee
Wate8 on Analytical Reagents of the American Chemi-
D 1192 Specifcation for Equipment for Sam-
piing Water and Steam'
D 1193 Specification for Reagent Wate8 'These test methods are under the jurisdiction of ASTM
Committee D-19 on Water and are the direct responsibility of
D 2777 Practice for Determination of Preci- SubcommitfeeD19.05 on Inorganic Constituents in Water.
sion and Bias of Methods of Committee Current edition approved Jan. 27, 1984. Published March
1984. Originally published as D 1339 - 54 T. Last previous
D- 19 on Wate? edition D 1339 - 78.
D 3370 Practices for Sampling Wate? Anniial B w k of ASTM Siandards, Vol 11.O 1.

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D 1339

cal Society, where such specifications are avail- 10. Apparatus

able.3 Other grades may be used, provided it is 10.1 Sample Tubes-The glass sample tubes?
first ascertained that the reagent is of sufficiently as shown in Fig. 1, have a nominal capacity of
high purity to permit its use without lessening 500 mL. The capacity of each tube shali be
the accuracy of the determination. determined to the nearest 1 mL.
5.2 Purity of Water-Unless othenvise indi- 10.2 Burets-The four 10-mL burets shall
cated, references to water shall be understood to have stopcock bores not greater than 2 mm and
mean reagent water conforming to Specification maximum tip diameters not exceeding 3 mm.
D 1193, Type II. 10.3 Stirrer-The motor-driven stirrer shall
be variable-speed and equipped with a glass pro-
6. Sampling
peller.
6.1 Collect the sample in accordance with 10.4 Dead-Stop Electrometric Titrator-The
Practices D 3370. electrometric dead-stop indicating apparatus’
6.2 For Method C, add 10 mL of EDTA so- shall be equipped with platinum electrodes. The
lution to the l-L sampling bottle before taking assembly shall be sensitive to the addition of 0.05
the sample. Fill the bottle to the brim, cap, and mL of 0.005 N sodium thiosulfate (Na2S203)
shake well to mix. The EDTA.solution com- solution to 500 mL of water.
plexes such ions as cobalt and copper, which
catalyze the rapid oxidation of sulfite when the 11. Reagents
sample is exposed to the air. +
1 1.1 HydrochloricAcid ( 1 1)-Mix 1 volume
NOTE1-To avoid premature oxidation of sulfite, of concentrated hydrochloric acid (HCi, sp gr
the titration should be camed out immediately after 1.19) with 1 volume of water.
collection. 1 1.2 Potassium Dichromat@-Heat potas-
sium dichromate (K2Cr207)in a platinum cru-
.METHOD A cible to a temperature just above its fusion point
(396“C), taking care to exclude all dust and or-
7. Scope ganic matter. After cooling, crush the fused salt
7.1 This test method is applicable to the de- to a powder in an agate mortar and preserve in
termination of sulfite ion in water, especially a glass-stoppered bottle.
boiler water and boiler feedwater, in which the 1 1.3 Potassium Iodate Solution, Standard
sulfite ion concenfration is 0.1 to 6 mg/L.. (0.025 N)-Dissolve x g of potassium iodate
7.2 The analyst should be aware that adequate (ao3),dried at 120”C, and 0.5 g of sodium
collaborative data for precision and bias state- bicarbonate (NaHC03) in water and dilute to 1
ments as required by Practice D2777 is not L ( x = 8.92 times the normality of the standard
provided. See Precision and Bias section for de- NazSz03solution, see 11.6). .
tails. 11.4 Potassium Iodide-The potassium io-
dide (KI)shall not impart a blue color when 1 g
8. Summary of Method is dissolved in 20 mL of freshly boiled water
8.1 The sample is taken in a tube of special “Reagent Chemicals, American Chemical Society Specifi-
design to exclude air until the sulfite has been cations,”Am. Chemical Soc., Washington, D.C. For suggestions
on the testing of reagents not listed b: the American Chemical
reacted with iodine chloride. The excess iodine Society, see “Reagent Chemicals and Standards,” by Joseph
chloride is determined by titration with thiosul- Rosin, D. Van Nostrand Co., Inc., New York, N.Y., and the
fate. The range of the method is limited by “United States Pharmacopeia.”
4McLean-type sampling tube, as modified by the Manne
reagent concentrations. Engineering Laboratory, U. S. Navy, and by the Heat Exchange
Institute. This tube is the same as that specified in ASTM
Methods D 888, Referee Methods B and C for DissolvedOxygen
9. Interferences in Water, Anntrul Book ofASTMSlundards, Part 31.
Ulmer, R. C., Reynar, J. M., and Decker, J. M., “Applica-
9.1 Other reducing agents such as sulfides and bility of Schwartz-Gurney Method for Determining Dissolved
certain heavy-metal ions react like sulfite with Oxygen in Boiler Feedwater, and Modification of the Method
iodine chloride and cause high results. Nitrite, if to Make it Especially Applicable in the Presence of Such Im-
purities as are Encountered in Power Plants,” Proceedings, Am.
present, will oxidize sulfite when the sample is Soc. Testing Mats., Vol 43, 1943, pp. 1261-63.
acidified. Reagent used for standardization purposes only.
7
7 -
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 D 1339

treated with 5 drops of 1 N sulfuric acid (H2S04) lution prepared in this manner will remain chem-
and 1 mL of freshly prepared starch solution. i d l y stable for I year.
1 1.5 Potassium Iodide Solution (50 g/L)- NOTE2-If the indicatoris not prepared as specified
Dissolve 50 g of iodate-free Ki and 0.5 g of or a proprietarystarch indicator preparation is used the
sodium bicarbonate (NaHC03) in freshly boiled report of analysis shaii speii out the deviation.
and cooled water and dilute to 1 L.
12. Procedure
i 1.6 Sodiiim Thiosulfate Solution, Standard
(0.10 N)-Using a 1000-mL volumetric flask, €2.1 sampling- Arrange the sample tube in
dissolve 24.82 g of sodium thiosulfate (NazSzO3. a support so that it is vertical, with its upper
5Hz0) in approximately 800 mL of water that outIet free of hose connections and at a level
has just been boiled and cooled, by inverting the higher than the valve for adjustment of sample
flask at reguIar short intervals. Stabilize the so- flow. Connect the lower end to the sampling line
lution by dissolving in it, in the same manner, l by means of rubber tubing. The sampling line
g of sodium carbonate (Nazco3), and make up shall contain a suitable cooling coil if the water
to 1 L with boiled water. Standardize against being sampled is above temperature, in which
KzCrz07,as follows: case the sample shall be cooled to ambient-air
11.6.1 Dissolve 2 g of iodate-free Ki and 2 g temperature. If a cooling coil is used, the valve
of NaHC03 in 300 mL of water in a 500-mL for dooling-water adjustment shaü be at the inlet
Erlenmeyer flask and add HCl (sp gr I. 19) slowly, to the cooling coil, and the overkìow shall be to
while swirling the flask, until carbon dioxide a point of lower elevation. The valve for adjusting
(COZ)gas evolution ceases. Add 10 mL excess of the flow of sample shall be at the outlet from the
HCI, mix, and thendissolve 0.098 g of dried cooling coil. Adjust the sample to a rate that will
K2Crz07(see 1 1.2). Wash down the inside of the fill the tube in 40 to 60 s and continue this flow
flask with a small amount of water without agi- long enough to provide at least ten changes of
tating the flask, and allow to stand for 10 min. water in the sampling tube. if the sampling line
11.6.2 Titrate with the Na&O3 solution, us- is used intermittently, alíow a suitably longer
time for the first sample to ensure adequate
ing starch solution as the indicator, until the color
just changes from blue to the green color of the flushing of the sampling line and cooling coil.
chromic salt. Close the upper stopcock of the tube, and im-
1 1.6.3 Calculate the normality of the Na2S203 mediately close the lower sfopcock and remove
solution, as follows: the tubing connection. If the line being sampled
is under such high pressure that the sampling
N = (A149.94B) X loo0 tubes or connecting tubing may burst with the
where: water hammer when the stopcocks are closed,
N = normality of the NazSz03solution, throttle the sample flow with the control valve
A = grams of KzCr207used, and just before the sample is removed, but do not
B = millilitres of NazSz03solution required for shut off the sample flow completely.
the titration. 12.2 Fixing-Fill the three burets with HCI
1 I .I Sodium Thiosulfate Solution. Standard (If. I), KI solution, and 0.025 N K I 0 3 solution,
(0.005 N)-Transfer 25 mL of the nominally respectively. Hick the water from the upper nip-
O. 10 NNaZSzO3solution to a 500-mLvolumetric ple of the sample tube and fill the nipple to the
flask. Dilute to the mark with water and mix upper calibration mark with HCl. If a bubble is
completely. This solution shall be prepared not entrapped in the nipple within or below the
more than 12 to 15 h before using. reagent, remove it by probing with a clean plati-
i 1.8 Starch Indicator-Mate a paste of 6 g of num wire until the bubble rises to the surface.
arrowroot starch or soluble iodometric starch Open the lower stopcock and admit the reagent
with cold water. Pour the paste into 1 L of boiling by control with the upper stopcock until the
water. Then add 20 g of potassium hydroxide meniscus in the nipple coincides with the lower
(KOH), mix thoroughly, and allow to stand for calibration mark. If the sample contains more
2 h. Add 6 mL of glacial acetic acid (99.5 %). than 800 mg/L of NaOH, add 2 mL more of
Mix thoroughly and then add sufficient HCl (sp acid for each IO00 mg/L of alkalinity or fraction
gr 1.19) to adjust the pH value of the solution to thereof in excess of 800 m a . Close both stop-
4.0. Store in a glass-stoppered bottle. Starch so- cocks and ense both nipples with a fine stream

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DI339

ofwater. Mix the contents by shaking or rotation, 14. Precision and Bias'
and flick out the excess water from each nipple. 14.1 The precision of this method may be
Invert the tube and fill what is now the upper expressed as follows:
nipple with KI solution to the 2-mL calibration
mark, Introduce the solution into the sample,
s, = 0.2
repeating the stopcock control, the rinsing of where:
both nipples, the shaking and rotating, and the S,= overall precision expressed in mg/L of
flicking of water from the nipples. Again invert NazSO3.
the tube and now introduce 2.0 mL of 0.025 N 14.2 The supporting data on this coilaborative
KIO3 solution into the sample foliowing the di- study do not include information on the number
rections given above for adding the reagents and of participating laboratories, water used, or sin-
rinsing the nipples. Once more, shake and rotate gle-operator precision or bias. It is the responsi-
the tube to mix the sample thoroughly. biiity of the analyst to assure the validity of the
12.3 Titration of Sample-Invert the sample method in a particular water.
tube and drain the sample into a clean 800-mL METHOD B
Giffin low-form beaker by opening both stop-
cocks. Do not rinse or blow into the sampling 15. Scope
tube, but shake the last drops from the nipple 15.1 This method covers the determination of
into the beaker. Add several drops of starch sulfite ion in wafer, especially boiler water and
indicator to indicate the approach of the end boiler feedwater, in which the sulfite concentra-
point. Insert the electrodes of the electrometric tion is 6 mg/L or higher.
dead-stop indicating apparatus into the sample, 15.2 The anaIyst shoald be aware that ade-
start the stirrer at low speed, and titrate the excess quate collaborativedata for precision and bias as
iodine chloride with 0.005 N Na2S2O3solution. required by Practice D 2777 is not provided. See
12.4 Determination ofBlank (Note 3)-Make Precision and Bias section for details.
a blank titration of 500 mL of water containing
no sulfife, to which have been added the three 16. Summary of Method
reagents that were added to the sample in 12.2. 16.1 Provision is made for excluding air from
NOTE3-Alternatively, if such tubes are available, the sample while it is being taken. Potassium
one sample of 500 mL and one sample of 250 mL are iodate is then added to form iodine chloride with
collected simultaneously, fixed as described in 12.2, potassium iodide and hydrochloric acid to oxi-
and titrated as described in 12.3. The difference in the dize the sulfite ion. The excess iodine chloride is
net amounts of 0.025 N Ki03solution used by the
sulfite content of the two samples will be the sulfite-ion titrated with sodium thiosulfate solution, using
equivalent of a 250-mL sample. an electrometric indicator to show the end point.
17. inferferences
13. Calculation 17.1 High results may be caused by the pres-
13.1 Calculate the concentrations of sulfite as ence of other reducing materials such as sulfide
milligrams per L of sodium sulfite (Na2S03),as and ferrous iron. Nitrite, if presenf, will oxidize
follows: sulfite when the sample is acidified.
Sulfite as Na2SO3, mg/L = 63000N (A - B)/S 18. Apparatus
where: 18.1 ErlenmeyerFlask, wide-mouth, 500-mL,
N = normality of the Na2S20ssolution, fitted with inlet, outlet, and siphon-leveling con-
A = millilitres of Na2SzO3solution needed to nections, as shown in Fig. 2.
titrate the blank, 18.2 Magnetic StirringApparatus, with swing-
B = millilitres of Na2Sz03 solution needed to ing support if electrometric end point-indicating
titrate the sample, and apparatus is used.
S = sampling-tube volume in millilitres minus 18.3 Dead-Stop End Point-Indicating Appa-
6.
13.2 To convert mg/L of Na2S03to mg/L '
Supporting data for these methods have been fded at ASTM
of sulfite ion, multiply by 0.635. Headquarters as R R D19-155.

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 D 1339
ratzcs-See 10.4. This apparatus is not necessary 21. Calculation
for less precise testing (see 1.2). 21.1 Calculate the concentration of sulfite as
milligrams per litre of sodium sulfite (N~~SOS),
19. Reagents as follows:
Suitïte as NazSon, mg/L = 126 N(A - B )
-+
19.1 Hydrochloric acid (1 1)-See 11.1.
19.2 Potassiiim Iodate Solution, Standard where:
(0.05 N)-Dissolve x g of potassium iodate N = normality of the Na2S203solution,
(KIOS), dried at 120°C and 0.5 g of sodium A = millilitres of Na2S203 solution needed to
bicarbonate (NaHC03) in water and dilute to titrate the blank, and
500 mL, in a volumetric flask, ( x = 8.92 times B = millilitres of Na2S203 solution required to
the normality of the standard Na2S203 solution, titrate the sample.
see 19.5). 21.2 To convert milligrams per litre of Na~S03
19.3 Potassium Iodide (50 g/L)-See 11.5. to milligrams per litre of sulfite ion, multiply by
19.4 Sodium Thiosulfate Solution, Standard 0.635.
(O. 10 N)-See 11.6.
19.5 Sodiiim Thiosulfate Solution. Standard 22. Precision and Bias’
(0.01 ¡“)-Transfer 50 mL of the O. 10 Nsodium 22.1 The single-operator, single-laboratory
thiosulfate (Na2SrO3) solution to a 500-mLvol- precision (SLo)of this method at a level of 10.3
umetric flask. Dilute to the mark with water and mg/L Na2SO3 may be expressed as follows:
mix completely. This solution should be pre- S, = 0.12 mg/L
pared not more than 12 to 15 h before using. 22.2 The supportingdata on this study do not
19.6 Starch Indicator-See 11.8. includewaters used or bias. It is the responsibility
of the analyst to assure the validity of the method
20. Procedure in a particular water.
20.1 Connect the sampling flask to fhe sample METHOD C
cooler with rubber tubing so that the sample, at
or slightly below room temperature, enters the 23. Scope
bottom of the flask and overflows from the top. 23.1 This test method is particularly applica-
Overflow an estimated volume of five times the ble for control tests where good precision is not
flask volume, allowing the siphon to fill during required and the sulfite content is 3 mg/L or
this step. Then close off the inlet connection and higher.
open the syphon to adjust the sample volume to 23.2 The analyst should be aware that ade-
500 mL. quate collaborative data for precision and bias
20.2 Fixing-Remove the stopper from the statements as required by Practice D 2777 is not
flask, set the flask on the magnetic stirrer plat- provided. See Precision and Bias section for de-
form, and operate the stirrer at low speed while tails.
5 mL of HCI, 5 mL of KI solution, and 5.0 mL
of KI03 solution are added immediately and in 24. Summary of Method
that order, If the sample contains more than 300 24.1 Iodine, liberated by potassium iodate so-
mg/L of sulfite, use correspondingly larger lution, reacts with the sulfite in the water sample.
amounts of reagents. An end point is reached when excess iodine is
20.3 Titration-Add several drops of starch present, as shown by the blue color produced
indicator solution to indicate the approach of the with starch indicator.
end point. Insert the electrodes of the end point
indicator into the sample and titrate the excess 25. Interferences
iodine chloride with 0.01 NNazSz03 solution. 25.1 EDTA is added to the sample to complex
20.4 Determination of Blank-Make a blank such metallic ions as copper that catalyze the
titration of 500 mL of water containing no sulfite oxidation of sulfite when the sample is exposed
to which have been added in the same way and to air. Other reducing agents such as sulfides and
in the same volume the reagents used to fur the ferrous iron will cause high results since they
sample (see 20.2). react like sulfite. Sulfamic acid is added to react
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 ASTM DI339 84 H 0757530 0023505 3
D1339
with nitrite, which would otherwise oxidize sul- tion used as S.Repeat the test, using 100 mL of
fite when the sample is acidified in the test. water instead of sample, and record the volume
of Klo3solution as B.
26. Reagents 28. Calculation
26.1 EDTA Solution (3.72 g/L)-Dissolve 28.1 Calculate the concentration of sulfite, as
3.72 g of disodium ethylenediamine tetraacetate SO3-- and as Na2S03, in milligrams per L, as
dihydrate in water and dilute to 1 L. follows:
+
26.2 HydroctilorìcAcid (1 1)-See 11.1, Sulfite as SO3- -O, mg/L = 6.35 (S- B)
26.3 Potassium Iodate Solution, Standard (1 Sulfite as Na2SOj, mg/L = 10 (S- B)
mL = 1 mg NazS03)-Dissolve 0.566 g of potas- where:
sium iodate (mo3)dried at 120”C, and 0.5 g of S = miiliíitres of Klo3solution required for
sodium bicarbonate (NaHC03) in water, and titration of the sample, and
dilute to 1 L in a volumetric flask. B = millilitres of KIOS solution required for
26.4 Potassium IodideSolution (50 g/L)-See titration of the water blank.
11.5.
26.5 Starch Itidicator-See 11.8. 29. Precision and Bias
26.6 Sulfamic Acid, crystalline. 29.1 The precision of this test method may be
expressed as follows:
27. Procedure so= 1
27.1 Pour 5 mL HCI (l”1) into a 250-mL, where:
wide-mouth Erlenmeyer flask and add 0.1 g of SO= the single-operator precision expressed in
sulfamic acid, Pipet 100 mL of the EDTA-stabi- milligrams per litre of Na2S03.
lized sample into the flask, keeping the pipet tip 29.2 The supportingdata on this collaborative
below the surface. Add 1 mL of starch solution study do not include information on the number
and 5 mL of KI soIufion. Immediately add KI03 of participatinglaboratones,waters used, or over-
solution dropwise from a buret while shaking the ali precision and bias. It is the responsibility of
flask, until the first persistent blue color appears the analyst to assure the validity of the method
in the sample. Record the volume of KI03 solu- in a particular water.

Rubber Retaining Washer

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FIG. 1 5W-Millilitre Sample Tube for Sulfite Determination

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