ASTM D1977-16
(Test Method)Standard Test Method for Nickel and Vanadium in FCC Equilibrium Catalysts by Hydrofluoric/Sulfuric Acid Decomposition and Atomic Spectroscopic Analysis
Standard Test Method for Nickel and Vanadium in FCC Equilibrium Catalysts by Hydrofluoric/Sulfuric Acid Decomposition and Atomic Spectroscopic Analysis
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.
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 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 and health practices and determine the applicability of regulatory limitations prior to use.
General Information
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Designation: D1977 −16
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 D1977; 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.
1. Scope 3. Terminology
1.1 This test method covers the determination of nickel and 3.1 Definitions—See Terminology D3766.
vanadium in equilibrium catalysts where the vanadium and
4. Summary of Test Method
nickel concentrations are greater than 50 and 25 mg/kg,
respectively.
4.1 The test specimen (as received) is decomposed with
hydrofluoricandsulfuricacids.Aftercompletevolatilizationof
1.2 The values stated in SI units are to be regarded as
thehydrofluoricacidandcooling,thesulfatesaltsaredilutedto
standard. No other units of measurement are included in this
the appropriate concentration range for analysis by flame
standard.
atomic absorption, direct current plasma emission, or induc-
1.3 This standard does not purport to address all of the
tivelycoupledplasmaemissionspectroscopies.Theinstrument
safety concerns, if any, associated with its use. It is the
is calibrated with matrix-matched standards. Solutions of the
responsibility of the user of this standard to establish appro-
test specimen are analyzed.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5. Significance and Use
5.1 This test method is a procedure by which catalyst
2. Referenced Documents
samples may be compared on an inter- or intra-laboratory
2
2.1 ASTM Standards:
basis. Catalyst producers and user should find this test method
D1193Specification for Reagent Water
to be of value.
D3766Terminology Relating to Catalysts and Catalysis
E105Practice for Probability Sampling of Materials
6. Interferences
E177Practice 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
E288Specification for Laboratory Glass Volumetric Flasks
needed to achieve the working ranges for vanadium and nickel
E456Terminology Relating to Quality and Statistics
must contain the sameAl O (7800 ppm) concentration as the
2 3
E691Practice for Conducting an Interlaboratory Study to
standards.
Determine the Precision of a Test Method
3
6.2 If using optical emission, consult tables showing inter-
2.2 U.S. Federal Specification:
fering line near analyte lines; if significant overlap occurs, one
Federal Specification NNN-P-395CTolerance for Class A
must apply interelement correction or choose an alternate
Pipets
emission line.
7. Apparatus
1
This test method is under the jurisdiction of ASTM Committee D32 on
7.1 Analytical Balance, capable of weighing to nearest
Catalysts and is the direct responsibility of Subcommittee D32.03 on Chemical
Composition. 0.1mg.
Current edition approved March 1, 2016. Published April 2016. Originally
7.2 Hot Plate, capable of maintaining 250 6 10°C at
approved in 1991. Last previous edition approved in 2008 as D1977–03 (2008).
DOI: 10.1520/D1977-16. surface.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
7.3 PTFE Fluorocarbon Beaker, 250 mL and PTFE watch
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 glass.
the ASTM website.
3
7.4 Volumetric Flasks, borosilicate glass, 50, 100, 250, 500,
Available from DLA Document Services, Building 4/D, 700 Robbins Ave.,
Philadelphia, PA 19111-5094, http://quicksearch.dla.mil. and 1000-mL capacity conforming to Specification E288.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D1977 − 16
7.5 Pipettes, borosilicate glass, 5, 10, and 25 mL, conform- 50.0mL of the 1000-mg/L solution to 1000-mL volumetric
ing to Federal Specification NNN-P-395C. flasks containing 200 mL of the 39000-mg⁄LAl O solution
2 3
and100mLconcentratedhydrochloricacid.Dilutesolutionsto
7.6 Bottles, polyethylene, 100 and 1000 mL.
volume with distilled water and store in polyethylene bottles.
8. Reagents
10.2 Vanadium—Prepare standard solutions containing 0,
8.1 Purity of Reagents—Reagent grade chemicals shall be 10.0, 25.0, 50.0 and 100.0 mg/L V in a matrix of 7800 mg/L
Al O and10%hydrochloricacidbytransferring0,10.0,25.0,
used in all tests. Unless otherwise indicated, it is intended that
2 3
all reagents conform to the specifications of the Commit
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D1977 − 03 (Reapproved 2008) D1977 − 16
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 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 25 mg/kg, respectively.
1.2 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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D3766 Terminology Relating to Catalysts and Catalysis
E105 Practice 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
3
2.2 U.S. Federal Specification:
Federal Specification NNN-P-395C Tolerance for Class A Pipets
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.
1
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 April 1, 2008March 1, 2016. Published April 2008April 2016. Originally approved in 1991. Last previous edition approved in 20032008 as
D1977–03. –03 (2008). DOI: 10.1520/D1977-03R08.10.1520/D1977-16.
2
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.
3
Available from Standardization Documents Order Desk, Bldg. 4 Section D, DLA Document Services, Building 4/D, 700 Robbins Ave., Philadelphia, PA 19111-5094,
Attn: NPODS.http://quicksearch.dla.mil.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D1977 − 16
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°C at surface.
7.3 TFEPTFE Fluorocarbon Beaker, 250 mL.mL and PTFE watch glass.
7.4 Volumetric Flasks, borosilicate glass, 50, 100, 250, 500, and 1000-mL capacity conforming to Specification E288.
7.5 Pipettes, borosilicate glass, 5, 10, and 25 mL, conforming to Federal Specification NNN-P-395C.
7.6 Bottles, polyethylene, 100 and 1000 mL.
8. Reagents
8.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that
...
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