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ASAP 2460
Micromeritics ASAP 2460 User Manual
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ASAP 2460 Operator’s Manual
Degas
246-42800-01 - Aug 2013
4-25
Degas
Unit > Degas
If a SmartPrep is not connected
to the analyzer
,
the menu options in this sect
ion are
disabled.
190
192
Table of Contents
Section 1
5
Default Chapter
5
Table of Contents
5
1 Using the Analyzer
13
Introduction
13
Organization of the Operator's Manual
13
Conventions
15
Equipment Description
16
Gas Requirements
17
Degasser Options
17
Controls, Indicators, and Connectors
18
Front Panel
18
Side Panel
19
Back Panel
20
Turning on the System
21
Turning off the System
21
Reports
22
Interactive Reports
22
Report Features
22
Using the Software
23
Shortcut Keys
23
Shortcut Menus
23
File Status and Description
24
Files
24
File Name Conventions
25
Libraries
26
Main Menu Bar
27
Menu Structure
27
Help Menu
28
Window Menu
28
Setup Program
29
2 Operational Procedures
31
Introduction
31
Working with Interactive Reports
31
Editing the Default Method
34
Creating Methods
36
Defining Sample Information Files
38
Advanced Format
38
Basic or Restricted Format
41
Opening Sample Information Files
42
Opening Files with a Status of Complete, Analyzing, or Entered
43
Opening Files with a Status of Preparing, Prepared, or no Analysis
44
Defining Parameter Files
46
Sample Tube
46
Degas Conditions
48
Analysis Conditions
49
Adsorptive Properties
51
Report Options
53
ASCII Text File Format Rules
55
Importing Manually Entered Isotherm Data from the Interactive Isotherm Window
55
Sample ASCII Text File
55
To Import the ASCII Text File
55
Copying / Pasting Manually Entered Isotherm Data
56
Preparing for Analysis
58
Cleaning and Labeling Sample Tubes
58
Determining the Sample Mass
60
Degassing the Sample
61
Installing Sample Tubes
63
Filling Dewars
64
Precautions
64
Filling an Analysis Dewar
65
Performing an Analysis
69
Standard Analysis
69
Krypton Analysis
72
High Throughput Analysis
74
Micropore Analysis
76
Generating Reports
77
Listing Files
79
Exporting Files
81
Generating Graph Overlays
83
Multiple Sample Overlays
83
Multiple Graph Overlays
88
3 File Menu
95
Introduction
95
Common Fields and Buttons - File Menu Options
95
New Sample
98
Open
99
Save
99
Save as
99
Save All
100
Close
101
Close All
101
List
101
Export
102
Convert
102
Exit
103
Sample Information Files
104
Degas Conditions File
107
Analysis Conditions Files
109
Common Fields and Buttons - Report Options
124
Report Options Files
125
Summary Report
127
Isotherm Report Options
129
Bet/Langmuir Surface Area Report Options
131
Freundlich Report Options
133
Temkin Isotherm Report Options
135
T-Plot Report Options
137
Alpha-S Method
140
F-Ratio Method
142
BJH Adsorption/Desorption Report Options
143
Tabular Report Options
145
Plot Options
147
Dollimore-Heal Adsorption/Desorption Report Options
148
Plot Options
152
Tabular Report Options
152
DFT Pore Size Report Options
154
DFT Surface Energy Report Options
156
Dubinin Report Options
157
Tabular Report Options
158
Transformed Isotherm Plot Options
158
Pore Volume Options
160
MP-Method Report Options
161
Tabular Report Options
162
Plot Options
163
User-Defined Reports
164
Options Report
166
Sample Log Report
166
Validation Report
166
4 Unit Menu
167
Introduction
167
Common Fields and Buttons - Unit Menu Options
168
Start Analysis
170
Start Krypton Analysis
174
Start High Throughput Analysis
178
Start Micropore Analysis
179
Enable Manual Control
180
Show Instrument Schematic
183
Show Dashboard
185
Show Status
188
Show Instrument Log
189
Degas
191
Show Smartprep Status
192
Start Smartprep Degas
193
Smartprep Configuration
194
Unit Configuration
195
Show All Readings
197
Diagnostics
198
Calibration
200
Save to File
200
Load from File
201
Service Test
201
5 Reports Menu
203
Introduction
203
Common Fields and Buttons - Reports Menu Options
203
Start Report
205
Close Reports
205
Open Report
206
SPC Report Options
207
Regression Report
209
Control Chart
212
Heat of Adsorption Report
215
Report Features and Shortcuts
217
Report Header
218
Report Tool Bar
219
Report Header Shortcuts
222
Report Shortcut Menus
222
Tabular Reports Shortcuts
223
Graph Shortcuts
224
Axis Cross-Hair
228
Other On-Screen Features
228
Zoom Feature
228
Report Examples
229
Isotherm Linear Plot
230
BET Surface Area Report
231
BET Surface Area Plot
232
T-Plot Report
233
BJH Adsorption: Cumulative Pore Volume
234
BJH Desorption: Cumulative Pore Volume
235
6 Options Menu
237
Introduction
237
Option Presentation
237
Restricted Format
237
Default Method
238
Manage Libraries
238
Units
240
Graph Grid Lines
240
Service Test Mode
241
7 Troubleshooting and Maintenance
243
Troubleshooting
243
Preventive Maintenance
246
Checking and Cleaning the Analysis Port Dewars
247
Replacing Analysis Port Filters
247
Replacing a Sample Tube O-Ring
249
Inspecting and Changing Vacuum Pump Fluid
251
Inspecting Fluid
251
Changing Fluid
252
Replacing the Alumina in the Oil Vapor Traps
255
Cleaning the Analyzer
258
Checking the Analysis Manifold Outgassing Rate
259
Replacing the Vacuum Pump Exhaust Filter
261
Testing the Analyzer for Leaks
261
Routine Maintenance
263
Changing Gases
263
Connecting a Gas Regulator to the Gas Supply
263
Guidelines for Connecting Gases to the Analyzer
263
Connecting the Gas Delivery Tubing to the Analyzer
265
Specifying Gas Ports
266
Cleaning and Verifying the Gas Line
267
Calibrating the System
269
Performing a Reference Material Analysis
269
8 Ordering Information
271
Analysis System Components and Accessories
271
Sample Tubes and Components
274
Forms
277
Sample Data Worksheet
279
Error Messages
281
2200 And 2400 Series
281
2500 Series
290
4000 Series
297
6100 Series
313
6200 Series
314
6500 Series
321
Calculations
325
Saturation Pressure
325
Relative Pressure Calculations
326
Equation of State
326
Quantity Adsorbed Calculations
327
Free Space
328
Measured
328
Calculated
329
Thermal Transpiration Correction
331
BET Surface Area
332
Langmuir Surface Area
333
Freundlich Isotherm
334
Temkin Isotherm
335
T-Plot
336
Alpha-S Method
337
F-Ratio Method
338
BJH Pore Volume and Area Distribution
338
Explanation of Terms
339
Calculations
340
Compendium of Variables
348
Dollimore-Heal Adsorption
349
Pore Diameter
349
Pore Length
349
Horvath-Kawazoe
350
Slit Pore Geometry (Original HK
350
Cylinder Pore Geometry (Saito/Foley
351
Sphere Pore Geometry (Cheng/Yang
352
Cheng/Yang Correction
353
Interaction Parameter
354
Additional Calculations
355
Interaction Parameter Components
356
DFT (Density Functional Theory
358
The Integral Equation of Adsorption
358
Application to Pore Size Distribution
359
Application to Surface Energy Distribution
359
Performing the Deconvolution
360
Regularization
360
Dubinin-Radushkevich
361
Dubinin-Astakhov
362
MP-Method
366
Thickness Curve Calculations
368
Broekoff-De Boer
368
Carbon Black STSA
368
Halsey
368
Harkins and Jura
368
Kruk-Jaroniec-Sayari
368
SPC Report Variables
369
Regression Chart Variables
369
Control Chart Variables
370
Summary Report
370
References
373
Free Space Correction
375
Measure
375
Calculate
375
Enter
376
Maintaining High Purity Gases
377
Using Metal Gas Lines
377
Removing Trapped Air
377
Purge Method
378
Evacuation Method
379
Dft Models
381
Models Based on Statistical Thermodynamics
381
Theoretical Background
381
Molecular Dynamics Method
382
Molecular Simulation Methods
382
Monte Carlo Method
382
Density Functional Formulation
383
Models Included
387
Non-Local Density Functional Theory with Density-Dependent Weights
387
Non-Local Density Functional Theory with Density-Independent Weights
387
Models Based on Classical Theories
393
Pore Size
393
Surface Energy
393
Kelvin Equation with Halsey Thickness Curve
394
Models Included
394
Kelvin Equation with Harkins and Jura Thickness Curve
395
Kelvin Equation with Broekhoff-De Boer Thickness Curve
396
References
397
Elements Used in this Manual
419
Contact Us
421
Section 2
423
1 About the Smart Vacprep
425
Specifications for the Smart Vacprep
427
Set the Voltage for the Smart Vacprep
428
2 About the Software
429
Add or Remove a Smart Vacprep
429
Add a Smart Vacprep Unit
430
Remove a Smart Vacprep Unit
430
Smart Vacprep Configuration
431
3 Operate the Smart Vacprep
433
Backfill the Smart Vacprep Ports
433
Evacuate the Smart Vacprep Ports
433
Quickstart Degas Conditions
435
Load Quickstart Degas Conditions into a Sample File
436
Start Smart Vacprep Degas
437
Show Smart Vacprep Dashboard
439
Show Smart Vacprep Log
440
Show Smart Vacprep Schematic
441
Smart Vacprep Schematic Shortcut Menus
442
Show Smart Vacprep Status
443
4 Smart Vacprep Calibration
445
Smart Vacprep Pressure Offset
445
Smart Vacprep Servo Valve Calibration
446
5 Smart Vacprep Diagnostics
447
6 Maintenance and Troubleshooting
458
Replace the Vacuum Pump Exhaust Filter
459
7 Parts and Accessories for the Smart Vacprep
461
8 Error Messages
463
Index Index
468
5
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Micromeritics ASAP 2460 Specifications
General
Brand
Micromeritics
Model
ASAP 2460
Category
Measuring Instruments
Language
English
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