ASTM D717-86(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: D717 − 86 (Reapproved 2020)
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 E97 Method of Test for Directional Reflectance Factor,
45-Deg 0-Deg, of Opaque Specimens by Broad-Band
1.1 These test methods cover the analysis of magnesium
Filter Reflectometry (Withdrawn 1991)
silicate pigment.
1.2 The values stated in SI units are to be regarded as the
3. Significance and Use
standard. The values given in parentheses are for information
3.1 These test methods may be used to confirm the stated
only.
SiO , CaO, and MgO content of magnesium silicate for quality
1.3 This standard does not purport to address all of the
control.
safety concerns, if any, associated with its use. It is the
4. Apparatus
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
4.1 Platinum Crucible.
mine the applicability of regulatory limitations prior to use.
4.2 Electric Furnace, capable of 1200°C.
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard-
5. Purity of Reagents
ization established in the Decision on Principles for the
5.1 Reagent grade chemicals shall be used in all tests.
Development of International Standards, Guides and Recom-
Unless otherwise indicated, it is intended that all reagents shall
mendations issued by the World Trade Organization Technical
conform to the specifications of the Committee on Analytical
Barriers to Trade (TBT) Committee.
Reagents of the American Chemical Society, where such
specifications are available. Other grades may be used, pro-
2. Referenced Documents
vided it is first ascertained that the reagent is of sufficiently
2.1 ASTM Standards:
high purity to permit its use without lessening the accuracy of
D234 Specification for Raw Linseed Oil (Withdrawn 2007)
the determination.
D280 Test Methods for Hygroscopic Moisture (and Other
5.2 Unless otherwise indicated, references to water shall be
Matter Volatile Under the Test Conditions) in Pigments
understood to mean Type II of Specification D1193.
D718 Test Methods for Analysis of Aluminum Silicate
Pigment
SILICON DIOXIDE
D1193 Specification for Reagent Water
D1208 Test Methods for Common Properties of Certain
6. Reagents
Pigments
6.1 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
D2448 Test Method for Water-Soluble Salts in Pigments by
chloric acid (HCl).
Measuring the Specific Resistance of the Leachate of the
6.2 Hydrochloric Acid (1+20)—Mix 1 volume of concen-
Pigment
trated hydrochloric acid (HCl, sp gr 1.19) with 20 volumes of
water.
1 6.3 Hydrofluoric Acid (48 %)—Concentrated hydrofluoric
These test methods are under the jurisdiction of ASTM Committee D01 on
Paint and Related Coatings, Materials, and Applications and are the direct acid (HF).
responsibility of Subcommittee D01.31 on Pigment Specifications.
6.4 Sodium Carbonate (Na CO ).
Current edition approved June 1, 2020. Published June 2020. Originally 2 3
approved in 1943. Last previous edition approved in 2014 as D717 – 86 (2014).
DOI: 10.1520/D0717-86R20.
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or ACS Reagent Chemicals, Specifications and Procedures for Reagents and
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standard-Grade Reference Materials, American Chemical Society, Washington,
Standards volume information, refer to the standard’s Document Summary page on DC. For suggestions on the testing of reagents not listed by theAmerican Chemical
the ASTM website. Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
The last approved version of this historical standard is referenced on U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
www.astm.org. copeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D717 − 86 (2020)
6.5 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid 9.3 Hydrochloric Acid (1+3)—Mix 1 volume of concen-
(H SO ). trated HCl (sp gr 1.19) with 3 volumes of water.
2 4
9.4 Methyl Red Indicator Solution—Dissolve 0.2 g of
7. Procedure
methyl red in 100 mL of methanol, ethanol, or isopropanol.
7.1 Transfer1gofthe sample weighed to 0.1 mg to a
9.5 Potassium Pyrosulfate—(K S O ).
2 2 7
platinum crucible and fuse with5gofNa CO until the entire
2 3
contents of the crucible are in a molten state. Continue heating
10. Procedure
for 20 min. Keep a close-fitting platinum cover on the crucible
during the fusion. When the fusion is complete, allow the
10.1 If an appreciable residue remains after the treatment
crucible and contents to cool, and transfer to a 600-mL
with HF in accordance with 7.4, fuse the residue with a small
porcelain casserole containing 200 mL of water (Note 1). Boil
amount of K S O until it is dissolved. Leach the pyrosulfate
2 2 7
until the melt is disintegrated.
melt out of the crucible with water and combine the solution
with the filtrate reserved in accordance with 7.3.
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,
10.2 Using the methyl red indicator solution, neutralize the
the subsequent removal of the melt is facilitated. Do not allow the water
combined solutions from the silica determination with NH OH
to enter the crucible while the contents are hot to avoid spattering.
and add an excess of 2 drops. Bring to a boil adding NH OH
7.2 Remove crucible and lid, being careful to scrub and
1 drop at a time if necessary to maintain a slight alkalinity.
rinse out any adhering particles of the melt. Carefully acidify
Allow the precipitate to settle (not more than 5 min) and filter.
the contents of the casserole with concentrated HCl (sp gr
Wash four times with hot NH Cl solution.
1.19); introduce the HCl in small portions, keeping a watch
10.3 Set aside the filtrate and transfer the precipitate and
glass over the crucible to avoid loss by spattering.Add 30 mL
filter paper to the same beaker in which the first precipitation
ofHClinexcessandevaporatetodrynessonasteambath;take
was effected. Dissolve the precipitate with 40 mL of hot HCl
care to break up any crusts that form. When the material
(1+3),dilutethesolutiontoabout100mL,andreprecipitatethe
appears completely dry, and no odor of HCl can be detected,
hydroxides as described in 10.2. Filter and wash the precipitate
remove the casserole from the steam bath, and allow to cool.
four times with hot NH Cl. Combine the filtrate and washings
7.3 Washdownthesidesofthecasserolewith20mLofHCl
with the filtrate set aside and reserve for the determination of
(sp gr 1.19) and then with water. Repeat the evaporation as
CaO (Section 10).
described in 7.2, then bake for1hinan oven at 105°C. Cool
10.4 Place the precipitate in a weighed platinum crucible,
the residue, drench with 25 mL of HCl (sp gr 1.19), add 175
heat slowly until the papers are charred, and finally ignite to
mLofwater,andwarm,whilestirring,untilallsolublesaltsare
constant weight at 1050 to 1100°C with care to prevent
dissolved. Filter off the silica on a close-texture paper, wash
reduction. Cool and weigh as R O (aluminum and iron
fivetimeswithHCl(1+20),washfivetimeswithhotwater,and 2 3
oxides).
reserve the filtrate for determination of other oxides (Section
9).
11. Calculation
7.4 Transfer the paper and washed silica to a clean platinum
11.1 Calculate the percent of R O as follows:
crucible, ignite, first gently until the filter paper is consumed,
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
where:
mL of HF. Evaporate to dryness on a steam bath, heat gently
P =R O,g,and
until H SO has been expelled, and ignite at 1200°C for 5 min.
2 4 2 2 3
S = sample used, g.
Cool and weigh. The loss in weight represents the SiO .
8. Calculation CALCIUM OXIDE
8.1 Calculate the percent of silica as follows:
12. Reagents
SiO,% 5 ~P/S! 3100 (1)
12.1 Ammonium Hydroxi
...