ASTM C225-85(2009)
(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:”
Test Method B-A is intended particularly for testing glass containers primarily destined for containment of products with a pH under 5.
Test Method B-W is intended particularly for testing glass containers to be used for products with a pH of 5.0 or over.
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.
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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 2009)
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 U.S. Department of Defense.
1. Scope D1193 Specification for Reagent Water
E11 Specification for Woven Wire Test Sieve Cloth and Test
1.1 These test methods cover the evaluation of the resis-
Sieves
tanceofglasscontainerstochemicalattack.Threetestmethods
E691 Practice for Conducting an Interlaboratory Study to
are presented, as follows:
Determine the Precision of a Test Method
1.1.1 Test Method B-A covers autoclave tests at 121°C on
bottles partially filled with dilute acid as the attacking medium.
3. Significance and Use
1.1.2 Test Method B-W covers autoclave tests at 121°C on
3.1 The solubility of glass in contact with food, beverages,
bottles partially filled with distilled water as the attacking
or pharmaceutical products is an important consideration for
medium.
the safe packaging and storage of such materials. Autoclave
1.1.3 Test Method P-W covers autoclave tests at 121°C on
conditions are specified since sterilization is often employed
powdered samples with pure water as the attacking medium.
for the packaging of the product. It also represents one of the
1.2 The values stated in SI units are to be regarded as the
most extreme conditions, particularly of temperature, that
standard. The values in parentheses are for information only.
containers will ordinarily experience. Any of the three test
methods described may be used to establish specifications for
1.3 This standard does not purport to address all of the
conformity to standard values, either as specified by a
safety concerns, if any, associated with its use. It is the
customer, an agency, or “The United States Pharmacopeia:”
responsibility of the user of this standard to establish appro-
3.1.1 Test Method B-A is intended particularly for testing
priate safety and health practices and determine the applica-
glasscontainersprimarilydestinedforcontainmentofproducts
bility of regulatory limitations prior to use.
with a pH under 5.
2. Referenced Documents
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
2.1 ASTM Standards:
over.
A569/A569M Specification for Steel, Carbon (0.15
3.1.3 Test Method P-W is a hydrolytic autoclave test primar-
Maximum,Percent),Hot-RolledSheetandStripCommer-
ily intended for evaluating samples from untreated glass
cial
containers. It is often useful for testing the resistance of
D1125 Test Methods for Electrical Conductivity and Resis-
containers of too small capacity to permit measurements of
tivity of Water
solubility on the unbroken article by the B-W test method.
Yielding the water resistance of the bulk glass, it can also be
These test methods are under the jurisdiction of ASTM Committee C14 on
used in conjunction with the B-W test method to distinguish
Glass and Glass Products and are the direct responsibility of Subcommittee C14.02
on Chemical Properties and Analysis. whether the internal surface of a container has been treated to
Current edition approved Nov. 1, 2009. Published January 2010. Originally
improve its durability.
approved in 1949. Last previous edition approved 2004 as C225 – 85 (2004). DOI:
3.2 All three test methods are suitable for specification
10.1520/C0225-85R09.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
acceptance.
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
4. Purity of Reagents
the ASTM website.
3 4.1 Reagent grade chemicals shall be used in all tests.
Withdrawn. The last approved version of this historical standard is referenced
on www.astm.org. Unless otherwise indicated, it is intended that all reagents shall
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C225 − 85 (2009)
conform to the specifications of the Committee on Analytical of the phthalate to a 250-mL Erlenmeyer flask and dissolve in
Reagents of the American Chemical Society, where such about 75 mL of CO -free water. Add five drops of phenol-
specifications are available. Other grades may be used, pro- phthalein indicator solution and titrate with the NaOH solution
vided it is first ascertained that the reagent is of sufficiently to the first persistent pink color. Adjust the standard NaOH
high purity to permit its use without lessening the accuracy of solution to 0.020N strength.
the determination.
6.4.1 Calculate the normality N of the NaOH solution as
follows:
4.2 Unless otherwise indicated, references to water shall be
understood to mean distilled water or other water meeting the N 5 0.9798/mL of NaOH (1)
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.
TO ATTACK BY DILUTE ACID
6.5.1 The source water shall be distilled, then passed
5. Apparatus
through a deionizer cartridge packed with a mixed bed of
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.
The autoclave shall be capable of accommodating at least six
NOTE 1—Copper tubing should not be used in the discharge lines.
and preferably twelve of the largest containers to be tested. It
TFE-fluorocarbon or pure tin are suitable.
shall be equipped with a rack for supporting the samples, a NOTE 2—Reference should be made to Specification D1193. Type I
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
25°C.
(NaOH) solution so that the titer of five drops of the indicator
The distillation step is essential to minimize or avoid cultivation of
solution in 100 mL of the special distilled water does not
microorganisms in the ion-exchange bed and consequent clogging of the
exceed 0.02 mL of 0.020N NaOH solution. In titrations using
membrane filter. When preceded by distillation, the ion-exchange bed
the methyl red indicator solution, the end point shall be taken
should have a long life, but as the conductivity begins to rise toward the
limit it should be replaced by a new bed.
at a pH of 5.6.
Distillation from phosphoric acid with a conductivity of the product
6.3 Phenolphthalein Indicator Solution—Dissolve 0.5 g of
between 0.5 and 1.0 µS/cm was specified as water for extraction in Test
phenolphthalein in 60 mL of ethyl alcohol (95 %) and dilute Methods C225.Water prepared as described herein gave results averaging
about 8 % higher than water prepared by distillation from phosphoric acid
with water to 100 mL.
when Test Method B-W was applied to soda-lime and borosilicate glass
6.4 Sodium Hydroxide Solution, Standard (0.020N)—
bottles in seven laboratories. The trend to slightly greater extraction may
Dissolve 100 g of NaOH in 100 mL of water in a 150-mL test 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
tube. Avoid wetting the top of the test tube. Stopper the tube
because water of less conductivity is readily obtained and when 0.15
loosely with a stopper covered with tinfoil and allow to stand
µS/cm is exceeded, the conductivity rises rapidly on further use of the
in a vertical position until the supernatant liquid is clear.
system.
Withdraw some of the clear solution in a measuring pipet and
6.6 Sulfuric Acid, Standard (0.020N) containing approxi-
deliver 1.3 mL into a paraffin-lined bottle containing 1 L of
mately 0.58 mL of concentrated sulfuric acid (H SO,spgr
2 4
carbon dioxide (CO )-free water. Stopper the bottle with a
1.84) in 1 L of solution. Prepare 0.1N H SO containing 3.0
2 4
two-hole stopper carrying a glass siphon tube (for delivering
mLof concentrated sulfuric acid (H SO , sp gr 1.84)/L. Dilute
2 4
the solution to a buret) and a soda-lime or soda-asbestos guard
200 mL of the 0.1N H SO to 1 L and standardize against
2 4
tube. Standardize the 0.020N NaOH solution against the
0.020N NaOH solution, using methyl red indicator solution.
National Institute of Standards and Technology Standard
Finally, adjust the standard H SO to 0.020N strength.
2 4
Sample No. 84h of acid potassium phthalate.Transfer 0.2000 g
6.7 Sulfuric Acid, Standard (0.0005N)—Mix 1 volume of
0.1N H SO with 199 volumes of water.Adjust the strength to
2 4
Reagent Chemicals, American Chemical Society Specifications, American
be 0.0005 6 0.000025N.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
6.8 Sulfuric Acid, Standard (0.0002N)—Mix 1 volume of
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
0.1N H SO with 499 volumes of water.Adjust the strength to
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, 2 4
MD. be 0.0002 6 0.00001N.
C225 − 85 (2009)
7. Preparation of Sample TEST METHOD B-W—RESISTANCE OF BOTTLES
TO ATTACK BY WATER
7.1 If the bottles are 168–cm (6-oz) capacity or over, select
threebottles.Ifthebottlesaresmallerthan6-ozcapacity,select
10. Apparatus
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 12.1 If the bottles are 168-cm (6-oz) capacity or over,
overflow capacity with the attacking medium. 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
combined to form three sets to give 100 mL/set. Rinse each
equivalent of 0.80 mL of 0.020N H SO , use 0.0005N H SO as the
2 4 2 4
container with two portions of the high-purity water as
attacking medium. Otherwise, use 0.0002N H SO as the attacking
2 4
described in 6.5.
medium.
8.2 Cover each container individually with a chemical-
13. Procedure
resistant glass beaker or cap that has been digested with water
13.1 Fill the containers, at room temperature, to 90 % of
foratleast24hat90°C(194°F)or1hat121°C(250°F).These
overflow capacity with the high-purity water. Continue as
covers shall be of such size that the bottoms of the beakers or
described in 8.2.
caps fit snugly down on the top rims of the containers. Place
13.2 Titration of Bottle Extract—Using a graduated
the containers on the rack in the autoclave. The sample rack
cylinder, transfer 100-mLportions of the test solution from the
must support the samples above water level. Close the cover
containers to 250-mL flasks of chemical-resistant glass. Add
securely, leaving the vent cock open. Heat until steam issues
five drops of methyl red indicator solution to each flask and
vigorously from the vent. Allow steam to issue from the vent
titratewith0.020NH SO (Note4).Thetimeelapsingbetween
2 4
for 10 min; then close the vent cock and increase the
opening the autoclave and titrating the solution should not
temperature at the rate of 1°C/min to 121°C taking 19 to 23
exceed 1 h.
min. Maintain the temperature at 121 6 0.5°C (250 6 0.9°F)
13.3 Blank—Titrate 100 mL of the high-purity water at the
for 1 h, counting from the time when the holding temperature
same temperature and using the same amount of indicator as in
is reached.At the end of the hour, cool at the rate of 0.5°C/min
titration of the bottle extract in accordance with 13.2.
to atmospheric pressure, venting to prevent formation of a
vacuum. The time to cool from 121°C to atmospheric pressure
14. Calculation and Report
should be from 38 to 46 min. Open the autoclave and remove
14.1 Report the results as millilitres of 0.020N H SO
2 4
the containers.
required for titration of the sample, minus millilitres required
8.3 Titration of Bottle Extract—Cool the containers and
for titration of the blank.
contents to room temperature. With a pipet, transfer 100-mL
TEST METHOD P-W—RESISTANCE OF
portions of the test solution from the containers to 250-mL
POWDERED SAMPLE TO ATTACK BY WATER
flasks of chemical-resistant glass.Add five drops of methyl red
indicator solution to each flask and titrate with 0.20N NaOH
15. Apparatus
solution.
15.1 Autoclave—See 5.1.
NOTE 4—When titrations are under 1 mL, a microburet should be used.
15.2 Flasks—Erlenmeyer flasks of 250-mL capacity, made
of chemical-resistant glass and suitably aged by previous
9. Calculation and Report
treatment similar to the test or by previous use.
9.1 Report the results as millilitres of 0.020N acid con-
15.3 Crushing Device—Either a special steel mortar or a
sumed in the test, A. Calculate as follows:
special steel
...
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