ASTM D4487-90(2014)

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it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D4487 − 90 (Reapproved 2008) D4487 − 90 (Reapproved 2014)
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 These test methods cover the analysis of the pigment commercially known as calcium borosilicate.
1.2 The test methods appear in the following order:
Test Methods Sections
Silicon Dioxide (SiO ) 6 – 9
Iron Oxide (Fe O ) 10 – 13
2 3
Boron Trioxide (B O ) 17 – 20
2 3
Calcium Oxide (CaO) 21 – 23
Moisture and Volatile Matter 24
Water of Hydration 25 to 26
Coarse Particles 27
Oil Absorption 28
1.3 Individual specimens may be used for the direct determinations of SiO , B O , and CaO. SiO and Fe O should be removed
2 2 3 2 2 3
before the determination of the B O and CaO.
2 3
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns, if any, 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.
2. Referenced Documents
2.1 ASTM Standards:
D185 Test Methods for Coarse Particles in Pigments
D280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments
D281 Test Method for Oil Absorption of Pigments by Spatula Rub-out
D1193 Specification for Reagent Water
3. Significance and Use
3.1 These test methods compile in one place, recommended procedures for analysis of the pigment known commercially as
calcium borosilicate. This pigment is used extensively in paints and the composition is important to the user and producer.
4. Reagents
4.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
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 Nov. 1, 2008Dec. 1, 2014. Published November 2008December 2014. Originally approved in 1985. Last previous edition approved in 20032008
as D4487 – 90 (2003).(2008). DOI: 10.1520/D4487-90R08.10.1520/D4487-90R14.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’sstandard’s Document Summary page on the ASTM website.
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4487 − 90 (2014)
4.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to
Type II of Specification D1193.
4.3 Concentration of Acids and Ammonium Hydroxide—When acids and ammonium hydroxide are specified by name or
chemical formula only, it should be understood that concentrated reagents of the following specific gravity are intended:
Hydrochloric acid (HCl) 1.19
Nitric acid, (HNO ) 1.42
Sulfuric acid (H SO ) 1.84
2 4
Ammonium hydroxide (NH OH) 0.90
5. Preparation of Samples
5.1 Thoroughly mix and comminute the sample before taking portions for analysis.
SILICON DIOXIDE
6. Apparatus
6.1 Evaporating Casserole, 250-mL capacity.
6.2 Hot Plate.
6.3 Porcelain Filtering Crucible, medium porosity, 30-mL capacity.
6.4 Drying Oven, maintained at 100 6 5°C.
6.5 Muffle Furnace.
7. Reagents
7.1 Hydrochloric Acid (1+1).
7.2 Hydrochloric Acid (1+19).
7.3 Hydrochloric Acid (1+99).
8. Procedure
8.1 Introduce a 1-g specimen, weighed to the nearest 0.1 mg into an evaporating casserole. Add 50 mL of HCl (1+1) and
thoroughly mix.
8.2 Place the casserole on a hot plate and evaporate carefully to dryness.
8.3 Place the casserole in the oven at 100°C for 2 h. Do not allow the oven temperature to exceed 105°C at any time. Remove
the casserole and allow to cool for 10 min.
8.4 Completely wet the residue with 25 mL of HCl (1+1) and cover the casserole with a watch glass. Warm just to boiling on
a hot plate and maintain for 10 min.
8.5 Add 25 mL of water, free any material from the sides of the casserole with a stirring rod, and immediately filter through
a tared porcelain crucible of medium porosity.
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 two 5-mL
portions of hot water. Save the combined filtrates for the determination of iron oxide (Sections 10 – 12).
8.7 Place the crucible containing the precipitate in the muffle furnace from 600 to 800°C and heat to constant weight (64 mg).
Cool in a desiccator and weigh.
9. Calculation
9.1 Calculate the percent of SiO , A, as follows:
A 5 R/S ~100! (1)
where:
R = weight of residue, g, and
S = weight of original specimen, g.
IRON OXIDE
10. Apparatus
10.1 Volumetric Flasks, 250-mL and 1000-mL capacity.
10.2 Buret, 10-mL capacity.
D4487 − 90 (2014)
11. Reagents
11.1 Potassium Iodate (0.01878 N)—Dry 1.0 g of KIO at 120°C for 2 h in a 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
11.2 Potassium Iodide (KI)—Iodate free.
11.3 Starch Indicator Solution—Make a homogeneous paste of 10 g of soluble starch in cold water. Add to this 1 L of boiling
water, stir rapidly, and cool. Salicylic acid (1.25 g/L) may be added to preserve the indicator. If long storage is required, the solution
should be kept in a refrigerator at 4 to 10°C. Prepare fresh indicator when the end point of the titration from blue to colorless fails
to be sharp.
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 mL of
2 2 3 2
water and dilute to 250 mL. Standardize as follows: Pipet 10 mL of the KIO solution into each of three 150-mL beakers. Dilute
each to 100 mL with water, add 2 g of KI and 5 mL of H SO (1+18), and dissolve the KI with stirring. Titrate the liberated iodine
2 4
with 0.025 N Na S O solution until the color of the solution becomes pale yellow. Add 2 mL of starch indicator and continue the
2 2 3
titration dropwise until the color changes from blue to colorless.
I 5 1 mL Na S O 5 0.01500/V g Fe O (2)
2 2 3 1 2 3
where:
I = iron oxide equivalent of Na S O solution,
2 2 3
V = Na S O required for titrations, mean, mL, and
1 2 2 3
0.01500 = (10.00 mL KIO ) × (0.001500 g Fe O /mL KIO ).
3 2 3 3
12. Procedure
12.1 Dilute the solution obtained from the procedure in 8.6 to 100 mL with water. Add 10 mL of HCl and 5 g KI. Dissolve the
KI with stirring.
12.2 Titrate with 0.025 N Na S O solution until the color becomes a pale yellow. Add 2 mL of starch indicator solution and
2 2 3
continue the titration until the color changes from blue to colorless.
13. Calculation
13.1 Calculate the percent of iron oxide, D, as follows:
D 5 ~I 3V !/S ~100! (3)
2 1
where:
V = Na S O solution required for titration, mL, and
2 2 2 3
S = weight of original specimen, g.
SOLUTION OF PIGMENT FOR THE DETERMINATION OF BORON TRIOXIDE AND CALCIUM OXIDE
14. Apparatus
14.1 Boiling Flask—300-mL capacity with ground glass connection.
14.2 Büchner Funnel, 56-mm diameter.
14.3 Filter Paper, 55-mm diameter.
14.4 Filter Flask, 250-mL capacity.
14.5 Hot Plate/Stirrer.
14.6 pH Meter.
14.7 Reflux Condenser, with ground glass connection, water cooled.
14.8 Sintered Glass Crucible, 50-mL capacity, medium porosity.
14.9 Volumetric Flask, 250-mL capacity.
15. Reagents
15.1 Hydrochloric Acid (1+1).
15.2 Hydrochloric Acid (1+25).
The sole source of supply of Whatman No. 50 Filter Paper, known to the committee at this time is Whatman, Inc. If you are aware of alternative suppliers, please provide
this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you
may attend.
D4487 − 90 (2014)
15.3 Nitric Acid (1+1).
15.4 Potassium Hydroxide, pellets.
15.5 Potassium Hydroxide Solution, 28 g/L.
16. Procedure
16.1 Introduce 2.5 g of sample, weighed to 0.1 mg, into the 300-mL boiling flask.
16.2 Add 50 mL of HCl (1+1) and 2 drops HNO (1+1). Place a magnetic stirring bar in the flask, connect the reflux condenser
to the flask, and reflux for 1 h on the hotplate with constant stirring.
16.3 Remove the hotplate and place an ice bath under the flask. After the solution has cooled, wash the condenser down with
a small amount of water (10 mL) and remove from the flask.
16.4 Filter the mixture through a Büchner funnel equipped with filter paper into a 250-mL filter flask. Wash the boiling flask
with several 5-mL portions of hot water to transfer all the material to the filter.
16.5 Cool the filtrate in an ice bath to a temperature of approximately 10°C, add
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