ASTM D4487-90(1999)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D 4487 – 90 (Reapproved 1999)
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 4. Reagents
1.1 These test methods cover the analysis of the pigment 4.1 Purity of Reagents—Reagent grade chemicals shall be
commercially known as calcium borosilicate. used in all tests. Unless otherwise indicated, it is intended that
1.2 The test methods appear in the following order: all reagents shall conform to the specifications of the Commit-
tee on Analytical Reagents of the American Chemical Society
Test Methods Sections
Silicon Dioxide (SiO ) 6-9
2 where such specifications are available. Other grades may be
Iron Oxide (Fe O ) 10-13
2 3
used, provided it is first ascertained that the reagent is of
Boron Trioxide (B O ) 17-20
2 3
sufficiently high purity to permit its use without lessening the
Calcium Oxide (CaO) 21-23
Moisture and Volatile Matter 24
accuracy of the determination.
Water of Hydration 25 to 26
4.2 Purity of Water—Unless otherwise indicated, references
Coarse Particles 27
Oil Absorption 28 to water shall be understood to mean reagent water conforming
to Type II of Specification D 1193.
1.3 Individual specimens may be used for the direct deter-
4.3 Concentration of Acids and Ammonium Hydroxide—
minations of SiO ,B O , and CaO. SiO and Fe O should be
2 2 3 2 2 3
When acids and ammonium hydroxide are specified by name
removed before the determination of the B O and CaO.
2 3
or chemical formula only, it should be understood that concen-
1.4 This standard does not purport to address all of the
trated reagents of the following specific gravity are intended:
safety concerns, if any, associated with its use. It is the
Hydrochloric acid (HCl) 1.19
responsibility of the user of this standard to establish appro-
Nitric acid, (HNO ) 1.42
priate safety and health practices and determine the applica-
Sulfuric acid (H SO ) 1.84
2 4
Ammonium hydroxide (NH OH) 0.90
bility of regulatory limitations prior to use.
5. Preparation of Samples
2. Referenced Documents
5.1 Thoroughly mix and comminute the sample before
2.1 ASTM Standards:
taking portions for analysis.
D 185 Test Methods for Coarse Particles in Pigments,
Pastes, and Paints
SILICON DIOXIDE
D 280 Test Methods for Hygroscopic Moisture (and Other
Matter Volatile Under the Test Conditions) in Pigments
6. Apparatus
D 281 Test Method for Oil Absorption of Pigments by
6.1 Evaporating Casserole, 250-mL capacity.
Spatula Rub-Out
6.2 Hot Plate.
D 1193 Specification for Reagent Water
6.3 Porcelain Filtering Crucible, medium porosity, 30-mL
capacity.
3. Significance and Use
6.4 Drying Oven, maintained at 100 6 5°C.
3.1 These test methods compile in one place, recommended
6.5 Muffle Furnace.
procedures for analysis of the pigment known commercially as
calcium borosilicate. This pigment is used extensively in paints
7. Reagents
and the composition is important to the user and producer.
7.1 Hydrochloric Acid (1+1).
7.2 Hydrochloric Acid (1+19).
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 May 25, 1990. Published July 1990. Originally Chemical Society, Washington, DC. For suggestions on the testing of reagents not
published as D 4487 – 85. Last previous edition D 4487 – 85. 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 06.01. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 11.01. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 4487
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 Introduce a 1-g specimen, weighed to the nearest 0.1 mg color changes from blue to colorless.
into an evaporating casserole. Add 50 mL of HCl (1+1) and
I 5 1mLNa S O 5 0.01500/V gFe O (2)
2 2 3 1 2 3
thoroughly mix.
where:
8.2 Place the casserole on a hot plate and evaporate care-
I 5 iron oxide equivalent of Na S O solution,
fully to dryness. 2 2 3
V 5 Na S O required for titrations, mean, mL, and
1 2 2 3
8.3 Place the casserole in the oven at 100°C for 2 h. Do not
0.01500 5 (10.00 mL KIO ) 3 (0.001500 g Fe O /mL
3 2 3
allow the oven temperature to exceed 105°C at any time.
KIO ).
Remove the casserole and allow to cool for 10 min.
8.4 Completely wet the residue with 25 mL of HCl (1+1)
12. Procedure
and cover the casserole with a watch glass. Warm just to
12.1 Dilute the solution obtained from the procedure in 7.6
boiling on a hot plate and maintain for 10 min.
to 100 mL with water. Add 10 mL of HCl and 5 g KI. Dissolve
8.5 Add 25 mL of water, free any material from the sides of
the KI with stirring.
the casserole with a stirring rod, and immediately filter through
12.2 Titrate with 0.025 N Na S O solution until the color
2 2 3
a tared porcelain crucible of medium porosity.
becomes a pale yellow. Add 2 mL of starch indicator solution
8.6 Wash the residue with two 5-mL portions of hot HCl
and continue the titration until the color changes from blue to
(1+19), one 5-mL portion of hot HCl (1+99), and finally with
colorless.
two 5-mL portions of hot water. Save the combined filtrates for
the determination of iron oxide (Sections 10-12).
13. Calculation
8.7 Place the crucible containing the precipitate in the
13.1 Calculate the percent of iron oxide, D, as follows:
muffle furnace from 600 to 800°C and heat to constant weight
(64 mg). Cool in a desiccator and weigh.
D 5 ~I 3 V !/S ~100! (3)
2 1
9. Calculation where:
V 5 Na S O solution required for titration, mL, and
2 2 2 3
9.1 Calculate the percent of SiO , A, as follows:
S 5 weight of original specimen, g.
A 5 R/S ~100! (1)
SOLUTION OF PIGMENT FOR THE
where:
DETERMINATION OF BORON TRIOXIDE AND
R 5 weight of residue, g, and
CALCIUM OXIDE
S 5 weight of original specimen, g.
14. Apparatus
IRON OXIDE
14.1 Boiling Flask—300-mL capacity with ground glass
10. Apparatus
connection.
14.2 Büchner Funnel, 56-mm diameter.
10.1 Volumetric Flasks, 250-mL and 1000-mL capacity.
14.3 Filter Paper, 55-mm diameter.
10.2 Buret, 10-mL capacity.
14.4 Filter Flask, 250-mL capacity.
11. Reagents 14.5 Hot Plate/Stirrer.
14.6 pH Meter.
11.1 Potassium Iodate (0.01878 N)—Dry 1.0 g of KIO at
14.7 Reflux Condenser, with ground glass connection, water
120°C for2hina drying oven. After cooling, weigh 0.6700 g
cooled.
and dissolve it in 100 mL of water. Dilute the solution to 1 L
14.8 Sintered Glass Crucible, 50-mL capacity, medium
in a volumetric flask. 1 mL 5 0.001500 g Fe O .
2 3
porosity.
11.2 Potassium Iodide (KI)—Iodate free.
14.9 Volumetric Flask, 250-mL capacity.
11.3 Starch Indicator Solution—Make a homogeneous
paste of 10 g of soluble starch in cold water. Add to this 1 L of
15. Reagents
boiling water, stir rapidly, and cool. Salicylic acid (1.25 g/L)
15.1 Hydrochloric Acid (1+1).
may be added to preserve the indicator. If long storage is
15.2 Hydrochloric Acid (1+25).
required, the solution should be kept in a refrigerator at 4 to
15.3 Nitric Acid (1+1).
10°C. Prepare fresh indicator when the end point of the
15.4 Potassium Hydroxide, pellets.
titration from blue to colorless fails to be sharp.
15.5 Potassium Hydroxide Solution, 28 g/L.
11.4 Sulfuric acid (H SO ) (1+18).
2 4
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
The sole source of supply of Whatman No. 50 Filter Paper, known to the
mL of water and dilute to 250 mL. Standardize as follows:
committee at this time is Whatman, Inc. If you are aware of alternative suppliers,
Pipet 10 mL of the KIO solution into each of three 150-mL
please provide this information to ASTM Headquarters. Your comments will receive
beakers. Dilute each to 100 mL with water, add2gofKIand
careful consideration at a meeting of the responsible technical committee, which
5mL ofH SO (1+18), and dissolve the KI with stirring. you may attend.
2 4
D 4487
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 a magnetic stirring bar in the flask, connect the reflux
standard.
condenser to the flask, and reflux for1honthe hotplate with
18.7 Sodium Hydroxide, Standard Solution (0.1 N)—
constant stirring.
Dissolve 4.0 g of NaOH pellets in 100 mL of water and dilute
16.3 Remove the hotplate and place an ice bath under the
to 1 L in a volumetric flask. Standardize as follows: Dry 2.0 g
flask. After the solution has cooled, wash the condenser down
of KHP for2hat 105°C in the oven and cool. Weigh 1.6420
with a small amount of water (10 mL) and re
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