ASTM C169-92(2011)

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Designation: C169 − 92(Reapproved 2011)
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 U.S. Department of Defense.
1. Scope responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
1.1 These test methods cover the quantitative chemical
bility of regulatory limitations prior to use.
analysis of soda-lime and borosilicate glass compositions for
both referee and routine analysis. This would be for the usual
2. Referenced Documents
constituents present in glasses of the following types: (1)
2.1 ASTM Standards:
soda-lime silicate glass, (2) soda-lime fluoride opal glass, and
C146Test Methods for Chemical Analysis of Glass Sand
(3) borosilicate glass. The following common oxides, when
C225Test Methods for Resistance of Glass Containers to
present in concentrations greater than indicated, are known to
Chemical Attack
interfere with some of the determinations in this method: 2%
D1193Specification for Reagent Water
barium oxide (BaO), 0.2% phosphorous pentoxide (P O ),
2 5
E50Practices for Apparatus, Reagents, and Safety Consid-
0.05% zinc oxide (ZnO), 0.05% antimony oxide (Sb O ),
2 3
erations for Chemical Analysis of Metals, Ores, and
0.05% lead oxide (PbO).
Related Materials
1.2 The analytical procedures, divided into two general
E60Practice for Analysis of Metals, Ores, and Related
groups, those for referee analysis, and those for routine
Materials by Spectrophotometry
analysis, appear in the following order:
Sections 3. Significance and Use
Procedures for Referee Analysis:
3.1 These test methods can be used to ensure that the
Silica 10
BaO, R O (Al O +P O ), CaO, and MgO 11–15
2 2 2 3 2 5 chemical composition of the glass meets the compositional
Fe O ,TiO ,ZrO by Photometry and Al O by Complexio- 16–22
2 3 2 2 2 3
specification required for the finished glass product.
metric Titration
Cr O by Volumetric and Photometric Methods 23–25
2 3
3.2 These test methods do not preclude the use of other
MnO by the Periodate Oxidation Method 26–29
methodsthatyieldresultswithinpermissiblevariations.Inany
Na O by the Zinc Uranyl Acetate Method and K Obythe 30–33
2 2
Tetraphenylborate Method case, the analyst should verify the procedure and technique
SO (Total Sulfur) 34 to 35
employed by means of a National Institute of Standards and
As O by Volumetric Method 36–40
2 3
Technology (NIST) standard reference material having a com-
Procedures for Routine Analysis:
Silica by the Single Dehydration Method 42–44 ponentcomparablewiththatofthematerialundertest.Alistof
Al O , CaO, and MgO by Complexiometric Titration, and BaO, 45–51
2 3
standard reference materials is given in the NIST Special
Na O, and K O by Gravimetric Method
2 2 3
Publication 260, current edition.
BaO, Al O , CaO, and MgO by Atomic Absorption; and Na O 52–59
2 3 2
and K O by Flame Emission Spectroscopy
3.3 Typical examples of products manufactured using soda-
SO (Total Sulfur) 60
lime silicate glass are containers, tableware, and flat glass.
B O 61 to 62
2 3
Fluorine by Pyrohydrolysis Separation and Specific Ion Electrode 63–66
3.4 Typical examples of products manufactured using boro-
Measurement
P O by the Molybdo-Vanadate Method 67–70 silicate glass are bakeware, labware, and fiberglass.
2 5
Colorimetric Determination of Ferrous Iron Using 1,10 71–76
3.5 Typical examples of products manufactured using fluo-
Phenan throline
ride opal glass are containers, tableware, and decorative
1.3 This standard does not purport to address all of the
glassware.
safety concerns, if any, associated with its use. It is the
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 Properties and Analysis. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Oct. 1, 2011. Published October 2011. Originally the ASTM website.
approvedin1941.Lastpreviouseditionapprovedin2005asC169–92(2005).DOI: Available from National Institute of Standards and Technology, Gaithersburg,
10.1520/C0169-92R11. MD 20899.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C169 − 92 (2011)
4. Purity of Reagents 7.2 The considerations of instrumentation given in Test
Methods C146 are equally applicable to these test methods.
4.1 Reagent grade chemicals shall be used throughout.
Unless otherwise indicated, it is intended that reagents shall
8. Preparation of Sample
conform to the specifications of the Committee on Analytical
8.1 Glass crushed in a steel mortar as described in Test
Reagents of the American Chemical Society, where such
Methods C225, and sieved through a 150-µm (No. 100) mesh
specifications are available. Other grades may be used, pro-
sieve, is generally suitable for analysis, except for the deter-
vided it is first ascertained that the reagent is of sufficiently
mination of iron oxide (Fe O ). After crushing and sieving,
2 3
high purity to permit its use without lessening the accuracy of
place the powder on a sheet of paper and pass a small magnet
the determination.
through it to remove adventitious iron. Then store in a tightly
4.2 Purity of Water—Unless otherwise indicated, reference
closed container and keep in a desiccator.
to water shall be understood to mean reagent water as defined
8.2 A sample prepared in an iron mortar is not recom-
by Type I, II, or III of Specification D1193.
mended for the determination of Fe O . Instead, glass should
2 3
be ground in an agate mortar after ascertaining it is free of
5. Concentration of Acids and Ammonium Hydroxide
contamination.
5.1 When acids and ammonium hydroxide are specified by
8.3 A sample prepared for the determination of fluorine
name or chemical formula only, concentrated reagents of the
should be sieved through a 75-µm (No. 200) mesh sieve rather
following percent concentrations are intended:
than a 150-µm (No. 100) sieve.
%
8.4 The practice of drying samples in a drying oven at 105
Hydrochloric acid (HCl) 36 to 38
Hydrofluoric acid (HF) 48 to 51
to 110°C after preparation is not recommended. Powdered
Nitric acid (HNO ) 69to71
glass can fix CO and water as readily at this temperature as at
Perchloric acid (HClO ) 70to72
room temperature.Afreshly prepared sample, if exposed but a
Sulfuric acid (H SO ) 95to98
2 4
Ammonium hydroxide (NH OH) 28 to 30
4 shorttimetotheatmosphere,willnothaveacquiredanignition
5.2 Concentrations of diluted acids and NH OH except loss of much analytical significance. If ignition loss is
when standardized are specified as a ratio, stating the number determined, use the following temperature schedules:
of volumes of the concentrated reagent to be added to a given
Soda-lime glass, 800°C for 1 h
Fluorine opal glass, 500 to 550°C for 1 h
number of volumes of water, as follows: HCl (1 + 99) means
Borosilicate glass, 800°C for 1 h
1 volume of concentrated HCl (approximately 37%) added to
Determine the ignition loss ona1to3-g sample in a
99 volumes of water.
platinum crucible.
5.3 The hygroscopic nature of the ignited precipitates of
9. Precision and Bias
silica, aluminum oxide, and calcium oxide obtained in the
methods to be described, requires the use of fresh and highly
9.1 The probable precision of results that can be expected
active desiccants. For this purpose, magnesium perchlorate
by the use of the procedures described in these test methods is
(Mg(ClO ) ) and barium oxide (BaO) are recommended.
4 2 shown in the following tabulation. Precision is given as
absolute error, and is dependent on the quantity of constituent
6. Filter Papers
present as well as the procedure used.
6.1 Throughout these test methods, filter papers will be
Probable Precision of Results, weight %
Constituent Referee Analysis Routine Analysis
designated as “coarse,” “medium,” or “fine,” without naming
Silica ±0.1 ±0.25
brandsormanufacturers.Allfilterpapersareofthedoubleacid
BaO ±0.02 ±0.05
washedashlesstype.“Coarse”filterpaperreferstotheporosity
Al O +P O ±0.05 ±0.10 (−P O )
2 3 2 5 2 5
CaO ±0.05 ±0.15
commonly used for the filtration of aluminum hydroxide.
MgO ±0.05 ±0.02 to 0.10
“Medium” filter paper refers to that used for filtration of
Fe O ±0.003 .
2 3
calcium oxalate, and “fine” filter paper to that used for barium
TiO ±0.005 .
ZrO ±0.001 to 0.005 .
sulfate. 2
Cr O (volumetric) ±0.005 .
2 3
Cr O (photometric) ±0.0001 to 0.001 .
2 3
7. Photometers and Photometric Practice
MnO ±0.001 to 0.005 .
Na O ±0.05 ±0.25 (flame emission)
7.1 Photometers and photometric practice prescribed in
K O ±0.02 to 0.05 ±0.02 to 0.10
these methods shall conform to Practice E60.
(flame emission)
SO ±0.02 ±0.05
As O ±0.005 .
2 3
P O . ±0.005 to 0.02
2 5
Reagent Chemicals, American Chemical Society Specifications, American
B O . ±0.05 to 0.15
2 3
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Fluorine . ±0.01 to 0.20
listed by the American Chemical Society, see Analar Standards for Laboratory
(0.1 to 6.0 %)
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 (2011)
9.3 Recorded results should be carried to one more signifi-
Number of Significant Figures
Percent
Retained After Rounding
cant figure than required in 9.2.
1to100 3
0.1to0.99 2
0.01 to 0.09 1 or 2
<0.01 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.
Results for SiO when analyzing fluorine opals may tend to be low by
anhydrous sodium carbonate (Na CO ) for soda-lime glass, or 2
2 3
0.2 to 0.3%. For an alternative, but more lengthy procedure, consult
2.0gofNa CO for borosilicate glass, into a clean 75-mL
2 3 6
Applied Inorganic Analysis.
platinum dish (see 10.1.1); mix well with a platinum or
NOTE 2—Boron in amounts less than 5% B O does not interfere.
2 3
Nichrome wire. Tap the charge so it lies evenly in the bottom
However, if boron is greater than 5%, proceed to the point of completing
the first dehydration (see 10.2), then add 20 mL of anhydrous methanol
of the dish. Cover with platinum lid and heat first at a dull red
saturated with dry HCl (gas), and evaporate to dryness on an air bath or
heat over a clean oxidizing flame; gradually raise the tempera-
under an infrared lamp. Repeat once more before proceeding.
ture until a clear melt is obtained. Properly carried out, little or
10.3 Evaporate the filtrate to dryness on the steam bath or
no spattering should occur and the fusion can be performed in
under an infrared lamp.When dry, cool, drench with 10 mLof
3 to 4 min. When melted, rotate the melt to spread it evenly
HCl (1+1) and again evaporate just to dryness; then bake in a
over the bottom and lower sides of the dish, gradually
drying oven at 105°C for 30 min. Cool, drench with 5 mL of
withdrawing from the flame. Cover and cool to room tempera-
HCl, and add 20 mLof hot water and a small bit of filter pulp.
ture.Duringfusion,thedishshouldbehandledatalltimeswith
Digesthotfor5minandfilterthrougha7-cmfinepaper.Police
platinum-tipped tongs and the fusion performed with a plati-
thedishwiththeaidofabitofpaperpulpandwashprecipitate
num (preferably 90% platinum and 10% rhodium alloy) or
andpapereighttimeswithhot2%HCl.Transferthepaperand
silica triangle.
precipitate to the dish containing the initial precipitation.Wipe
10.1.1 To obtain accurate repeat weighings, platinum ware
the stirring rod and the periphery of the funnel with a piece of
shall be kept scrupulously clean on the outside of the vessel as
damp filter paper and add to the dish containing the precipitate
well as on the inside. It should be polished brightly with fine,
for ignition.
round grain sand and protected from dirty surfaces. It is
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
for 30 min. Carefully and completely cover the dish before
10.2 Add 20 to 25 mL of HCl (1 + 1) (Note 1) under the
removing it from the furnace and transfer to a desiccator. Cool
platinumcoveranddigestonasteambathorhotplateuntilthe
toroomtemperatureandweighthecovereddish(W ).Moisten
melt has completely disintegrated; it is also possible to digest
thesilicawith1to2mLofwaterandadd4to5mLofHFand
the melt in the cold overnight. Police and rinse the lid with a
0.5 g of oxalic acid crystals. Evaporate to dryness on a sand
finejetofwater;rinsedownthesidesofthedishandevaporate
bath or under an infrared lamp. Carefully sublime any remain-
todrynessonasteambathorunderaninfraredlamp.Keepthe
ing oxalic acid, cover the dish with its platinum cover, heat to
dish covered with a raised cover glass during evaporation.
1000°C for 2 min, cool, and weigh (W ) as before.
Whenevaporationiscomplete(Note2)(absenceofHCl),cool,
drench the residue with 5 mL of HCl, and then add 20 mL of
10.5 Calculation—Calculate the percent of SiO as follows:
hot water. Digest for 5 min and filter through a 9-cm medium
SiO,% 5 W 2 W 3100 (1)
~ !
2 1 2
filter paper. Catch the filtrate in a 250-mL platinum dish.
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 sub
...