Standard Test Methods for Analysis of Aluminum Silicate Pigment

SCOPE
1.1 These test methods cover the analysis of aluminum silicate pigment.  
1.2 This standard does not purport to address the safety problems 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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09-Jul-1999
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ASTM D718-86(1999) - Standard Test Methods for Analysis of Aluminum Silicate Pigment
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 718 – 86 (Reapproved 1999)
Standard Test Methods for
Analysis of Aluminum Silicate Pigment
This standard is issued under the fixed designation D 718; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 5. Purity of Reagents
1.1 These test methods cover the analysis of aluminum 5.1 Reagent grade chemicals shall be used in all tests.
silicate pigment. Unless otherwise indicated, it is intended that all reagents shall
1.2 This standard does not purport to address the safety conform to the specifications of the Committee on Analytical
concerns associated with its use. It is the responsibility of the Reagents of the American Chemical Society, where such
user of this standard to establish appropriate safety and health specifications are available. Other grades may be used, pro-
practices and determine the applicability of regulatory limita- vided it is first ascertained that the reagent is of sufficiently
tions prior to use. high purity to permit its use without lessening the accuracy of
the determination.
2. Referenced Documents
5.2 Unless otherwise indicated, references to water shall be
2.1 ASTM Standards:
understood to mean Type II of Specification D 1193.
D 234 Specification for Raw Linseed Oil
SILICON DIOXIDE
D 280 Test Methods for Hygroscopic Moisture (and Other
Matter Volatile Under the Test Conditions) in Pigments
6. Procedure
D 717 Test Methods for Analysis of Magnesium Silicate
2 6.1 Determine the silicon dioxide content in accordance
Pigment
3 with Test Methods D 717.
D 1193 Specification for Reagent Water
D 1208 Test Methods for Common Properties of Certain
ALUMINUM OXIDE
Pigments
D 2448 Test Methods for Water-Soluble Salts in Pigments
7. Reagents
by Measuring the Specific Resistance of the Leachate of
7.1 Ammonium Acetate (20 %)—Dissolve 200 g of ammo-
the Pigment
nium acetate (NH C H O ) in 1 L of distilled water.
4 2 3 2
E 11 Specification for Wire-Cloth Sieves for Testing Pur-
7.2 Ammonium Chloride Solution (20 g/L)—Dissolve 20 g
poses
of ammonium chloride (NH Cl) in water and dilute to 1 L.
7.3 Ammonium Hydroxide (sp gr 0.90)—Concentrated am-
3. Significance and Use
monium hydroxide (NH OH).
3.1 These test methods may be used to confirm the stated
7.4 Diphenylamine Indicator Solution (1 g/100 mL)—
aluminum oxide and SiO content of aluminum silicate for
Dissolve1gof diphenylamine in 100 mL of concentrated
quality control.
sulfuric acid (H SO , sp gr 1.84).
2 4
7.5 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
4. Apparatus
chloric acid (HCl).
4.1 Platinum Crucible.
7.6 Hydrochloric Acid (1+3)—Mix 1 volume of concen-
4.2 Electric furnace (or gas burner), capable of 1050 to
trated HCl (sp gr 1.19) with 3 volumes of water.
1100°C.
7.7 Hydrofluoric Acid (48 %)—Concentrated hydrofluoric
4.3 Volumetric flask, 100 and 250 mL.
acid (HF).
4.4 Colorimeter, with transmission range from 400 to 550
7.8 Hydrogen Peroxide (H O , 3 %, freshly prepared)—
2 2
nm.
Mix 1 volume of H O (30 %) with 9 volumes of distilled
2 2
4.5 High Silica Crucible.
water.
7.9 Hydroxylamine Hydrochloride (10 %)—Dissolve 10 g
These test methods are under the jurisdiction of ASTM Committee D-1 on Paint
and Related Coatings, Materials, and Applications and are the direct responsibility
of Subcommittee D01.31 on Pigment Specifications. Reagent Chemicals, American Chemical Society Specifications, American
Current edition approved April 25, 1986. Published June 1986. Originally Chemical Society, Washington, DC. For suggestions on the testing of reagents not
e1
published as D 718 – 43. Last previous edition D 718 – 73 (1979) . listed by the American Chemical Society, see Analar Standards for Laboratory
Annual Book of ASTM Standards, Vol 06.03. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 11.01. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 14.02. MD.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 718
of NH OH · HCl in 100 mL of distilled water. Prepare fresh increasing the heat gradually until the oxides have all dis-
weekly. solved. Take up the melt with 5 mL of H SO (1+1) in 150 mL
2 4
7.10 Iron Standard—Dissolve 0.1 g of analytical grade iron of water and warm to effect solution. Transfer the solution to a
wire in 10 mL of HCl (1+1) and dilute to 1 L. Each millilitre 250-mL volumetric flask, dilute to volume, and mix well.
contains 0.1 mg of Fe. Reserve for TiO and Fe O determinations.
2 2 3
7.11 Mercuric Chloride Solution (HgCl ), saturated. 8.5 Determine the percent of TiO as follows: Pipet an
2 2
7.12 Methyl Red Indicator Solution— Dissolve 0.2 g of aliquot containing 0.2 to 3.0 mg of TiO into a 100-mL
methyl red in 100 mL of methanol, ethanol, or isopropanol. volumetric flask. For samples containing 0.5 to 3 % TiO ,a
7.13 Potassium Dichromate, Standard Solution (0.05 N)— 20-mL aliquot is suitable. Add 5 mL of H O (3 %), dilute to
2 2
Dissolve 2.457 g of potassium dichromate (K Cr O ) in water volume with H SO (1+9) and mix well. Obtain the colorimet-
2 2 7 2 4
and dilute to 1 L. Standardize against National Bureau of ric reading in a suitable colorimeter using a filter with
Standards’ standard sample No. 27b of Sibley iron ore, using transmission limits of 400 to 450 nm or at 410 nm with a prism
such an amount as to give approximately the same titration as or grating spectrometer. Compare the readings to a curve
the sample to be analyzed. plotted from a set of TiO standards similarly treated and read
7.14 Phosphoric Acid (H PO , 85 %)—Concentrated phos- on the same instrument.
3 4
phoric acid. 8.6 Determine the percent of Fe O as follows: Pipet a
2 3
7.15 Potassium Pyrosulfate (K S O ). 25-mL aliquot into a 100-mL volumetric flask. Add the
2 2 7
7.16 o-Phenanthroline (0.1 %)—Dissolve 1.0 g of following in the order given, mixing well after each addition:
o-phenanthroline in 1 L of hot distilled water. 2mLofNH OH · HCl (10 %), 10 mL of NH C H O (20 %),
2 4 2 3 2
7.17 Stannous Chloride Solution (5 g/100 mL)—Dissolve 5
and 10 mL of o-phenanthroline (0.1 %). Roll a small piece of
g of stannous chloride (SnCl ,2H O) in 10 mL of concentrated congo red paper into a ball and introduce into the flask. Add
3 2
HCl (sp gr 1.19) and dilute to 100 mL with water. Add scraps
concentrated NH OH dropwise until indicator turns red and 1
of iron-free granulated tin, and boil until the solution is clear. drop in excess. Dilute to volume and let stand for 10 to 20 min.
Keep the solution in a closed dropping bottle containing
Obtain the colorimetric reading in a suitable colorimeter using
metallic tin. a filter with transmission limits 485 to 550 nm, or at 510 nm
7.18 Sulfuric Acid (1+1)—Add carefully 1 volume of con-
with a prism or grating spectrometer. Compare the readings to
centrated sulfuric acid (H SO , sp gr 1.84) to 1 volume of a curve plotted from a set of Fe O standards similarly treated
2 4 2 3
distilled water. and read on the same instrument.
7.19 Sulfuric Acid (1+9)—Add carefully 1 volume of con- 8.7 Alternatively the Fe O may be determined by titration
2 3
centrated H SO (sp gr 1.84) to 9 volumes of distilled water.
as follows: Fuse1gof sample with 10 g of K S O in a
2 4
2 2 7
high-silica crucible starting at low temperature and increasing
8. Procedure
the heat gradually until the crucible glows with a dull red color
8.1 If an
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