D32.05 - Zeolites

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 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 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 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 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 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 and health practices and determine the applicability of regulatory limitations prior to use.

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 and health practices and determine the applicability of regulatory limitations prior to use.

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 and health practices and determine the applicability of regulatory limitations prior to use.

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 and health practices and determine the applicability of regulatory limitations prior to use.

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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
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.
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.
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.
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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
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.
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.
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. In addition, one may use the test method solely to determine the unit cell dimension, in which case no correlation is needed.
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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
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.  
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.
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.
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.
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 and health practices and determine the applicability of regulatory limitations prior to use.

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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
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.
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.
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.
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 of 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 "% XRD intensity/NaA."
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.

SIGNIFICANCE AND USE
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.  
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.
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.
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 determining relative zeolite diffraction intensities.  
1.2 The term "zeolite" here is restricted to those zeolites having the faujasite crystal structure, including X and Y zeolites, the various cation exchange forms, and the dealuminized, decationated, and ultrastable forms. These zeolites have cubic symmetry with unit cell parameter within the limits 24.2 and 25.0 A (2.42 and 2.50 nm). The samples contemplated include zeolite preparations in the various forms and catalysts 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 The 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 other zeolite, 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
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.
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.
Users of the 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 method solely to determine the unit cell dimension, in which case no correlation is needed.
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 (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 and health practices and determine the applicability of regulatory limitations prior to use.

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 and health practices and determine the applicability of regulatory limitations prior to use.

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 of 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 "% XRD intensity/NaA."
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.

SCOPE
1.1 This test method covers determining relative zeolite diffraction intensities.  
1.2 The term "zeolite" here is restricted to those zeolites having the faujasite crystal structure, including X and Y zeolites, the various cation exchange forms, and the dealuminized, decationated, and ultrastable forms. These zeolites have cubic symmetry with unit cell parameter within the limits 24.2 and 25.0 A (2.42 and 2.50 nm). The samples contemplated include zeolite preparations in the various forms and catalysts 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 The 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 other zeolite, 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 and health practices and determine the applicability of regulatory limitations prior to use.

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 (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.
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.