ASTM C169-92(1996)
(Test Method)Standard Test Methods for Chemical Analysis of Soda-Lime and Borosilicate Glass
Standard Test Methods for Chemical Analysis of Soda-Lime and Borosilicate Glass
SCOPE
1.1 These test methods cover the quantitative chemical analysis of soda-lime and borosilicate glass compositions for both referee and routine analysis. This would be for the usual constituents present in glasses of the following types: (1) soda-lime silicate glass, (2) soda-lime fluoride opal glass, and (3) borosilicate glass. The following common oxides, when present in concentrations greater than indicated, are known to interfere with some of the determinations in this method: 2 % barium oxide (BaO), 0.2 % phosphorous pentoxide (P2O5), 0.05 % zinc oxide (ZnO), 0.05 % antimony oxide (Sb2O3), 0.05 % lead oxide (PbO).
1.2 The analytical procedures, divided into two general groups, those for referee analysis, and those for routine analysis, appear in the following order: SectionsProcedures for Referee Analysis:Silica10BaO, R2O2 (Al2O3 + P2O5), CaO, and MgO11-15Fe2O3, TiO2, ZrO2 by Photometry and Al2O3 by Complexio-metric Titration16-22Cr2O3 by Volumetric and Photometric Methods23-25MnO by the Periodate Oxidation Method26-29Na2O by the Zinc Uranyl Acetate Method and K2O by the Tetraphenylborate Method30-33SO3 (Total Sulfur)34 to 35As2O3 by Volumetric Method36-40Procedures for Routine Analysis:Silica by the Single Dehydration Method42-44Al2O3, CaO, and MgO by Complexiometric Titration, and BaO, Na2O, and K2O by Gravimetric Method45-51BaO, Al2O3, CaO, and MgO by Atomic Absorption; and Na2O and K 2O by Flame Emission Spectroscopy52-59SO3 (Total Sulfur)60B2O361 to 62Fluorine by Pyrohydrolysis Separation and Specific Ion Electrode Measurement63-66P2O5 by the Molybdo-Vanadate Method67-70Colorimetric Determination of Ferrous Iron Using 1,10 Phenanthroline71-76
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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Designation: C 169 – 92 (Reapproved 1996)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Methods for
Chemical Analysis of Soda-Lime and Borosilicate Glass
This standard is issued under the fixed designation C 169; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope bility of regulatory limitations prior to use.
1.1 These test methods cover the quantitative chemical
2. Referenced Documents
analysis of soda-lime and borosilicate glass compositions for
2.1 ASTM Standards:
both referee and routine analysis. This would be for the usual
C 146 Test Methods for Chemical Analysis of Glass Sand
constituents present in glasses of the following types: (1)
C 225 Test Methods for Resistance of Glass Containers to
soda-lime silicate glass, (2) soda-lime fluoride opal glass, and
Chemical Attack
(3) borosilicate glass. The following common oxides, when
D 1193 Specification for Reagent Water
present in concentrations greater than indicated, are known to
E 50 Practices for Apparatus, Reagents, and Safety Precau-
interfere with some of the determinations in this method: 2 %
tions for Chemical Analysis of Metals
barium oxide (BaO), 0.2 % phosphorous pentoxide (P O ),
2 5
E 60 Practice for Photometric and Spectrophotometric
0.05 % zinc oxide (ZnO), 0.05 % antimony oxide (Sb O ),
2 3
Methods for Chemical Analysis of Metals
0.05 % lead oxide (PbO).
1.2 The analytical procedures, divided into two general
3. Significance and Use
groups, those for referee analysis, and those for routine
3.1 These test methods can be used to ensure that the
analysis, appear in the following order:
chemical composition of the glass meets the compositional
Sections
specification required for the finished glass product.
Procedures for Referee Analysis:
Silica 10
3.2 These test methods do not preclude the use of other
BaO, R O (Al O +P O ), CaO, and MgO 11-15
2 2 2 3 2 5
methods that yield results within permissible variations. In any
Fe O ,TiO , ZrO by Photometry and Al O by Complexio- 16-22
2 3 2 2 2 3
case, the analyst should verify the procedure and technique
metric Titration
Cr O by Volumetric and Photometric Methods 23-25
2 3 employed by means of a National Institute of Standards and
MnO by the Periodate Oxidation Method 26-29
Technology (NIST) standard reference material having a com-
Na O by the Zinc Uranyl Acetate Method and K Obythe 30-33
2 2
ponent comparable with that of the material under test. A list of
Tetraphenylborate Method
SO (Total Sulfur) 34 to 35
3 standard reference materials is given in the NIST Special
As O by Volumetric Method 36-40
2 3
Publication 260, current edition.
Procedures for Routine Analysis:
3.3 Typical examples of products manufactured using soda-
Silica by the Single Dehydration Method 42-44
Al O , CaO, and MgO by Complexiometric Titration, and BaO, 45-51
2 3
lime silicate glass are containers, tableware, and flat glass.
Na O, and K O by Gravimetric Method
2 2
3.4 Typical examples of products manufactured using boro-
BaO, Al O , CaO, and MgO by Atomic Absorption; and Na O 52-59
2 3 2
silicate glass are bakeware, labware, and fiberglass.
and K O by Flame Emission Spectroscopy
SO (Total Sulfur) 60
3 3.5 Typical examples of products manufactured using fluo-
B O 61 to 62
2 3
ride opal glass are containers, tableware, and decorative
Fluorine by Pyrohydrolysis Separation and Specific Ion Electrode 63-66
glassware.
Measurement
P O by the Molybdo-Vanadate Method 67-70
2 5
Colorimetric Determination of Ferrous Iron Using 1,10 Phenan- 71-76
4. Purity of Reagents
throline
4.1 Reagent grade chemicals shall be used throughout.
1.3 This standard does not purport to address all of the
Unless otherwise indicated, it is intended that reagents shall
safety concerns, if any, associated with its use. It is the
conform to the specifications of the Committee on Analytical
responsibility of the user of this standard to establish appro-
Reagents of the American Chemical Society, where such
priate safety and health practices and determine the applica-
1 2
These test methods are under the jurisdiction of ASTM Committee C-14 on Annual Book of ASTM Standards, Vol 15.02.
Glass and Glass Products and are the direct responsibility of Subcommittee C14.02 Annual Book of ASTM Standards, Vol 11.01.
on Chemical Analysis. Annual Book of ASTM Standards, Vol 03.05.
Current edition approved May 15, 1992. Published September 1992. Originally Available from National Institute of Standards and Technology, Gaithersburg,
published as C 169 – 41 T. Last previous edition C 169 – 89. MD 20899.
C 169
specifications are available. Other grades may be used, pro- place the powder on a sheet of paper and pass a small magnet
vided it is first ascertained that the reagent is of sufficiently through it to remove adventitious iron. Then store in a tightly
high purity to permit its use without lessening the accuracy of closed container and keep in a desiccator.
the determination.
8.2 A sample prepared in an iron mortar is not recom-
4.2 Purity of Water—Unless otherwise indicated, reference
mended for the determination of Fe O . Instead, glass should
2 3
to water shall be understood to mean reagent water as defined
be ground in an agate mortar after ascertaining it is free of
by Type I, II, or III of Specification D 1193.
contamination.
8.3 A sample prepared for the determination of fluorine
5. Concentration of Acids and Ammonium Hydroxide
should be sieved through a 75-μm (No. 200) mesh sieve rather
5.1 When acids and ammonium hydroxide are specified by
than a 150-μm (No. 100) sieve.
name or chemical formula only, concentrated reagents of the
8.4 The practice of drying samples in a drying oven at 105
following percent concentrations are intended:
to 110°C after preparation is not recommended. Powdered
%
glass can fix CO and water as readily at this temperature as at
Hydrochloric acid (HCl) 36 to 38
room temperature. A freshly prepared sample, if exposed but a
Hydrofluoric acid (HF) 48 to 51
Nitric acid (HNO ) 69to71
3 short time to the atmosphere, will not have acquired an ignition
Perchloric acid (HClO ) 70to72
loss of much analytical significance. If ignition loss is deter-
Sulfuric acid (H SO ) 95to98
2 4
mined, use the following temperature schedules:
Ammonium hydroxide (NH OH) 28 to 30
Soda-lime glass, 800°C for 1 h
5.2 Concentrations of diluted acids and NH OH except Fluorine opal glass, 500 to 550°C for 1 h
Borosilicate glass, 800°C for 1 h
when standardized are specified as a ratio, stating the number
of volumes of the concentrated reagent to be added to a given
Determine the ignition loss ona1to3-g sample in a
number of volumes of water, as follows: HCl (1 + 99) means
platinum crucible.
1 volume of concentrated HCl (approximately 37 %) added to
99 volumes of water.
9. Precision and Bias
5.3 The hygroscopic nature of the ignited precipitates of
silica, aluminum oxide, and calcium oxide obtained in the 9.1 The probable precision of results that can be expected
methods to be described, requires the use of fresh and highly
by the use of the procedures described in these test methods is
active desiccants. For this purpose, magnesium perchlorate shown in the following tabulation. Precision is given as
(Mg(ClO ) ) and barium oxide (BaO) are recommended.
absolute error, and is dependent on the quantity of constituent
4 2
present as well as the procedure used.
6. Filter Papers
Probable Precision of Results, weight %
Constituent Referee Analysis Routine Analysis
6.1 Throughout these test methods, filter papers will be
Silica 60.1 60.25
designated as “coarse,” “medium,” or “fine,” without naming
BaO 60.02 60.05
brands or manufacturers. All filter papers are of the double acid
Al O +P O 60.05 60.10 (−P O )
2 3 2 5 2 5
CaO 60.05 60.15
washed ashless type. “Coarse” filter paper refers to the porosity
MgO 60.05 60.02 to 0.10
commonly used for the filtration of aluminum hydroxide.
Fe O 60.003 .
2 3
“Medium” filter paper refers to that used for filtration of
TiO 60.005 .
ZrO 60.001 to 0.005 .
calcium oxalate, and “fine” filter paper to that used for barium 2
Cr O (volumetric) 60.005 .
2 3
sulfate.
Cr O (photometric) 60.0001 to 0.001 .
2 3
MnO 60.001 to 0.005 .
7. Photometers and Photometric Practice
Na O 60.05 60.25 (flame emission)
K O 60.02 to 0.05 60.02 to 0.10
7.1 Photometers and photometric practice prescribed in
(flame emission)
these methods shall conform to Practice E 60.
SO 60.02 60.05
As O 60.005 .
7.2 The considerations of instrumentation given in Test
2 3
P O . 60.005 to 0.02
2 5
Methods C 146 are equally applicable to these test methods.
B O . 60.05 to 0.15
2 3
Fluorine . 60.01 to 0.20
8. Preparation of Sample
(0.1 to 6.0 %)
8.1 Glass crushed in a steel mortar as described in Test
9.2 It is recommended that reported results be rounded as
Methods C 225, and sieved through a 150-μm (No. 100) mesh
follows:
sieve, is generally suitable for analysis, except for the deter-
mination of iron oxide (Fe O ). After crushing and sieving, Number of Significant Figures
2 3
Percent
Retained After Rounding
1 to 100 3
0.1 to 0.99 2
Reagent Chemicals, American Chemical Society Specifications, American
0.01 to 0.09 1 or 2
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
<0.01 1 or 2
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
9.3 Recorded results should be carried to one more signifi-
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. cant figure than required in 9.2.
C 169
PROCEDURES FOR REFEREE ANALYSIS
Results for SiO when analyzing fluorine opals may tend to be low by
SILICA
0.2 to 0.3 %. For an alternative, but more lengthy procedure, consult
10. Procedure Applied Inorganic Analysis.
NOTE 2—Boron in amounts less than 5 % B O does not interfere.
2 3
10.1 Weigh 1.000 g of powdered sample and 1.5 g of
However, if boron is greater than 5 %, proceed to the point of completing
anhydrous sodium carbonate (Na CO ) for soda-lime glass, or
2 3
the first dehydration (see 10.2), then add 20 mL of anhydrous methanol
2.0gofNa CO for borosilicate glass, into a clean 75-mL
2 3
saturated with dry HCl (gas), and evaporate to dryness on an air bath or
platinum dish (see 10.1.1); mix well with a platinum or
under an infrared lamp. Repeat once more before proceeding.
Nichrome wire. Tap the charge so it lies evenly in the bottom
10.3 Evaporate the filtrate to dryness on the steam bath or
of the dish. Cover with platinum lid and heat first at a dull red
under an infrared lamp. When dry, cool, drench with 10 mL of
heat over a clean oxidizing flame; gradually raise the tempera-
HCl (1 + 1) and again evaporate just to dryness; then bake in a
ture until a clear melt is obtained. Properly carried out, little or
drying oven at 105°C for 30 min. Cool, drench with 5 mL of
no spattering should occur and the fusion can be performed in
HCl, and add 20 mL of hot water and a small bit of filter pulp.
3 to 4 min. When melted, rotate the melt to spread it evenly
Digest hot for 5 min and filter through a 7-cm fine paper. Police
over the bottom and lower sides of the dish, gradually
the dish with the aid of a bit of paper pulp and wash precipitate
withdrawing from the flame. Cover and cool to room tempera-
and paper eight times with hot 2 % HCl. Transfer the paper and
ture. During fusion, the dish should be handled at all times with
precipitate to the dish containing the initial precipitation. Wipe
platinum-tipped tongs and the fusion performed with a plati-
the stirring rod and the periphery of the funnel with a piece of
num (preferably 90 % platinum and 10 % rhodium alloy) or
damp filter paper and add to the dish containing the precipitate
silica triangle.
for ignition.
10.1.1 To obtain accurate repeat weighings, platinum ware
10.4 Partially cover the dish with its platinum lid but leave
shall be kept scrupulously clean on the outside of the vessel as
enough space so air can circulate during ignition. Place the dish
well as on the inside. It should be polished brightly with fine,
in a cold muffle furnace and bring the temperature to 1200°C
round grain sand and protected from dirty surfaces. It is
for 30 min. Carefully and completely cover the dish before
recommended that porcelain plates be used for cooling fusions,
removing it from the furnace and transfer to a desiccator. Cool
and that platinum be set on paper towels or other clean material
to room temperature and weigh the covered dish (W ). Moisten
during filtration.
the silica with 1 to 2 mL of water and add 4 to 5 mL of HF and
10.2 Add 20 to 25 mL of HCl (1 + 1) (Note 1) under the
0.5 g of oxalic acid crystals. Evaporate to dryness on a sand
platinum cover and digest on a steam bath or hot plate until the
bath or under an infrared lamp. Carefully sublime any remain-
melt has completely disintegrated; it is also possible to digest
ing oxalic acid, cover the dish with its platinum cover, heat to
the melt in the cold overnight. Police and rinse the lid with a
1000°C for 2 min, cool, and weigh (W ) as before.
fine jet of water; rinse down the sides of the dish and evaporate
10.5 Calculation—Calculate the percent of SiO as follows:
to dryness on a steam bath or under an infrared lamp. Keep the
SiO,% 5 ~W 2 W ! 3 100 (1)
2 1 2
dish covered with a raised cover glass during evaporation.
When evaporation is complete (Note 2) (absence of HCl), cool,
BaO, R O (Al O +P O ), CaO, AND MgO
2 3 2 3 2 5
drench the residue with 5 mL of HCl, and then add 20 mL of
hot water. Digest for 5 min and filter through a 9-cm medium
11. General Considerations
filter paper. Catch the filtrate in a 250-mL platinum dish.
11.1 The detailed analysis described below may be desirable
Transfer the precipitated silica to the filter with the aid of a
only infrequently. Several steps may be omitted without undue
policeman and a bit of paper pulp, and wash the precipitate and
loss of accuracy, for example, the hydrogen sulfide (H S) and
paper twelve times with hot 2 % HCl. Transfer the paper and
the cupferron precipitations. Many glasses contain insignificant
precipitate to the dish used for fusion and dehydration and
amounts of BaO (less than 0.1 %), in which case BaO also may
...
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