ASTM D1394-76(2020)

Standard Test Methods for Chemical Analysis of White Titanium Pigments

ABSTRACT
These test methods cover procedures for the chemical analysis of white titanium dioxide pigments. The analytical procedures appear in the following order: sample preparation, qualitative analysis, moisture content determination, total titanium content determination by Jones Reductor and Aluminum Reduction methods, aluminum oxide content determination, and silica content determination. The reagents to be used shall include ammonium hydroxide, ammonium sulfate, hydrochloric acid, hydrogen peroxide, hydrogen sulfide, sulfuric acid, tartaric acid, tin, zinc, carbon steel, iron, ferric sulfate solution, nitric acid, sodium oxalate, potassium permanganate, aluminum metal foil, ammonium thiocyanate indicator solution, ferritic ammonium sulfate solution, sodium bicarbonate solution, sulfuric acid, titanium dioxide, acetic acid, ammonium phosphate, EDTA solution, methyl orange indicator solution, sodium bisulfate monohydrate, sodium fluoride, xylenol orange indicator solution, and zinc sulfate solution.
SCOPE
1.1 These test methods cover procedures for the chemical analysis of white titanium dioxide pigments.  
1.2 The analytical procedures appear in the following order:    
Sections  
Preparation of Sample  
4  
Qualitative Analysis  
5 and 6  
Moisture  
7  
Total Titanium:  
Jones Reductor Method  
8 – 12  
Aluminum Reduction Method  
13 – 17  
Aluminum Oxide  
18 – 22  
Silica  
23 – 29  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. A specific hazard statement is given in Section 19.  
1.5 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.

General Information

• Status: Published
• Publication Date: 31-May-2020
• ICS: 87.060.10 - Pigments and extenders
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.31 - Pigment Specifications

Relations

• Referred By: ASTM D4563-02(2022) - Standard Test Method for Determination by Atomic Absorption Spectroscopy of Titanium Dioxide Content of Pigments Recovered From Whole Paint
• Effective Date: 01-Jun-2020
• Referred By: ASTM D476-15(2021) - Standard Classification for Dry Pigmentary Titanium Dioxide Products
• Effective Date: 01-Jun-2020
• Referred By: ASTM D4764-01(2023) - Standard Test Method for Determination by X-ray Fluorescence Spectroscopy of Titanium Dioxide Content in Paint
• Effective Date: 01-Jun-2020
• Referred By: ASTM D3280-85(2020) - Standard Test Methods for Analysis of White Zinc Pigments
• Effective Date: 01-Jun-2020
• Referred By: ASTM D4797-17(2022) - Standard Test Methods for Gravimetric Analysis of White and Yellow Thermoplastic Pavement Marking
• Effective Date: 01-Jun-2020

Standards Content (Sample)

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: D1394 − 76 (Reapproved 2020)
Standard Test Methods for
1
Chemical Analysis of White Titanium Pigments
This standard is issued under the fixed designation D1394; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope E50Practices for Apparatus, Reagents, and Safety Consid-
erations for Chemical Analysis of Metals, Ores, and
1.1 These test methods cover procedures for the chemical
Related Materials
analysis of white titanium dioxide pigments.
1.2 Theanalyticalproceduresappearinthefollowingorder:
3. Reagents
Sections
3.1 Purity of Reagent—Reagent grade chemicals shall be
Preparation of Sample 4
used in all tests. Unless otherwise indicated, it is intended that
Qualitative Analysis 5 and 6
Moisture 7 all reagents shall conform to the specifications of the Commit-
Total Titanium:
tee onAnalytical Reagents of theAmerican Chemical Society,
Jones Reductor Method 8–12
3
where such specifications are available. Other grades may be
Aluminum Reduction Method 13–17
Aluminum Oxide 18–22
used, provided it is first ascertained that the reagent is of
Silica 23–29
sufficiently high purity to permit its use without lessening the
1.3 The values stated in SI units are to be regarded as
accuracy of the determination.
standard. No other units of measurement are included in this
3.2 Unless otherwise indicated, references to water shall be
standard.
understood to mean reagent water conforming to Type IV of
1.4 This standard does not purport to address all of the
Specification D1193.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Preparation of Sample
priate safety, health, and environmental practices and deter-
4.1 The sample shall, in all cases, be thoroughly mixed and
mine the applicability of regulatory limitations prior to use. A
comminuted before taking portions for analysis.
specific hazard statement is given in Section 19.
1.5 This international standard was developed in accor-
QUALITATIVE ANALYSIS
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the 5. Reagents
Development of International Standards, Guides and Recom-
5.1 Ammonium Hydroxide (sp gr 0.90)—Concentrated am-
mendations issued by the World Trade Organization Technical
monium hydroxide (NH OH).
4
Barriers to Trade (TBT) Committee.
5.2 Ammonium Sulfate—((NH ) SO ).
4 2 4
2. Referenced Documents
5.3 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
2
chloric acid (HCl).
2.1 ASTM Standards:
D280Test Methods for Hygroscopic Moisture (and Other
5.4 Hydrogen Peroxide (30 %)—Concentrated hydrogen
Matter Volatile Under the Test Conditions) in Pigments
peroxide (H O ).
2 2
D1193Specification for Reagent Water
5.5 Hydrogen Sulfide (H S).
2
5.6 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
1
These test methods are under the jurisdiction of ASTM Committee D01 on
(H SO ).
2 4
Paint and Related Coatings, Materials, and Applications and are the direct
responsibility of Subcommittee D01.31 on Pigment Specifications.
Current edition approved June 1, 2020. Published June 2020. Originally
3
approved in 1956. Last previous edition approved in 2014 as D1394–76(2014). ACS Reagent Chemicals, Specifications and Procedures for Reagents and
DOI: 10.1520/D1394-76R20. Standard-Grade Reference Materials, American Chemical Society, Washington,
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or DC. For suggestions on the testing of reagents not listed by theAmerican Chemical
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
Standards volume information, refer to the standard’s Document Summary page on U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
the ASTM website. copeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D1394 − 76 (2020)
5.7 Sulfuric Acid (1+19)—Carefully mix 1 volume of
H SO (sp gr 1.84) with 19 volumes of water.
2 4
5.8 Tartaric Acid.
5.9 Tin or Zinc Metal.
6. Procedure
6.1 Place about 0.5 g of the sample in a 250-mL glass
4
beaker, and add 20 mLof H
...