ASTM C146-94a(2004)
(Test Method)Standard Test Methods for Chemical Analysis of Glass Sand
Standard Test Methods for Chemical Analysis of Glass Sand
SIGNIFICANCE AND USE
These test methods can be used to ensure that the chemical composition of the glass sand meets the compositional specification required for this raw material.
These test methods do not preclude the use of other methods that yield results within permissible variations. In any case, the analyst should verify the procedure and technique used by means of a National Institute of Standards and Technology (NIST) standard reference material or other similar material of known composition having a component comparable with that of the material under test. A list of standard reference materials is given in the NIST Special Publication 260, current edition.
SCOPE
1.1 These test methods cover the chemical analysis of glass sands. They are useful for either high-silica sands (99% + silica (SiO )) or for high-alumina sands containing as much as 12 to 13% alumina (Al O ). Generally nonclassical, the test methods are rapid and accurate. They include the determination of silica and of total R O (see 11.2.4), and the separate determination of total iron as iron oxide (Fe O ), titania (TiO ), chromium oxide (Cr O ), zirconia (ZrO ), and ignition loss. Included are procedures for the alkaline earths and alkalies. High-alumina sands may contain as much as 5 to 6% total alkalies and alkaline earths. It is recommended that the alkalies be determined by flame photometry and the alkaline earths by absorption spectrophotometry.
1.2 These test methods, if followed in detail, will provide interlaboratory agreement of results. Note 1-For additional information, see Test Methods C169 and Practices E50.
1.3 The test methods appear in the following order: Procedures for Referee Analysis: Section Silica (SiO2)--Double Dehydration 10 Total R2O3--Gravimetric 11 Fe2O3, TiO2, ZrO2, Cr2O3, by Photometric Methods and 12-17 Al2O3 by Complexiometric Titration Preparation of the Sample for Determination of Iron 12 Oxide, Titania, Alumina, and Zirconia Iron oxide (as Fe2O3) by 1,10-Phenanthroline Method 13 Titania (TiO2) by the Tiron Method 14 Alumina (Al2O3) by the CDTA Titration Method 15 Zirconia (ZrO2) by the Pyrocatechol Violet Method 16 Chromium Oxide (Cr2O3) by the 1,5-Diphenylcarbo- 17 hydrazide Method Procedures for Routine Analysis: Silica (SiO2)--Single Dehydration 19 Al2O3, CaO, and MgO--Atomic Absorption Spectro- 20-25 photometry Na2O and K2O--Flame Emission Spectrophotometry 26-27 Loss on Ignition (LOI) 28
1.4 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:C146–94a (Reapproved 2004)
Standard Test Methods for
Chemical Analysis of Glass Sand
This standard is issued under the fixed designation C146; 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.
1. Scope
Na O and K O—Flame Emission Spectrophotometry 26-27
2 2
Loss on Ignition (LOI) 28
1.1 These test methods cover the chemical analysis of glass
1.4 This standard does not purport to address all of the
sands. They are useful for either high-silica sands
(99%+silica (SiO )) or for high-alumina sands containing as safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
much as 12 to 13% alumina (Al O ). Generally nonclassical,
2 3
the test methods are rapid and accurate. They include the priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
determination of silica and of total R O (see 11.2.4), and the
2 3
separate determination of total iron as iron oxide (Fe O ),
2 3
2. Referenced Documents
titania (TiO ), chromium oxide (Cr O ), zirconia (ZrO ), and
2 2 3 2
2.1 ASTM Standards:
ignition loss. Included are procedures for the alkaline earths
C169 Test Methods for Chemical Analysis of Soda-Lime
and alkalies. High-alumina sands may contain as much as 5 to
and Borosilicate Glass
6% total alkalies and alkaline earths. It is recommended that
C429 Test Method for SieveAnalysis of Raw Materials for
the alkalies be determined by flame photometry and the
Glass Manufacture
alkaline earths by absorption spectrophotometry.
D1193 Specification for Reagent Water
1.2 These test methods, if followed in detail, will provide
E11 SpecificationforWovenWireTestSieveClothandTest
interlaboratory agreement of results.
Sieves
NOTE 1—For additional information, see Test Methods C169 and
E50 Practices for Apparatus, Reagents, and Safety Consid-
Practices E50.
erations for Chemical Analysis of Metals, Ores, and
1.3 The test methods appear in the following order:
Related Materials
Procedures for Referee Analysis: Section
E60 Practice for Analysis of Metals, Ores, and Related
Materials by Molecular Absorption Spectrometry
Silica (SiO )—Double Dehydration 10
2.2 Other Documents:
Total R O —Gravimetric 11
2 3
Fe O ,TiO ,ZrO ,Cr O , by Photometric Methods and 12-17
2 3 2 2 2 3
NIST Special Publication 260
Al O by Complexiometric Titration
2 3
Preparation of the Sample for Determination of Iron 12
3. Significance and Use
Oxide, Titania, Alumina, and Zirconia
Iron Oxide (as Fe O ) by 1,10-Phenanthroline Method 13
2 3
3.1 These test methods can be used to ensure that the
Titania (TiO ) by the Tiron Method 14
chemical composition of the glass sand meets the composi-
Alumina (Al O ) by the CDTA Titration Method 15
2 3
Zirconia (ZrO ) by the Pyrocatechol Violet Method 16 tional specification required for this raw material.
Chromium Oxide (Cr O ) by the 1,5-Diphenylcarbo- 17
2 3
3.2 These test methods do not preclude the use of other
hydrazide Method
methods that yield results within permissible variations. In any
Procedures for Routine Analysis: case, the analyst should verify the procedure and technique
used by means of a National Institute of Standards and
Silica (SiO )—Single Dehydration 19
Technology(NIST)standardreferencematerialorothersimilar
Al O , CaO, and MgO—Atomic Absorption Spec- 20–25
2 3
trophotometry
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
These test methods are under the jurisdiction of ASTM Committee C14 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Glass and Glass Products and are the direct responsibility of Subcommittee C14.02 Standards volume information, refer to the standard’s Document Summary page on
on Chemical Properties and Analysis. the ASTM website.
Current edition approved Oct. 1, 2004. Published October 2004. Originally Standard samples available from the National Institute of Standards and
approved in 1939 . Last previous edition apporved in 1999 as C146–94a(1999). Technology are listed in U.S. Dept. of Commerce, NIST, Special Publication 260
DOI: 10.1520/C0146-94AR04. (current edition), Washington, DC 20234.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C146–94a (2004)
material of known composition having a component compa- 8. Preparation of Sample
rable with that of the material under test. A list of standard
8.1 General Considerations—The acquisition and prepara-
reference materials is given in the NIST Special Publication
tion of the sample shall follow the principles stated in Test
260, current edition.
Method C429.
8.2 Thelaboratorysampleisreducedforanalysisto10to20
4. Photometers and Photometric Practice
g by use of a small riffle with openings preferably of 6.4-mm
( ⁄4-in.) size. The analytical sample is then ground in an agate
4.1 Photometers and photometric practice prescribed in
mortar to pass a 150-µm (No. 100) sieve. If the laboratory
these test methods shall conform to Practice E60.
sampleasreceivedcontainsanylargeparticlesthatareretained
on a 850-µm (No. 20) sieve, these shall be sieved out, crushed
5. Purity of Reagents
(withoutcontamination)soastopassthesieve,andthenmixed
5.1 Reagent grade chemicals shall be used throughout.
back into the laboratory sample before riffling.
Unless otherwise indicated, it is intended that reagents shall
conform to the specifications of the Committee on Analytical
9. Precision and Bias
Reagents of theAmerican Chemical Society, where suchspeci-
9.1 Precision—Theprobableprecisionofresultsthatcanbe
fications are available. Other grades may be used, provided it
expected by the use of procedures described in these test
is first ascertained that the reagent is of sufficiently high purity
methods is shown in the following tabulation. Precision is
to permit its use without lessening the accuracy of the
given as absolute error and is dependent on the quantity of the
determination.
constituent present as well as the procedure used.
5.2 Unless otherwise indicated, references to water shall be
Probable Precision of Results, Weight %
understood to mean reagent water as defined by Type I, II, or
Constituent Referee Analysis Routine Analysis
III of Specification D1193.
SiO (99 %) 60.1 60.25
SiO (85–90 %) 60.1 60.25
6. Concentration of Acids and Ammonium Hydroxide
R O (1 %) 60.05 60.10
2 3
R O (10–15 %) 60.1 60.15
(NH OH) 2 3
Al O (1 %) 60.05 60.10
2 3
Al O (10–15 %) 60.1 60.1
6.1 When acids and ammonium hydroxide are specified by
2 3
Fe O 60.003 .
2 3
name or chemical formula only, concentrated reagents of the
TiO 60.005 .
following percent concentrations are intended:
ZrO 60.001 to 0.005 .
Cr O 60.0001 to 0.001 .
Sp Gr % 2 3
CaO . 60.001
MgO . 60.001
Hydrochloric acid (HCl) 1.2 36 to 38
Na O . 60.001
Hydrofluoric acid (HF) 1.2 48 to 51 2
K O . 60.001
Nitric acid (HNO ) 1.4 69 to 71 2
Perchloric acid (HClO ) 1.8 70 to 72
9.2 Bias—Standard reference materials or other similar
Sulfuric acid (H SO ) 1.8 95 to 98
2 4
Ammonium hydroxide (NH OH) 0.9 28 to 30 materials of known composition should be analyzed whenever
possible to determine the bias of the results.
6.2 Concentrations of diluted acids and NH OH, except
when standardized, are specified as a ratio stating the number
PROCEDURES FOR REFEREE ANALYSIS
of volumes of the concentrated reagent to be added to a given
10. Silica (SiO ) by the Double Dehydration Method
number of volumes of water, as in the following example: HCl
10.1 Weigh 1.000 g of the powdered sample and 2.0 g of
(1+99) means 1 volume of concentrated HCl (sp gr 1.19)
added to 99 volumes of water. anhydrous sodium carbonate (Na CO ) into a clean 75-mL
2 3
platinumdish(Note2);mixwellwithaplatinumorNichrome
wire.Tap the charge so it lies evenly in the bottom of the dish.
7. Filter Papers
Cover evenly with an additional 1.0 g of Na CO . Cover with
2 3
7.1 Throughout these test methods, filter papers will be
the platinum lid and heat first at a dull red heat over a clean
designated as “coarse,” “medium,” or “fine” without naming
oxidizing flame; gradually raise the temperature until a clear
brands or manufacturers. All filter papers are of the double-
melt is obtained. Properly carried out, little or no spattering
acid-washed ashless type. “Coarse” filter paper refers to the
should occur, and the fusion can be performed in 3 to 4 min.
porositycommonlyusedforthefiltrationofaluminumhydrox-
When melted, rotate the melt to spread it evenly over the
ide. “Medium” filter paper refers to that used for filtration of
bottom and lower sides of the dish, gradually withdrawing
calcium oxalate, and “fine” filter paper to that used for barium
from the flame. Cover and cool to room temperature. During
sulfate.
fusion, the dish should be handled at all times with platinum-
tipped tongs and the fusion performed with a platinum (pref-
erably 90% platinum and 10% rhodium alloy) or silica
Reagent Chemicals, American Chemical Society Specifications, American
triangle.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia Requirements for sieves are given in ASTM Specification E11.
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, Nichrome is a registered trademark of the Driver-Harris Co., 308 Middlesex
MD. St., Harrison, NJ 07029.
C146–94a (2004)
NOTE 2—To obtain accurate repeat weighings, platinum ware must be
suspected to be present. Sands low in Al O (0.05 to 0.5%)
2 3
kept scrupulously clean on the outside of the vessel as well as on the
requirea5-to10-gsample;sandswithlargeramountsofAl O
2 3
inside. It should be polished brightly with fine, round grain sand and
require a 0.5- to 1.0-g sample. Usually experience or prior
protected from dirty surfaces. It is recommended that porcelain plates be
information will indicate a satisfactory sample weight. The
usedforcoolingfusions,andthatplatinumbesetonpapertowelsorother
total R O serves as a check on the sum of the R O oxides
2 3 2 3
clean material during filtration.
determined separately. It also helps to identify an unknown
10.2 Add 20 to 25 mL of HCl (1+1) under the platinum
sand as a low- or high-alumina type.
cover and digest on a steam bath or hot plate until the melt has
11.2 Procedure:
completelydisintegrated;itisalsopossibletodigestthemeltin
11.2.1 Weigh a suitable weight of sample into an 80- to
the cold HCl overnight. Police and rinse the lid with a fine jet
100-mLplatinumdish,moisten,andadd10mLofHFforeach
of water; rinse down the sides of the dish and evaporate to
gram of sample taken; add 4 mL of H SO (1+1) and
2 4
dryness on a steam bath or under an infrared lamp. Keep the
7 evaporate to the first fuming of H SO (Note 3). Cool,
2 4
dish covered with a raised cover glass during evaporation.
carefully wash down the sides of the dish with a minimum of
When evaporation is complete (absence of HCl), cool, drench
water, and evaporate to the cessation of H SO fumes. Cool,
2 4
theresiduewith5mLofHCl,andthenadd20mLofhotwater.
add10to15mLofHCl(1+1),20mLofhotwater,anddigest
Digest for 5 min and filter through a 9-cm medium filter paper.
hotuntilthesaltsareinsolution.Iftheydonotdissolvereadily,
Catch the filtrate in a 250-mL platinum dish. Transfer the
transfer to a beaker, police the dish, and boil the solution until
precipitated silica to the filter with the aid of a policeman and
the sulfates have dissolved (Note 4).
a bit of paper pulp, and wash the precipitate and paper twelve
times with hot 2% HCl. Transfer the paper and precipitate to
NOTE 3—Some sands may contain small amounts of organic matter as
the dish used for fusion and dehydration and reserve for
shown by the presence of carbon or carbonaceous material in the
subsequent ignition. Wipe the stirring rod and the periphery of concentrated H SO . If this is the case, add 2 to 3 mLof HNO and 10 to
2 4 3
15 drops of HClO , and proceed.
thefunnelwithapieceofdampfilterpaper,andaddtothedish 4
NOTE 4—High-alumina sands are generally mixtures of quartz and
containing the precipitate for ignition.
aluminum silicates of the feldspar group. Some of these silicates can
10.3 Evaporate the filtrate to dryness on the steam bath or
contain barium. If a fine, white, insoluble precipitate persists, it is
under an infrared lamp.When dry, cool, drench with 10 mLof
probably barium sulfate. In this case, partially neutralize the HCl until the
HCl (1+1), and again evaporate just to dryness; then bake in
solution is about 1 to 2% acid, add about ten drops of H SO (1+1) and
2 4
a drying oven at 105°C for 30 min. Cool, drench with 5 mLof
boil gently for about 30 min. Cool, and after 1 to 2 h, filter the solution
HCl, and add 20 mLof hot water and a small bit of filter pulp.
through a fine paper. The precipitate may be ignited and weighed and
subsequently tested for barium. If the precipitate is not barium sulfate, it
Digesthotfor5minandfilterthrougha7-cmfinepaper.Police
should be tested for silica. If the precipitate is neither of these, it can be
thedishwiththeaidofabitofpaperpulpandwashprecipitate
considered R O and added to the R O found by ammonia precipitation.
2 3 2 3
andpapereighttimeswithhot2%HCl.Transferthepaperand
precipitate to the dish containing the initial precipitation.Wipe
11.2.2 If the expected R O is about 10 mg, dilute the
2 3
the stirring rod and the periphery of the funnel with a piece of
sample to about 75 to 100 mL; if much larger, dilute to about
dampfilterpaper,andaddtothedishcontainingtheprecipitate
200 to 250 mL. Add approximately2gofNH Cl, heat to
for ignition.
boiling,addthreetofourdropsofmethylredindicatorsolution
10.4 Partially cover the dish with its platinum lid, but leave
and precipitate the R O with the addition of NH OH (1+1).
2 3 4
enoughspacesoaircancirculateduringignition.Placethedish
Add the NH OH slowly, stirring to obtain a sharp end point;
in a cold muffle furnace, and bring the temperature to 1200°C
finally add about four drops in excess for small amounts of
for 30 min. Carefully and completely cover the dish before
precipitate and up to eight drops for large amounts. Boil the
removing it from the furnace and transfer to a desiccator. Cool
solutionforabout2minandfilterthroughacoarsepaper;there
toroomtemperatureandweighthecovereddish(W ).Moisten
1 is no
...
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