ASTM D717-86(1999)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 717 – 86 (Reapproved 1999)
Standard Test Methods for
Analysis of Magnesium Silicate Pigment
This standard is issued under the fixed designation D 717; 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 conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society, where such
1.1 These test methods cover the analysis of magnesium
specifications are available. Other grades may be used, pro-
silicate pigment.
vided it is first ascertained that the reagent is of sufficiently
1.2 This standard does not purport to address the safety
high purity to permit its use without lessening the accuracy of
concerns associated with its use. It is the responsibility of the
the determination.
user of this standard to establish appropriate safety and health
5.2 Unless otherwise indicated, references to water shall be
practices and determine the applicability of regulatory limita-
understood to mean Type II of Specification D 1193.
tions prior to use.
SILICON DIOXIDE
2. Referenced Documents
2.1 ASTM Standards:
6. Reagents
D 234 Specification for Raw Linseed Oil
6.1 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
D 280 Test Methods for Hygroscopic Moisture (and Other
chloric acid (HCl).
Matter Volatile Under the Test Conditions) in Pigments
6.2 Hydrochloric Acid (1+20)—Mix 1 volume of concen-
D 718 Test Methods for Analysis of Aluminum Silicate
trated hydrochloric acid (HCl, sp gr 1.19) with 20 volumes of
Pigment
water.
D 1193 Specification for Reagent Water
6.3 Hydrofluoric Acid (48 %)—Concentrated hydrofluoric
D 1208 Test Methods for Common Properties of Certain
acid (HF).
Pigments
6.4 Sodium Carbonate (Na CO ).
2 3
D 2448 Test Method for Water-Soluble Salts in Pigments by
6.5 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
Measuring the Specific Resistance of the Leachate of the
(H SO ).
2 4
Pigment
E 97 Test Method for Directional Reflectance Factor, 45-
7. Procedure
deg 0-deg, of Opaque Specimens by Broad-Band Filter
7.1 Transfer1gofthe sample weighed to 0.1 mg to a
Reflectometry
platinum crucible and fuse with5gofNa CO until the entire
2 3
contents of the crucible are in a molten state. Continue heating
3. Significance and Use
for 20 min. Keep a close-fitting platinum cover on the crucible
3.1 These test methods may be used to confirm the stated
during the fusion. When the fusion is complete, allow the
SiO , CaO, and MgO content of magnesium silicate for quality
crucible and contents to cool, and transfer to a 600-mL
control.
porcelain casserole containing 200 mL of water (Note 1). Boil
until the melt is disintegrated.
4. Apparatus
NOTE 1—If, during the cooling period, the crucible is partially im-
4.1 Platinum Crucible.
mersed several times in cold water to chill the outer portions of the melt,
4.2 Electric Furnace, capable of 1200°C.
the subsequent removal of the melt is facilitated. Do not allow the water
to enter the crucible while the contents are hot to avoid spattering.
5. Purity of Reagents
7.2 Remove crucible and lid, being careful to scrub and
5.1 Reagent grade chemicals shall be used in all tests.
rinse out any adhering particles of the melt. Carefully acidify
Unless otherwise indicated, it is intended that all reagents shall
the contents of the casserole with concentrated HCl (sp gr
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
Reagent Chemicals, American Chemical Society Specifications, American
of Subcommittee D01.31 on Pigment Specifications.
Current edition approved April 25, 1986. Published June 1986. Originally Chemical Society, Washington, DC. For suggestions on the testing of reagents not
e2
published as D 717 – 43. Last previous edition D 717 – 73 (1979) . 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 11.01. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Discontinued; see 1992 Annual Book of ASTM Standards, Vol 14.02. MD.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 717
1.19); introduce the HCl in small portions, keeping a watch was effected. Dissolve the precipitate with 40 mL of hot HCl
glass over the crucible to avoid loss by spattering. Add 30 mL (1+3), dilute the solution to about 100 mL, and reprecipitate the
of HCl in excess and evaporate to dryness on a steam bath; take hydroxides as described in 10.2. Filter and wash the precipitate
care to break up any crusts that form. When the material four times with hot NH Cl. Combine the filtrate and washings
appears completely dry, and no odor of HCl can be detected, with the filtrate set aside and reserve for the determination of
remove the casserole from the steam bath, and allow to cool. CaO (Section 10).
7.3 Wash down the sides of the casserole with 20 mL of HCl 10.4 Place the precipitate in a weighed platinum crucible,
(sp gr 1.19) and then with water. Repeat the evaporation as heat slowly until the papers are charred, and finally ignite to
described in 7.2, then bake for1hinan oven at 105°C. Cool constant weight at 1050 to 1100°C with care to prevent
the residue, drench with 25 mL of HCl (sp gr 1.19), add 175 reduction. Cool and weigh as R O (aluminum and iron
2 3
mL of water, and warm, while stirring, until all soluble salts are oxides).
dissolved. Filter off the silica on a close-texture paper, wash
11. Calculation
five times with HCl (1+20), wash five times with hot water, and
reserve the filtrate for determination of other oxides (Section 11.1 Calculate the percent of R O as follows:
2 3
9).
R O ,% 5 ~P /S! 3 100 (2)
2 3 2
7.4 Transfer the paper and washed silica to a clean platinum
crucible, ignite, first gently until the filter paper is consumed, where:
P 5 R O ,g,and
and then at 1200°C for 20 min, cool, and weigh. Moisten the
2 2 3
S 5 sample used, g.
residue with water, add 5 drops of H SO (sp gr 1.84), and 15
2 4
mL of HF. Evaporate to dryness on a steam bath, heat gently
CALCIUM OXIDE
until H SO has been expelled, and ignite at 1200°C for 5 min.
2 4
Cool and weigh. The loss in weight represents the SiO .
12. Reagents
8. Calculation 12.1 Ammonium Hydroxide (1+1)—Mix 1 volume of con-
centrated NH OH (sp gr 0.90) with 1 volume of water.
8.1 Calculate the percent of silica as follows:
12.2 Ammonium Oxalate Solution—((NH ) C O ·H O),
4 2 2 4 2
SiO ,% 5 ~P/S! 3 100 (1)
saturated.
12.3 Ammonium Oxalate Solution (1 g/L)—Dilute 1.0 g of
where:
ammonium oxalate ((NH ) C O ·H O) in 1 L of water.
P 5 SiO ,g,and 4 2 2 4 2
12.4 Hydrochloric Acid (1+3)—See 9.3.
S 5 sample used, g.
12.5 Hydrochloric Acid (1+1)—Mix 1 volume of concen-
AMMONIUM HYDROXIDE GROUP
trated hydrochloric acid (HCl, sp gr 1.19) with 1 volume of
(Alumina and Iron Oxide)
water.
12.6 Methyl Red Indicator Solution— See 9.4.
9. Reagents
13. Procedure
9.1 Ammonium Chloride Solution (2 g/100 mL)—Dissolve
2 g of ammonium chloride (NH Cl) in 100 mL of water.
13.1 Acidify the combined filtrates obtained in the precipi-
9.2 Ammonium Hydroxide (sp gr 0.90)—Concentrated am-
tations of the ammonium hydroxide group (Section 10) with
monium hydroxide (NH OH).
HCl and evaporate them to a volume of about 300 mL. Add 5
9.3 Hydrochloric Acid (1+3)—Mix 1 volume of concen-
mL of HCl (1+1), a few drops of methyl red indicator solution,
trated HCl (sp gr 1.19) with 3 volumes of water.
and 30 mL of warm ammonium oxalate solution (saturated).
9.4 Methyl Red Indicator Solution— Dissolve 0.2 g of
Heat the solution to 70 to 80°C and add NH OH (1+1)
methyl red in 100 mL of methanol, ethanol, or isopropanol.
dropwise while stirring, until the color changes from red to
9.5 Potassium Pyrosulfate—(K S O ).
yellow. Allow the solution to stand without further heating for
2 2 7
1 h (no
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