ASTM D717-86(2003)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D717–86(Reapproved2003)
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 4. Apparatus
1.1 These test methods cover the analysis of magnesium 4.1 Platinum Crucible.
silicate pigment. 4.2 Electric Furnace, capable of 1200°C.
1.2 The values stated in SI units are to be regarded as the
5. Purity of Reagents
standard. The values given in parentheses are for information
only. 5.1 Reagent grade chemicals shall be used in all tests.
Unless otherwise indicated, it is intended that all reagents shall
1.3 This standard does not purport to address the safety
concerns associated with its use. It is the responsibility of the conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society, where such
user of this standard to establish appropriate safety and health
practices and determine the applicability of regulatory limita- specifications are available. Other grades may be used, pro-
vided it is first ascertained that the reagent is of sufficiently
tions prior to use.
high purity to permit its use without lessening the accuracy of
2. Referenced Documents
the determination.
2.1 ASTM Standards: 5.2 Unless otherwise indicated, references to water shall be
D 234 Specification for Raw Linseed Oil understood to mean Type II of Specification D 1193.
D 280 Test Methods for Hygroscopic Moisture (and Other
SILICON DIOXIDE
Matter Volatile Under the Test Conditions) in Pigments
D 718 Test Methods for Analysis of Aluminum Silicate
6. Reagents
Pigment
3 6.1 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
D 1193 Specification for Reagent Water
chloric acid (HCl).
D 1208 Test Methods for Common Properties of Certain
6.2 Hydrochloric Acid (1+20)—Mix 1 volume of concen-
Pigments
trated hydrochloric acid (HCl, sp gr 1.19) with 20 volumes of
D 2448 TestMethodforWater-SolubleSaltsinPigmentsby
water.
Measuring the Specific Resistance of the Leachate of the
2 6.3 Hydrofluoric Acid (48 %)—Concentrated hydrofluoric
Pigment
acid (HF).
E 97 Test Method for Directional Reflectance Factor, 45-
6.4 Sodium Carbonate (Na CO ).
2 3
deg 0-deg, of Opaque Specimens by Broad-Band Filter
6.5 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
Reflectometry
(H SO ).
2 4
3. Significance and Use
7. Procedure
3.1 These test methods may be used to confirm the stated
7.1 Transfer1gofthe sample weighed to 0.1 mg to a
SiO , CaO, and MgO content of magnesium silicate for quality
platinum crucible and fuse with5gofNa CO until the entire
2 3
control.
contents of the crucible are in a molten state. Continue heating
for 20 min. Keep a close-fitting platinum cover on the crucible
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. Reagent Chemicals, American Chemical Society Specifications, American
Current edition approved Oct. 1, 2003. Published October 2003. Originally Chemical Society, Washington, DC. For suggestions on the testing of reagents not
approved in 1943. Last previous edition approved in 1986 as D 717 - 86 (1999). 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 International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D717–86 (2003)
during the fusion. When the fusion is complete, allow the amount of K S O until it is dissolved. Leach the pyrosulfate
2 2 7
crucible and contents to cool, and transfer to a 600-mL melt out of the crucible with water and combine the solution
porcelain casserole containing 200 mL of water (Note 1). Boil with the filtrate reserved in accordance with 7.3.
until the melt is disintegrated. 10.2 Using the methyl red indicator solution, neutralize the
combined solutions from the silica determination with NH OH
NOTE 1—If, during the cooling period, the crucible is partially im-
and add an excess of 2 drops. Bring to a boil adding NH OH
mersed several times in cold water to chill the outer portions of the melt,
1 drop at a time if necessary to maintain a slight alkalinity.
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. Allow the precipitate to settle (not more than 5 min) and filter.
Wash four times with hot NH Cl solution.
7.2 Remove crucible and lid, being careful to scrub and
10.3 Set aside the filtrate and transfer the precipitate and
rinse out any adhering particles of the melt. Carefully acidify
filter paper to the same beaker in which the first precipitation
the contents of the casserole with concentrated HCl (sp gr
was effected. Dissolve the precipitate with 40 mL of hot HCl
1.19); introduce the HCl in small portions, keeping a watch
(1+3),dilutethesolutiontoabout100mL,andreprecipitatethe
glass over the crucible to avoid loss by spattering.Add 30 mL
hydroxides as described in 10.2. Filter and wash the precipitate
ofHClinexcessandevaporatetodrynessonasteambath;take
four times with hot NH Cl. Combine the filtrate and washings
care to break up any crusts that form. When the material
with the filtrate set aside and reserve for the determination of
appears completely dry, and no odor of HCl can be detected,
CaO (Section 10).
remove the casserole from the steam bath, and allow to cool.
10.4 Place the precipitate in a weighed platinum crucible,
7.3 Washdownthesidesofthecasserolewith20mLofHCl
heat slowly until the papers are charred, and finally ignite to
(sp gr 1.19) and then with water. Repeat the evaporation as
constant weight at 1050 to 1100°C with care to prevent
described in 7.2, then bake for1hinan oven at 105°C. Cool
reduction. Cool and weigh as R O (aluminum and iron
2 3
the residue, drench with 25 mL of HCl (sp gr 1.19), add 175
oxides).
mLofwater,andwarm,whilestirring,untilallsolublesaltsare
dissolved. Filter off the silica on a close-texture paper, wash
11. Calculation
fivetimeswithHCl(1+20),washfivetimeswithhotwater,and
11.1 Calculate the percent of R O as follows:
2 3
reserve the filtrate for determination of other oxides (Section
R O ,% 5 P /S 3 100 (2)
~ !
2 3 2
9).
7.4 Transfer the paper and washed silica to a clean platinum
where:
crucible, ignite, first gently until the filter paper is consumed,
P =R O,g,and
2 2 3
and then at 1200°C for 20 min, cool, and weigh. Moisten the
S = sample used, g.
residue with water, add 5 drops of H SO (sp gr 1.84), and 15
2 4
CALCIUM OXIDE
mL of HF. Evaporate to dryness on a steam bath, heat gently
untilH SO hasbeenexpelled,andigniteat1200°Cfor5min.
2 4
12. Reagents
Cool and weigh. The loss in weight represents the SiO .
12.1 Ammonium Hydroxide (1+1)—Mix 1 volume of con-
8. Calculation centrated NH OH (sp gr 0.90) with 1 volume of water.
12.2 Ammonium Oxalate Solution—((NH ) C O ·H O),
4 2 2 4 2
8.1 Calculate the percent of silica as follows:
saturated.
SiO,% 5 P/S! 3 100 (1)
~
12.3 Ammonium Oxalate Solution (1 g/L)—Dilute 1.0 g of
ammonium oxalate ((NH ) C O ·H O) in 1 L of water.
where: 4 2 2 4 2
12.4 Hydrochloric Acid (1+3)—See 9.3.
P = SiO,g,and
12.5 Hydrochloric Acid (1+1)—Mix 1 volume of concen-
S = sample used, g.
trated hydrochloric acid (HCl, sp gr 1.19) with 1 volume of
AMMONIUM HYDROXIDE GROUP
water.
(Alumina and Iron Oxide)
12.6 Methyl Red Indicator Solution— See 9.4.
9. Reagents 13. Procedure
9.1 Ammonium Chloride Solution (2 g/100 mL)—Dissolve 13.1 Acidify the combined filtrates obtained in the precipi
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