ASTM C169-92(2000)
(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.
General Information
Relations
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:C169–92(Reapproved 2000)
Standard Test Methods for
Chemical Analysis of Soda-Lime and Borosilicate Glass
This standard is issued under the fixed designation C169; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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 priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
1.1 These test methods cover the quantitative chemical
analysis of soda-lime and borosilicate glass compositions for
2. Referenced Documents
both referee and routine analysis. This would be for the usual
2.1 ASTM Standards:
constituents present in glasses of the following types: (1)
C146 Test Methods for Chemical Analysis of Glass Sand
soda-lime silicate glass, (2) soda-lime fluoride opal glass, and
C225 Test Methods for Resistance of Glass Containers to
(3) borosilicate glass. The following common oxides, when
Chemical Attack
present in concentrations greater than indicated, are known to
D1193 Specification for Reagent Water
interfere with some of the determinations in this method: 2%
E50 Practices forApparatus, Reagents, and Safety Precau-
barium oxide (BaO), 0.2% phosphorous pentoxide (P O ),
2 5
tions for Chemical Analysis of Metals
0.05% zinc oxide (ZnO), 0.05% antimony oxide (Sb O ),
2 3
E 60 Practice for Photometric and Spectrophotometric
0.05% lead oxide (PbO).
Methods for Chemical Analysis of Metals
1.2 The analytical procedures, divided into two general
groups, those for referee analysis, and those for routine
3. Significance and Use
analysis, appear in the following order:
3.1 These test methods can be used to ensure that the
Sections
chemical composition of the glass meets the compositional
Procedures for Referee Analysis:
Silica 10
specification required for the finished glass product.
BaO, R O (Al O +P O ), CaO, and MgO 11-15
2 2 2 3 2 5
3.2 These test methods do not preclude the use of other
Fe O ,TiO,ZrO by Photometry and Al O by Complexio- 16-22
2 3 2 2 2 3
methods that yield results within permissible variations. In any
metric Titration
Cr O by Volumetric and Photometric Methods 23-25
2 3 case, the analyst should verify the procedure and technique
MnO by the Periodate Oxidation Method 26-29
employed by means of a National Institute of Standards and
Na O by the Zinc Uranyl Acetate Method and KObythe 30-33
2 2
Technology (NIST) standard reference material having a com-
Tetraphenylborate Method
SO (Total Sulfur) 34 to 35
3 ponentcomparablewiththatofthematerialundertest.Alistof
As O by Volumetric Method 36-40
2 3
standard reference materials is given in the NIST Special
Procedures for Routine Analysis:
Publication 260, current edition.
Silica by the Single Dehydration Method 42-44
Al O , CaO, and MgO by Complexiometric Titration, and BaO, 45-51
2 3 3.3 Typical examples of products manufactured using soda-
Na O, and K O by Gravimetric Method
2 2
lime silicate glass are containers, tableware, and flat glass.
BaO, Al O , CaO, and MgO by Atomic Absorption; and Na O 52-59
2 3 2
3.4 Typical examples of products manufactured using boro-
and K O by Flame Emission Spectroscopy
SO (Total Sulfur) 60
silicate glass are bakeware, labware, and fiberglass.
B O 61 to 62
2 3
3.5 Typical examples of products manufactured using fluo-
Fluorine by Pyrohydrolysis Separation and Specific Ion Electrode 63-66
ride opal glass are containers, tableware, and decorative
Measurement
P O by the Molybdo-Vanadate Method 67-70
2 5 glassware.
Colorimetric Determination of Ferrous Iron Using 1,10 Phenan- 71-76
throline
4. Purity of Reagents
1.3 This standard does not purport to address all of the
4.1 Reagent grade chemicals shall be used throughout.
safety concerns, if any, associated with its use. It is the
Unless otherwise indicated, it is intended that reagents shall
responsibility of the user of this standard to establish appro-
1 2
These test methods are under the jurisdiction of ASTM Committee C14 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 C169–41T. Last previous edition C169–89. MD 20899.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C169–92 (2000)
conform to the specifications of the Committee on Analytical sieve, is generally suitable for analysis, except for the deter-
Reagents of the American Chemical Society, where such mination of iron oxide (Fe O ). After crushing and sieving,
2 3
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 D1193. 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.Afreshly prepared sample, if exposed but a
Hydrofluoric acid (HF) 48 to 51
shorttimetotheatmosphere,willnothaveacquiredanignition
Nitric acid (HNO) 69to71
loss of much analytical significance. If ignition loss is deter-
Perchloric acid (HClO) 70to72
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
9. Precision and Bias
99 volumes of water.
5.3 The hygroscopic nature of the ignited precipitates of
9.1 The probable precision of results that can be expected
silica, aluminum oxide, and calcium oxide obtained in the
by the use of the procedures described in these test methods is
methods to be described, requires the use of fresh and highly
shown in the following tabulation. Precision is given as
active desiccants. For this purpose, magnesium perchlorate
absolute error, and is dependent on the quantity of constituent
(Mg(ClO ) ) and barium oxide (BaO) are recommended.
present as well as the procedure used.
4 2
Probable Precision of Results, weight %
6. Filter Papers
Constituent Referee Analysis Routine Analysis
Silica 60.1 60.25
6.1 Throughout these test methods, filter papers will be
BaO 60.02 60.05
designated as “coarse,” “medium,” or “fine,” without naming
Al O +P O 60.05 60.10 (−P O )
2 3 2 5 2 5
brandsormanufacturers.Allfilterpapersareofthedoubleacid CaO 60.05 60.15
MgO 60.05 60.02 to 0.10
washedashlesstype.“Coarse”filterpaperreferstotheporosity
Fe O 60.003 .
2 3
commonly used for the filtration of aluminum hydroxide.
TiO 60.005 .
“Medium” filter paper refers to that used for filtration of ZrO 60.001 to 0.005 .
Cr O (volumetric) 60.005 .
2 3
calcium oxalate, and “fine” filter paper to that used for barium
Cr O (photometric) 60.0001 to 0.001 .
2 3
sulfate.
MnO 60.001 to 0.005 .
Na O 60.05 60.25 (flame emission)
7. Photometers and Photometric Practice K O 60.02 to 0.05 60.02 to 0.10
(flame emission)
7.1 Photometers and photometric practice prescribed in
SO 60.02 60.05
As O 60.005 .
these methods shall conform to Practice E60.
2 3
P O . 60.005 to 0.02
2 5
7.2 The considerations of instrumentation given in Test
B O . 60.05 to 0.15
2 3
Methods C146 are equally applicable to these test methods.
Fluorine . 60.01 to 0.20
(0.1 to 6.0 %)
8. Preparation of Sample
9.2 It is recommended that reported results be rounded as
8.1 Glass crushed in a steel mortar as described in Test
follows:
Methods C225, and sieved through a 150-µm (No. 100) mesh
Number of Significant Figures
Percent
Retained After Rounding
1to100 3
Reagent Chemicals, American Chemical Society Specifications, American
0.1to0.99 2
Chemical Society, Washington, DC. For suggestions on the testing of reagents not 0.01 to 0.09 1 or 2
listed by the American Chemical Society, see Analar Standards for Laboratory <0.01 1 or 2
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.
C169–92 (2000)
PROCEDURES FOR REFEREE ANALYSIS
before filtration, be made in a drying oven for 30 to 45 min at 105°C.
SILICA
Results for SiO when analyzing fluorine opals may tend to be low by
0.2 to 0.3%. For an alternative, but more lengthy procedure, consult
10. Procedure
Applied Inorganic Analysis.
10.1 Weigh 1.000 g of powdered sample and 1.5 g of
NOTE 2—Boron in amounts less than 5% B O does not interfere.
2 3
anhydrous sodium carbonate (Na CO ) for soda-lime glass, or
2 3 However, if boron is greater than 5%, proceed to the point of completing
2.0gofNa CO for borosilicate glass, into a clean 75-mL the first dehydration (see 10.2), then add 20 mL of anhydrous methanol
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
of the dish. Cover with platinum lid and heat first at a dull red
10.3 Evaporate the filtrate to dryness on the steam bath or
heat over a clean oxidizing flame; gradually raise the tempera-
under an infrared lamp. When dry, cool, drench with 10 mLof
ture until a clear melt is obtained. Properly carried out, little or
HCl (1+1) and again evaporate just to dryness; then bake in a
no spattering should occur and the fusion can be performed in
drying oven at 105°C for 30 min. Cool, drench with 5 mL of
3 to 4 min. When melted, rotate the melt to spread it evenly
HCl, and add 20 mLof hot water and a small bit of filter pulp.
over the bottom and lower sides of the dish, gradually
Digesthotfor5minandfilterthrougha7-cmfinepaper.Police
withdrawing from the flame. Cover and cool to room tempera-
thedishwiththeaidofabitofpaperpulpandwashprecipitate
ture.Duringfusion,thedishshouldbehandledatalltimeswith
andpapereighttimeswithhot2%HCl.Transferthepaperand
platinum-tipped tongs and the fusion performed with a plati-
precipitate to the dish containing the initial precipitation.Wipe
num (preferably 90% platinum and 10% rhodium alloy) or
the stirring rod and the periphery of the funnel with a piece of
silica triangle.
damp filter paper and add to the dish containing the precipitate
10.1.1 To obtain accurate repeat weighings, platinum ware
for ignition.
shall be kept scrupulously clean on the outside of the vessel as 10.4 Partially cover the dish with its platinum lid but leave
well as on the inside. It should be polished brightly with fine,
enoughspacesoaircancirculateduringignition.Placethedish
round grain sand and protected from dirty surfaces. It is in a cold muffle furnace and bring the temperature to 1200°C
recommendedthatporcelainplatesbeusedforcoolingfusions,
for 30 min. Carefully and completely cover the dish before
andthatplatinumbesetonpapertowelsorothercleanmaterial removing it from the furnace and transfer to a desiccator. Cool
during filtration.
toroomtemperatureandweighthecovereddish(W ).Moisten
10.2 Add 20 to 25 mL of HCl (1 + 1) (Note 1) under the thesilicawith1to2mLofwaterandadd4to5mLofHFand
platinumcoveranddigestonasteambathorhotplateuntilthe
0.5 g of oxalic acid crystals. Evaporate to dryness on a sand
melt has completely disintegrated; it is also possible to digest
bath or under an infrared lamp. Carefully sublime any remain-
the melt in the cold overnight. Police and rinse the lid with a
ing oxalic acid, cover the dish with its platinum cover, heat to
finejetofwater;rinsedownthesidesofthedishandevaporate
1000°C for 2 min, cool, and weigh (W ) as before.
to dryness on a steam bath or under an infrared lamp. Keep the
10.5 Calculation—CalculatethepercentofSiO asfollows:
dish covered with a raised cover glass during evaporation.
SiO,% 5 W 2W 3100 (1)
~ !
2 1 2
Whenevaporationiscomplete(Note2)(absenceofHCl),cool,
drench the residue with 5 mL of HCl, and then add 20 mL of
BaO, R O (Al O +P O ), CaO, AND MgO
2 3 2 3 2 5
hot water. Digest for 5 min and filter through a 9-cm medium
filter paper. Catch the filtrate in a 250-mL platinum dish.
11. General Considerations
Transfer the precipitated silica to the filter with the aid of a
11.1 Thedetailedanalysisdescribedbelowmaybedesirable
policemanandabitofpaperpulp,andwashtheprecipitateand
only infrequently. Several steps may be omitted without undue
paper twelve times with hot 2% HCl. Transfer the paper and
loss of accuracy, for example, the hydrogen sulfide (H S) and
precipitate to the dish used for fusion and dehydration and
thecupferronprecipitations.Manyglassescontaininsignificant
reserve for subsequent ignition. Wipe the stirring rod and the
amountsofBaO(lessthan0.1%),inwhichcaseBaOalsomay
periphery of the funnel with a piece of damp filter paper and
be ignored. Thus, if the separation of BaO and the H S
add to the dish containing the precipitate for
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.