ASTM D1977-03(2008)
(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
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.
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Designation:D1977 −03(Reapproved 2008)
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.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
nickel concentrations are greater than 50 and 25 mg/kg,
4. Summary of Test Method
respectively.
4.1 The test specimen (as received) is decomposed with
1.2 The values stated in SI units are to be regarded as
hydrofluoricandsulfuricacids.Aftercompletevolatilizationof
standard. No other units of measurement are included in this
thehydrofluoricacidandcooling,thesulfatesaltsaredilutedto
standard.
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
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
2. Referenced Documents
5.1 This test method is a procedure by which catalyst
samples may be compared on an inter- or intra-laboratory
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
ASTM Test Methods
6.1 The enhancement of alumina in the samples are over-
E288Specification for Laboratory Glass Volumetric Flasks
come by using matrix-matched standards. Any dilutions
E456Terminology Relating to Quality and Statistics
needed to achieve the working ranges for vanadium and nickel
E691Practice for Conducting an Interlaboratory Study to
must contain the sameAl O (7800 ppm) concentration as the
2 3
Determine the Precision of a Test Method
standards.
2.2 U.S. Federal Specification:
6.2 If using optical emission, consult tables showing inter-
Federal Specification NNN-P-395CTolerance for Class A
fering line near analyte lines; if significant overlap occurs, one
Pipets
must apply interelement correction or choose an alternate
emission line.
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
7.1 Analytical Balance, capable of weighing to nearest
Composition.
Current edition approved April 1, 2008. Published April 2008. Originally
0.1mg.
approved in 1991. Last previous edition approved in 2003 as D1977–03. DOI:
10.1520/D1977-03R08. 7.2 Hot Plate, capable of maintaining 250 6 10°C at
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
surface.
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 7.3 TFE Fluorocarbon Beaker, 250 mL.
the ASTM website.
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 E288.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1977−03 (2008)
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/L Al 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,
10.0, 25.0, 50.0 and 100.0 mg/L V in a matrix of 7800 mg/L
8.1 Purity of Reagents—Reagent grade chemicals shall be
Al O and10%hydrochloricacidbytransferring0,10.0,25.0,
used in all tests. Unless otherwise indicated, it is intended that
2 3
50.0, and 100.0 mL of the 1000-mg/L solution to 1000-mL
all reagents conform to the specifications of the Committee on
volumetricflaskscontaining200mLofthe39000-mg/LAl O
Analytical Reagents of theAmerican Chemical Society, where
2 3
solution and 100 mL concentrated hydrochloric acid. Dilute
such specifications are available. Other grades may be used,
solutions to volume with distilled water and store in polyeth-
provided it is first ascertained that the reagent is of sufficient
ylene bottles.
purity to permit its use without lessening the accuracy of the
determination.
11. Procedure
8.2 Purity of Water—Unless otherwise indicated, references
11.1 Weigh three test specimens of approximately 2.0 g
to water shall be understood to mean type IVreagent water, as
each to the nearest 0.1 mg and transfer to 250-mL TFE-
defined in Specification D1193.
fluorocarbon beakers.Areagent blank should be carried along
8.3 Required Reagents: with each set of samples.
8.3.1 Hydrofluoric Acid (HF), concentrated, 48%.
11.2 Add 10 mL 48% sulfuric acid, 10 mL concentrated
8.3.2 Sulfuric Acid, (H SO ), concentrated, 98%.
2 4
nitric acid, and 10 mL concentrated hydrofluoric acid.
8.3.3 SulfuricAcid,49volume%,addslowly,whilestirring,
11.3 Transfer beaker and contents to a hot plate (no hotter
one part of concentrated
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:D1977–98 Designation: D 1977 – 03 (Reapproved 2008)
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
1.1This test method is intended for 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
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
2.1 ASTM Standards:
D 1193Specifications for Reagent Water Specification for Reagent Water
D 3766 Terminology Relating to Catalysts and Catalysis
E 105 Practice for Probability Sampling ofOf Materials
E 177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E 288 Specification for Laboratory Glass Volumetric Flasks
E 456 Terminology Relating to Quality and Statistics
E 691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
2.2 U.S. Federal Specification
4 3
Federal Spec NNN-P-395CTolerance for Class A Pipets U.S. Federal Specification:
Federal Specification NNN-P-395C Tolerance for Class A Pipets
3. Summary of Test Method
3.1The 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. Terminology
3.1 Definitions—See Terminology D 3766.
4. Significance and Use
4.1This 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. 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
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 published as D1977–91. Last previous edition D1977–91.
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, 2008. Published April 2008. Originally approved in 1991. Last previous edition approved in 2003 as D 1977–03.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 11.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
Annual Book of ASTM Standards, Vol 14.02.
Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 1977 – 03 (2008)
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
5.1The6.1 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 sameAl O (7800 ppm) concentration as the standards.
2 3
5.2If6.2 If using optical emission, consult tables showing interfering line near analyte lines; if significant overlap occurs, one
must apply inter-element correction or choose an alternate emission line.
6.7. Apparatus
6.1Analytical balance, capable of weighing to nearest 0.1 mg.
6.2Hot plate, capable of maintaining 250°C 6 10°C at surface.
6.3TFE fluorocarbon beaker
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 TFE Fluorocarbon Beaker, 250 mL.
6.4Volumetric flasks
7.4 Volumetric Flasks, borosilicate glass, 50, 100, 250, 500, and 1000-mL capacity conforming to Specification E 288.
6.5
7.5 Pipettes, borosilicate glass, 5, 10, and 25 mL, conforming to Federal Specification NNN-P-395C.
6.6
7.6 Bottles, polyethylene, 100 and 1000 mL.
7.
8. Reagents
7.1
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.
7.2
8.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean type IV reagent water, as
defined in Specification D 1193.
7.3
8.3 Required Reagents:
7.3.1Hydrofluoric acid
8.3.1 Hydrofluoric Acid (HF), concentrated, 48 %.
7.3.2Sulfuric acid
8.3.2 Sulfuric Acid,(H SO ), concentrated, 98 %.
2 4
7.3.3Sulfuric acid
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.
7.3.48.3.4 Hydrochloric acidAcid, concentrated, 38 %.
7.3.5Hydrochloric acid
8.3.5 Hydrochloric Acid, 19 volume %, add slowly, while stirring, one part of concentrated HCl (38 %) to one part of water,
then cool.
7.3.6
8.3.6 Nitric Acid (HNO ) , concentrated, 70 %.
7.3.7
Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
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 Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
D 1977 – 03 (2008)
8.3.7 Reference Standard Solution—1000 mg/L nickel.
7.3.8—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.
7.3.9Aluminum chloride—1000 mg/L vanadium (see Note 1).
8.3.9 Aluminum Chloride, reagent grade, Al
...
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