ASTM D4487-90(2003)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D4487–90(Reapproved2003)
Standard Test Methods for
Analysis of Calcium Borosilicate
This standard is issued under the fixed designation D 4487; 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 3. Significance and Use
1.1 These test methods cover the analysis of the pigment 3.1 These test methods compile in one place, recommended
commercially known as calcium borosilicate. procedures for analysis of the pigment known commercially as
1.2 The test methods appear in the following order: calciumborosilicate.Thispigmentisusedextensivelyinpaints
and the composition is important to the user and producer.
Test Methods Sections
Silicon Dioxide (SiO)6-9
Iron Oxide (Fe O ) 10-13
4. Reagents
2 3
Boron Trioxide (B O ) 17-20
2 3
4.1 Purity of Reagents—Reagent grade chemicals shall be
Calcium Oxide (CaO) 21-23
Moisture and Volatile Matter 24
used in all tests. Unless otherwise indicated, it is intended that
Water of Hydration 25 to 26
all reagents shall conform to the specifications of the Commit-
Coarse Particles 27
tee on Analytical Reagents of the American Chemical Society
Oil Absorption 28
where such specifications are available. Other grades may be
1.3 Individual specimens may be used for the direct deter-
used, provided it is first ascertained that the reagent is of
minations of SiO ,B O , and CaO. SiO and Fe O should be
2 2 3 2 2 3
sufficiently high purity to permit its use without lessening the
removed before the determination of the B O and CaO.
2 3
accuracy of the determination.
1.4 The values stated in SI units are to be regarded as the
4.2 Purity of Water—Unless otherwise indicated, references
standard. The values given in parentheses are for information
to water shall be understood to mean reagent water conforming
only.
to Type II of Specification D 1193.
1.5 This standard does not purport to address all of the
4.3 Concentration of Acids and Ammonium Hydroxide—
safety concerns, if any, associated with its use. It is the
When acids and ammonium hydroxide are specified by name
responsibility of the user of this standard to establish appro-
or chemical formula only, it should be understood that concen-
priate safety and health practices and determine the applica-
trated reagents of the following specific gravity are intended:
bility of regulatory limitations prior to use.
Hydrochloric acid (HCl) 1.19
Nitric acid, (HNO ) 1.42
2. Referenced Documents
Sulfuric acid (H SO ) 1.84
2 4
Ammonium hydroxide (NH OH) 0.90
2.1 ASTM Standards: 4
D 185 Test Methods for Coarse Particles in Pigments,
5. Preparation of Samples
Pastes, and Paints
5.1 Thoroughly mix and comminute the sample before
D 280 Test Methods for Hygroscopic Moisture (and Other
taking portions for analysis.
Matter Volatile Under the Test Conditions) in Pigments
D 281 Test Method for Oil Absorption of Pigments by
SILICON DIOXIDE
Spatula Rub-Out
D 1193 Specification for Reagent Water
6. Apparatus
6.1 Evaporating Casserole, 250-mL capacity.
6.2 Hot Plate.
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 Dec. 1, 2003. Published December 2003. Originally Reagent Chemicals, American Chemical Society Specifications, American
approved in 1985. Last previous edition approved in 1990 as D 4487 – 90 (1999). Chemical Society, Washington, DC. For suggestions on the testing of reagents not
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4487–90 (2003)
6.3 Porcelain Filtering Crucible, medium porosity, 30-mL 10°C. Prepare fresh indicator when the end point of the
capacity. titration from blue to colorless fails to be sharp.
6.4 Drying Oven, maintained at 100 6 5°C. 11.4 Sulfuric acid (H SO ) (1+18).
2 4
6.5 Muffle Furnace. 11.5 Sodium Thiosulfate, Standard Solution (0.025 N)—
Dissolve 1.5 g of sodium thiosulfate (Na S O ·5H O) in 50
2 2 3 2
7. Reagents
mL of water and dilute to 250 mL. Standardize as follows:
Pipet 10 mL of the KIO solution into each of three 150-mL
7.1 Hydrochloric Acid (1+1).
beakers. Dilute each to 100 mL with water, add2gofKIand
7.2 Hydrochloric Acid (1+19).
5mLofH SO (1+18), and dissolve the KI with stirring.
2 4
7.3 Hydrochloric Acid (1+99).
Titrate the liberated iodine with 0.025 N Na S O solution
2 2 3
until the color of the solution becomes pale yellow.Add 2 mL
8. Procedure
of starch indicator and continue the titration dropwise until the
8.1 Introducea1-gspecimen,weighedtothenearest0.1mg
color changes from blue to colorless.
into an evaporating casserole. Add 50 mL of HCl (1+1) and
I 51mLNa S O 5 0.01500/V gFe O (2)
thoroughly mix. 2 2 3 1 2 3
8.2 Place the casserole on a hot plate and evaporate care-
where:
fully to dryness.
I = iron oxide equivalent of Na S O solution,
2 2 3
8.3 Place the casserole in the oven at 100°C for 2 h. Do not
V =Na S O required for titrations, mean, mL, and
1 2 2 3
allow the oven temperature to exceed 105°C at any time.
0.01500 = (10.00 mL KIO ) 3 (0.001500 g Fe O /mL
3 2 3
Remove the casserole and allow to cool for 10 min.
KIO ).
8.4 Completely wet the residue with 25 mL of HCl (1+1)
and cover the casserole with a watch glass. Warm just to
12. Procedure
boiling on a hot plate and maintain for 10 min.
12.1 Dilute the solution obtained from the procedure in 8.6
8.5 Add 25 mLof water, free any material from the sides of
to 100 mLwith water.Add 10 mLof HCl and 5 g KI. Dissolve
the casserole with a stirring rod, and immediately filter through
the KI with stirring.
a tared porcelain crucible of medium porosity.
12.2 Titrate with 0.025 N Na S O solution until the color
2 2 3
8.6 Wash the residue with two 5-mL portions of hot HCl
becomes a pale yellow. Add 2 mL of starch indicator solution
(1+19), one 5-mL portion of hot HCl (1+99), and finally with
and continue the titration until the color changes from blue to
two 5-mLportions of hot water. Save the combined filtrates for
colorless.
the determination of iron oxide (Sections 10-12).
8.7 Place the crucible containing the precipitate in the
13. Calculation
muffle furnace from 600 to 800°C and heat to constant weight
13.1 Calculate the percent of iron oxide, D, as follows:
(64 mg). Cool in a desiccator and weigh.
D 5 ~I 3 V !/S ~100! (3)
2 1
9. Calculation
where:
9.1 Calculate the percent of SiO , A, as follows:
V =Na S O solution required for titration, mL, and
2 2 2 3
A 5 R/S 100! (1)
~ S = weight of original specimen, g.
where:
SOLUTION OF PIGMENT FOR THE
R = weight of residue, g, and
DETERMINATION OF BORON TRIOXIDE AND
S = weight of original specimen, g.
CALCIUM OXIDE
IRON OXIDE
14. Apparatus
14.1 Boiling Flask—300-mL capacity with ground glass
10. Apparatus
connection.
10.1 Volumetric Flasks, 250-mL and 1000-mL capacity.
14.2 Büchner Funnel, 56-mm diameter.
10.2 Buret, 10-mL capacity.
14.3 Filter Paper, 55-mm diameter.
14.4 Filter Flask, 250-mL capacity.
11. Reagents
14.5 Hot Plate/Stirrer.
11.1 Potassium Iodate (0.01878 N)—Dry 1.0 g of KIO at
14.6 pH Meter.
120°C for2hina drying oven.After cooling, weigh 0.6700 g
14.7 Reflux Condenser, with ground glass connection, water
and dissolve it in 100 mL of water. Dilute the solution to 1 L
cooled.
in a volumetric flask. 1 mL = 0.001500 g Fe O .
2 3
11.2 Potassium Iodide (KI)—Iodate free.
11.3 Starch Indicator Solution—Make a homogeneous
The sole source of supply of Whatman No. 50 Filter Paper, known to the
paste of 10 g of soluble starch in cold water.Add to this 1 Lof
committee at this time is Whatman, Inc. If you are aware of alternative suppliers,
boiling water, stir rapidly, and cool. Salicylic acid (1.25 g/L)
please provide this information to ASTM International Headquarters. Your com-
may be added to preserve the indicator. If long storage is
ments will receive careful consideration at a meeting of the responsible technical
required, the solution should be kept in a refrigerator at 4 to committee, which you may attend.
D4487–90 (2003)
14.8 Sintered Glass Crucible, 50-mL capacity, medium 17.4 Drying Oven, maintained at 105 6 2°C.
porosity.
18. Reagents
14.9 Volumetric Flask, 250-mL capacity.
18.1 Hydrochloric Acid (1+19).
15. Reagents
18.2 Mannitol.
18.3 Phenolphthalein Indicator Solution— Dissolve 0.10 g
15.1 Hydrochloric Acid (1+1).
phenolphthalein in 50 mL of ethyl alcohol. Dilute to 100 mL
15.2 Hydrochloric Acid (1+25).
with water.
15.3 Nitric Acid (1+1).
18.4 Thymol Blue Indicator Solution— Dissolve 0.1 g of
15.4 Potassium Hydroxide, pellets.
thymol blue in 50 mL of 0.01 N sodium hydroxide. Dilute to
15.5 Potassium Hydroxide Solution, 28 g/L.
100 mL with ethyl alcohol.
16. Procedure
18.5 Mixed Indicator Solution—Mix 25 mL of thymol blue
indicator solution with 75 mL of phenolphthalein indicator
16.1 Introduce 2.5 g of sample, weighed to 0.1 mg, into the
solution. Adjust the pH from 6.0 to 7.0 on a pH meter with
300-mL boiling flask.
either HCl (1+19) or NaOH (0.1 N).
16.2 Add 50 mL of HCl (1+1) and 2 drops HNO (1+1).
18.6 Potassium Hydrogen Phthalate (KHP)—Acidimetric
Place
...