Standard Test Methods for Analysis of Aluminum Silicate Pigment

SIGNIFICANCE AND USE
3.1 These test methods may be used to confirm the stated aluminum oxide and SiO2 content of aluminum silicate for quality control.
SCOPE
1.1 These test methods cover the analysis of aluminum silicate pigment.  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.3 This standard does not purport to address the safety concerns 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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Publication Date
30-Nov-2014
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D718 − 86 (Reapproved 2014)
Standard Test Methods for
Analysis of Aluminum Silicate Pigment
This standard is issued under the fixed designation D718; 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.
1. Scope 4. Apparatus
1.1 These test methods cover the analysis of aluminum 4.1 Platinum Crucible.
silicate pigment.
4.2 Electric furnace (or gas burner), capable of 1050 to
1.2 The values stated in SI units are to be regarded as the 1100°C.
standard. The values given in parentheses are for information
4.3 Volumetric flask, 100 and 250 mL.
only.
4.4 Colorimeter, with transmission range from 400 to 550
1.3 This standard does not purport to address the safety
nm.
concerns associated with its use. It is the responsibility of the
4.5 High Silica Crucible.
user of this standard to establish appropriate safety and health
practices and determine the applicability of regulatory limita-
5. Purity of Reagents
tions prior to use.
5.1 Reagent grade chemicals shall be used in all tests.
2. Referenced Documents Unless otherwise indicated, it is intended that all reagents shall
conform to the specifications of the Committee on Analytical
2.1 ASTM Standards:
3 Reagents of the American Chemical Society, where such
D234 Specification for Raw Linseed Oil (Withdrawn 2007)
specifications are available. Other grades may be used, pro-
D280 Test Methods for Hygroscopic Moisture (and Other
vided it is first ascertained that the reagent is of sufficiently
Matter Volatile Under the Test Conditions) in Pigments
high purity to permit its use without lessening the accuracy of
D717 Test Methods for Analysis of Magnesium Silicate
the determination.
Pigment
D1193 Specification for Reagent Water
5.2 Unless otherwise indicated, references to water shall be
D1208 Test Methods for Common Properties of Certain understood to mean Type II of Specification D1193.
Pigments
SILICON DIOXIDE
D2448 Test Method for Water-Soluble Salts in Pigments by
Measuring the Specific Resistance of the Leachate of the
6. Procedure
Pigment
6.1 Determine the silicon dioxide content in accordance
E11 Specification for Woven Wire Test Sieve Cloth and Test
with Test Methods D717.
Sieves
ALUMINUM OXIDE
3. Significance and Use
3.1 These test methods may be used to confirm the stated 7. Reagents
aluminum oxide and SiO content of aluminum silicate for
7.1 Ammonium Acetate (20 %)—Dissolve 200 g of ammo-
quality control.
nium acetate (NH C H O ) in 1 L of distilled water.
4 2 3 2
7.2 Ammonium Chloride Solution (20 g/L)—Dissolve 20 g
These test methods are under the jurisdiction of ASTM Committee D01 on
of ammonium chloride (NH Cl) in water and dilute to 1 L.
Paint and Related Coatings, Materials, and Applications and are the direct
7.3 Ammonium Hydroxide (sp gr 0.90—Concentrated am-
responsibility of Subcommittee D01.31 on Pigment Specifications.
Current edition approved Dec. 1, 2014. Published December 2014. Originally
monium hydroxide (NH OH).
approved in 1943. Last previous edition approved in 2008 as D718 – 86 (2008).
DOI: 10.1520/D0718-86R14.
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Reagent Chemicals, American Chemical Society Specifications, American
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Standards volume information, refer to the standard’s Document Summary page on listed by the American Chemical Society, see Analar Standards for Laboratory
the ASTM website. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
The last approved version of this historical standard is referenced on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
www.astm.org. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D718 − 86 (2014)
7.4 Diphenylamine Indicator Solution (1 g/100 mL)— mL of HCl, add a few drops of methyl red indicator solution,
Dissolve1gof diphenylamine in 100 mL of concentrated and heat to boiling. Add concentrated NH OH (sp gr 0.90)
sulfuric acid (H SO , sp gr 1.84). dropwise until 1 drop changes the color of the solution to a
2 4
distinct yellow. Reheat the solution containing the precipitated
7.5 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
hydroxides to boiling, boil for 1 or 2 min, and filter. Wash the
chloric acid (HCl).
precipitate once by decantation and then slightly on the filter
7.6 Hydrochloric Acid (1+3)—Mix 1 volume of concen-
with hot NH Cl.
trated HCl (sp gr 1.19) with 3 volumes of water.
8.3 Transfer the precipitate and paper to the original beaker
7.7 Hydrofluoric Acid (48 %)—Concentrated hydrofluoric
inwhichtheprecipitationwasmade.Dissolvetheprecipitatein
acid (HF).
hot HCl (1+3), dilute to 100 mL, and precipitate again as
described in 8.2. After filtering, wash the precipitate ten times
7.8 Hydrogen Peroxide (H O , 3 %, freshly prepared)—
2 2
Mix 1 volume of H O (30 %) with 9 volumes of distilled with small portions of hot NH Cl solution. Transfer the
2 2 4
precipitate to a weighed platinum crucible, heat slowly until
water.
the paper is charred, and finally ignite to constant weight at
7.9 Hydroxylamine Hydrochloride (10 %)—Dissolve 10 g
1050 to 1100°C in an electric furnace or over a burner, taking
of NH OH · HCl in 100 mL of distilled water. Prepare fresh
care to avoid reduction. Weigh the precipitate as
weekly.
Al O +TiO +Fe O .
2 3 2 2 3
7.10 Iron Standard—Dissolve 0.1 g of analytical grade iron
8.4 Fuse the combined oxides from 8.3with9to10gof
wire in 10 mL of HCl (1+1) and dilute to 1 L. Each millilitre
K S O in a platinum crucible, starting at low temperature and
2 2 7
contains 0.1 mg of Fe.
increasing the heat gradually until the oxides have all dis-
7.11 Mercuric Chloride Solution (HgCl ), saturated.
solved. Take up the melt with 5 mLof H SO (1+1) in 150 mL
2 4
7.12 Methyl Red Indicator Solution—Dissolve 0.2 g of of water and warm to effect solution. Transfer the solution to a
250-mL volumetric flask, dilute to volume, and mix well.
methyl red in 100 mL of methanol, ethanol, or isopropanol.
Reserve for TiO and Fe O determinations.
2 2 3
7.13 Potassium Dichromate, Standard Solution (0.05 N
8.5 Determine the percent of TiO as follows: Pipet an
)—Dissolve 2.457 g of potassium dichromate (K Cr O)in
2 2 7 2
water and dilute to 1 L. Standardize against National Bureau of aliquot containing 0.2 to 3.0 mg of TiO into a 100-mL
volumetric flask. For samples containing 0.5 to 3 % TiO,a
Standards’ standard sample No. 27b of Sibley iron ore, using
such an amount as to give approximately the same titration as 20-mL aliquot is suitable. Add 5 mL of H O (3 %), dilute to
2 2
volume with H SO (1+9) and mix well. Obtain the colorimet-
the sample to be analyzed.
2 4
ric reading in a suitable colorimeter using a filter with
7.14 Phosphoric Acid (H PO , 85 %)—Concentrated phos-
3 4
transmission limits of 400 to 450 nm or at 410 nm with a prism
phoric acid.
or grating spectrometer. Compare the readings to a curve
7.15 Potassium Pyrosulfate (K S O ).
2 2 7
plotted from a set of TiO standards similarly treated and read
7.16 o-Phenanthroline (0.1 %)—Dissolve 1.0 g of on the same instrument.
o-phenanthroline in 1 L of hot distilled water.
8.6 Determine the percent of Fe O as follows: Pipet a
2 3
7.17 Stannous Chloride Solution (5 g/100 mL)—Dissolve 5 25-mL aliquot into a 100-mL volumetric flask. Add the
following in the order given, mixing well after each addition:
g of stannous chloride (SnCl ,2H O) in 10 mLof concentrated
3 2
HCl (sp gr 1.19) and dilute to 100 mL with water. Add scraps 2mLofNH OH · HCl (10 %), 10 mL of NH C H O (20 %),
2 4 2 3 2
and 10 mL of o-
...


This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D718 − 86 (Reapproved 2008) D718 − 86 (Reapproved 2014)
Standard Test Methods for
Analysis of Aluminum Silicate Pigment
This standard is issued under the fixed designation D718; 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.
1. Scope
1.1 These test methods cover the analysis of aluminum silicate pigment.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 This standard does not purport to address the safety concerns 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.
2. Referenced Documents
2.1 ASTM Standards:
D234 Specification for Raw Linseed Oil (Withdrawn 2007)
D280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments
D717 Test Methods for Analysis of Magnesium Silicate Pigment
D1193 Specification for Reagent Water
D1208 Test Methods for Common Properties of Certain Pigments
D2448 Test Method for Water-Soluble Salts in Pigments by Measuring the Specific Resistance of the Leachate of the Pigment
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
3. Significance and Use
3.1 These test methods may be used to confirm the stated aluminum oxide and SiO content of aluminum silicate for quality
control.
4. Apparatus
4.1 Platinum Crucible.
4.2 Electric furnace (or gas burner), capable of 1050 to 1100°C.
4.3 Volumetric flask, 100 and 250 mL.
4.4 Colorimeter, with transmission range from 400 to 550 nm.
4.5 High Silica Crucible.
5. Purity of Reagents
5.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform
to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are
available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use
without lessening the accuracy of the determination.
These test methods are under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and are the direct responsibility of
Subcommittee D01.31 on Pigment Specifications.
Current edition approved Feb. 1, 2008Dec. 1, 2014. Published February 2008December 2014. Originally approved in 1943. Last previous edition approved in 20032008
as D718 – 86 (2003).(2008). DOI: 10.1520/D0718-86R08.10.1520/D0718-86R14.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’sstandard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
Reagent Chemicals, American Chemical Society Specifications, American 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 and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D718 − 86 (2014)
5.2 Unless otherwise indicated, references to water shall be understood to mean Type II of Specification D1193.
SILICON DIOXIDE
6. Procedure
6.1 Determine the silicon dioxide content in accordance with Test Methods D717.
ALUMINUM OXIDE
7. Reagents
7.1 Ammonium Acetate (20 %)—Dissolve 200 g of ammonium acetate (NH C H O ) in 1 L of distilled water.
4 2 3 2
7.2 Ammonium Chloride Solution (20 g/L)—Dissolve 20 g of ammonium chloride (NH Cl) in water and dilute to 1 L.
7.3 Ammonium Hydroxide (sp gr 0.90—Concentrated ammonium hydroxide (NH OH).
7.4 Diphenylamine Indicator Solution (1 g/100 mL)—Dissolve 1 g of diphenylamine in 100 mL of concentrated sulfuric acid
(H SO , sp gr 1.84).
2 4
7.5 Hydrochloric Acid (sp gr 1.19)—Concentrated hydrochloric acid (HCl).
7.6 Hydrochloric Acid (1+3)—Mix 1 volume of concentrated HCl (sp gr 1.19) with 3 volumes of water.
7.7 Hydrofluoric Acid (48 %)—Concentrated hydrofluoric acid (HF).
7.8 Hydrogen Peroxide (H O , 3 %, freshly prepared)—Mix 1 volume of H O (30 %) with 9 volumes of distilled water.
2 2 2 2
7.9 Hydroxylamine Hydrochloride (10 %)—Dissolve 10 g of NH OH · HCl in 100 mL of distilled water. Prepare fresh weekly.
7.10 Iron Standard—Dissolve 0.1 g of analytical grade iron wire in 10 mL of HCl (1+1) and dilute to 1 L. Each millilitre
contains 0.1 mg of Fe.
7.11 Mercuric Chloride Solution (HgCl ), saturated.
7.12 Methyl Red Indicator Solution—Dissolve 0.2 g of methyl red in 100 mL of methanol, ethanol, or isopropanol.
7.13 Potassium Dichromate, Standard Solution (0.05 N )—Dissolve 2.457 g of potassium dichromate (K Cr O ) in water and
2 2 7
dilute to 1 L. Standardize against National Bureau of Standards’Standards’ standard sample No. 27b of Sibley iron ore, using such
an amount as to give approximately the same titration as the sample to be analyzed.
7.14 Phosphoric Acid (H PO , 85 %)—Concentrated phosphoric acid.
3 4
7.15 Potassium Pyrosulfate (K S O ).
2 2 7
7.16 o-Phenanthroline (0.1 %)—Dissolve 1.0 g of o-phenanthroline in 1 L of hot distilled water.
7.17 Stannous Chloride Solution (5 g/100 mL)—Dissolve 5 g of stannous chloride (SnCl , 2H O) in 10 mL of concentrated HCl
3 2
(sp gr 1.19) and dilute to 100 mL with water. Add scraps of iron-free granulated tin, and boil until the solution is clear. Keep the
solution in a closed dropping bottle containing metallic tin.
7.18 Sulfuric Acid (1+1)—Add carefully 1 volume of concentrated sulfuric acid (H SO , sp gr 1.84) to 1 volume of distilled
2 4
water.
7.19 Sulfuric Acid (1+9)—Add carefully 1 volume of concentrated H SO (sp gr 1.84) to 9 volumes of distilled water.
2 4
8. Procedure
8.1 If an appreciable residue remains after the treatment with HF in accordance with 7.4 of Test Methods D717, fuse the residue
with a small amount of K S O until it is dissolved. Leach the pyrosulfate melt out of the crucible with water and combine the
2 2 7
solution with the filtrate reserved in accordance with 7.3 or Test Methods D717.
8.2 Bring the volume of the combined solution to 250 mL, and, if necessary, add HCl in order to ensure a total of 10 to 15 mL
of HCl, add a few drops of methyl red indicator solution, and heat to boiling. Add concentrated NH OH (sp gr 0.90) dropwise until
1 drop changes the color of the solution to a distinct yellow. Reheat the solution containing the precipitated hydroxides to boiling,
boil for 1 or 2 min, and filter. Wash the precipitate once by decantation and then slightly on the filter with hot NH Cl.
8.3 Transfer the precipitate and paper to the original beaker in which the precipitation was made. Dissolve the precipitate in hot
HCl (1+3), dilute to 100 mL, and precipitate again as described in 8.2. After filtering, wash the precipitate ten times with small
portions of hot NH Cl solution. Transfer the precipitate to a weighed platinum crucible, heat slowly until the paper is charred, and
finally ignite to constant weight at 1050 to 1100°C in an electric furnace or over a burner, taking care to avoid reduction. Weigh
the precipitate as Al O + TiO + Fe O .
2 3 2 2 3
D718 − 86 (2014)
8.4 Fuse the combined oxides from 8.3 with 9 to 10 g of K S O in a platinum crucible, starting at low temperature and
2 2 7
increasing the heat gradually until the oxid
...

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