ASTM D717-86(2008)
(Test Method)Standard Test Methods for Analysis of Magnesium Silicate Pigment
Standard Test Methods for Analysis of Magnesium Silicate Pigment
SIGNIFICANCE AND USE
These test methods may be used to confirm the stated SiO2, CaO, and MgO content of magnesium silicate for quality control.
SCOPE
1.1 These test methods cover the analysis of magnesium silicate pigment.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 This standard does not purport to address the safety concerns 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.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D717 − 86 (Reapproved2008)
Standard Test Methods for
Analysis of Magnesium Silicate Pigment
This standard is issued under the fixed designation D717; 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 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
conform to the specifications of the Committee on Analytical
concerns associated with its use. It is the responsibility of the
Reagents of the American Chemical Society, where such
user of this standard to establish appropriate safety and health
specifications are available. Other grades may be used, pro-
practices and determine the applicability of regulatory limita-
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
D234 Specification for Raw Linseed Oil (Withdrawn 2007)
understood to mean Type II of Specification D1193.
D280 Test Methods for Hygroscopic Moisture (and Other
Matter Volatile Under the Test Conditions) in Pigments
SILICON DIOXIDE
D718 Test Methods for Analysis of Aluminum Silicate
6. Reagents
Pigment
D1193 Specification for Reagent Water
6.1 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
D1208 Test Methods for Common Properties of Certain
chloric acid (HCl).
Pigments
6.2 Hydrochloric Acid (1+20)—Mix 1 volume of concen-
D2448 Test Method for Water-Soluble Salts in Pigments by
trated hydrochloric acid (HCl, sp gr 1.19) with 20 volumes of
Measuring the Specific Resistance of the Leachate of the
water.
Pigment
6.3 Hydrofluoric Acid (48 %)—Concentrated hydrofluoric
E97 Method of Test for Directional Reflectance Factor,
acid (HF).
45-Deg 0-Deg, of Opaque Specimens by Broad-Band
Filter Reflectometry (Withdrawn 1991)
6.4 Sodium Carbonate (Na CO ).
2 3
3. Significance and Use
6.5 Sulfuric Acid (sp gr 1.84—Concentrated sulfuric acid
(H SO ).
3.1 These test methods may be used to confirm the stated 2 4
SiO , CaO, and MgO content of magnesium silicate for quality
7. Procedure
control.
7.1 Transfer1gofthe sample weighed to 0.1 mg to a
platinum crucible and fuse with5gofNa CO until the entire
These test methods are under the jurisdiction of ASTM Committee D01 on
2 3
Paint and Related Coatings, Materials, and Applications and are the direct
contents of the crucible are in a molten state. Continue heating
responsibility of Subcommittee D01.31 on Pigment Specifications.
for 20 min. Keep a close-fitting platinum cover on the crucible
Current edition approved Feb. 1, 2008. Published February 2008. Originally
approved in 1943. Last previous edition approved in 2003 as D717 - 86 (2003).
DOI: 10.1520/D0717-86R08.
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Reagent Chemicals, American Chemical Society Specifications, American
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Standards volume information, refer to the standard’s Document Summary page on listed by the American Chemical Society, see Analar Standards for Laboratory
the ASTM website. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
The last approved version of this historical standard is referenced on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
www.astm.org. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D717 − 86 (2008)
during the fusion. When the fusion is complete, allow the 10. Procedure
crucible and contents to cool, and transfer to a 600-mL
10.1 If an appreciable residue remains after the treatment
porcelain casserole containing 200 mL of water (Note 1). Boil
with HF in accordance with 7.4, fuse the residue with a small
until the melt is disintegrated.
amount of K S O until it is dissolved. Leach the pyrosulfate
2 2 7
melt out of the crucible with water and combine the solution
NOTE 1—If, during the cooling period, the crucible is partially im-
mersed several times in cold water to chill the outer portions of the melt, with the filtrate reserved in accordance with 7.3.
the subsequent removal of the melt is facilitated. Do not allow the water
10.2 Using the methyl red indicator solution, neutralize the
to enter the crucible while the contents are hot to avoid spattering.
combined solutions from the silica determination with NH OH
7.2 Remove crucible and lid, being careful to scrub and
and add an excess of 2 drops. Bring to a boil adding NH OH
rinse out any adhering particles of the melt. Carefully acidify
1 drop at a time if necessary to maintain a slight alkalinity.
the contents of the casserole with concentrated HCl (sp gr
Allow the precipitate to settle (not more than 5 min) and filter.
1.19); introduce the HCl in small portions, keeping a watch
Wash four times with hot NH Cl solution.
glass over the crucible to avoid loss by spattering.Add 30 mL
10.3 Set aside the filtrate and transfer the precipitate and
ofHClinexcessandevaporatetodrynessonasteambath;take
filter paper to the same beaker in which the first precipitation
care to break up any crusts that form. When the material
was effected. Dissolve the precipitate with 40 mL of hot HCl
appears completely dry, and no odor of HCl can be detected,
(1+3),dilutethesolutiontoabout100mL,andreprecipitatethe
remove the casserole from the steam bath, and allow to cool.
hydroxides as described in 10.2. Filter and wash the precipitate
7.3 Washdownthesidesofthecasserolewith20mLofHCl
four times with hot NH Cl. Combine the filtrate and washings
(sp gr 1.19) and then with water. Repeat the evaporation as
with the filtrate set aside and reserve for the determination of
described in 7.2, then bake for1hinan oven at 105°C. Cool
CaO (Section 10).
the residue, drench with 25 mL of HCl (sp gr 1.19), add 175
10.4 Place the precipitate in a weighed platinum crucible,
mLofwater,andwarm,whilestirring,untilallsolublesaltsare
heat slowly until the papers are charred, and finally ignite to
dissolved. Filter off the silica on a close-texture paper, wash
constant weight at 1050 to 1100°C with care to prevent
fivetimeswithHCl(1+20),washfivetimeswithhotwater,and
reduction. Cool and weigh as R O (aluminum and iron
2 3
reserve the filtrate for determination of other oxides (Section
oxides).
9).
7.4 Transfer the paper and washed silica to a clean platinum 11. Calculation
crucible, ignite, first gently until the filter paper is consumed,
11.1 Calculate the percent of R O as follows:
2 3
and then at 1200°C for 20 min, cool, and weigh. Moisten the
R O ,% 5 P /S 3100 (2)
~ !
2 3 2
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
where:
until H SO has been expelled, and ignite at 1200°C for 5 min.
2 4
P =R O,g,and
2 2 3
Cool and weigh. The loss in weight represents the SiO .
S = sample used, g.
8. Calculation
CALCIUM OXIDE
8.1 Calculate the percent of silica as follows:
12. Reagents
SiO,% 5 P/S 3100 (1)
~ !
12.1 Ammonium Hydroxide (1+1)—Mix 1 volume of con-
where:
centrated NH OH (sp gr 0.90) with 1 volume of water.
P = SiO,g,and
12.2 Ammonium Oxalate Solution—((NH ) C O ·H O),
4 2 2 4 2
S = sample used, g.
saturated.
AMMONIUM HYDROXIDE GROUP 12.3 Ammonium Oxalate Solution (1 g/L)—Dilute 1.0 g of
(Alumina and Iron Oxide)
ammonium oxalate ((NH ) C O ·H O) in 1 L of water.
4 2 2 4 2
12.4 Hydrochloric Acid (1+3)—See 9.3.
9. Reagents
12.5 Hydrochloric Acid (1+1)—Mix 1 volume of concen-
9.1 Ammonium Chloride Soluti
...
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