ASTM D1977-98

Standard Test Method for Nickel and Vanadium in FCC Equilibrium Catalysts by Hydrofluoric/Sulfuric Acid Decomposition and Atomic Spectroscopic Analysis

SCOPE
1.1 This test method evaluates the effect of a circulating engine coolant on metal test specimens and automotive cooling system components under controlled, essentially isothermal laboratory conditions.
1.2 This test method specifies test material, cooling system components, type of coolant, and coolant flow conditions that are considered typical of current automotive use.
1.3 The values stated in either SI or inch-pound units are to be regarded as the standard. The values given in parentheses are approximate equivalents for information only.
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 and health practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 6.

General Information

• Status: Historical
• Publication Date: 09-Mar-1998
• ICS: 77.120.40 - Nickel, chromium and their alloys
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.03 - Chemical Composition

Relations

• Replaced By: ASTM D1977-03 - Standard Test Method for Nickel and Vanadium in FCC Equilibrium Catalysts by Hydrofluoric/Sulfuric Acid Decomposition and Atomic Spectroscopic Analysis
• Effective Date: 01-Oct-2003
• Referred By: ASTM D7085-04(2018) - Standard Guide for Determination of Chemical Elements in Fluid Catalytic Cracking Catalysts by X-ray Fluorescence Spectrometry (XRF)
• Effective Date: 10-Mar-1998

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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.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 1977 – 98
Standard Test Method for
Nickel and Vanadium in FCC Equilibrium Catalysts by
Hydrofluoric/Sulfuric Acid Decomposition and Atomic
Spectroscopic Analysis
This standard is issued under the fixed designation D 1977; 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. Significance and Use
1.1 This test method is intended for the determination of 4.1 This test method is a procedure by which catalyst
nickel and vanadium in equilibrium catalysts where the vana- samples may be compared on an inter- or intra-laboratory
dium and nickel concentrations are greater than 50 and 25 basis. Catalyst producers and user should find this test method
mg/kg, respectively. to be of value.
1.2 This standard does not purport to address all of the
5. Interferences
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 5.1 The enhancement of alumina in the samples are over-
come by using matrix-matched standards. Any dilutions
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. needed to achieve the working ranges for vanadium and nickel
must contain the same Al O (7800 ppm) concentration as the
2 3
2. Referenced Documents
standards.
2.1 ASTM Standards: 5.2 If using optical emission, consult tables showing inter-
D 1193 Specifications for Reagent Water fering line near analyte lines; if significant overlap occurs, one
E 105 Practice for Probability Sampling of Materials must apply inter-element correction or choose an alternate
E 177 Practice for Use of the Terms Precision and Bias in emission line.
ASTM Test Methods
6. Apparatus
E 288 Specification for Laboratory Glass Volumetric
Flasks 6.1 Analytical balance, capable of weighing to nearest 0.1
mg.
E 456 Terminology Relating to Quality and Statistics
E 691 Practice for Conducting an Interlaboratory Study to 6.2 Hot plate, capable of maintaining 250°C 6 10°C at
surface.
Determine the Precision of a Test Method
2.2 U.S. Federal Specification 6.3 TFE fluorocarbon beaker, 250 mL.
6.4 Volumetric flasks, borosilicate glass, 50, 100, 250, 500,
Federal Spec NNN-P-395C Tolerance for Class A Pipets
and 1000-mL capacity conforming to Specification E 288.
3. Summary of Test Method
6.5 Pipettes, borosilicate glass, 5, 10, and 25 mL, conform-
3.1 The test specimen (as received) is decomposed with ing to Federal Specification NNN-P-395C.
hydrofluoric and sulfuric acids. After complete volatilization of 6.6 Bottles, polyethylene, 100 and 1000 mL.
the hydrofluoric acid and cooling, the sulfate salts are diluted to
7. Reagents
the appropriate concentration range for analysis by flame
atomic absorption, direct current plasma emission, or induc- 7.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
tively coupled plasma emission spectroscopies. The instrument
is calibrated with matrix-matched standards. Solutions of the all reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society, where
test specimen are analyzed.
such specifications are available. Other grades may be used,
provided it is first ascertained that the reagent is of sufficient
This test method is under the jurisdiction of ASTM Committee D-32 on
Catalyst and is the direct responsibility of Subcommittee D-32.03 on Chemical
Composition.
Current edition approved March 10, 1998. Published October 1998. Originally “Reagent Chemicals, American Chemical Society Specifications, American
published as D 1977–91. Last previous edition D 1977–91. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Annual Book of ASTM Standards, Vol 11.01. listed by the American Chemical Society, see “Analar Standards for Laboratory
Annual Book of ASTM Standards, Vol 14.02. U.K. Chemicals,” BDH Ltd., Poole, Dorset, and the United States Pharamacopeia
Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 and National Formulary, U. S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. MD.
Copyright © ASTM, 100 Barr Harbor Drive, 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 1977
purity to permit its use without lessening the accuracy of the 10.3 Transfer beaker and contents to a hot plate (no hotter
determination. than 250°C to avoid melting the beaker) and evaporate to near
7.2 Purity of Water—Unless otherwise indicated, references dryness.
to water shall be understood to mean type IV reagent water, as 10.4 Remove beaker from hot plate and cool to ambient
defined in Specification D 1193. temperature.
7.3 Required Reagents: 10.5 Add 20 mL 19 % hydrochloric acid and 30 mL 3%
7.3.1 Hydrofluoric acid (HF), concentrated, 48 %. hydrogen peroxide, cover with watch glass and return beaker to
7.3.2 Sulfuric acid,(H SO ), concentrated, 98 %. hot plate.
2 4
7.3.3 Sulfuric acid, 49 volume %, add slowly, while stirring, 10.6 Heat solution to boiling and continue to boil until all
one part of concentrated H SO (98 %) to one part of water, the salts are dissolved.
2 4
then cool. 10.7 After dissolution is complete, remove beaker from hot
7.3.4 Hydrochloric acid, concentrated, 38 %. plate and cool to ambient temperature.
7.3.5 Hydrochloric acid, 19 volume %, add slowly, while 10.8 Wash watch glass, catching washings in the beaker,
stirring, one part o
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