Standard Test Methods for Analysis of Aluminum Silicate Pigment

SIGNIFICANCE AND USE
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-Sep-2003
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ASTM D718-86(2003) - Standard Test Methods for Analysis of Aluminum Silicate Pigment
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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(Reapproved2003)
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 4.2 Electric furnace (or gas burner), capable of 1050 to
1100°C.
1.1 These test methods cover the analysis of aluminum
4.3 Volumetric flask, 100 and 250 mL.
silicate pigment.
4.4 Colorimeter, with transmission range from 400 to 550
1.2 The values stated in SI units are to be regarded as the
nm.
standard. The values given in parentheses are for information
4.5 High Silica Crucible.
only.
1.3 This standard does not purport to address the safety
5. Purity of Reagents
concerns associated with its use. It is the responsibility of the
5.1 Reagent grade chemicals shall be used in all tests.
user of this standard to establish appropriate safety and health
Unless otherwise indicated, it is intended that all reagents shall
practices and determine the applicability of regulatory limita-
conform to the specifications of the Committee on Analytical
tions prior to use.
Reagents of the American Chemical Society, where such
2. Referenced Documents specifications are available. Other grades may be used, pro-
vided it is first ascertained that the reagent is of sufficiently
2.1 ASTM Standards:
high purity to permit its use without lessening the accuracy of
D 234 Specification for Raw Linseed Oil
the determination.
D 280 Test Methods for Hygroscopic Moisture (and Other
5.2 Unless otherwise indicated, references to water shall be
Matter Volatile Under the Test Conditions) in Pigments
understood to mean Type II of Specification D 1193.
D 717 Test Methods for Analysis of Magnesium Silicate
Pigment
SILICON DIOXIDE
D 1193 Specification for Reagent Water
D 1208 Test Methods for Common Properties of Certain
6. Procedure
Pigments
6.1 Determine the silicon dioxide content in accordance
D 2448 Test Method forWater-Soluble Salts in Pigments by
with Test Methods D 717.
Measuring the Specific Resistance of the Leachate of the
Pigment
ALUMINUM OXIDE
E 11 Specification for Wire Cloth and Sieves for Testing
7. Reagents
Purposes
7.1 Ammonium Acetate (20 %)—Dissolve 200 g of ammo-
3. Significance and Use
nium acetate (NH C H O ) in 1 L of distilled water.
4 2 3 2
3.1 These test methods may be used to confirm the stated
7.2 Ammonium Chloride Solution (20 g/L)—Dissolve 20 g
aluminum oxide and SiO content of aluminum silicate for
of ammonium chloride (NH Cl) in water and dilute to 1 L.
quality control.
7.3 Ammonium Hydroxide (sp gr 0.90)—Concentrated am-
monium hydroxide (NH OH).
4. Apparatus
7.4 Diphenylamine Indicator Solution (1 g/100 mL)—
4.1 Platinum Crucible.
Dissolve1gof diphenylamine in 100 mL of concentrated
sulfuric acid (H SO , sp gr 1.84).
2 4
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. Reagent Chemicals, American Chemical Society Specifications, American
Current edition approved Oct. 1, 2003. Published October 2003. Originally Chemical Society, Washington, DC. For suggestions on the testing of reagents not
approved in 1943. Last previous edition approved in 1986 as D 718 – 86 (1999). 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 International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D718–86 (2003)
7.5 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro- hot HCl (1+3), dilute to 100 mL, and precipitate again as
chloric acid (HCl). described in 8.2. After filtering, wash the precipitate ten times
7.6 Hydrochloric Acid (1+3)—Mix 1 volume of concen- with small portions of hot NH Cl solution. Transfer the
trated HCl (sp gr 1.19) with 3 volumes of water. precipitate to a weighed platinum crucible, heat slowly until
7.7 Hydrofluoric Acid (48 %)—Concentrated hydrofluoric the paper is charred, and finally ignite to constant weight at
acid (HF). 1050 to 1100°C in an electric furnace or over a burner, taking
7.8 Hydrogen Peroxide (H O , 3 %, freshly prepared)— care to avoid reduction. Weigh the precipitate as Al O +TiO
2 2 2 3
Mix 1 volume of H O (30 %) with 9 volumes of distilled 2+Fe O .
2 2 2 3
water.
8.4 Fuse the combined oxides from 8.3 with 9 to 10 g of
7.9 Hydroxylamine Hydrochloride (10 %)—Dissolve 10 g
K S O in a platinum crucible, starting at low temperature and
2 7
of NH OH · HCl in 100 mL of distilled water. Prepare fresh
2 increasing the heat gradually until the oxides have all dis-
weekly.
solved. Take up the melt with 5 mLof 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
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
2 2 7
volume with H SO (1+9) and mix well. Obtain the colorimet-
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-
3 4
on the same instrument.
phoric acid.
8.6 Determine the percent of Fe O as follows: Pipet a
2 3
7.15 Potassium Pyrosulfate (K S O ).
2 2 7
25-mL aliquot into a 100-mL volumetric flask. Add the
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 mLof 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 mLof concentrated
3 2
congo red paper into a ball and introduce into the flask. Add
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 carefull
...

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