ASTM C169-92(2005)

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Designation:C169–92(Reapproved 2005)
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 (´) 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 1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 These test methods cover the quantitative chemical
responsibility of the user of this standard to establish appro-
analysis of soda-lime and borosilicate glass compositions for
priate safety and health practices and determine the applica-
both referee and routine analysis. This would be for the usual
bility of regulatory limitations prior to use.
constituents present in glasses of the following types: (1)
soda-lime silicate glass, (2) soda-lime fluoride opal glass, and
2. Referenced Documents
(3) borosilicate glass. The following common oxides, when
2.1 ASTM Standards:
present in concentrations greater than indicated, are known to
C146 Test Methods for Chemical Analysis of Glass Sand
interfere with some of the determinations in this method: 2%
C225 Test Methods for Resistance of Glass Containers to
barium oxide (BaO), 0.2% phosphorous pentoxide (P O ),
2 5
Chemical Attack
0.05% zinc oxide (ZnO), 0.05% antimony oxide (Sb O ),
2 3
D1193 Specification for Reagent Water
0.05% lead oxide (PbO).
E50 Practices for Apparatus, Reagents, and Safety Consid-
1.2 The analytical procedures, divided into two general
erations for Chemical Analysis of Metals, Ores, and
groups, those for referee analysis, and those for routine
Related Materials
analysis, appear in the following order:
E60 Practice for Analysis of Metals, Ores, and Related
Sections
Materials by Molecular Absorption Spectrometry
Procedures for Referee Analysis:
Silica 10
BaO, R O (Al O +P O ), CaO, and MgO 11-15
2 2 2 3 2 5 3. Significance and Use
Fe O ,TiO,ZrO by Photometry and Al O by Complexio- 16-22
2 3 2 2 2 3
3.1 These test methods can be used to ensure that the
metric Titration
Cr O by Volumetric and Photometric Methods 23-25
chemical composition of the glass meets the compositional
2 3
MnO by the Periodate Oxidation Method 26-29
specification required for the finished glass product.
Na O by the Zinc Uranyl Acetate Method and KObythe 30-33
2 2
3.2 These test methods do not preclude the use of other
Tetraphenylborate Method
SO (Total Sulfur) 34 to 35
3 methods that yield results within permissible variations. In any
As O by Volumetric Method 36-40
2 3
case, the analyst should verify the procedure and technique
Procedures for Routine Analysis:
employed by means of a National Institute of Standards and
Silica by the Single Dehydration Method 42-44
Al O , CaO, and MgO by Complexiometric Titration, and BaO, 45-51
2 3 Technology (NIST) standard reference material having a com-
Na O, and K O by Gravimetric Method
2 2
ponentcomparablewiththatofthematerialundertest.Alistof
BaO, Al O , CaO, and MgO by Atomic Absorption; and Na O 52-59
2 3 2
standard reference materials is given in the NIST Special
and K O by Flame Emission Spectroscopy
SO (Total Sulfur) 60
Publication 260, current edition.
B O 61 to 62
2 3
3.3 Typical examples of products manufactured using soda-
Fluorine by Pyrohydrolysis Separation and Specific Ion Electrode 63-66
Measurement lime silicate glass are containers, tableware, and flat glass.
P O by the Molybdo-Vanadate Method 67-70
2 5 3.4 Typical examples of products manufactured using boro-
Colorimetric Determination of Ferrous Iron Using 1,10 71-76
silicate glass are bakeware, labware, and fiberglass.
Phenan throline
1 2
These test methods are under the jurisdiction of ASTM Committee C14 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Glass and Glass Products and are the direct responsibility of Subcommittee C14.02 contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
on Chemical Analysis. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Sept. 1, 2005. Published November 2005. Originally the ASTM website.
approvedin1941.Lastpreviouseditionapprovedin2000asC169–89(2000).DOI: Available from National Institute of Standards and Technology, Gaithersburg,
10.1520/C0169-92R05. MD 20899.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C169–92 (2005)
3.5 Typical examples of products manufactured using fluo- 7.2 The considerations of instrumentation given in Test
ride opal glass are containers, tableware, and decorative Methods C146 are equally applicable to these test methods.
glassware.
8. Preparation of Sample
4. Purity of Reagents
8.1 Glass crushed in a steel mortar as described in Test
4.1 Reagent grade chemicals shall be used throughout.
Methods C225, and sieved through a 150-µm (No. 100) mesh
Unless otherwise indicated, it is intended that reagents shall
sieve, is generally suitable for analysis, except for the deter-
conform to the specifications of the Committee on Analytical
mination of iron oxide (Fe O ). After crushing and sieving,
2 3
Reagents of the American Chemical Society, where such
place the powder on a sheet of paper and pass a small magnet
specifications are available. Other grades may be used, pro-
through it to remove adventitious iron. Then store in a tightly
vided it is first ascertained that the reagent is of sufficiently
closed container and keep in a desiccator.
high purity to permit its use without lessening the accuracy of
8.2 A sample prepared in an iron mortar is not recom-
the determination.
mended for the determination of Fe O . Instead, glass should
4.2 Purity of Water—Unless otherwise indicated, reference 2 3
be ground in an agate mortar after ascertaining it is free of
to water shall be understood to mean reagent water as defined
contamination.
by Type I, II, or III of Specification D1193.
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
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
4 Fluorine opal glass, 500 to 550°C for 1 h
when standardized are specified as a ratio, stating the number Borosilicate glass, 800°C for 1 h
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
absolute error, and is dependent on the quantity of constituent
(Mg(ClO ) ) and barium oxide (BaO) are recommended.
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
brandsormanufacturers.Allfilterpapersareofthedoubleacid
Al O +P O 60.05 60.10 (−P O )
2 3 2 5 2 5
CaO 60.05 60.15
washedashlesstype.“Coarse”filterpaperreferstotheporosity
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 E60.
SO 60.02 60.05
As O 60.005 .
2 3
P O . 60.005 to 0.02
2 5
B O . 60.05 to 0.15
Reagent Chemicals, American Chemical Society Specifications, American 2 3
Fluorine . 60.01 to 0.20
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
(0.1 to 6.0 %)
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
9.2 It is recommended that reported results be rounded as
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. follows:
C169–92 (2005)
Number of Significant Figures <0.01 1 or 2
Percent
Retained After Rounding
1to100 3
9.3 Recorded results should be carried to one more signifi-
0.1to0.99 2
cant figure than required in 9.2.
0.01 to 0.09 1 or 2
PROCEDURES FOR REFEREE ANALYSIS
exception: after the fusion has been made and before addition of the acid
SILICA
(see 10.2), add 10 mL of aluminum chloride (AlCl ) solution (10
mL=200 mg of Al) to complex fluorine. If evaporation is made on a
10. Procedure
steambath,itisdifficulttodrytheresidue.Itissuggestedthatfinaldrying,
10.1 Weigh 1.000 g of powdered sample and 1.5 g of
before filtration, be made in a drying oven for 30 to 45 min at 105°C.
anhydrous sodium carbonate (Na CO ) for soda-lime glass, or
2 3
Results for SiO when analyzing fluorine opals may tend to be low by
2.0gofNa CO for borosilicate glass, into a clean 75-mL
0.2 to 0.3%. For an alternative, but more lengthy procedure, consult
2 3
platinum dish (see 10.1.1); mix well with a platinum or Applied Inorganic Analysis.
NOTE 2—Boron in amounts less than 5% B O does not interfere.
Nichrome wire. Tap the charge so it lies evenly in the bottom 2 3
However, if boron is greater than 5%, proceed to the point of completing
of the dish. Cover with platinum lid and heat first at a dull red
the first dehydration (see 10.2), then add 20 mL of anhydrous methanol
heat over a clean oxidizing flame; gradually raise the tempera-
saturated with dry HCl (gas), and evaporate to dryness on an air bath or
ture until a clear melt is obtained. Properly carried out, little or
under an infrared lamp. Repeat once more before proceeding.
no spattering should occur and the fusion can be performed in
10.3 Evaporate the filtrate to dryness on the steam bath or
3 to 4 min. When melted, rotate the melt to spread it evenly
under an infrared lamp.When dry, cool, drench with 10 mLof
over the bottom and lower sides of the dish, gradually
HCl (1+1) and again evaporate just to dryness; then bake in a
withdrawing from the flame. Cover and cool to room tempera-
drying oven at 105°C for 30 min. Cool, drench with 5 mL of
ture.Duringfusion,thedishshouldbehandledatalltimeswith
HCl, and add 20 mLof hot water and a small bit of filter pulp.
platinum-tipped tongs and the fusion performed with a plati-
Digesthotfor5minandfilterthrougha7-cmfinepaper.Police
num (preferably 90% platinum and 10% rhodium alloy) or
thedishwiththeaidofabitofpaperpulpandwashprecipitate
silica triangle.
andpapereighttimeswithhot2%HCl.Transferthepaperand
10.1.1 To obtain accurate repeat weighings, platinum ware
precipitate to the dish containing the initial precipitation.Wipe
shall be kept scrupulously clean on the outside of the vessel as
the stirring rod and the periphery of the funnel with a piece of
well as on the inside. It should be polished brightly with fine,
damp filter paper and add to the dish containing the precipitate
round grain sand and protected from dirty surfaces. It is
for ignition.
recommendedthatporcelainplatesbeusedforcoolingfusions,
10.4 Partially cover the dish with its platinum lid but leave
andthatplatinumbesetonpapertowelsorothercleanmaterial
enoughspacesoaircancirculateduringignition.Placethedish
during filtration.
in a cold muffle furnace and bring the temperature to 1200°C
10.2 Add 20 to 25 mL of HCl (1 + 1) (Note 1) under the
for 30 min. Carefully and completely cover the dish before
platinumcoveranddigestonasteambathorhotplateuntilthe
removing it from the furnace and transfer to a desiccator. Cool
melt has completely disintegrated; it is also possible to digest
toroomtemperatureandweighthecovereddish(W ).Moisten
the melt in the cold overnight. Police and rinse the lid with a
thesilicawith1to2mLofwaterandadd4to5mLofHFand
finejetofwater;rinsedownthesidesofthedishandevaporate
0.5 g of oxalic acid crystals. Evaporate to dryness on a sand
todrynessonasteambathorunderaninfraredlamp.Keepthe
bath or under an infrared lamp. Carefully sublime any remain-
dish covered with a raised cover glass during evaporation.
ing oxalic acid, cover the dish with its platinum cover, heat to
Whenevaporationiscomplete(Note2)(absenceofHCl),cool,
1000°C for 2 min, cool, and weigh (W ) as before.
drench the residue with 5 mL of HCl, and then add 20 mL of
10.5 Calculation—CalculatethepercentofSiO asfollows:
hot water. Digest for 5 min and filter through a 9-cm medium
SiO,% 5 ~W 2W ! 3100 (1)
filter paper. Catch the filtrate in a 250-mL platinum dish.
2 1 2
Transfer the precipitated silica to the filter with the aid of a
BaO, R O (Al O +P O ), CaO, AND MgO
2 3 2 3 2 5
policemanandabitofpaperpulp,andwashtheprecipitateand
paper twelve times with hot 2% HCl. Transfer the paper and
11. General Considerations
precipitate to the dish used for fusion and dehydration and
11.1 Thedetailedanalysisdescribedbelowmaybedesirable
reserve for subseque
...