ASTM C225-85(2004)
(Test Method)Standard Test Methods for Resistance of Glass Containers to Chemical Attack
Standard Test Methods for Resistance of Glass Containers to Chemical Attack
SIGNIFICANCE AND USE
The solubility of glass in contact with food, beverages, or pharmaceutical products is an important consideration for the safe packaging and storage of such materials. Autoclave conditions are specified since sterilization is often employed for the packaging of the product. It also represents one of the most extreme conditions, particularly of temperature, that containers will ordinarily experience. Any of the three test methods described may be used to establish specifications for conformity to standard values, either as specified by a customer, an agency, or “The United States Pharmacopeia:”
3.1.1 Test Method B-A is intended particularly for testing glass containers primarily destined for containment of products with a pH under 5.
3.1.2 Test Method B-W is intended particularly for testing glass containers to be used for products with a pH of 5.0 or over.
3.1.3 Test Method P-W is a hydrolytic autoclave test primarily intended for evaluating samples from untreated glass containers. It is often useful for testing the resistance of containers of too small capacity to permit measurements of solubility on the unbroken article by the B-W test method. Yielding the water resistance of the bulk glass, it can also be used in conjunction with the B-W test method to distinguish whether the internal surface of a container has been treated to improve its durability.
All three test methods are suitable for specification acceptance.
SCOPE
1.1 These test methods cover the evaluation of the resistance of glass containers to chemical attack. Three test methods are presented, as follows:
1.1.1 Test Method B-A covers autoclave tests at 121°C on bottles partially filled with dilute acid as the attacking medium.
1.1.2 Test Method B-W covers autoclave tests at 121°C on bottles partially filled with distilled water as the attacking medium.
1.1.3 Test Method P-W covers autoclave tests at 121°C on powdered samples with pure water as the attacking medium.
1.2 The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only.
1.3 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.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information.
Designation:C225–85 (Reapproved 2004)
Standard Test Methods for
Resistance of Glass Containers to Chemical Attack
This standard is issued under the fixed designation C225; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope D1125 Test Methods for Electrical Conductivity and Resis-
tivity of Water
1.1 These test methods cover the evaluation of the resis-
D1193 Specification for Reagent Water
tanceofglasscontainerstochemicalattack.Threetestmethods
E11 SpecificationforWovenWireTestSieveClothandTest
are presented, as follows:
Sieves
1.1.1 Test Method B-A covers autoclave tests at 121°C on
E691 Practice for Conducting an Interlaboratory Study to
bottles partially filled with dilute acid as the attacking medium.
Determine the Precision of a Test Method
1.1.2 Test Method B-W covers autoclave tests at 121°C on
bottles partially filled with distilled water as the attacking
3. Significance and Use
medium.
3.1 The solubility of glass in contact with food, beverages,
1.1.3 Test Method P-W covers autoclave tests at 121°C on
or pharmaceutical products is an important consideration for
powdered samples with pure water as the attacking medium.
the safe packaging and storage of such materials. Autoclave
1.2 The values stated in SI units are to be regarded as the
conditions are specified since sterilization is often employed
standard. The values in parentheses are for information only.
for the packaging of the product. It also represents one of the
1.3 This standard does not purport to address all of the
most extreme conditions, particularly of temperature, that
safety concerns, if any, associated with its use. It is the
containers will ordinarily experience. Any of the three test
responsibility of the user of this standard to establish appro-
methods described may be used to establish specifications for
priate safety and health practices and determine the applica-
conformity to standard values, either as specified by a cus-
bility of regulatory limitations prior to use.
tomer, an agency, or “The United States Pharmacopeia:”
2. Referenced Documents 3.1.1 Test Method B-A is intended particularly for testing
glasscontainersprimarilydestinedforcontainmentofproducts
2.1 ASTM Standards:
with a pH under 5.
A569/A569M Specification for Steel, Carbon (0.15 Maxi-
3.1.2 Test Method B-W is intended particularly for testing
mum Percent), Hot-Rolled Sheet and Strip Commercial
3 glass containers to be used for products with a pH of 5.0 or
Quality
over.
3.1.3 Test Method P-W is a hydrolytic autoclave test prima-
These test methods are under the jurisdiction of ASTM Committee C14 on
rily intended for evaluating samples from untreated glass
Glass and Glass Products and are the direct responsibility of Subcommittee C14.02
containers. It is often useful for testing the resistance of
on Chemical Properties and Analysis.
containers of too small capacity to permit measurements of
Current edition approved Oct. 1, 2004. Published October 2004. Originally
approved in 1949. Last previous edition approved 1999 as C225 – 85 (1999). DOI:
solubility on the unbroken article by the B-W test method.
10.1520/C0225-85R04.
Yielding the water resistance of the bulk glass, it can also be
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
used in conjunction with the B-W test method to distinguish
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on whether the internal surface of a container has been treated to
the ASTM website.
improve its durability.
Withdrawn.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C225–85 (2004)
3.2 All three test methods are suitable for specification two-hole stopper carrying a glass siphon tube (for delivering
acceptance. the solution to a buret) and a soda-lime or soda-asbestos guard
tube. Standardize the 0.020N NaOH solution against the
4. Purity of Reagents
National Institute of Standards and Technology Standard
Sample No. 84h of acid potassium phthalate.Transfer 0.2000 g
4.1 Reagent grade chemicals shall be used in all tests.
of the phthalate to a 250-mL Erlenmeyer flask and dissolve in
Unless otherwise indicated, it is intended that all reagents shall
about 75 mL of CO -free water. Add five drops of phenol-
conform to the specifications of the Committee on Analytical
phthalein indicator solution and titrate with the NaOH solution
Reagents of the American Chemical Society, where such
to the first persistent pink color. Adjust the standard NaOH
specifications are available. Other grades may be used, pro-
solution to 0.020N strength.
vided it is first ascertained that the reagent is of sufficiently
6.4.1 Calculate the normality N of the NaOH solution as
high purity to permit its use without lessening the accuracy of
the determination. follows:
4.2 Unless otherwise indicated, references to water shall be
N 5 0.9798/mL of NaOH (1)
understood to mean distilled water or other water meeting the
requirements for one of the types of reagent water covered by
6.5 High-Purity Water—This water shall be free of heavy
Specification D1193.
metals, particularly copper, as shown by a dithizone test and
have a conductivity (consult Test Methods D1125) not exceed-
TEST METHOD B-A—RESISTANCE OF BOTTLES
ing 0.15 µS/cm.
TOATTACK BY DILUTE ACID
6.5.1 The source water shall be distilled, then passed
through a deionizer cartridge packed with a mixed bed of
5. Apparatus
nuclear-grade resin, then through a cellulose ester membrane
5.1 Autoclave or Steam Sterilizer, capable of withstanding a
having openings not exceeding 0.45 µm. Pass the purified
pressure of 165 kPa (24 psi) and, preferably, equipped with a
water through an in-line conductivity cell to verify its purity.
constant-pressure regulator or other means for maintaining the
After flushing discharge lines, suitable water should be dis-
temperature at 121 6 0.5°C (250 6 0.9°F). This temperature
pensed directly into the test vessels.
shall be checked by means of a suitably calibrated instrument.
NOTE 1—Copper tubing should not be used in the discharge lines.
The autoclave shall be capable of accommodating at least six
TFE-fluorocarbon or pure tin are suitable.
and preferably twelve of the largest containers to be tested. It
NOTE 2—Reference should be made to Specification D1193. Type I
shall be equipped with a rack for supporting the samples, a
reagent water as defined therein complies with the present 6.5.Inthe
thermometer, a pressure gage, and a vent cock.
interest of practicality and demonstrated sufficiency, 6.5 allows the
following deviations from Type I reagent water specifications.
6. Reagents and Materials
(1) Source water is unspecified whereas Type I specifies source water
6.1 Acetone, USP grade. having a maximum conductivity of 20 µS/cm at 25°C.
(2) The final step is filtration through a membrane having openings not
6.2 Methyl Red Indicator Solution—Dissolve 24 mg of the
exceeding 0.45 µm. Type I directs filtration through a 0.2-µm membrane.
sodium salt of methyl red in 100 mL of water. If necessary,
(3) The conductivity immediately before dispensing is required not to
neutralizetheindicatorsolutionwith0.020Nsodiumhydroxide
exceed 0.15 µS/cm at 25°C whereas Type I is limited to 0.06 µS/cm at
(NaOH) solution so that the titer of five drops of the indicator
25°C.
solution in 100 mL of the special distilled water does not
The distillation step is essential to minimize or avoid cultivation of
exceed 0.02 mL of 0.020N NaOH solution. In titrations using
microorganisms in the ion-exchange bed and consequent clogging of the
the methyl red indicator solution, the end point shall be taken
membrane filter. When preceded by distillation, the ion-exchange bed
should have a long life, but as the conductivity begins to rise toward the
at a pH of 5.6.
limit it should be replaced by a new bed.
6.3 Phenolphthalein Indicator Solution—Dissolve 0.5 g of
Distillation from phosphoric acid with a conductivity of the product
phenolphthalein in 60 mL of ethyl alcohol (95 %) and dilute
between 0.5 and 1.0 µS/cm was specified as water for extraction in Test
with water to 100 mL.
Methods C225.Water prepared as described herein gave results averaging
6.4 Sodium Hydroxide Solution, Standard (0.020N)—
about 8 % higher than water prepared by distillation from phosphoric acid
Dissolve 100 g of NaOH in 100 mL of water in a 150-mL test
when Test Method B-W was applied to soda-lime and borosilicate glass
tube. Avoid wetting the top of the test tube. Stopper the tube
bottles in seven laboratories. The trend to slightly greater extraction may
loosely with a stopper covered with tinfoil and allow to stand be associated with the higher average purity of this water. The limit on
conductivity of 0.15 µS/cm for water prepared by this means was set
in a vertical position until the supernatant liquid is clear.
because water of less conductivity is readily obtained and when 0.15
Withdraw some of the clear solution in a measuring pipet and
µS/cm is exceeded, the conductivity rises rapidly on further use of the
deliver 1.3 mL into a paraffin-lined bottle containing 1 L of
system.
carbon dioxide (CO )-free water. Stopper the bottle with a
6.6 Sulfuric Acid, Standard (0.020N) containing approxi-
mately 0.58 mL of concentrated sulfuric acid (H SO,spgr
2 4
1.84) in 1 L of solution. Prepare 0.1N H SO containing 3.0
Reagent Chemicals, American Chemical Society Specifications, American
2 4
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
mLof concentrated sulfuric acid (H SO , sp gr 1.84)/L. Dilute
2 4
listed by the American Chemical Society, see Analar Standards for Laboratory
200 mL of the 0.1N H SO to 1 L and standardize against
2 4
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
0.020N NaOH solution, using methyl red indicator solution.
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. Finally, adjust the standard H SO to 0.020N strength.
2 4
C225–85 (2004)
6.7 Sulfuric Acid, Standard (0.0005N)—Mix 1 volume of
B = 0.020N NaOH solution used in the titration of 100
0.1N H SO with 199 volumes of water.Adjust the strength to
2 4 mL of bottle extract, mL; and
be 0.0005 6 0.000025N.
0.98 = factor applied to the titration of the bottle extract to
6.8 Sulfuric Acid, Standard (0.0002N)—Mix 1 volume of
correct that titration for loss of attacking medium
0.1N H SO with 499 volumes of water.Adjust the strength to
during cooling of the autoclave.
2 4
be 0.0002 6 0.00001N.
TEST METHOD B-W—RESISTANCE OF BOTTLES
7. Preparation of Sample
TO ATTACK BY WATER
7.1 If the bottles are 168–cm (6-oz) capacity or over, select
10. Apparatus
threebottles.Ifthebottlesaresmallerthan6-ozcapacity,select
a sufficient number so the contents can be combined to form
10.1 See Section 5.
three sets to give 100 mL/set. Rinse each container with two
portions of the high-purity water, follow with two similar
11. Reagents
rinsings using acetone and dry with a stream of clean dry air.
11.1 See 6.2-6.6.
8. Procedure
12. Preparation of Sample
8.1 Fill the containers, at room temperature, to 90 % of 3
12.1 If the bottles are 168-cm (6-oz) capacity or over,
overflow capacity with the attacking medium. 3
select three bottles. If the bottles are smaller than 168–cm
capacity, select a sufficient number so that the contents can be
NOTE 3—If the bottles to be tested will neutralize more than the
equivalent of 0.80 mL of 0.020N H SO , use 0.0005N H SO as the
combined to form three sets to give 100 mL/set. Rinse each
2 4 2 4
attacking medium. Otherwise, use 0.0002N H SO as the attacking
2 4 container with two portions of the high-purity water as
medium.
described in 6.5.
8.2 Cover each container individually with a chemical-
13. Procedure
resistant glass beaker or cap that has been digested with water
foratleast24hat90°C(194°F)or1hat121°C(250°F).These
13.1 Fill the containers, at room temperature, to 90 % of
covers shall be of such size that the bottoms of the beakers or
overflow capacity with the high-purity water. Continue as
caps fit snugly down on the top rims of the containers. Place
described in 8.2.
the containers on the rack in the autoclave. The sample rack
13.2 Titration of Bottle Extract—Using a graduated cylin-
must support the samples above water level. Close the cover
der, transfer 100-mL portions of the test solution from the
securely, leaving the vent cock open. Heat until steam issues
containers to 250-mL flasks of chemical-resistant glass. Add
vigorously from the vent. Allow steam to issue from the vent
five drops of methyl red indicator solution to each flask and
for 10 min; then close the vent cock and increase the
titratewith0.020NH SO (Note4).Thetimeelapsingbetween
2 4
temperature at the rate of 1°C/min to 121°C taking 19 to 23
opening the autoclave and titrating the solution should not
min. Maintain the temperature at 121 6 0.5°C (250 6 0.9°F)
exceed 1 h.
for 1 h, counting from the time when the holding temperature
13.3 Blank—Titrate 100 mL of the high-purity water at the
is reached.At the end of the hour, cool at the rate of 0.5°C/min
same temperature and using the same amount of indicator as in
to atmospheric pressure, venting to prevent formation of a
titration of the bottle extract in accordance with 13.2.
vacuum. The time to cool from 121°C to atmospheric pressure
should be from 38 to 46 min. Open the autoclave and remove
14. Calculation and Report
the containers.
14.1 Report the results as millilitres of 0.020N H SO
2 4
8.3 Titration of Bottle Extract—Cool the containers and
required for titration of the sample, minus millilitres required
contents to room temperature. With a pipet, transfer 100-mL
for titration of the blank.
portions of the test solution from the containers to 250-mL
flasks of chemical-resistant glass.Add five drops of methyl red
TEST METHOD P-W—RESISTANCE OF
indicator solution to each flask and titrate with 0.20N NaOH
POWDERED SAMPLE TO ATTACK BY WATER
solution.
NOTE 4—When titrations are under 1 mL, a microburet should be used. 15. Apparatus
15.1 Autoclave—See 5.1.
9. Calculation and Report
15.2 Flasks—Erlenmeyer flasks of 250-mL capacity, made
9.1 Report the results as millilitres of 0.020N acid con-
of chemical-resistant glass and suitably aged by previous
sumed in the test,
...
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