ASTM C323-56(2011)

Standard Test Methods for Chemical Analysis of Ceramic Whiteware Clays

ABSTRACT
These test methods cover the chemical analysis of clays used in the manufacture of ceramic whitewares. Determine moisture on the sample in its ordinary air-dried condition. Determine all other percentage compositions on moisture-free samples and report accordingly on a moisture-free basis. Make blank determinations on the reagents for each constituent in the whiteware clay and deduct this blank in each case. The sample shall be heated to a constant weight at a given temperature; the loss in weight is recorded as moisture. For the determination of the silica blank, approximately 0.25 g of alumina should be added as aluminium chloride. The procedure for the determination of iron, aluminium, and titanium oxide blank are presented in details. The procedure for the determination of iron oxide, titania, alumina, lime, magnesia, and alkalies blank are discussed and presented in details.
SCOPE
1.1 These test methods cover the chemical analysis of clays used in the manufacture of ceramic whitewares.
1.2 The analytical procedures appear in the following order:

General Information

• Status: Historical
• Publication Date: 28-Feb-2011
• ICS: 91.100.25 - Terracotta building products
• Technical Committee: C21 - Ceramic Whitewares and Related Products
• Drafting Committee: C21.04 - Raw Materials

Relations

• Replaces: ASTM C323-56(2006) - Standard Test Methods for Chemical Analysis of Ceramic Whiteware Clays
• Effective Date: 01-Mar-2011
• Replaced By: ASTM C323-56(2016) - Standard Test Methods for Chemical Analysis of Ceramic Whiteware Clays (Withdrawn 2024)
• Effective Date: 01-Jul-2016

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: C323 − 56(Reapproved 2011)
Standard Test Methods for
Chemical Analysis of Ceramic Whiteware Clays
This standard is issued under the fixed designation C323; 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 (´) indicates an editorial change since the last revision or reapproval.
Hillebrand and Lundell and to similar publications. Particularly in the
1. Scope
determination of alumina, reference should be made to Scientific Paper
1.1 These test methods cover the chemical analysis of clays
No. 286 of the National Bureau of Standards.
used in the manufacture of ceramic whitewares.
1.3 The values stated in acceptable metric units are to be
1.2 The analytical procedures appear in the following order:
regarded as the standard. The values given in parentheses are
for information only.
Section
Moisture 7
1.4 This standard does not purport to address all of the
Loss on Ignition 8
safety concerns, if any, associated with its use. It is the
Silica 9
Iron, Aluminum, and Titanium Oxides 10
responsibility of the user of this standard to establish appro-
Iron Oxide 11
priate safety and health practices and determine the applica-
Titania 12
Alumina 13 bility of regulatory limitations prior to use.
Lime 14
Magnesia 15
2. Referenced Documents
Alkalies 16
2.1 ASTM Standards:
NOTE 1—These test methods have been compiled as standard proce-
C322 Practice for Sampling Ceramic Whiteware Clays
dures for use in referee analyses. These test methods, however, when the
E11 Specification for Woven Wire Test Sieve Cloth and Test
determination of iron oxide as Fe O is involved, are not intended to
2 3
Sieves
preclude the use of other procedures that give results within the permis-
sible variations. For the sake of uniformity the classical Zimmerman-
3. Reagents
Reinhardt procedure is specified for the determination of iron oxide. It is
recognized that numerous other procedures are equally accurate and often
3.1 Unless otherwise indicated, it is intended that all re-
more convenient. The other procedures commonly in use include reduc-
agents shall conform to the specifications of the Committee on
tion of an oxidized solution with zinc or other metal, and titration with
Analytical Reagents of theAmerican Chemical Society, where
standard potassium permanganate (KMnO ) or potassium dichromate
(K Cr O )solution,aswellastitrationwithastandardsolutionoftitanous
such specifications are available. Other grades may be used,
2 2 7
chloride in an oxidized solution. These procedures shall be considered
provided it is first ascertained that the reagent is of sufficiently
acceptable, provided the analyst has obtained results by his special
high purity to permit its use without lessening the accuracy of
procedurethatcheckwiththeZimmerman-Reinhardtprocedurewithinthe
the determination. Unless otherwise indicated, references to
limits specified in Section 17. It is suggested that National Institute of
Standards and Technology standard samples be used for checking the water shall be understood to mean distilled water. Paragraphs
accuracy of procedures.
3.1.1-3.1.16 include those reagents common to two or more of
It will be understood that the making of a complete analysis of a
ceramic whiteware clay is a difficult procedure requiring a wide knowl-
Hillebrand,W. F., and Lundell, G. E. F., Applied Inorganic Analysis,Wiley and
edge of the chemistry involved in the operations and a thorough training
Son, New York, 1929.
in carrying out the work. A skilled analyst of good training is therefore
Blum, W., “Determination of Alumina as Oxide,” National Bureau of
required to do the work.The descriptions here given cover the vital points
Standards, Scientific Paper No. 286.
of procedure, but frequent reference in regard to the details of the various
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
manipulations should be made to “Applied Inorganic Analysis” by
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
1 5
These test methods are under the jurisdiction of ASTM Committee C21 on Reagent Chemicals, American Chemical Society Specifications, American
Ceramic Whitewares and Related Productsand are the direct responsibility of Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Subcommittee C21.04 on Raw Materials. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved March 1, 2011. Published March 2011. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
approved in 1956. Last previous edition approved in 2006 as C323 - 56 (2006). and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
DOI: 10.1520/C0323-56R11. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C323 − 56 (2011)
the analytical procedures. Other reagents will be found listed porous glass, or porcelain filter, and keep in a dark place.
with the particular test method in which they are prescribed. Standardize against the National Institute of Standards and
3.1.1 Concentrated Acids and Ammonium Hydroxide— Technology standard Sample No. 40c of sodium oxalate.
Concentrated acids and ammonium hydroxide of approxi- 3.1.13 Potassium Permanganate, Standard Solution
mately the following specific gravities or concentrations will
(0.04N)—Dissolve 2.5 g of KMnO in water and make up to 2
be required: L.Allow to stand for one week, filter through an asbestos mat,
porous glass, or porcelain filter, and keep in a dark place.
Hydrochloric acid (HCl) 1.19 sp gr
Nitric acid (HNO ) 1.42spgr
3 Standardize against the National Institute of Standards and
Sulfuric acid (H SO ) 1.84spgr
2 4
Technology standard Sample No. 40c of sodium oxalate.
Hydrofluoric acid (HF) 40 %
A
3.1.14 Sodium Arsenite, Standard Solution— Dissolve
Perchloric acid (HClO ) 60to70%,cp
B
Sulfurous acid (H SO ) 6 % solution
2 3
0.908 g of arsenious oxide, (As O ), in a small amount of hot
2 3
Ammonium hydroxide (NH OH) 0.90 sp gr
sodium carbonate (Na CO ) solution, cool, filter, and dilute to
2 3
___________
A 1 L. Standardize against a steel of known manganese content.
Lower purity varieties may contain aluminum oxide, (Al O ), as an impurity.
2 3
B
As supplied by reagent manufacturers.
3.1.15 Stannous Chloride Solution (50 g/L)—Dissolve 50 g
of SnCl in 100 mLof HCl and dilute to 1000 mL. Keep a few
3.1.2 DilutedAcidsandAmmoniumHydroxide—Thediluted
pieces of metallic tin in the bottle.
acids and ammonium hydroxide referred to are of varying
3.1.16 Titania, Standard Solution—Weigh out 0.05 g of
percentages by volume. They shall be made up by mixing
calcined titanium dioxide (TiO ). Fuse with 10 g of K S O in
2 2 2 7
proportional volumes of the concentrated reagent and water.
a clean platinum crucible, keeping the temperature as low as
The diluted sulfuric acid mixtures shall be made up by slowly
possible to maintain fluidity. Cool, and dissolve in about 300
stirring the acid into the water. These diluted acids and
mL of H SO (1 + 5). Cool, transfer to a 500-mL volumetric
2 4
ammoniumhydroxidearedesignatedinthemethodsas(1 + 4),
flask, dilute to the mark with water, and mix thoroughly. To
(1 + 9), and so forth, except very diluted solutions which are
standardize the solution, take two 50-mL portions in 400-mL
referred to by the percent of reagent added. The designation in
beakers, dilute, boil, and precipitate with NH OH. Filter, and
parentheses indicates the ratio of the volume of the concen-
wash with hot water. Place the papers in the original beakers,
trated reagent to the volume of water; for example, H SO
2 4
add 15 mL of HCl, stir to macerate the paper, dilute, and
(1 + 9) contains 10 volume % of H SO (sp gr 1.84). The
2 4
precipitate again with NH OH. Filter, and wash with hot water
following will be required:
untilfreeofalkalisalts.Ignitecarefully,blast,andweigh.From
Volume %
the weight determined, calculate the strength of the solution.
HCl 50
H SO 50
2 4
4. Sampling
4.1 Selection of Sample—Obtain the sample in accordance
HNO 30
with Practice C322.
NH OH 50
4.2 Crushthesampleinasmalljaworroll-typecrusherwith
hardenedtool-steelfacestopassa2.36-mm(No.8)sieve(Note
3.1.3 Ammonium Chloride (2 %) —Dissolve2gofNH Cl
2). Crush the sample to pass a 850-µm (No. 20) sieve, mix, and
in 100 mL of water.
quarter to about 50 g. Grind this 50-g sample so that it will all
3.1.4 Ammonium Oxalate Solution (Saturated)—Dissolve 4
pass a 150-µm (No. 100) sieve, unless otherwise specified, mix
gof(NH ) C O in 100 mL of water.
4 2 2
thoroughly, and place in a container that will ensure freedom
3.1.5 Chloroplatinic Acid Solution (10 %).
from contamination. Do fine grinding in a suitable mortar
3.1.6 Diammonium Phosphate Solution—Dissolve 10 g of
(agate, mullite, alumina, or boron carbide) to prevent the
(NH ) HPO in 100 mL of water.
4 2 4
introduction of impurities. Take precautions to prevent con-
3.1.7 Ethyl Alcohol (80 %) —Prepare a solution containing
tamination of the sample by steel particles from the sampling
80 volume % of ethyl alcohol in water.
equipment during crushing or grinding.
3.1.8 Ethyl Alcohol (Absolute)—Certain commercial brands
NOTE 2—Detailed requirements for these sieves are given in Specifi-
of denatured absolute alcohol are satisfactory as well as being
cation E11.
considerably less expensive than the reagent grade absolute
alcohol.
5. Method of Analysis
3.1.9 Hydrogen Peroxide (30 %) (H O ).
2 2
3.1.10 Manganese Sulfate Solution—Dissolve 70 g of crys- 5.1 Determine moisture on the sample in its ordinary
talline MnSO in 500 mLof water.Add 140 mLof phosphoric
air-dried condition. Determine all other percentage composi-
acid (H PO , sp gr 1.7), and 130 mL of sulfuric acid (H SO , tions on moisture-free samples and report accordingly on a
3 4 2 4
sp gr 1.84). Dilute to 1 L.
moisture-free basis. The drying temperature recommended for
3.1.11 Mercuric Chloride Solution (Saturated)—Prepare a all moisture determinations is 105 to 110°C. Whenever a
saturated solution of HgCl .
sample is weighed out for any determination other than
3.1.12 Potassium Permanganate, Standard Solution moisture,itshallbemoisture-free.Ifpreferred,thesamplemay
(0.1N)—Dissolve 3.25 g of KMnO in 1000 mL of water. be dried in a weighing bottle from which the required samples
Allow to stand for one week, filter through an asbestos mat, shall be weighed out.
C323 − 56 (2011)
6. Blank Determinations 10. Iron, Aluminum, and Titanium Oxides
6.1 Make blank determinations on the reagents for each 10.1 Fuse the residue with1gof fused potassium pyrosul-
constituent in the whiteware clay and deduct this blank in each fate (K S O ) or sodium pyrophosphate (Na S O ), dissolve in
2 2 7 2 2 7
case. For the determination of the silica (SiO ) blank, approxi- a small amount of water, and add to the filtrate from the silica
mately 0.25 g ofAl O should be added as aluminum chloride. determination (Section 9).Add5gofNH Cl and three drops
2 3 4
of 0.1 % methyl red solution. Heat the solution almost to
7. Moisture
boiling, and add slowly NH OH (1 + 1) until the indicator has
changed to a yellow color. Boil for several minutes to remove
7.1 Weigh 1.00 g of the sample and heat to constant weight
the excess ammonia. Allow to settle for 30 min and decant
at a temperature not under 105 nor over 110°C. Record the loss
through an open, rapid-filtering acid-washed filter paper, trans-
in weight as moisture.
ferring the precipitate to the paper and washing the beaker and
8. Loss on Ignition
paper several times with a warm 2 % NH Cl solution. Reserve
the filtrate, “A,” for the determination of calcium oxide (CaO)
8.1 Weigh 1.000 g of the moisture-free (105 to 110°C)
and magnesium oxide (MgO) (Section 14). Return the precipi-
sample and heat to constant weight over a blast lamp, or in an
tate and paper to the original beaker, add 50 mL of hot water
electric muffle furnace, at 900 to 1000°C. Record the loss in
and 10 mL of HCl (sp gr 1.19). Stir until the precipitate is
weight as the ignition loss.
dissolved and the paper is well macerated. Dilute to about 200
mL with hot water, precipitate and filter as before. Combine
9. Silica
this filtrate “B” with filtrate “A.” Wash the paper and precipi-
9.1 Weigh 0.5000 g of the moisture-free (105 to 110°C)
tate with a warm 2 % NH Cl solution. Place the precipitate in
sample into a platinum crucible containing about5gof
a weighed platinum crucible and ignite. Continue the ignition
powdered anhydrous Na CO and mix well with a platinum
2 3
at 1200°C to constant weight (15 to 20 min is usually
wire. Cover the mixture with a little more Na CO . Heat
2 3
sufficient). Cool in a desiccator, and weigh with the crucible
gradually to the full heat of a good burner (1000 to 1100°C)
covered with the lid.The R O consists of the aluminum oxide
2 3
maintained for about 1 h until complete solution is obtained.
(Al O ), TiO , and Fe O present in the sample. In addition,
2 3 2 2 3
Place the crucible cover on a triangle, and when the melt has
there may be small amounts of phosphoric anhydride (P O ),
2 5
partially cooled, pour it on the lid (Note 3). When cool, place
zirconium oxide (ZrO ), vanadium pentoxide (V O ), and
2 2 5
the crucible and lid in a 150-mL beaker, placing the button on
chromic oxide (Cr O ).
2 3
a watch glass above the beaker. Add 30 mL of HCl (1 + 1).
When solution is complete wash off the crucible and lid with
11. Iron Oxide
HCl (1 + 4), taking care to remove all SiO . Place the button in
11.1 Procedure A: Fe O Determined on R O Sample—
the solution. Transfer the contents of the beaker to an evapo- 2 3 2 3
Heat the R O precipitate (Note 4) obtained in the determina-
rating dish and evaporate to dryness on a steam bath. Bake for 2 3
tion of iron, aluminum, and titanium oxides (Section 10), with
1hat110°C.Add20to30mLofHCl(1 + 1)and50mLofhot
fused K S O or Na S O until solution is complete. Dissolve
water. When all salts have been dissolved, allow to settle for 2 2 7 2 2 7
the fusion in 50 mL of H SO (1 + 9) and evaporate to fumes.
several minutes and then filter through a general-purpose grade 2 4
Cool, dilute with water, and filter off the SiO , washing with
acid-washed medium-retention filter paper. Wash the SiO 2
hot water. Reserve the filtrate for the determination of Fe O
three times by decantation using 20- to 30-mL portions of first 2 3
an
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