ASTM D1977-03

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

SIGNIFICANCE AND USE
This test method is a procedure by which catalyst samples may be compared on an inter- or intra-laboratory basis. Catalyst producers and user should find this test method to be of value.
SCOPE
1.1 This test method covers the determination of nickel and vanadium in equilibrium catalysts where the vanadium and nickel concentrations are greater than 50 and 25 mg/kg, respectively.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses re for information only.
1.3 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.

General Information

• Status: Historical
• Publication Date: 30-Sep-2003
• ICS: 77.120.40 - Nickel, chromium and their alloys
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.03 - Chemical Composition

Relations

• Replaces: ASTM D1977-98 - 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
• Replaced By: ASTM D1977-03(2008) - Standard Test Method for Nickel and Vanadium in FCC Equilibrium Catalysts by Hydrofluoric/Sulfuric Acid Decomposition and Atomic Spectroscopic Analysis
• Effective Date: 01-Apr-2008
• 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: 01-Oct-2003

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 1977 – 03
Standard Test Method for
Nickel and Vanadium in FCC Equilibrium Catalysts by
Hydrofluoric/Sulfuric Acid Decomposition and Atomic
1
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 3. Terminology
1.1 This test method covers the determination of nickel and 3.1 Definitions—See Terminology D 3766.
vanadium in equilibrium catalysts where the vanadium and
4. Summary of Test Method
nickel concentrations are greater than 50 and 25 mg/kg,
4.1 The test specimen (as received) is decomposed with
respectively.
1.2 The values stated in SI units are to be regarded as the hydrofluoricandsulfuricacids.Aftercompletevolatilizationof
thehydrofluoricacidandcooling,thesulfatesaltsaredilutedto
standard. The values given in parentheses are for information
only. the appropriate concentration range for analysis by flame
atomic absorption, direct current plasma emission, or induc-
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the tively coupled plasma emission spectroscopies.The instrument
is calibrated with matrix-matched standards. Solutions of the
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- test specimen are analyzed.
bility of regulatory limitations prior to use.
5. Significance and Use
2. Referenced Documents
5.1 This test method is a procedure by which catalyst
2
samples may be compared on an inter- or intra-laboratory
2.1 ASTM Standards:
D 1193 Specification for Reagent Water basis. Catalyst producers and user should find this test method
to be of value.
D 3766 Terminology Relating to Catalysts and Catalysis
E 105 Practice for Probability Sampling of Materials
6. Interferences
E 177 Practice for Use of the Terms Precision and Bias in
6.1 The enhancement of alumina in the samples are over-
ASTM Test Methods
come by using matrix-matched standards. Any dilutions
E 288 Specification for Laboratory Glass Volumetric Flasks
needed to achieve the working ranges for vanadium and nickel
E 456 Terminology Relating to Quality and Statistics
must contain the same Al O (7800 ppm) concentration as the
E 691 Practice for Conducting an Interlaboratory Study to
2 3
standards.
Determine the Precision of a Test Method
6.2 If using optical emission, consult tables showing inter-
2.2 U.S. Federal Specification
3
fering line near analyte lines; if significant overlap occurs, one
Federal Spec NNN-P-395C Tolerance for Class A Pipets
must apply inter-element correction or choose an alternate
emission line.
1
This test method is under the jurisdiction of ASTM Committee D32 on
7. Apparatus
Catalysts and is the direct responsibility of Subcommittee D32.03 on Chemical
Composition.
7.1 Analytical Balance, capable of weighing to nearest 0.1
Current edition approved Oct. 1, 2003. Published October 2003. Originally
mg.
approved in 1991. Last previous edition approved in 1998 as D 1977–98.
2
7.2 Hot Plate, capable of maintaining 250 6 10°C at
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
surface.
Standards volume information, refer to the standard’s Document Summary page on
7.3 TFE Fluorocarbon Beaker, 250 mL.
the ASTM website.
3 7.4 Volumetric Flasks, borosilicate glass, 50, 100, 250, 500,
AvailablefromStandardizationDocumentsOrderDesk,Bldg.4SectionD,700
Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. and 1000-mL capacity conforming to Specification E 288.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D1977–03
7.5 Pipettes, borosilicate glass, 5, 10, and 25 mL, conform- 50.0, and 100.0 mL of the 1000–mg/L solution to 1000-mL
ing to Federal Specification NNN-P-395C. volumetric flasks containing 200 mL of the 39 000– mg/L
7.6 Bottles, polyethylene, 100 and 1000 mL. Al O solution and 100 mL concentrated hydrochloric acid.
2 3
Dilute solutions to volume with distilled water and store in
8. Reagents
polyethylene bottles.
8.1 Purity of Reagents—Reagent grade chemicals shall be
10. Sampling
used in all tests. Unless otherwise indicated, it is intended that
all reagents conform to the specifications of the Committee on
10.1 The selection of a representative analytical sample
Analytical Reagents of theAmerican Chemical Society, where
from the bulk material is outside the scope of
...