ASTM D4487-90(2020)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4487 − 90 (Reapproved 2020)
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 D280Test Methods for Hygroscopic Moisture (and Other
Matter Volatile Under the Test Conditions) in Pigments
1.1 These test methods cover the analysis of the pigment
D281Test Method for Oil Absorption of Pigments by
commercially known as calcium borosilicate.
Spatula Rub-out
1.2 The test methods appear in the following order:
D1193Specification for Reagent Water
Test Methods Sections
Silicon Dioxide (SiO ) 6–9
3. Significance and Use
Iron Oxide (Fe O ) 10–13
2 3
Boron Trioxide (B O ) 17–20
2 3
3.1 These test methods compile in one place, recommended
Calcium Oxide (CaO) 21–23
proceduresforanalysisofthepigmentknowncommerciallyas
Moisture and Volatile Matter 24
Water of Hydration 25 to 26
calciumborosilicate.Thispigmentisusedextensivelyinpaints
Coarse Particles 27
and the composition is important to the user and producer.
Oil Absorption 28
1.3 Individual specimens may be used for the direct deter-
4. Reagents
minations of SiO,B O , and CaO. SiO and Fe O should be
2 2 3 2 2 3
4.1 Purity of Reagents—Reagent grade chemicals shall be
removed before the determination of the B O and CaO.
2 3
used in all tests. Unless otherwise indicated, it is intended that
1.4 The values stated in SI units are to be regarded as
all reagents shall conform to the specifications of the Commit-
standard. No other units of measurement are included in this
tee onAnalytical Reagents of theAmerican Chemical Society
standard. 3
where such specifications are available. Other grades may be
1.5 This standard does not purport to address all of the
used, provided it is first ascertained that the reagent is of
safety concerns, if any, associated with its use. It is the
sufficiently high purity to permit its use without lessening the
responsibility of the user of this standard to establish appro-
accuracy of the determination.
priate safety, health, and environmental practices and deter-
4.2 Purity of Water—Unless otherwise indicated, references
mine the applicability of regulatory limitations prior to use.
towatershallbeunderstoodtomeanreagentwaterconforming
1.6 This international standard was developed in accor-
to Type II of Specification D1193.
dance with internationally recognized principles on standard-
4.3 Concentration of Acids and Ammonium Hydroxide—
ization established in the Decision on Principles for the
When acids and ammonium hydroxide are specified by name
Development of International Standards, Guides and Recom-
or chemical formula only, it should be understood that concen-
mendations issued by the World Trade Organization Technical
trated reagents of the following specific gravity are intended:
Barriers to Trade (TBT) Committee.
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
D185Test Methods for Coarse Particles in Pigments
5. Preparation of Samples
5.1 Thoroughly mix and comminute the sample before
1 taking portions for analysis.
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.
CurrenteditionapprovedJune1,2020.PublishedJuly2020.Originallyapproved
in 1985. Last previous edition approved in 2014 as D4487–90(2014). DOI: ACS Reagent Chemicals, Specifications and Procedures for Reagents and
10.1520/D4487-90R20. Standard-Grade Reference Materials, American Chemical Society, Washington,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or DC. For suggestions on the testing of reagents not listed by theAmerican Chemical
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
Standards volume information, refer to the standard’s Document Summary page on U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
the ASTM website. copeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4487 − 90 (2020)
SILICON DIOXIDE 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
6. Apparatus
11.2 Potassium Iodide (KI)—Iodate free.
6.1 Evaporating Casserole, 250-mL capacity.
11.3 Starch Indicator Solution—Makeahomogeneouspaste
6.2 Hot Plate.
of 10 g of soluble starch in cold water. Add to this 1 L of
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
6.4 Drying Oven, maintained at 100 6 5°C.
required, the solution should be kept in a refrigerator at 4 to
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)—
7.2 Hydrochloric Acid (1+19).
Dissolve1.5gofsodiumthiosulfate(Na S O ·5H O)in50mL
2 2 3 2
7.3 Hydrochloric Acid (1+99).
ofwateranddiluteto250mL.Standardizeasfollows:Pipet10
mL of the KIO solution into each of three 150-mL beakers.
8. Procedure
Dilute each to 100 mL with water, add2gofKIand5mLof
8.1 Introducea1-gspecimen,weighedtothenearest0.1mg
H SO (1+18), and dissolve the KI with stirring. Titrate the
2 4
into an evaporating casserole. Add 50 mL of HCl (1+1) and
liberated iodine with 0.025 N Na S O solution until the color
2 2 3
thoroughly mix.
of the solution becomes pale yellow. Add 2 mL of starch
8.2 Place the casserole on a hot plate and evaporate care-
indicator and continue the titration dropwise until the color
fully to dryness.
changes from blue to colorless.
8.3 Place the casserole in the oven at 100°C for 2 h. Do not
I 51mLNa S O 5 0.01500/V gFe O (2)
2 2 3 1 2 3
allow the oven temperature to exceed 105°C at any time.
where:
Remove the casserole and allow to cool for 10 min.
I = iron oxide equivalent of Na S O solution,
2 2 3
8.4 Completely wet the residue with 25 mL of HCl (1+1)
V =Na S O required for titrations, mean, mL, and
1 2 2 3
and cover the casserole with a watch glass. Warm just to
0.01500 = (10.00 mL KIO ) × (0.001500 g Fe O /mL
3 2 3
boiling on a hot plate and maintain for 10 min.
KIO ).
8.5 Add 25 mLof water, free any material from the sides of
thecasserolewithastirringrod,andimmediatelyfilterthrough 12. Procedure
a tared porcelain crucible of medium porosity.
12.1 Dilute the solution obtained from the procedure in 8.6
8.6 Wash the residue with two 5-mL portions of hot HCl
to100mLwithwater.Add10mLofHCland5gKI.Dissolve
(1+19), one 5-mL portion of hot HCl (1+99), and finally with
the KI with stirring.
two5-mLportionsofhotwater.Savethecombinedfiltratesfor
12.2 Titrate with 0.025 N Na S O solution until the color
the determination of iron oxide (Sections10–12). 2 2 3
becomes a pale yellow. Add 2 mL of starch indicator solution
8.7 Place the crucible containing the precipitate in the
and continue the titration until the color changes from blue to
muffle furnace from 600 to 800°C and heat to constant weight
colorless.
(64 mg). Cool in a desiccator and weigh.
13. Calculation
9. Calculation
9.1 Calculate the percent of SiO , A, as follows:
13.1 Calculate the percent of iron oxide, D, as follows:
A 5 R/S ~100! (1)
D 5 ~I 3 V !/S ~100! (3)
2 1
where:
where:
R = weight of residue, g, and
V =Na S O solution required for titration, mL, and
2 2 2 3
S = weight of original specimen, g.
S = weight of original specimen, g.
IRON OXIDE
SOLUTION OF PIGMENT FOR THE
DETERMINATION OF BORON TRIOXIDE AND
10. Apparatus
CALCIUM OXIDE
10.1 Volumetric Flasks, 250-mL and 1000-mL capacity.
14. Apparatus
10.2 Buret, 10-mL capacity.
14.1 Boiling Flask—300-mL capacity with ground glass
11. Reagents
connection.
11.1 Potassium Iodate (0.01878 N)—Dry 1.0 g of KIO at
120°C for2hina drying oven.After cooling, weigh 0.6700 g 14.2 Büchner Funnel, 56-mm diameter.
D4487 − 90 (2020)
14.3 Filter Paper, 55-mm diameter. hot water. Swirl the acidic solution around in the flask to
dissolve any iron precipitate adhering to the sides of the flask.
14.4 Filter Flask, 250-mL capacity.
16.8 Repeat the neutralization step (16.5) and filter the
14.5 Hot Plate/Stirrer.
solution through the sintered glass crucible into the flask
14.6 pH Meter.
containing the first filtrate (16.7).
14.7 Reflux Condenser, with ground glass connection, water
16.9 Wash the flask used in the neutralization with two
cooled.
5-mL portions of water, and then wash the precipitate in the
14.8 Sintered Glass Crucible, 50-mL capacity, medium
crucible.
porosity.
16.10 Transfer the filtrate quantitatively to a 250-mL volu-
14.9 Volumetric Flask, 250-mL capacity.
metric flask and dilute to volume. Use this filtrate for the
determinationofborontrioxide(Sections17–19)andcalcium
15. Reagents
oxide (Sections20–22).
15.1 Hydrochloric Acid (1+1).
BORON TRIOXIDE
15.2 Hydrochloric Acid (1+25).
17. Apparatus
15.3 Nitric Acid (1+1).
17.1 pH Meter.
15.4 Potassium Hydroxide, pellets.
17.2 Buret, 25-mL capacity.
15.5 Potassium Hydroxide Solution, 28 g/L.
17.3 Volumetric Flasks, 1000-mL and 100-mL capacity.
16. Procedure
17.4 Drying Oven, maintained at 105 6 2°C.
16.1 Introduce 2.5 g of sample, weighed to 0.1 mg, into the
300-mL boiling flask.
18. Reagents
16.2 Add 50 mL of HCl (1+1) and 2 drops HNO (1+1).
18.1 Hydrochloric Acid (1+19).
Place a magnetic st
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