ASTM D4487-90(2008)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D4487 − 90(Reapproved 2008)
Standard Test Methods for
Analysis of Calcium Borosilicate
This standard is issued under the fixed designation D4487; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Significance and Use
3.1 These test methods compile in one place, recommended
1.1 These test methods cover the analysis of the pigment
proceduresforanalysisofthepigmentknowncommerciallyas
commercially known as calcium borosilicate.
calciumborosilicate.Thispigmentisusedextensivelyinpaints
1.2 The test methods appear in the following order:
and the composition is important to the user and producer.
Test Methods Sections
Silicon Dioxide (SiO ) 6-9
4. Reagents
Iron Oxide (Fe O ) 10-13
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
used in all tests. Unless otherwise indicated, it is intended that
Moisture and Volatile Matter 24
Water of Hydration 25 to 26
all reagents shall conform to the specifications of the Commit-
Coarse Particles 27
tee onAnalytical Reagents of theAmerican 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
4.2 Purity of Water—Unless otherwise indicated, references
standard. No other units of measurement are included in this towatershallbeunderstoodtomeanreagentwaterconforming
standard.
to Type II of Specification D1193.
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-
trated reagents of the following specific gravity are intended:
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
Hydrochloric acid (HCl) 1.19
Nitric acid, (HNO ) 1.42
Sulfuric acid (H SO ) 1.84
2 4
2. Referenced Documents
Ammonium hydroxide (NH OH) 0.90
2.1 ASTM Standards:
5. Preparation of Samples
D185Test Methods for Coarse Particles in Pigments
D280Test Methods for Hygroscopic Moisture (and Other 5.1 Thoroughly mix and comminute the sample before
Matter Volatile Under the Test Conditions) in Pigments taking portions for analysis.
D281Test Method for Oil Absorption of Pigments by
SILICON DIOXIDE
Spatula Rub-out
D1193Specification for Reagent Water
6. Apparatus
6.1 Evaporating Casserole, 250-mL capacity.
These test methods are under the jurisdiction of ASTM Committee D01 on 6.2 Hot Plate.
Paint and Related Coatings, Materials, and Applications and are the direct
responsibility of Subcommittee D01.31 on Pigment Specifications.
Current edition approved Nov. 1, 2008. Published November 2008. Originally
approved in 1985. Last previous edition approved in 2003 as D4487–90(2003). Reagent Chemicals, American Chemical Society Specifications, American
DOI: 10.1520/D4487-90R08. 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.
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D4487 − 90 (2008)
6.3 Porcelain Filtering Crucible, medium porosity, 30-mL boiling water, stir rapidly, and cool. Salicylic acid (1.25 g/L)
capacity. may be added to preserve the indicator. If long storage is
required, the solution should be kept in a refrigerator at 4 to
6.4 Drying Oven, maintained at 100 6 5°C.
10°C. Prepare fresh indicator when the end point of the
6.5 Muffle Furnace.
titration from blue to colorless fails to be sharp.
7. Reagents
11.4 Sulfuric acid (H SO ) (1+18).
2 4
7.1 Hydrochloric Acid (1+1).
11.5 Sodium Thiosulfate, Standard Solution (0.025 N)—
Dissolve1.5gofsodiumthiosulfate(Na S O ·5H O)in50mL
2 2 3 2
7.2 Hydrochloric Acid (1+19).
ofwateranddiluteto250mL.Standardizeasfollows:Pipet10
7.3 Hydrochloric Acid (1+99).
mL of the KIO solution into each of three 150-mL beakers.
Dilute each to 100 mL with water, add2gofKIand5mLof
8. Procedure
H SO (1+18), and dissolve the KI with stirring. Titrate the
2 4
8.1 Introducea1-gspecimen,weighedtothenearest0.1mg
liberated iodine with 0.025 N Na S O solution until the color
2 2 3
into an evaporating casserole. Add 50 mL of HCl (1+1) and
of the solution becomes pale yellow. Add 2 mL of starch
thoroughly mix.
indicator and continue the titration dropwise until the color
8.2 Place the casserole on a hot plate and evaporate care- changes from blue to colorless.
fully to dryness.
I 51mLNa S O 50.01500/V gFe O (2)
2 2 3 1 2 3
8.3 Place the casserole in the oven at 100°C for 2 h. Do not
where:
allow the oven temperature to exceed 105°C at any time.
I = iron oxide equivalent of Na S O solution,
2 2 3
Remove the casserole and allow to cool for 10 min.
V =Na S O required for titrations, mean, mL, and
1 2 2 3
8.4 Completely wet the residue with 25 mL of HCl (1+1)
0.01500 = (10.00 mL KIO ) × (0.001500 g Fe O /mL
3 2 3
and cover the casserole with a watch glass. Warm just to
KIO ).
boiling on a hot plate and maintain for 10 min.
12. Procedure
8.5 Add 25 mLof water, free any material from the sides of
thecasserolewithastirringrod,andimmediatelyfilterthrough 12.1 Dilute the solution obtained from the procedure in 8.6
a tared porcelain crucible of medium porosity.
to100mLwithwater.Add10mLofHCland5gKI.Dissolve
the KI with stirring.
8.6 Wash the residue with two 5-mL portions of hot HCl
(1+19), one 5-mL portion of hot HCl (1+99), and finally with
12.2 Titrate with 0.025 N Na S O solution until the color
2 2 3
two5-mLportionsofhotwater.Savethecombinedfiltratesfor becomes a pale yellow. Add 2 mL of starch indicator solution
the determination of iron oxide (Sections 10-12).
and continue the titration until the color changes from blue to
colorless.
8.7 Place the crucible containing the precipitate in the
muffle furnace from 600 to 800°C and heat to constant weight
13. Calculation
(64 mg). Cool in a desiccator and weigh.
13.1 Calculate the percent of iron oxide, D, as follows:
9. Calculation
D 5 ~I 3 V !/S ~100! (3)
2 1
9.1 Calculate the percent of SiO , A, as follows:
where:
A 5 R/S ~100! (1)
V =Na S O solution required for titration, mL, and
2 2 2 3
where: S = weight of original specimen, g.
R = weight of residue, g, and
SOLUTION OF PIGMENT FOR THE
S = weight of original specimen, g.
DETERMINATION OF BORON TRIOXIDE AND
CALCIUM OXIDE
IRON OXIDE
10. Apparatus
14. Apparatus
10.1 Volumetric Flasks, 250-mL and 1000-mL capacity.
14.1 Boiling Flask—300-mL capacity with ground glass
connection.
10.2 Buret, 10-mL capacity.
14.2 Büchner Funnel, 56-mm diameter.
11. Reagents
14.3 Filter Paper, 55-mm diameter.
11.1 Potassium Iodate (0.01878 N)—Dry 1.0 g of KIO at
14.4 Filter Flask, 250-mL capacity.
120°C for2hina drying oven.After cooling, weigh 0.6700 g
and dissolve it in 100 mL of water. Dilute the solution to 1 L
in a volumetric flask. 1 mL=0.001500 g Fe O .
2 3
The sole source of supply of Whatman No. 50 Filter Paper, known to the
11.2 Potassium Iodide (KI)—Iodate free. committee at this time is Whatman, Inc. If you are aware of alternative suppliers,
please provide this information to ASTM International Headquarters. Your com-
11.3 Starch Indicator Solution—Makeahomogeneouspaste
ments will receive careful consideration at a meeting of the responsible technical
of 10 g of soluble starch in cold water. Add to this 1 L of committee, which you may attend.
D4487 − 90 (2008)
14.5 Hot Plate/Stirrer. 16.10 Transfer the filtrate quantitatively to a 250-mL volu-
metric flask and dilute to volume. Use this filtrate for the
14.6 pH Meter.
determination of boron trioxide (Sections 17-19) and calcium
14.7 Reflux Condenser, with ground glass connection, water
oxide (Sections 20-22).
cooled.
BORON TRIOXIDE
14.8 Sintered Glass Crucible, 50-mL capacity, medium
porosity.
17. Apparatus
14.9 Volumetric Flask, 250-mL capacity.
17.1 pH Meter.
15. Reagents
17.2 Buret, 25-mL capacity.
15.1 Hydrochloric Acid (1+1).
17.3 Volumetric Flasks, 1000-mL and 100-mL capacity.
15.2 Hydrochloric Acid (1+25).
17.4 Drying Oven, maintained at 105 6 2°C.
15.3 Nitric Acid (1+1).
18. Reagents
15.4 Potassium Hydroxide, pellets.
18.1 Hydrochloric Acid (1+19).
15.5 Potassium Hydroxide Solution, 28 g/L.
18.2 Mannitol.
16. Procedure
18.3 Phenolphthalein Indicator Solution—Dissolve 0.10 g
16.1 Introduce 2.5 g of sample, weighed to 0.1 mg, into the
phenolphthalein in 50 mL of ethyl alcohol. Dilute to 100 mL
300-mL boiling flask.
with water.
16.2 Add 50 mL of HCl (1+1) and 2 drops HNO (1+1).
18.4 Thymol Blue Indicator Solution—Dissolve 0.1 g of
Place a magnetic stirring bar in the flask, connect the reflux
thymol blu
...