ASTM D3366-95

Standard Test Method for Color of Maleic Anhydride and Phthalic Anhydride in the Molten State and After Heating (Platinum-Cobalt Scale)

SCOPE
1.1 This test method covers the determination of the visual measurement of the color of maleic and phthalic anhydride melt before and after prolonged heating under specified conditions of time and temperature. Color values are expressed in terms of platinum-cobalt standards.  
1.2 This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this standard to consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific precautionary statements see 7.2.

General Information

• Status: Historical
• Publication Date: 14-Sep-1995
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.02 - Oxygenated Aromatics

Relations

• Replaced By: ASTM D3366-95(2003)e1 - Standard Test Method for Color of Maleic Anhydride and Phthalic Anhydride in the Molten State and After Heating (Platinum-Cobalt Scale) (Withdrawn 2012)
• Effective Date: 10-Feb-2003

Standards Content (Sample)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.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 3366 – 95
Standard Test Method for
Color of Maleic Anhydride and Phthalic Anhydride in the
Molten State and After Heating (Platinum-Cobalt Scale)
This standard is issued under the fixed designation D 3366; 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 OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
1910.1200
1.1 This test method covers the determination of the visual
measurement of the color of maleic and phthalic anhydride
3. Summary of Test Method
melt before and after prolonged heating under specified con-
3.1 A freshly melted specimen is filled to mark into a
ditions of time and temperature. Color values are expressed in
Nessler tube and compared with Platinum-Cobalt color stan-
terms of platinum-cobalt standards. This test method covers the
dards.
range 0 to 100 color standard numbers.
3.2 After heating for2hata prescribed temperature, the
1.2 The following applies to all specified limits in this
specimen is again compared to the color standards.
standard: for purposes of determining conformance with this
standard, an observed value or a calculated value shall be
4. Significance and Use
rounded of “to the nearest unit” in the last right-hand digit used
4.1 The color of maleic anhydride and phthalic anhydride
in expressing the specification limit, in accordance with the
can be an indication of the purity of these materials. High
rounding-off method of Practice E 29.
colors normally indicate contamination.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5. Apparatus
responsibility of the user of this standard to establish appro-
5.1 Color Comparison Tubes—Matched sets of 50-mL
priate safety and health practices and determine the applica-
Nessler tubes having a total length of about 300 mm. The
bility of regulatory limitations prior to use. For specific hazard
height of the 50-mL gradation mark shall be within 200 to 250
statements see Section 7.
mm above the exterior bottom of the tube. In a given set the
graduation marks shall not vary by more than 3 mm. The use
2. Referenced Documents
of heat resistant glass is required.
2.1 ASTM Standards:
2 5.2 Color Comparator, constructed to permit visual com-
D 1193 Specification for Reagent Water
parison of light transmitted through the 50-mL Nessler tubes in
D 1209 Test Method for Color of Clear Liquids (Platinum-
3 the direction of their longitudinal axes. (The comparator should
Cobalt Scale)
be constructed so that white light is reflected off a white plate
D 3438 Practice for Sampling and Handling Naphthalene,
and directed with equal intensity through the tubes, and should
Maleic Anhydride, and Phthalic Anhydride
be shielded so that no light enters the tubes from the side.)
E 29 Practice for Using Significant Digits in Test Data to
Determine Conformance With Specifications
NOTE 1—For convenience of operation, an electrically heated, insulated
comparator tube may be used to prevent the solidification of maleic or
2.2 Other Document:
phthalic anhydride.
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Available from Superintendent of Documents, U.S. Government Printing
Subcommittee D16.02 on Oxygenated Aromatics. Office, Washington, D.C. 20402.
Current edition approved Sept. 15, 1995. Published November 1995. Originally Kimble No. 45315A-50 or H5315B-50 Nessler tubes have been found
published as D 3366 – 74. Last previous edition D 3366 – 90. satisfactory for this test; available from Fisher Scientific, VWR Scientific and other
Annual Book of ASTM Standards, Vol 11.01. laboratory supply houses (Fisher Scientific, Corporate Headquarters, 111 Forbes
Annual Book of ASTM Standards, Vol 06.04. Avenue, Pittsburgh, PA 15219; VWR Scientific, Marketing Department, P.O. Box
Annual Book of ASTM Standards, Vol 14.02. 13645, Philadelphia, PA 19101).
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, 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 3366
5.3 Electric Heating Block —An electrically heated alumi- Safety Data Sheets, and local regulations for materials used in
num block, such as shown in Fig. 1, having the following this test method.
8. Sampling
8.1 Sample in accordance with Practice D 3438.
9. Standards
9.1 Platinum-Cobalt Stock Solution —Dissolve 1.245 g of
K PtCl and 1.000 g of CoCl ·6H O in water. Add 100 mL of
2 6 2 2
HCl and dilute to 1 L with water. This solution is defined as
color standard No. 500.
9.2 Platinum Cobalt Standards —From the stock solution,
prepare color standards by diluting the required volumes as
given in Table 1, to 50 mL with water in the Nessler tubes.
A
TABLE 1 Platinum—Cobalt Color Standards
Color Stock Color Stock
Standard Solution Standard Solution
No. mL No. mL
5 0.5 35 3.5
10 1.0 40 4.0
FIG. 1 Heat Stability Block
15 1.5 50 5.0
20 2.0 60 6.0
25 2.5 70 7.0
operating characteristics:
30 3.0 100 10.0
Maleic anhydride temperature regulation,° C 140 6 2
A
Other color standards may be prepared by proportional dilution in steps of 20
Heating time for sample from 60 to 140°C, minutes 25 6 5
as follows: No. 120, No. 140, No. 160, etc.
Phthalic anhydride temperature regulation,° C 250 6 2
Heating time for sample from 150 to 250°C, minutes 25 6 5
Temperature gradient, sample well to thermometer well, °C max 2
When not in use, protect these standards from contamination
The operating characteristics of the heating block used are
and evaporation by the use of suitable caps on the tubes.
critical.
10. Procedure
6. Reagents
10.1 Melt an approximately 75-g sample (Note 2) and
6.1 Purity of Reagents—Reagent grade chemicals shall be
simultaneously preheat a Nessler tube in an oven, electric
used in all tests. Unless otherwise indicated it is intended that
heating block, or other similar equipmen
...