D32 - Catalysts

SIGNIFICANCE AND USE
4.1 This test method can be used to determine particle size distributions for material specifications, manufacturing control, and research and development work in the particle size range usually encountered in fluidizable cracking catalysts.
SCOPE
1.1 This test method covers the determination of particle size distribution of catalyst and catalyst carrier (see Terminology D3766) particles using an electroconductive sensing method and is one of several valuable methods for the measurement of particle size.  
1.2 The range of particle sizes investigated was 20 μm to 150 μm (see IEEE/ASTM SI 10) equivalent spherical diameter. The technique is capable of measuring particles above and below this range. The instrument used for this method is an electric current path of small dimensions that is modulated by individual particle passage through an aperture, and produces individual pulses of amplitude proportional to the particle volume.  
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, health, and environmental 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.

SCOPE
1.1 This terminology covers definitions of terms related to catalysts and catalysis.
Note 1: The Manual of Symbols and Terminology for Physicochemical Quantities and Units presents authoritative descriptions of many terms used in the field of catalysis.2  
1.2 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.

SIGNIFICANCE AND USE
5.1 This test method can be used to determine the acidity of catalysts and catalyst carriers by ammonia chemisorption for materials specifications, manufacturing control, and research and development in the evaluation of catalysts.
SCOPE
1.1 This test method covers the determination of acidity of catalysts and catalyst carriers by ammonia chemisorption. A volumetric measuring system is used to obtain the amount of chemisorbed ammonia.  
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 This test method is a means of determining the crushing strength of a catalyst in a bed. Techniques to measure the crushing strength of formed catalyst particles is limited to crushing of individual particles, which may not be related to how the catalyst will crush in a reactor or bed. For some catalysts, such as granules, this technique may be the only viable method for obtaining crushing strength. The production of fines in a reactor is not desired because of the potential of bed compaction and the pressure buildup in the reactor.
SCOPE
1.1 This test method covers the determination of bulk crush strength of a bed of formed catalyst particles 1/32 to 3/16 in. (0.8 to 4.8 mm) in diameter and is intended to provide information concerning the ability of the catalyst material to maintain physical integrity.  
1.2 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered 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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 This test method has been found useful for the determination of the specific surface area of catalysts and catalyst carriers in the range from 0.05 m2/g to 10 m2/g for materials specification, manufacturing control, and research and development in the evaluation of catalysts. The determination of surface area of catalysts and catalyst carriers above 10 m2/g is addressed in Test Method D3663 – Surface Area of Catalyst and Catalyst Carriers – and is appropriate for most samples with specific surface areas above 1 m2/g.
SCOPE
1.1 This test method covers the determination of the specific surface area of catalysts and catalyst carriers in the range from 0.05 m2/g to 10 m2/g. A volumetric measuring system is used to obtain at least three data points which fall within the linear BET region.  
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.

SIGNIFICANCE AND USE
5.1 This test method is to be used for measuring the vibratory packing density of formed particles that will not break up during sampling, filling, or vibrating of the measuring cylinder under test conditions.
SCOPE
1.1 This test method covers the determination of the vibratory packing density of formed catalyst and catalyst carriers. For the purpose of this test, catalyst particles are defined as extrudates, spheres, or formed pellets of 0.8-mm to 4.8-mm (1/32-in. to 3/16-in.) nominal diameter.  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are 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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 This test method is used for measuring the vibratory packing density of formed particles used in fixed bed reactors, driers, and so forth.
SCOPE
1.1 This test method covers the determination of the vibratory packing density of formed catalyst and catalyst carrier particles that will not break up significantly under test conditions. For the purpose of this test, catalyst particles are defined as extrudates, spheres or formed pellets greater than 4.8 mm.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
4.1 This test method can be used to determine particle size distributions of catalysts and supports for materials specifications, manufacturing control, and research and development work.
SCOPE
1.1 This test method covers the determination of particle size distribution of catalytic powder material using a sieving instrument and is one of several found valuable for the measurement of particle size. This test method is particularly suitable for particles in the 20 to 420 μm range. (See Terminology D3766.)  
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.  
1.2.1 Exception—In 5.2, mesh size is the standard unit of measure.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 This test method is intended to provide information concerning the ability of a powdered catalyst to resist particle size reduction during use in a fluidized environment.  
5.2 This test method is suitable for specification acceptance, manufacturing control, and research and development purposes.
SCOPE
1.1 This test method covers the determination of the relative attrition characteristics of FCC catalysts by means of air jet attrition. Other fine powder catalysts can be analyzed by this test method, but the precision of this test method has been determined only for FCC catalysts. It is applicable to spherically or irregularly shaped particles which range in size between 10 and 180 μm, have skeletal densities between 2.4 and 3.0 g/cm3 (2400 and 3000 kg/m3) (see IEEE/ASTM SI-10) and are insoluble in water. Particles less than 20 μm are considered fines. (See Terminology D3766.)  
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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 This test method is intended to provide information concerning the ability of a catalyst shape to retain physical integrity during use.
SCOPE
1.1 This test method covers determining the resistance of formed catalysts and catalyst carriers to compressive force and is applicable to regular catalyst shapes such as tablets and spheres. Other formed catalysts and catalyst carriers extrudates, granular materials, and other irregular shapes are specifically excluded.  
1.2 This test method determines the average crush strength in the range from 0 to 50 lbf (0 to 220 N). Some materials may have crush strengths above 50 lbf (220N); the test method is applicable to these materials, but the precision of the test is not known.  
1.3 Units—The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
4.1 This test method sets forth a procedure by which catalyst samples may be compared either on an interlaboratory or intralaboratory basis. It is anticipated that catalyst producers and users will find this test method to be of value.
SCOPE
1.1 This test method covers the determination of cobalt (expressed as the oxide) in fresh cobalt-molybdenum catalyst, in the range of 0.5 to 10 % cobalt oxide.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
4.1 This test method is for measuring the apparent packing density of catalyst or catalyst carrier powders that are smaller than 0.8 mm in diameter.
SCOPE
1.1 This test method covers the determination of the apparent packing density of fine catalyst and catalyst carrier powders smaller than 0.8 mm in diameter.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 This test method provides for the measurement of volume of pores that are in the range of catalytic importance and possibly for adsorption processes. This test method requires the use of mercury in order to perform the measurements.
SCOPE
1.1 This test method covers the determination of the total pore volume of catalysts and catalyst carriers, that is, the volume of pores having pore diameter between approximately 14 µm and 0.4 nm (4 Å).  
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 Warning—Mercury has been designated by many regulatory agencies as a hazardous material that can cause central nervous system, kidney, and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution should be taken when handling mercury and mercury containing products. See the applicable product Material Safety Data Sheet (MSDS) for details and EPA’s website—http://www.epa.gov/mercury/faq.htm—for additional information. Users should be aware that selling mercury or mercury containing products, or both, into your state or country may be prohibited by law.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 8. Warning statements are given in 10.1.4, 10.1.7, and 10.1.11.  
1.5 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.

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 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, health, and environmental 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.

SIGNIFICANCE AND USE
4.1 This test method provides a means of determining the palladium content in fresh catalysts containing molecular sieves.  
4.2 This test method is not intended to cover samples containing precious metals other than palladium.
SCOPE
1.1 This test method covers the determination of palladium in molecular sieve-containing fresh catalysts with about 0.5 weight % of palladium.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 Particle size and shape are important in predicting the performance of catalytic materials. They influence the bulk density of the final product and thereby the effectiveness of performance.  
5.2 Establishing a verification reference for the analyzer that is commercially available and dimensionally reliable to close tolerances enables different analyzers to be easily checked to equivalent standards.  
5.3 This practice may also be followed to analyze catalytic materials for quality manufacturing purposes. Sections 9 and 10 instruct on sample count determination as well as sampling recommendations. Test Method D6299 may be utilized to monitor performance of the analyzer in measuring the size and shape of catalytic materials.
SCOPE
1.1 This practice covers the calibration and verification of Dynamic Imaging Analyzers (analyzers) using catalytic and non-catalytic reference materials. The measurement range of analyzers covers from 500 µm to 20 000 µm.  
1.2 This practice may also be used to analyze catalytic materials once the analyzer has been calibrated and verified.  
1.3 Units—The values stated in SI units are to be regarded as standard; however, English and mesh units are also acceptable with conversions provided in Appendix X3.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
5.1 The chemical composition of catalyst and catalyst materials is an important indicator of catalyst performance and is a valuable tool for assessing parameters in a FCCU process. This practice will be useful to catalyst manufacturers and petroleum refiners for quality verification and performance evaluation, and to environmental authorities at the state and federal levels for evaluation and verification of various compliance programs.3, 4, 5  
5.2 Catalysts and catalyst type materials are difficult to prepare for analysis by ICP, and although the techniques presented in this practice are common, there is wide variation among laboratories in sample pretreatment and digestion recipes. This practice is intended to standardize these variables in order to facilitate the utility of comparative data among manufacturers, refiners, and regulatory agencies.
SCOPE
1.1 This practice covers uniform dissolution techniques for preparing samples of fluid catalytic cracking catalysts (FCC) and exchanged zeolitic materials for analysis by Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES). These techniques describe standardized approaches to well-known, widely used laboratory practices of sample preparation utilizing acid digestions and borate salt fusions. This practice is applicable to fresh and equilibrium FCC catalysts, catalytic materials used to manufacture catalyst, and exchanged zeolite materials.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 The chemical composition of catalysts and catalyst materials is an important indicator of catalyst performance and is a valuable tool for assessing parameters in a FCCU process. This practice will be useful to catalyst manufacturers and petroleum refiners for quality verification and performance evaluation, and to environmental authorities at the state and federal levels for evaluation and verification of various compliance programs (1, 2, 3).
SCOPE
1.1 This practice describes the analysis of fluid catalytic cracking catalysts, rare earth exchanged zeolitic materials, additive and related materials when analyzed by ICP-OES for the six most common rare earth elements.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this Practice.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. See Appendix X3.  
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.

SIGNIFICANCE AND USE
5.1 This guide provides an alternative way to measure the porosity of catalytic materials without the use of mercury porosimetry. It is useful for research and development as well as quality control purposes. (See Test Methods D4284 and D6761.)
SCOPE
1.1 This guide describes how to measure the pore volume of catalytic materials by water immersion with the excess water removed with a centrifuge. The measured pore volume is converted to the dry pore volume by using the loss on ignition (LOI) of the material. It is generally applicable to both powdered materials and particles greater than about 1 mm.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 The jet cup attrition test will provide an estimate of the relative attrition resistance of fluid catalytic cracking (FCC) catalyst, catalyst additives, and catalytic materials.  
5.2 The test is designed to simulate the attrition a catalyst or additive undergoes in a fluid catalytic cracking unit but at an accelerated rate.  
5.3 The data from this test can be used to rank catalyst according to attrition rate.  
5.4 The test requires a relatively small sample size of 5 g [0.175 oz] and a relatively short analysis time of 40 min. This test should be useful to quality control facilities that require fast turnaround time and research and development (R&D) facilities that have limited sample material.
SCOPE
1.1 The jet cup attrition test is applicable to fluid catalytic cracking (FCC) catalysts, catalyst additives, and catalytic materials.  
1.2 Applications for other powdered catalysts have been reported in the literature. The round robin test samples included two FCC catalysts and one powdered alumina.  
1.3 Units—The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system are not necessarily exact equivalents; therefore, to ensure conformance with the standard, each system shall be used independently of the other, and values from the two systems shall not be combined.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
5.1 This guide is intended to determine meso- and macropore volume which affects heavy oil cracking performance of a catalyst. The information is useful for materials specification, manufacturing control, and research and development in the evaluation of catalytic materials.  
5.2 It has been reported in literature the existence of a correlation between the pore volume obtained from this guide and that from Test Method D4284.3
SCOPE
1.1 This guide measures pore volume of powdered catalysts and catalyst carriers by titration with water. The water does not react with material. The range of pore volume is 0.25 mL/g to 0.46 mL/g.  
1.2 This guide is suitable for fine catalysts such as fluid catalytic cracking (FCC) catalysts (fresh or equilibrium), catalyst additives and spray dried catalyst carriers or finished catalysts, or a combination thereof, and is typically applicable to powders with the majority of particles (above 90 %) in the distribution range between 20 and 150 µm equivalent spherical diameter (determined by Test Method D4464) and with an average particle size between 60 and 100 µm.
Note 1: This technique is capable of measuring particles below and above this range (for example, from 1 to 300 µm) but no precision data is available.  
1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
4.1 ZSM-5 is a siliceous zeolite that can be crystallized with SiO2/Al2O3 ratio in the range of 20 to greater than 1000. ZSM-5, upon modification to the H-cation form (HZSM-5) in a post-crystallization step, has been used since the 1970s as a shape selective, acid-site catalyst for petroleum refining and petrochemicals production, including such processes as alkylation, isomerization, fluid cracking catalysis (FCC), and methanol-to-gasoline. The most siliceous member of the ZSM-5 family, sometimes called silicalite, is hydrophobic and it is used for selective sorption of organic molecules from water-containing systems.  
4.2 This X-ray procedure is designed to allow a reporting of the relative degree of crystallization upon manufacture of ZSM-5. The relative crystallinity/ZSM-5 number has proven useful in technology, research, and specifications.  
4.3 The Integrated Peak Area Method (Procedure A) is preferred over the Peak Height Method (Procedure B) since it calculates XRD intensity as a sum from several peaks rather than utilizing just one peak. Drastic changes in intensity of individual peaks in the XRD pattern of ZSM-5 can result from changes in distribution of electron density within the unit cell of the ZSM-5 zeolite. The electron density distribution is dependent upon the following factors:  
4.3.1 Extent of filling of pores with guest molecules and the nature of these guest molecules.  
4.3.2 Type of cations and extent of their presence (these cations may also affect the absorption of X rays by the ZSM-5 sample).  
4.3.3 In this XRD method, the guest molecule H2O completes the filling of the pores. Other guest molecule types may also be present, including one of numerous amines, diamines, and quarternary ammonium cations that can function as a template for crystallization of the ZSM-5 structure.  
4.3.4 Because of the factors mentioned in 4.3.1 to 4.3.3 that could vary the intensities of the XRD peaks in ZSM-5, this XRD method will provide the best de...
SCOPE
1.1 This test method covers a procedure for determination of the relative crystallinity of zeolite ZSM-5 using selected peaks from the X-ray diffraction pattern of the zeolite.  
1.2 The test method provides a number that is the ratio of intensity of a portion of the XRD pattern of the sample ZSM-5 to intensity of the corresponding portion of the pattern of a reference ZSM-5. The intensity ratio, expressed as a percentage, is then labeled percent XRD relative crystallinity/ZSM-5. This type of comparison is commonly used in zeolite technology and is often referred to as percent crystallinity.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
4.1 This test method sets forth a procedure by which catalyst samples can be compared either on an interlaboratory or intralaboratory basis. It is anticipated that catalyst producers and users will find this method of value.
SCOPE
1.1 This test method covers the determination of nickel in fresh alumina-base catalysts and has been tested at nickel concentrations from 2.5 to 60 weight %, expressed as nickel oxide (NiO).  
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, health, and environmental 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.

SIGNIFICANCE AND USE
4.1 This test method sets forth a procedure by which catalyst samples can be compared either on an interlaboratory or intralaboratory basis. It is anticipated that catalyst producers and users will find this method of value.
SCOPE
1.1 This test method covers the determination of molybdenum in alumina-base catalysts and has been cooperatively tested at molybdenum concentrations from 8 to 18 weight %, expressed as MoO3. Any component of the catalyst other than molybdenum such as iron, tungsten, etc., which is capable of being oxidized by either ferric or ceric ions after being passed through a zinc-amalgam reductor column (Jones reductor) will interfere.  
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 Many catalysts that contain molybdenum also contain other metals, nickel for example, that may be regulated by the EPA. Go to the material safety data sheet for the catalyst material being analyzed. More information can be found at EPA.gov. Additional information on nickel containing catalysts can be found in Test Method D4481.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
5.1 This guide is intended to provide information concerning the ability of formed catalysts or catalyst carriers to resist particle size reduction during use. It can be used by itself or in conjunction with other methods to assess catalytic material integrity, such as Test Methods D4058 and D7084.  
5.2 There are no known restrictions on sample geometry, as spheres, pellets, and hollow cylinders are suitable for testing.  
5.3 This guide, as written, is suitable for use for catalytic materials from about 1/8 in. to about 3/4 in. It can also be used for larger parts, but this requires using a larger diameter pipe.  
5.4 This guide is suitable for specification acceptance, manufacturing control, and research and development processes.
SCOPE
1.1 The resistance to breakage of formed catalysts, catalyst carriers, or catalyst pieces is determined by dropping a quantity of sample through a 25 ft length of 1 in. internal diameter pipe onto a steel plate.  
1.2 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.3 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.

SIGNIFICANCE AND USE
4.1 This test method sets forth a procedure by which duplicate catalyst samples can be compared either on an interlaboratory or intralaboratory basis. It is anticipated that catalyst producers and users will find this test method of value.  
4.2 Discrimination of the samples for which this procedure is recommended must be exercised when considering carrier (support) materials that sorb appreciable quantities of hydrogen or could cause an alteration of the state of the catalyst during pretreatment, or both, (that is, sintering or metal occlusion). These materials must be identified by the user and experimented with to determine the most significant conditions of measurement.  
4.3 This test method provides a measure of the total hydrogen uptake (volume of hydrogen at STP, cm3/g of catalyst) without specifying the nature of the hydrogen-platinum interaction. Persons interested in using hydrogen uptake data to calculate percent platinum dispersion in a specific catalyst should be aware of carrier (support) interactions, spillover effects, and other phenomena related to the hydrogen uptake capabilities of the catalyst in question.
SCOPE
1.1 This test method covers the determination of the chemisorption of hydrogen at 298 K (25 °C) on supported platinum catalysts that have been reduced in flowing hydrogen at 723 K (450 °C). It incorporates a static volumetric vacuum technique at constant volume.  
1.2 The test method is intended for use on unused supported platinum on alumina catalysts of loadings greater than 0.3 weight %. Data on other supports and lower platinum loadings were not tested.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
4.1 This test method is for estimating the relative amount of gamma alumina in calcined catalyst or catalyst carrier samples, assuming that the X-ray powder diffraction peak occurring at about 67 °2θ is attributable to gamma alumina. Gamma alumina is defined as a transition alumina formed after heating in the range from 500 to 550 °C, and may include forms described in the literature as eta, chi, and gamma aluminas. Delta alumina has a diffraction peak in the same region, but is formed above 850 °C, a temperature to which most catalysts of this type are not heated. There are other possible components which may cause some interference, such as alpha-quartz and zeolite Y, as well as aluminum-containing spinels formed at elevated temperatures. If the presence of interfering material is suspected, the diffraction pattern should be examined in greater detail. More significant interference may be caused by the presence of large amounts of heavy metals or rare earths, which exhibit strong X-ray absorption and scattering. Comparisons between similar materials, therefore, may be more appropriate than those between widely varying materials.
SCOPE
1.1 This test method covers the determination of gamma alumina and related transition aluminas in catalysts and catalyst carriers containing silica and alumina by X-ray powder diffraction, using the diffracted intensity of the peak occurring at about 67 °2θ when copper Kα radiation is employed.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 The test method has two main functions: first, it provides data useful for establishing the pore size distribution of catalyst materials, which in turn may influence their performance; and second, it serves as a laboratory test which may be used to study porosity changes that may occur during the manufacture and evaluation of catalysts.
SCOPE
1.1 This test method covers the determination of nitrogen adsorption and desorption isotherms of catalysts and catalyst carriers at the boiling point of liquid nitrogen.2 A static volumetric measuring system is used to obtain sufficient equilibrium adsorption points on each branch of the isotherm to adequately define the adsorption and desorption branches of the isotherm. Thirty points evenly spread over the isotherm is considered to be the minimum number of points that will adequately define the isotherm.  
1.2 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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, health, and environmental 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.

ABSTRACT
This test method establishes the standard procedure for determining the surface areas of catalyst and catalyst carriers that have Type II or IV nitrogen adsorption isotherms, and specified minimum area. A volumetric measuring system is used to obtain at least four data points which fit on the linear BET line. The surface area of a catalyst or catalyst carrier is determined by measuring the volume of nitrogen gas adsorbed at various low-pressure levels by the catalyst sample. Pressure differentials caused by introducing the catalyst surface area to a fixed volume of nitrogen in the test apparatus are measured and used to calculate BET surface area.
SCOPE
1.1 This test method covers the determination of surface areas of catalyst and catalyst carriers that have Type II or IV nitrogen adsorption isotherms, and at least 1 m2/g of area. A volumetric measuring system is used to obtain at least four data points which fit on the linear BET2 equation line.  
1.2 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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, health, and environmental 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.

SIGNIFICANCE AND USE
4.1 Zeolite Beta is a siliceous zeolite that can be crystallized with SiO2/Al2O3 ratio greater than 20. Zeolite Beta, upon modification to the H-cation form in a post-crystallization step, has been used in catalytic NOx reduction, isomerization of waxes, alkylation of aromatics, hydrocarbon adsorption from exhaust gas emission, etc.  
4.2 This X-ray procedure is designed to allow a reporting of the relative degree of crystallinity upon manufacture of zeolite Beta. The relative crystallinity of zeolite Beta number has proven useful in technology, research, and specifications.  
4.3 The Integrated Peak Area Method (Procedure A) is preferred over the Peak Height Method (Procedure B) since it calculates XRD intensity as a sum from several peaks rather than utilizing just one peak. Drastic changes in intensity of individual peaks in the XRD pattern of zeolite Beta can result from changes in distribution of electron density within the unit cell of the zeolite Beta. The electron density distribution is dependent upon the following factors:  
4.3.1 Extent of filling of pores with guest molecules and the nature of these guest molecules.  
4.3.2 Type of cations and extent of their presence (these cations may also affect the absorption of X rays by the zeolite Beta sample).  
4.3.3 In this XRD method, the guest molecule H2O completes the filling of the pores. Other guest molecule types may also be present, including one of numerous amines, diamines, and quaternary ammonium cations that can function as a template for crystallization of the zeolite Beta structure.  
4.3.4 Because of the factors mentioned in 4.3.1 – 4.3.3 that could vary the intensities of the XRD peaks in zeolite Beta, this XRD method will provide the best determination of relative crystallinity when the reference zeolite Beta and sample zeolite Beta have a similar history of preparation and composition.  
4.4 If crystalline phases other than zeolite Beta are present in the sample, their diffraction peaks...
SCOPE
1.1 This test method covers a procedure for determination of the relative crystallinity of zeolite Beta containing samples using selected peaks from the X-ray diffraction (XRD) pattern of the zeolite.  
1.2 The test method provides a number that is the ratio of intensity of a portion of the XRD pattern of the sample zeolite Beta to intensity of the corresponding portion of the pattern of a reference zeolite Beta. The intensity ratio, expressed as a percentage, is then labeled percent XRD relative crystallinity of zeolite Beta. This type of comparison is commonly used in zeolite technology and is often referred to as percent crystallinity.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
4.1 This test method is considered to be a measure of the propensity of a catalyst to produce fines in the course of transportation, handling, and use. However, there is no absolute level of acceptability. The values obtained are significant principally in relation to values for other materials (or other samples of the same material) of comparable size.
SCOPE
1.1 This test method covers the determination of the attrition and abrasion resistance of catalysts and catalyst carriers. It is applicable to tablets, extrudate, spheres, and irregularly shaped particles larger than about 1/16 in. (1.6 mm) and smaller than about 3/4 in. (19 mm). The materials used in developing the method exhibited losses on attrition less than 7 %; however, the method should be applicable to materials giving much higher attritions.  
1.2 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered 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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 It is important to recognize that the results obtained by this test method or any other method for particle size determination utilizing different physical principles may disagree. The results are strongly influenced by physical principles employed by each method of particle size analysis. The results of any particle sizing method should be used only in a relative sense and should not be regarded as absolute when comparing results obtained by other methods. Particularly for fine materials (that is, average particle size 3  
5.2 Light scattering theories (Fraunhofer Diffraction4 and Mie Scattering5) that are used for determination of particle size have been available for many years. Several manufacturers of testing equipment now have units based on these principles. Although each type of testing equipment utilizes the same basic principles for light scattering as a function of particle size, different assumptions pertinent to application of the theory and different models for converting light measurements to particle size, may lead to different results for each instrument. Furthermore, any particles which are outside the size measurement range of the instrument will be ignored, causing an increase in the reported percentages within the detectable range. A particle size distribution which ends abruptly at the detection limit of the instrument may indicate that particles outside the range are present. Therefore, use of this test method cannot guarantee directly comparable results from different types of instruments.  
5.3 This test method can be used to determine particle size distributions of catalysts, supports, and catalytic raw materials for specifications, manufacturing control, and research and development work.  
5.4 For fine materials (that is, average particle size 6
SCOPE
1.1 This test method covers the determination of the particle size distribution of catalyst, catalyst carrier, and catalytic raw material particles and is one of several found valuable for the measurement of particle size. The range of average particle sizes investigated was from 1 to 300 μm equivalent spherical diameter. The technique is capable of measuring particles above and below this range. The angle and intensity of laser light scattered by the particles are selectively measured to permit calculation of a volume distribution using light-scattering techniques.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 This gas adsorption method complements the X-ray procedure of Test Method D3906. This test method will be useful to laboratories that do not have X-ray diffractometers. Each test method can be calibrated by use of an appropriate series of mechanical mixtures to provide what may be termed percent zeolite. If there is disorder in the zeolite, the adsorption method will yield higher values than the X-ray method. The reverse will be true if some zeolite pores (micropores) are blocked or filled.
SCOPE
1.1 This test method covers the determination of total surface area and mesopore area. From these results are calculated the zeolite area and micropore volume of a zeolite containing catalyst. The micropore volume is related to the percent zeolite in the catalyst. The zeolite area, a number related to the surface area within the zeolite pores, may also be calculated. Zeolite area, however, is difficult to interpret in physical terms because of the manner in which nitrogen molecules pack within the zeolite.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For a specific precautionary statement, see Note 3.  
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.

SIGNIFICANCE AND USE
5.1 This test method is useful for determining the specific surface area of catalysts and catalyst carriers for material specifications, manufacturing control, and research and development in the evaluation of catalysts.
SCOPE
1.1 This test method covers the single-point determination of the surface area of catalysts and catalyst carriers that exhibit Type II or Type IV nitrogen adsorption isotherms using a nitrogen-helium flowing gas mixture. This test method is applicable for the determination of total surface areas from 0.1 to 300 m2, where rapid surface area determinations are desired.  
1.2 Because the single-point method uses an approximation of the BET equation, the multipoint BET method (Test Method D3663) is preferred to the single-point method.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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 consult and establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
5.1 The fluidized bed test provides data to assess the relative performances of FCC catalysts. Because results are affected by catalyst pretreatment, feedstock characteristics, and operating parameters, this test method is written specifically to address the accuracy and precision when a common catalyst and oil are tested under the same conditions but at different sites, using Kayser Technologies Advanced Catalytic Evaluation (ACE) unit.4,5 Analytical procedures may vary among the sites. However, significant variations are not expected.
Note 1: ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility.  
5.2 The standard reaction temperature for purposes of the accuracy and precision statement is 532 °C [990 °F]. Other reaction temperatures can be used in practice; however, yield data developed at temperatures other than 532 °C [990 °F] will not be the same. Also, test precision may be different at other reaction temperatures.
SCOPE
1.1 This test method covers determining the activity and coke selectivity of either equilibrium or laboratory deactivated fluid catalytic cracking (FCC) catalysts. The activity is evaluated on the basis of mass percent conversion of gas oil feed in a fluidized bed reactor. The coke yield is defined as the mass of carbon laid down on the catalyst, also expressed as a percent of the gas oil feed. The scope of the round robin will be limited to the determination of activity and coke. All other analyses are thus beyond this scope and should be noted as “optional.”  
1.2 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system are not necessarily exact equivalents; therefore, to ensure conformance with the standard, each system shall be used independently of the other, and values from the two systems shall not be combined.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
4.1 Zeolites Y and  X, particularly for catalyst and adsorbent applications, are a major article of manufacture and commerce. Catalysts and adsorbents comprising these zeolites in various forms plus binder and other components have likewise become important. Y-based catalysts are used for fluid catalytic cracking (FCC) and hydrocracking of petroleum, while X-based adsorbents are used for desiccation, sulfur compound removal, and air separation.  
4.2 This X-ray procedure is designed to monitor these Y and X zeolites and catalysts and adsorbents, providing a number more or less closely related to percent zeolite in the sample. This number has proven useful in technology, research, and specifications.  
4.3 Drastic changes in intensity of individual peaks in the XRD patterns of Y and X can result from changes of distribution of electron density within the unit cell of the zeolite. The electron density distribution is dependent upon the extent of filling of pores in the zeolite with guest molecules, and on the nature of the guest molecules. In this XRD method, the guest molecule H2O completely fills the pores. Intensity changes may also result if some or all of the cations in Y and  X are exchanged by other cations.  
4.3.1 Because of the factors mentioned in 4.3 that could vary the intensities of the XRD peaks, this XRD method will provide the best determination of relative crystallinity when the reference and sample have a similar history of preparation and composition.  
4.4 Corrections are possible that can make this XRD method accurate for measuring percent zeolite in many specific situations. These corrections are well known to those skilled in X-ray diffraction. It is not practical to specify those corrections here.
SCOPE
1.1 This test method covers the determination of relative X-ray diffraction intensities of zeolites having the faujasite crystal structure, including synthetic Y and X zeolites, their modifications such as the various cation exchange forms, and the dealuminized, decationated, and ultrastable forms of Y. These zeolites have cubic symmetry with a unit cell parameter usually within the limits of 24.2 and 25.0 Å (2.42 and 2.50 nm).  
1.2 The samples include zeolite preparations in the various forms, and catalysts and adsorbents containing these zeolites.  
1.3 The term “intensity of an X-ray powder diffraction (XRD) peak” is the “integral intensity,” either the area of counts under the peak or the product of the peak height and the peak width.  
1.4 This test method provides a number that is the ratio of intensity of portions of the XRD pattern of the sample to intensity of the corresponding portion of the pattern of a reference zeolite, NaY. (Laboratories may use a modified Y or  X, for example, REY as a secondary standard.) The intensity ratio, expressed as a percentage, is then labeled “% XRD intensity/NaY.”  
1.5 Under certain conditions such a ratio is the percent zeolite in the sample. These conditions include:  
1.5.1 The zeolite in the sample is the same as the reference zeolite.  
1.5.2 The absorption for the X-rays used is the same for the zeolite and the nonzeolite portions of the sample.  
1.6 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.7 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.

SIGNIFICANCE AND USE
4.1 In general, steam treatment of FCC catalyst can be used either to compare a series of cracking catalysts at a simulated equilibrium condition or conditions, or to simulate the equilibrium condition of a specific cracking unit and a specific catalyst. This guide gives an example for the first purpose and an approach for the latter purpose.
SCOPE
1.1 This guide covers the deactivation of fresh fluid catalytic cracking (FCC) catalyst by hydrothermal treatment prior to the determination of the catalytic cracking activity in the microactivity test (MAT) or the Advanced Cracking Evaluation (ACE) test.  
1.2 The hydrothermal treatment of fresh FCC catalyst, prior to the MAT or the ACE test, is important because the catalytic activity of the catalyst in its fresh state is an inadequate measure of its true commercial performance. During operation in a commercial cracking unit, the catalyst is deactivated by thermal, hydrothermal, and chemical degradation. Therefore, to maintain catalytic activity, fresh catalyst is added (semi) continuously to the cracking unit, to replace catalyst lost through the stack or by withdrawal, or both. Under steady state conditions, the catalyst inventory of the unit is called equilibrium catalyst. This catalyst has an activity level substantially below that of fresh catalyst. Therefore, artificially deactivating a fresh catalyst prior to determination of its cracking activity should provide more meaningful catalyst performance data.  
1.3 Due to the large variations in properties among fresh FCC catalyst types as well as between commercial cracking unit designs or operating conditions, or both, no single set of steam deactivation conditions is adequate to artificially simulate the equilibrium catalyst for all purposes.  
1.3.1 In addition, there are many other factors that will influence the properties and performance of the equilibrium catalyst. These include, but are not limited to: deposition of heavy metals such as Ni, V, and Cu; deposition of light metals such as Na; and contamination from attrited refractory linings of vessel walls. Furthermore, commercially derived equilibrium catalyst represents a distribution of catalysts of different ages (from fresh to >300 days). Despite these apparent problems, it is possible to obtain reasonably close agreement between the performances of steam deactivated and equilibrium catalysts. It is also recognized that it is possible to steam deactivate a catalyst so that its properties and performance poorly represent the equilibrium. It is therefore recommended that when assessing the performance of different catalyst types, a common steaming condition be used. Catalyst deactivation by metals deposition is not addressed in this guide, but is addressed in Guide D7206/D7206M.  
1.4 This guide offers two approaches to steam deactivate fresh catalysts. The first part provides specific sets of conditions (time, temperature, and steam pressure) that can be used as general pre-treatments prior to comparison of fresh FCC catalyst MAT activities (Test Method D3907) or activities plus selectivities (Test Methods D5154 and D7964).  
1.4.1 The second part provides guidance on how to pretreat catalysts to simulate their deactivation in a specific FCCU and suggests catalyst properties which can be used to judge adequacy of the simulation. This technique is especially useful when examining how different types of catalyst may perform in a specific FCCU, provided no other changes (catalyst addition rate, regenerator temperature, contaminant metals levels, etc.) occur. This approach covers catalyst physical properties that can be used as monitors to indicate the closeness to equilibrium catalyst properties.  
1.5 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system are not necessarily exact equivalents; therefore, to ensure conformance with the standard, each s...

SIGNIFICANCE AND USE
4.1 This guide describes techniques of deactivation that can be used to compare a series of cracking catalysts at equilibrium conditions or to simulate the equilibrium conditions of a specific commercial unit and a specific catalyst.
SCOPE
1.1 This guide covers the deactivation of fluid catalytic cracking (FCC) catalyst in the laboratory as a precursor to small scale performance testing such as catalyst activities (Test Method D3907) or activities plus selectivities (Test Methods D5154 and D7964). FCC catalysts are deactivated in the laboratory in order to simulate the aging that occurs during continuous use in a commercial fluid catalytic cracking unit (FCCU). Deactivation for purposes of this guide constitutes hydrothermal deactivation of the catalyst and metal poisoning by nickel and vanadium. Hydrothermal treatment is used to simulate the physical changes that occur in the FCC catalyst through repeated regeneration cycles. Hydrothermal treatment (steaming) destabilizes the faujasite (zeolite Y), resulting in reduced crystallinity and surface area. Further decomposition of the crystalline structure occurs in the presence of vanadium, and to a lesser extent in the presence of nickel. Vanadium is believed to form vanadic acid in a hydrothermal environment resulting in destruction of the zeolitic portion of the catalyst. Nickel’s principle effect is to poison the selectivity of the FCC catalyst. Hydrogen and coke production is increased in the presence of nickel, due to the dehydrogenation activity of the metal. Vanadium also exhibits significant dehydrogenation activity, the degree of which can be influenced by the oxidation and reduction conditions prevailing throughout the deactivation process. The simulation of the metal effects that one would see commercially is part of the objective of deactivating catalysts in the laboratory. Catalyst deactivation by hydrothermal treatment only is addressed in Guide D4463/D4463M.  
1.2 The two basic approaches to laboratory-scale simulation of commercial equilibrium catalysts described in this guide are as follows:  
1.2.1 Cyclic Propylene Steaming (CPS) Method, in which the catalyst is impregnated with the desired metals via an incipient wetness procedure (Mitchell method)2 followed by a prescribed steam deactivation.  
1.2.2 Crack-on Methods,  in which fresh catalyst is subjected to a repetitive sequence of cracking (using a feed with enhanced metals concentrations), stripping, and regeneration in the presence of steam. Two specific procedures are presented here, a procedure with alternating metal deposition and deactivation steps and a modified Two-Step procedure, which includes a cyclic deactivation process to target lower vanadium dehydrogenation activity.  
1.3 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system are not necessarily exact equivalents; therefore, to ensure conformance with the standard, each system shall be used independently of the other, and values from the two systems shall not be combined.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
5.1 The microactivity test provides data to assess the relative performance of FCC catalysts. Because results are affected by catalyst pretreatment, feedstock characteristics, test equipment, and operating parameters, adherence to this test method is a prerequisite for correct interpretation of results. Apparatus, test conditions, and analytical procedures actually used should closely resemble those described in this test method.  
5.2 Caution should be used in interpreting results above 80 mass % conversion due to the significance of overcracking.
SCOPE
1.1 This test method covers determining the activity of equilibrium or laboratory-deactivated fluid catalytic cracking (FCC) catalysts, or both. This is evaluated on the basis of mass percent conversion of gas oil feed in a microactivity unit. The selectivity of FCC catalysts can be determined using Test Method D5154.  
1.2 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system are not necessarily exact equivalents; therefore, to ensure conformance with the standard, each system shall be used independently of the other, and values from the two systems shall not be combined.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 This test method is intended to provide information on the ability of an extruded catalyst to retain physical integrity during use.
SCOPE
1.1 This test method covers and is suitable for determining the resistance of extruded catalysts and catalyst carriers to compressive force from the side.  
1.2 This test method was developed using extruded catalyst and catalyst carriers from 1/16 to 1/8 in. in diameter (0.159 to 0.318 cm) and limited to pieces with a length to diameter ratio greater than or equal to 1:1. This test method may be applicable to other diameters.  
1.3 This test method is suitable for the determination of mean crush strength per millimetre in the range of 0 to 15 lbf/mm (0 to 65 N/mm).  
1.4 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard.  
1.5 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 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.

SIGNIFICANCE AND USE
4.1 Zeolite NaA has been used as an active component in molecular sieves employed as desiccants for natural gas, process gas streams, sealed insulated windows, and as a builder (water softener) in household laundry detergents.  
4.2 This X-ray procedure is designed to allow a reporting of the relative degree of crystallization of NaA in the manufacture of NaA. The relative crystallinity number has proven useful in technology, research, and specifications.  
4.3 Drastic changes in intensity of individual peaks in the XRD pattern of NaA can result from changes in distribution of electron density within the unit cell of the NaA zeolite. The electron density distribution is dependent upon the extent of filling of pores in the zeolite with guest molecules, and on the nature of the guest molecules. In this XRD method, the guest molecule H2O completely fills the pores. Intensity changes may also result if some or all of the sodium cations in NaA are exchanged by other cations.  
4.4 Drastic changes in overall intensity can result from changes in X-ray absorption attributed to non-crystalline phases, if present, in a NaA sample. If non-zeolite crystalline phases are present, their diffraction peaks may overlap with some of the NaA diffraction peaks selected for this test method. If there is reason to suspect the presence of such components, then NaA peaks free of interference should be chosen for analysis.
SCOPE
1.1 This test method covers a procedure for determining the relative crystallinity of zeolite sodium A (zeolite NaA) using selected peaks from the X-ray diffraction pattern of the zeolite.  
1.2 The term “intensity of an X-ray powder diffraction (XRD) peak” refers to the “integral intensity,” either the area or counts under the peak or the product of the peak height and the peak width at half height.  
1.3 This test method provides a number that is the ratio of intensity of portions of the XRD pattern of the sample to intensity of the corresponding portion of the pattern of a reference zeolite NaA. The intensity ratio, expressed as a percentage, is then labeled relative crystallinity of NaA.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 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.

SIGNIFICANCE AND USE
4.1 Zeolites Y and X, particularly for catalyst and adsorbent applications, are a major article of manufacture and commerce. Catalysts and adsorbents comprising these zeolites in various forms plus binder and other components have likewise become important. Y-based catalysts are used for fluid catalytic cracking (FCC) and hydrocracking of petroleum, while X-based adsorbents are used for desiccation, sulfur compound removal, and air separation.  
4.2 The unit cell dimension of a freshly synthesized faujasite-type zeolite is a sensitive measure of composition which, among other uses, distinguishes between the two synthetic faujasite-type zeolites, X and Y. The presence of a matrix in a Y-containing catalyst precludes determination of the zeolite framework composition by direct elemental analysis.  
4.3 Users of the test method should be aware that the correlation between framework composition and unit cell dimension is specific to a given cation form of the zeolite. Steam or thermal treatments, for example, may alter both composition and cation form. The user must therefore determine the correlation that pertains to his zeolite containing samples.3 In addition, one may use the test method solely to determine the unit cell dimension, in which case no correlation is needed.  
4.4 Other crystalline components may be present in the sample whose diffraction pattern may cause interference with the selected faujasite-structure diffraction peaks. If there is reason to suspect the presence of such components, then a full diffractometer scan should be obtained and analyzed to select faujasite-structure peaks free of interference.
SCOPE
1.1 This test method covers the determination of the unit cell dimension of zeolites having the faujasite crystal structure, including synthetic Y and X zeolites, their modifications such as the various cation exchange forms, and the dealuminized, decationated, and ultra stable forms of Y. These zeolites have cubic symmetry with a unit cell parameter usually within the limits of 24.2 and 25.0 Å (2.42 and 2.50 nm).  
1.2 The samples include zeolite preparation in the various forms, and catalysts and adsorbents containing these zeolites. The zeolite may be present in amounts as low as 5 %, such as in a cracking catalyst.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
4.1 The chemical composition of fresh FCC catalyst and equilibrium FCC catalyst is a predictor of catalyst performance. The analysis of catalyst fines also provides information on the performance of the FCC unit and the fines collection device(s).  
4.2 The chemical composition of equilibrium FCC catalyst is a measure of the hazardous nature or toxicity of the material for purposes of disposal or secondary use.
SCOPE
1.1 This guide covers several comparable procedures for the quantitative chemical analysis of up to 29 elements in fluid catalytic cracking (FCC) catalyst by X-ray fluorescence spectrometry (XRF). Additional elements may be added.  
1.2 This guide is applicable to fresh FCC catalyst, equilibrium FCC catalyst, spent FCC catalyst, and FCC catalyst fines.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3.1 The units of ppm (mg/kg) are used instead of wt% in Tables X2.3-X2.5 for reporting concentration of certain elements because of industry convention and because most of these elements are present at trace levels.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
5.1 This test method is for measuring the mechanically tapped packing density of powders that are smaller than 0.8 mm in diameter, such as Fluidized Catalytic Cracking Catalysts (FCC).
SCOPE
1.1 This test method covers the determination of the mechanically tapped packing density of fine catalyst and catalyst carrier particles smaller than 0.8 mm in diameter.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 The microactivity test provides data to assess the relative performance of FCC catalysts. Because results are affected by catalyst pretreatment, feedstock characteristics, test equipment, and operating parameters, adherence to this test method is a prerequisite for correct interpretation of results. Apparatus, test conditions, and analytical procedures actually used should closely resemble those described in this test method. Significant variations in apparatus, test conditions and/or analytical procedures may result in activity and selectivity data which do not correlate with data developed by other laboratories on identical catalyst/feedstock samples.  
5.2 The standard method reaction temperature is 516 °C [960 °F]. Other reaction temperatures can be used; however, catalyst selectivity data developed at temperatures other than 516 °C [960 °F] may not correlate with selectivity data developed at 516 °C [960 °F]. Also, precision at other reaction temperatures may change compared to data obtained at 516 °C [960 °F].
SCOPE
1.1 This test method covers determining the activity and selectivity of either equilibrium or laboratory deactivated fluid catalytic cracking (FCC) catalysts. The activity is evaluated on the basis of mass percent conversion of gas oil feed in a microactivity unit. The selectivities are evaluated on the basis of mass percent yields of specifically defined products resulting from the catalytic cracking of gas oil feed.  
1.2 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the 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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 This test method is to be used for measuring the mechanically tapped packing density of formed particles that will not break up during sampling, filling, or tapping of the measuring cylinder under test conditions.
SCOPE
1.1 This test method covers the determination of the mechanically tapped density of formed catalyst and catalyst carriers. For the purpose of this test method, catalyst particles are defined as extrudates, spheres, or formed pellets of 0.8 to 4.8-mm (1/32 to 3/16-in.) nominal diameter.  
1.2 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.3 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.

ABSTRACT
This specification covers fired chemical-resistant ceramic tower installation packings formed from naturally occurring clays or compounded bodies. The number of dumped pieces of cylindrical-type packing material should conform to the requirements for each ring, packing, and saddle size. Material properties such as crushing strength, water absorption, and acid resistance should also fall within the given values for both porcelain and stoneware packings.
SCOPE
1.1 This specification covers fired ceramic shapes formed from naturally occurring clays and from compounded bodies that are used as packing in tower installations. These ceramic units are designed primarily for use in process equipment for the chemical or allied industries.  
1.2 The physical and chemical properties that affect quality of packing materials are covered in this specification. Properties that affect actual operational efficiency or characteristics of processing towers are not covered.  
1.3 The values stated in inch-pound units are to be regarded as the standard. The values given in parentheses are for information only.  
1.4 The following precautionary statement pertains to the test method portion only, Section 7, of this standard. 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
5.1 This test method is intended to determine the volume distribution of pores in catalysts and catalyst carriers with respect to the apparent diameter of the entrances to the pores. In general, both the size and volume of pores in a catalyst affect its performance. Thus, the pore volume distribution is useful in understanding a catalyst's performance and in specifying a catalyst that can be expected to perform in a desired manner.
SCOPE
1.1 This test method covers the determination of the pore volume distributions of catalysts and catalyst carriers by the method of mercury intrusion porosimetry. The range of apparent diameters of pores for which it is applicable is fixed by the operant pressure range of the testing instrument. This range is typically between apparent pore entrance diameters of about 100 and 0.003 μm (3 nm).  
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 WARNING—Mercury has been designated by many regulatory agencies as a hazardous material that can cause central nervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution should be taken when handling mercury and mercury containing products. See the applicable product Material Safety Data Sheet (MSDS) for details and EPA’s website—http://www.epa.gov/mercury/faq.htm—for additional information. Users should be aware that selling mercury and/or mercury containing products into your state or country may be prohibited by law.  
1.4 This standard does not purport to address all of the safety problems, 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 hazard information is given in Section 8.

SIGNIFICANCE AND USE
5.1 Pore volume distribution curves obtained from nitrogen sorption isotherms provide one of the best means of characterizing the pore structure in porous catalysts, provided that the limitations of the method are kept in mind. Used in conjunction with the BET treatment for surface area determination (5), these methods provide an indispensable means for studying the structure associated with pores usually important in catalysts. This practice is particularly useful in studying changes in a series of closely related samples caused by treatments, such as heat, compression, or extrusion often used in catalyst manufacturing. Pore volume distribution curves can often provide valuable information during mechanistic studies dealing with catalyst deactivation.
SCOPE
1.1 This practice covers the calculation of pore size distributions for catalysts and catalyst carriers from nitrogen desorption isotherms. The computational procedure is particularly useful for determining how the pore volume is distributed in catalyst samples containing pores whose sizes range from approximately 1.5 to 100 nm (15 to 1000 Å) in radius. It should be used with caution when applied to isotherms for samples containing pores both within this size range and pores larger than 100 nm (1000 Å) in radius. In such instances the isotherms rise steeply near P/Po  = 1 and the total pore volume cannot be well defined. The calculations should begin at a point on the isotherm near saturation preferably in a region near P/Po  = 0.99, establishing an upper limit on the pore size distribution range to be studied. Simplifications are necessary regarding pore shape. A cylindrical pore model is assumed, and the method treats the pores as non-intersecting, open-ended capillaries which are assumed to function independently of each other during the adsorption or desorption of nitrogen.  
Note 1: This practice is designed primarily for manual computation and a few simplifications have been made for this purpose. For computer computation, the simplified expressions may be replaced by exact expressions.  
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.

SIGNIFICANCE AND USE
4.1 This test method provides a means of determining the platinum content of fresh reforming catalysts where the platinum is supported on an all alumina substrate.4  
4.2 This test method is not intended to cover samples containing metals other than platinum. Palladium, rhenium, and rhodium in particular interfere with the spectrophotometric determination of platinum.
SCOPE
1.1 This test method covers the determination of platinum in nonzeolitic, fresh reforming catalysts containing platinum as the only precious metal, in the range of concentration of 0.200 to 0.700 weight %.  
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.