CCP14
Shadow Peak Profiling Manual in Scanned GIF Format
CCP14 homepage is at http://www.ccp14.ac.uk/
Scanned (no OCR at Present) to ensure accuracy of the text
- Titlepage
- Shadow, A system for X-ray Powder Diffraction Analysis by S.A. Howard.
Preface, Table of Contents and Figure Titles
- Page 1-1
- An Overview of the Shadow System
- Page 1-2
- An Overview of the Shadow System - The Programs Comprising the Shadow Pattern Analysis System; Shadow
- Page 1-3
- Page 1-4
- RRXRD, CONPLT; The Files Used in the Shadow System - Control Files, pattern Files, Plot Files
- Page 1-5
- The File extensions used in the Shadow Program.
- Page 1-6
- Annotated Program Listings and Demonstration Control Files
- Page 1-7
2. Program Shadow: A General Description
- Page 2-1
- The Default Parameter File: Shadow.DFT; The Instrument Calibration Data File: WGSDAT
- Page 2-2
- Radiation Parameters, Lorentz Polarisation and Monochromator; Instrument Profile Parameters
- Page 2-3
- Two Theta Correction Coefficients; Navigating From the Main Menu, Open a Pattern File for Analysis,
Background Determination.
- Page 2-4
- Search a Pattern for Peaks, Refine Profile Parameters
- Page 2-5
- Line list Features, Read/Write Parameter File, Batch Control Functions, Exit Program;
The Default Plot File Format Generated By Program Shadow
- Page 2-6
- Page 3-1
- The Background Determination File; The Necessity for Determining Background
- Page 3-2
- The Use of Background in the Peak Search; The Use of Background in Profile Refinement;
Sampling the pattern for Background Points.
- Page 3-3
- The Polynomial Model for Background
- Page 3-4
- The Empirical Model for Background
- Page 3-5
- Page 3-6
- The Relationship Between the Angular Range for Data Collection and
the Model Used to Describe the Background.
- Page 3-7
- A Description of the Background Evaluation Menu Options and Their Default Values.
- Page 3-8
4. Peak Search
- Page 4-1
- The Peak Search Menu; General Description
- Page 4-2
- The Criteria for Peak Acceptance; The Background Threshold Level
- Page 4-3
- Minimum Relative Peak Intensity, The Sliding Second Order Polynomial Peak Finder;
Secondary Tests: Peak Proximity and Line List Overflow
- Page 4-4
- How the Printed Values of the Intensities and Peak Positions are Determined;
The Peak Search Parameters, Threshold Limit in Standard Deviations, Minimum Relative Intensity
- Page 4-5
- Number of Points Used in Peak Detection, Type of Digital Filter, Smoothing Filter Moment, Filter Width
- Page 4-6
- Specifying the Plot File Output
- Page 4-7
- A Description of the Search Menu Options and Their Default Values; Minimum Standard
Deviation Above Background for Peak Acceptance.
- Page 4-8
- Minimum Relative Intensity, Number of POints Used in the Peak Search
- Page 4-9
- Number of Points to Use in Data Smoothing, Type of Filter for Data Smoothing, Digital Filter Moment
- Page 4-10
- Plotting of the Search Results
- Page 4-1
- The Profile Refinement Menu
- Page 5-2
- General Condierations in Profile Refinement; The Angular Range for Refinement,
The Number of Parameters to be Refined, The Optimisation Algorithms
- Page 5-3
- The Convergence Criteria for the Optimisation Algorithms
- Page 5-4
- The Least-Squares Error Criterion for Refinement; Profile-Shape Function (PSF)
- Page 5-5
- Split Profile-Shape Functions, Compound Profile-Shape Functions
- Page 5-6
- Page 5-7
- Lorentz/polarization Corrections
- Page 5-8
- Shape Constraints: Constraining the Shape of all Profiles to be Identical;
Specification of the Refinement Parameters
- Page 5-9
- The Refinement Region, Entering Lines Found During a Peak Search into the Refinement Line List,
Manually Adding Lines to the Refinement Line List, The Refinemetn Options,
Directing SHADOW to Add the Alpha2 Lines when using a Single Line PSF
- Page 5-10
- Specifying the Plot File Output
- Page 5-11
- Results from the Refinement
- Page 5-12
- Adding Lines and Repeating the Optimisation Process
- Page 5-13
- The Recording of the Refined Line Parameters
- Page 5-14
- Determining the Serial Number of a Refined Parameter
- Page 5-15
- Page 5-16
- A Description of the Refinement Menu Options and Their Default Values;
Default Refinement Profile-Shape Function
- Page 5-17
- Split Profile, Compound Profile, Consterain All PSF Shapes,
Refine the Alpha1/Alpha2 Ratio for Compound Profiles
- Page 5-18
- FWHM Multiplier, Constrains on Convoluted Profile Broadening as a Function of Angle
- Page 5-19
- Initial Estimates of Crystallite Size and Strain, Pattern Asymmetry Factor
- Page 5-20
- Lorentz/Polarization Correction for Lines in Compound Profiles,
Background Accommodation During the Refinement Process
- Page 5-21
- Page 5-22
- Page 5-23
- Optimisation Algorithm, Refinement Error Criterion, Maximum Number of Refinement Cycles
- Page 5-24
- Limits for Profile Generation, Plotting of the Refinement Results
6. Line List Functions
- Page 6-1
- The Line-List Menu, General Description
- Page 6-2
- Clearing the Line List,
Using the Line List to Determine X-ray Crystallite Size and/or Strain,
Evaluation of Size and Strain
- Page 6-3
- Plotting the Results from the Size/Strain Analysis; Residual Stress Analysis
- Page 6-4
- Page 6-5
- Alpha-2/Alpha-1 Intensity Ratio Analysis; Writing the Line List to a Profile-Data-File;
Writing the Line List to a Plot File; Default Parameters in the Shadow.dft File.
Statistical Weighting During Line list Regression Analysis
- Page 6-6
- Page 7-1
- The Parameter-File Menu; General Description
- Page 7-2
- The Parameters on File, Background Parameters, Peak Search Results, Refined Line Parameters,
Instrument Parameters.
8. Batch Control Function
- Page 8-1
- The Batch-Control Menu; General Descriptions, The Interactive Mode
- Page 8-2
- The Batch-Setup Mode, The Batch-Execute Mode; Batch Setup Mode
- Page 8-3
- Batch Execute Mode; Template Processing; Auto-Setup for Refinement
- Page 8-4
- Page 9-1
- General Description, Annotated Program Listings, Program INSCAL
- Page 9-2
- Choice of Calibration Standards; STEP 1: Creating the WSGDAT File
- Page 9-3
- STEP 2: Establishing the Radiation Parameters, Record a High Angle Line Profile,
Refine the Profile parameters Using Program SHADOW
- Page 9-4
- Use Program INSCAL to Determine the Radiation Wavelength Function W,
Store the Radiation Parameters in File WSGDAT;
STEP 3: Establishing the Instrument Profile Curves,
Collect the Necessary Scans from the Standards.
- Page 9-5
- Refine the Profile Parameters Using Program SHADOW,
Use Program INSCAL to Determine the Profile Calibration Curve.
- Page 9-6
- Store the Profile Coefficients in File WSGDAT;
STEP 4: Establishing the Two-Theta Correction Curve,
Measure a Set of Standard Lines, Refine the Profile Parameters Using Program SHADOW,
Use Program INSCAL to Determine the Two-Theta Correction Curve.
- Page 9-7
- Store the Correction Curve in File WSGDAT
10. The Convolution Process Used in Program Shadow
- Page 10-1
- Page 10-2
- The Profile-Shape-Function for the Instrument Profile (W*G),
W - The Factor Determining the Number of Lines in the Instrument PSF
- Page 10-3
- The Number of Parameters in the Instrument PSF, Corrections for the Lorentz and Polarisation Factors;
The Instrument Profile Curves; Generation for the Instrument and Speciment Profiles.
- Page 10-4
- The Top-Down Process of Profile Generation,
Generation of the (W*G) Profiles, Generation fo the Specimen Profile.
- Page 10-5
- Convolution of the Instrument Profile and Specimen Profile, Numerical Convolution of (W*G) and S,
Maintaining the Definition of the Convolute Profile.
- Page 10-6
- Page 10-7
- Broadening as a Function of Angle: Crystallite Size and Strain Constraints
- Page 10-8
- Annotated Program Listing
11. XRDPLT - Plotting
- Page 11-1
- Page 11-2
- Plotting a Plot File, The Attributes for Data Groups, Freqency Codes, Offset, Pen Code, Symbol.
- Page 11-3
- The Axis Parameters for the Graph, Section per Plot, Draw Axis System, Size of Plot,
Reverse X Axis Numbering, Min Value for Y Axis, X Axis Label, Y Axis Label.
- Page 11-4
- Plotting a Pattern File, The Attributes for the Pattern, The Axis Parameters;
The Graph Editing Options Menu.
- Page 11-5
- Navigating From the Main Menu
- Page 11-6
- A Description of the Program Defaults and Their Values.
- Page 11-7
- Page 11-8
- Page 11-9
