ASTM D1977-22

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Designation: D1977 − 16 D1977 − 22
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 D1977; 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
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 2525 mg mg/kg, ⁄kg, respectively.
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this
standard.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.4 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.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D3766 Terminology Relating to Catalysts and Catalysis
D4481 Test Method for Total Nickel in Fresh Alumina-Base Catalysts
D7442 Practice for Sample Preparation of Fluid Catalytic Cracking Catalysts and Zeolites for Elemental Analysis by Inductively
Coupled Plasma Optical Emission Spectroscopy
E105 Guide for Probability Sampling of Materials
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E288 Specification for Laboratory Glass Volumetric Flasks
E456 Terminology Relating to Quality and Statistics
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
2.2 U.S. Federal Specification:
Federal Specification NNN-P-395C Tolerance for Class A Pipets
This test method is under the jurisdiction of ASTM Committee D32 on Catalysts and is the direct responsibility of Subcommittee D32.03 on Chemical Composition.
Current edition approved March 1, 2016Aug. 1, 2022. Published April 2016August 2022. Originally approved in 1991. Last previous edition approved in 20082016 as
D1977D1977 – 16.–03 (2008). DOI: 10.1520/D1977-16.10.1520/D1977-22.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
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D1977 − 22
3. Terminology
3.1 Definitions—See Terminology D3766.
4. Summary of Test Method
4.1 The test specimen (as received) is decomposed with hydrofluoric and sulfuric acids. After complete volatilization of the
hydrofluoric acid and cooling, the sulfate salts are diluted to the appropriate concentration range for analysis by flame atomic
absorption, direct current plasma emission, or inductively coupled plasma emission spectroscopies. The instrument is calibrated
with matrix-matched standards. Solutions of the test specimen are analyzed.
5. Significance and Use
5.1 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.
6. Interferences
6.1 The enhancement of alumina in the samples are overcome by using matrix-matched standards. Any dilutions needed to achieve
the working ranges for vanadium and nickel must contain the same Al O (7800 ppm) concentration as the standards.
2 3
6.2 If using optical emission, consult tables showing interfering line near analyte lines; if significant overlap occurs, one must
apply interelement correction or choose an alternate emission line.
7. Apparatus
7.1 Analytical Balance, capable of weighing to nearest 0.1 mg.
7.2 Hot Plate, capable of maintaining 250 6 10°C10 °C at surface.
7.3 PTFE Fluorocarbon Beaker, 250 mL and PTFE watch glass.
7.4 Volumetric Flasks, borosilicate glass, 50, 100, 250, 500, and 1000-mL1000 mL capacity conforming to Specification E288.
7.5 Pipettes, borosilicate glass, 5, 10, and 25 mL, 25 mL, conforming to Federal Specification NNN-P-395C.
7.6 Bottles, polyethylene, 100 and 1000 mL.1000 mL.
7.7 Laboratory Fume Hood suitable for use with hydrofluoric acid.
8. Reagents
8.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such
specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficient purity to
permit its use without lessening the accuracy of the determination.
8.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean type IV reagent water or better,
as defined in Specification D1193.
8.3 Required Reagents:
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed by
the American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USP), Rockville, MD.
D1977 − 22
8.3.1 Hydrofluoric Acid (HF), concentrated, 48 %.
8.3.2 Sulfuric Acid, (H SO ), concentrated, 98 %.
2 4
8.3.3 Sulfuric Acid, 49 volume %, add slowly, while stirring, one part of concentrated H SO (98 %) to one part of water, then
2 4
cool.
8.3.4 Hydrochloric Acid, concentrated, 38 %.
8.3.5 Hydrochloric Acid, 19 volume %, add slowly, while stirring, one part of concentrated HCl (38 %) to one part of water, then
cool.
8.3.6 Nitric Acid (HNO ), concentrated, 70 %.
8.3.7 Reference Standard Solution—1000 mg/L nickel (see Note 1).
NOTE 1—If emission spectrometry is to be used, standards must contain no interfering element(s) in concentration(s) great enough to yield an interference
of more than 0.1% of the analytical response.
8.3.8 Reference Standard Solution—1000 mg/L vanadium (see Note 1).
8.3.9 Aluminum Chloride, reagent grade, AlCl ·6H O
3 2
8.3.10 Aluminum Stock Solution—39 000 mg/L Al O , dissolve 184.5 g of AlCl ·6H O in water and dilute to 1 L and store in a
2 3 3 2
polyethylene bottle.
8.3.11 Hydrogen Peroxide—3 % solution.
9. Sampling
9.1 The selection of a representative analytical sample from the bulk material is outside the scope of this test method. Parties using
this test method for comparison purposes will have agreed on the selection of an analytical sample. If a sampling procedure is
desired, Practice E105 is recommended.
10. Preparation of Standards
10.1 Nickel—Prepare standard solutions containing 0, 5.0, 20.0, and 50.0 mg/L Ni in a matrix of 7800 mg/L Al O and 10 %
2 3
hydrochloric acid by transferring 0, 5.0, 20.0, and 50.0 mL of the 1000-mg/L solution to 1000-mL1000 mL volumetric flasks
containing 200 mL of the 39 000-mg39 000 mg ⁄L Al O
...