Ventura - CE201COV.CHPAccelerated Surface Area and Porosimetry System (S/N: 2001 and higher)
Operator’s Manual
201-42821-01 October 2002
Windows is a registered trademark of Microsoft Corporation. DFT Plus is a registered trademark of Micromeritics Instrument Corporation.
©Micromeritics Instrument Corporation, 2002. All rights reserved. The software described in this manual is furnished under a license agreement and may be used or copied only in accordance with the terms of the agreement.
WARRANTY MICROMERITICS INSTRUMENT CORPORATION warrants for one year from the date of shipment each instrument manufactured by it to be free from defects in material and workmanship impairing its usefulness under normal use and service conditions except as noted herein.
Our liability under this warranty is limited to repair, servicing and adjustment, free of charge at our plant, of any instrument or defective parts, when returned prepaid to us, and which our examination discloses to have been defective. The purchaser is responsible for all transportation charges involving the shipment of materials for warranty repairs. Failure of any instrument or product due to operator error, improper installation, unauthorized repair or alteration, failure of utilities, or environmental contamination will not constitute a warranty claim. The materials of construction used in MICROMERITICS instruments and other products were chosen after extensive testing and experience for their reliability and durability. However, these materials cannot be totally guaranteed against wear and/or decomposition by chemical action (corrosion) as a result of normal use.
Repair parts are warranted to be free from defects in material and workmanship for 90 days from the date of shipment.
No instrument or product shall be returned to MICROMERITICS prior to notification of alleged defect and authorization to return the instrument or product. All repairs or replacements are made subject to factory inspection of returned parts.
MICROMERITICS shall be released from all obligations under its warranty in the event repairs or modifications are made by persons other than its own authorized service personnel unless such work is authorized in writing by MICROMERITICS.
The obligations of this warranty will be limited under the following conditions:
1. Certain products sold by MICROMERITICS are the products of reputable manufacturers, sold under their respective brand names or trade names. We, therefore, make no express or implied warranty as to such products. We shall use our best efforts to obtain from the manufacturer, in accordance with his customary practice, the repair or replacement of such of his products that may prove defective in workmanship or materials. Service charges made by such manufacturer are the responsibility of the ultimate purchaser. This states our entire liability in respect to such products, except as an authorized person of MICROMERITICS may otherwise agree to in writing.
2. If an instrument or product is found defective during the warranty period, replacement parts may, at the discretion of MICROMERITICS, be sent to be installed by the purchaser, e.g., printed circuit boards, check valves, seals, etc.
3. Expendable items, e.g., sample tubes, detector source lamps, indicator lamps, fuses, valve plugs (rotor) and stems, seals and O-rings, ferrules, etc., are excluded from this warranty except for manufacturing defects. Such items which perform satisfactorily during the first 45 days after the date of shipment are assumed to be free of manufacturing defects.
Purchaser agrees to hold MICROMERITICS harmless from any patent infringement action brought against MICROMERITICS if, at the request of the purchaser, MICROMERITICS modifies a standard product or manufactures a special product to the purchaser’s specifications.
MICROMERITICS shall not be liable for consequential or other type damages resulting from the use of any of its products other than the liability stated above. This warranty is in lieu of all other warranties, express or implied, including, but not limited to the implied warranties of merchantability or fitness for use.
One Micromeritics Drive • Norcross, GA 30093-1877 • Fax: (770) 662-3696 Domestic Sales — (770) 662-3633 Domestic Repair Service — (770) 662-3666 International Sales — (770) 662-3660 Customer Service — (770) 662-3636
Form No. 008-42104-00 Rev. 12/95
TABLE OF CONTENTS
1. GENERAL INFORMATION
Organization of the Manual . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1 Conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-2 Equipment Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3 Gas Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4 Analysis Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5 Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-7
2. INSTALLATION AND CALIBRATION
Unpacking and Inspection . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1 Equipment Damage or Loss During Shipment . . . . . . . . . . . . . 2-1 Equipment Return . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
Setting up the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-2 Installing the Vacuum Pumps . . . . . . . . . . . . . . . . . . . . . . 2-2
Removing the Rear Panel . . . . . . . . . . . . . . . . . . . . . 2-3 Preparing and Installing the Oil Vapor Traps . . . . . . . . . . 2-3 Adding Vacuum Pump Fluid . . . . . . . . . . . . . . . . . . . 2-4 Connecting the Vacuum Pumps . . . . . . . . . . . . . . . . . . 2-4 Connecting the Degas and Analysis Systems to the Vacuum Pump . . . . . . . . . . . . . . . . . . . . . . 2-4 Installing the Vacuum Pump Exhaust Filters . . . . . . . . . . 2-6 Verifying Line Voltage Selection . . . . . . . . . . . . . . . . . 2-6
Installing the Analyzer Control Panel . . . . . . . . . . . . . . . . . 2-7 Installing the Cold Trap Tubes . . . . . . . . . . . . . . . . . . . . . 2-9 Installing Saturation Pressure (Psat) Tube . . . . . . . . . . . . . . . 2-9 Selecting the Control Module Power Input . . . . . . . . . . . . . . 2-10 Inserting the Line Fuse . . . . . . . . . . . . . . . . . . . . . . . . . 2-10 Installing the Board . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-12 Connecting the Analyzer and the Interface Controller . . . . . . . . 2-13 Connecting the Cables . . . . . . . . . . . . . . . . . . . . . . . . . . 2-15 Turning On the System . . . . . . . . . . . . . . . . . . . . . . . . . 2-16 Turning Off the System . . . . . . . . . . . . . . . . . . . . . . . . . 2-17 Installing the Analysis Program . . . . . . . . . . . . . . . . . . . . . 2-17 Changing Your Hardware Configuration . . . . . . . . . . . . . . . . 2-19 Connecting Regulators and Delivery Tubes . . . . . . . . . . . . . . 2-20
Nitrogen System . . . . . . . . . . . . . . . . . . . . . . . . . . 2-20 Krypton System . . . . . . . . . . . . . . . . . . . . . . . . . . 2-21
ASAP 2010 Table of Contents
Jan 01 i
Changing Analysis or Backfill Gas . . . . . . . . . . . . . . . . . . . 2-22 Connecting the Gas Supply to the Analyzer . . . . . . . . . . . 2-23 Selecting the Analysis Gas in the Unit Configuration Dialog Box . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-24 Selecting the Psat Gas in the Unit Configuration Dialog Box . 2-24 Selecting Adsorptive Properties and Analysis Conditions . . . . 2-25
Verifying Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-26 Calibrating the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . 2-28
Calibrating the Manifold Temperature Sensor . . . . . . . . . . 2-28 Method 1 . . . . . . . . . . . . . . . . . . . . . . . . . . 2-28 Method 2 . . . . . . . . . . . . . . . . . . . . . . . . . . 2-29
Calibrating the Pressure Gauge . . . . . . . . . . . . . . . . . . 2-31 Calibrating the Pressure Scale . . . . . . . . . . . . . . . . . . . 2-32 Calibrating the System Volume . . . . . . . . . . . . . . . . . . 2-33
Cleaning and Labeling Sample Tubes . . . . . . . . . . . . . . . . . 2-36 Weighing Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-40 Degassing the Sample . . . . . . . . . . . . . . . . . . . . . . . . . . 2-42 Unloading the Sample Following Degassing . . . . . . . . . . . . . . 2-47 Transferring the Degassed Sample to the Analysis Port . . . . . . . . 2-48 Installing Dewars . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-50
Precautions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-50 Cold Trap Dewar . . . . . . . . . . . . . . . . . . . . . . . . . . 2-51 Analysis Dewar . . . . . . . . . . . . . . . . . . . . . . . . . . 2-52
Unit Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-54
3. GENERAL OPERATING INSTRUCTIONS
Front and Rear Panel Controls and Indicators . . . . . . . . . . . . . . . . 3-1 Front Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
Degas Section . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2 Auto Degas and Manual Valves . . . . . . . . . . . . . . 3-2 Heater Control . . . . . . . . . . . . . . . . . . . . . . . 3-4 Vacuum . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-5
Analysis Section . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6 High Vacuum Pump Switch (Micropore and Krypton only) . . 3-7
Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-8 Using the Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-9
Mouse . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-9 Keyboard . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-10 Windows . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-11 Main Menu Bar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-12 Dialog Boxes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-16
Subdialog Boxes . . . . . . . . . . . . . . . . . . . . . . . . . . 3-21 Selecting Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-22 Opening Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-24 File Name Conventions . . . . . . . . . . . . . . . . . . . . . . . . . 3-24 Selecting Data Presentation Default Values . . . . . . . . . . . . . . . 3-25 Using Help . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-25
Table of Contents ASAP 2010
ii Jan 01
4. DEFINING ANALYSIS VARIABLES
Sample Information Files . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1 Creating a Default Sample Information File . . . . . . . . . . . . . . . . . 4-2
Basic Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-2 Advanced Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-5
Defining Sample Information Files . . . . . . . . . . . . . . . . . . . . . . 4-8 Basic Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-8 Advanced Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-10
Defining Analysis Conditions . . . . . . . . . . . . . . . . . . . . . . . . . 4-12 Defining Adsorptive Properties . . . . . . . . . . . . . . . . . . . . . . . . 4-14 Defining Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-16 Collected Data and Entered Data . . . . . . . . . . . . . . . . . . . . . . 4-18
5. PERFORMING ANALYSES
Preparing Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1 Choosing Sample Tubes . . . . . . . . . . . . . . . . . . . . . . . . . 5-1 Determining Amount of Sample to Use . . . . . . . . . . . . . . . . 5-2
Performing the Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3 Analysis Gas . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3 Psat Gas . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4 Automatic Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4 Pre-Entered Custom Analysis . . . . . . . . . . . . . . . . . . . . . . 5-5 Online Custom Analysis . . . . . . . . . . . . . . . . . . . . . . . . . 5-6
Monitoring an Analysis with the Status Control Screen . . . . . . . . . . 5-8 Manifold Status . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-8 Optional Push Buttons . . . . . . . . . . . . . . . . . . . . . . . . . . 5-9 System Diagram . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-11 Analysis Detail . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-15
Isotherm . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-15 Status summary . . . . . . . . . . . . . . . . . . . . . . . . . . 5-15
6. FILE MAINTENANCE
File Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-1 Open . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-3
Sample Information . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-4 Basic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-5 Advanced format . . . . . . . . . . . . . . . . . . . . . . . . . . 6-6 Restricted Format . . . . . . . . . . . . . . . . . . . . . . . . . 6-8
Analysis Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . 6-9 Adsorptive Properties . . . . . . . . . . . . . . . . . . . . . . . . . . 6-24 Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-26
Save . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-27 Save As . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-27 Save All . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-28 Close . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-29
ASAP 2010 Table of Contents
Jan 01 iii
Close All . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-29 Print . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-30 List . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-32 Export . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-34 Convert . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-36 Exit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-39
7. REPORTS
Format Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-1 Reports Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-2
Start Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-2 Cancel Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-4 Rate of Adsorption (ROA) . . . . . . . . . . . . . . . . . . . . . . . . 7-4 DFT Plus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-4
Reports Displayed on the Screen . . . . . . . . . . . . . . . . . . . . . . . 7-5 Tabular Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-5
Optional Push Buttons for Tabular Reports . . . . . . . . . . . 7-5 Graphs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-6
Printed Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-8 Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-10 Defining Standard Report Options . . . . . . . . . . . . . . . . . . . . . . 7-13
BET Surface Area Report Options . . . . . . . . . . . . . . . . . . . 7-13 Langmuir Surface Area Report Options . . . . . . . . . . . . . . . . 7-16 Isotherm Report Options . . . . . . . . . . . . . . . . . . . . . . . . . 7-18 t-Plot Method Options . . . . . . . . . . . . . . . . . . . . . . . . . . 7-20 BJH Adsorption/Desorption Report Options . . . . . . . . . . . . . . 7-23 BJH Tabular Report Options . . . . . . . . . . . . . . . . . . . . . . 7-27 BJH Plot Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-30
Defining Micropore Report Options . . . . . . . . . . . . . . . . . . . . . . 7-33 Horvath-Kawazoe Report Options . . . . . . . . . . . . . . . . . . . . 7-33
Horvath-Kawazoe Tabular Report Column Options . . . . . . . 7-37 Horvath-Kawazoe Plot Options . . . . . . . . . . . . . . . . . . 7-38
Dubinin Report Options . . . . . . . . . . . . . . . . . . . . . . . . . 7-40 Dubinin Tabular Report Options . . . . . . . . . . . . . . . . . 7-42 Dubinin Plot Options . . . . . . . . . . . . . . . . . . . . . . . 7-43
Dubinin Transformed Isotherm Options . . . . . . . . . 7-43 Dubinin Pore Volume Options . . . . . . . . . . . . . . . 7-44
MP-Method Report Options . . . . . . . . . . . . . . . . . . . . . . . 7-46 MP-Method Tabular Report Options . . . . . . . . . . . . . . . 7-48 MP-Method Plot Options . . . . . . . . . . . . . . . . . . . . . 7-49
Use of Graph Overlays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-52 Multiple Samples Overlay Implementation . . . . . . . . . . . . . . . 7-53 Multiple Graphs Overlay Implementation . . . . . . . . . . . . . . . 7-58
Sample Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-61 Analysis Log . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-62 Isotherm Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-66 BET Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-69
Table of Contents ASAP 2010
iv Jan 01
BET Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-71 BJH Adsorption Report: BJH Pore Distribution Report . . . . . . . . 7-73 BJH Adsorption Report: Cumulative Pore Volume Plot . . . . . . . . 7-74 BJH Adsorption Report: dV/dlog(D) Pore Volume Plot . . . . . . . . 7-75 BJH Desorption Report: BJH Pore Distribution Report . . . . . . . . 7-76 BJH Desorption Report: Cumulative Pore Volume Plot . . . . . . . . 7-77 BJH Desorption Report: dV/dlog(D) Desorption Pore Volume Plot . 7-78 Micropore Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-79 Summary Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-86 Overlay Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-87
Multiple Sample Example . . . . . . . . . . . . . . . . . . . . . 7-87 Multiple Graph Example . . . . . . . . . . . . . . . . . . . . . 7-88
8. SYSTEM OPTIONS
Status/Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-4 Manually Controlling the System . . . . . . . . . . . . . . . . . . . . 8-5 Opening and Closing Valves . . . . . . . . . . . . . . . . . . . . . . 8-6 Raising and Lowering Dewars . . . . . . . . . . . . . . . . . . . . . 8-7
Sample Defaults . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-8 Basic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-8 Advanced Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-10
Data Presentation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-13 System Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-15 Parameter Files Directory . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-16
9. TROUBLESHOOTING AND MAINTENANCE
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-1 Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-1 Preventive Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-5
Lubricating the Elevator Screw . . . . . . . . . . . . . . . . . . . . . 9-6 Checking the Analysis Port Dewar . . . . . . . . . . . . . . . . . . . 9-6 Replacing the Port Filters . . . . . . . . . . . . . . . . . . . . . . . . 9-7
Analysis Port . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-7 Degas Port . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-8
Cleaning the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . 9-9 Replacing the Vacuum Pump Exhaust Filter . . . . . . . . . . . . . . 9-9 Inspecting and Changing Vacuum Pump Fluid . . . . . . . . . . . . 9-11
Inspecting Fluid . . . . . . . . . . . . . . . . . . . . . . . . . . 9-11 Changing Fluid . . . . . . . . . . . . . . . . . . . . . . . . . . 9-12
Lubricating the High Vacuum Pump (Krypton, Chemi, and Micropore Units Only) . . . . . . . . . . . . . 9-14
ASAP 2010 Table of Contents
Jan 01 v
Resetting the High Vacuum Pump Timer (Krypton, Chemi and Micropore Units Only) . . . . . . . . . . . . . 9-14 Calibrating the Manifold Temperature Sensor . . . . . . . . . . . . . 9-15 Checking the Heating Mantle Stability . . . . . . . . . . . . . . . . . 9-15 Cleaning the Cold Trap Tubes . . . . . . . . . . . . . . . . . . . . . . 9-16 Replacing the Alumina in the Oil Vapor Traps . . . . . . . . . . . . 9-17 Testing the Analyzer for Leaks . . . . . . . . . . . . . . . . . . . . . 9-20 Replacing the Calibration Chamber Cap O-ring . . . . . . . . . . . . 9-21 Performing a Reference Material Run . . . . . . . . . . . . . . . . . 9-21 Calibrating the System Volume . . . . . . . . . . . . . . . . . . . . . 9-22 Checking the Degas Pressure Switch . . . . . . . . . . . . . . . . . . 9-22 Replacing the Sample Tube O-ring . . . . . . . . . . . . . . . . . . . 9-23 Checking Analyzer Outgassing Rate . . . . . . . . . . . . . . . . . . 9-24
Analysis Manifold . . . . . . . . . . . . . . . . . . . . . . . . . 9-24 Degas Manifold . . . . . . . . . . . . . . . . . . . . . . . . . . 9-25
Checking the Vacuum Sets . . . . . . . . . . . . . . . . . . . . . . . 9-25 Analysis VAC SET . . . . . . . . . . . . . . . . . . . . . . . . . 9-25 Degas VACUUM SET . . . . . . . . . . . . . . . . . . . . . . . 9-26
Routine Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-27 Overhauling the Analyzer Valves . . . . . . . . . . . . . . . . . . . . 9-27
Degas Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-27 Analysis Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-30
10. ORDERING INFORMATION
Control Module Error Messages . . . . . . . . . . . . . . . . . . . . B-1 Interface Controller Error Messages . . . . . . . . . . . . . . . . . . B-39
Appendix C: Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . C-1 Saturation Pressure (Po) . . . . . . . . . . . . . . . . . . . . . . . . . C-1 Relative Pressure Calculations . . . . . . . . . . . . . . . . . . . . . . C-1 Volume Adsorbed Calculations . . . . . . . . . . . . . . . . . . . . . C-3
Free Space . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-3 Volume Adsorbed . . . . . . . . . . . . . . . . . . . . . . . . . C-4
Equilibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-5 Data Smoothing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-6 Thermal Transpiration Correction Calculations . . . . . . . . . . . . . C-7 BET Surface Area Calculations3 . . . . . . . . . . . . . . . . . . . . C-8 Langmuir Surface Area Calculations . . . . . . . . . . . . . . . . . . C-9 t-Plot Calculations5 . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-11 BJH Pore Volume and Area Distribution Calculations . . . . . . . . . C-13
Explanation of Terms . . . . . . . . . . . . . . . . . . . . . . . C-13 Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-14
Table of Contents ASAP 2010
vi Jan 01
Slit Pore Geometry (original HK) . . . . . . . . . . . . . . . . C-23 Cylinder Pore Geometry (Saito/Foley)11 . . . . . . . . . . . . . C-25 Sphere Pore Geometry (Cheng/Yang)12 . . . . . . . . . . . . . C-26 Cheng/Yang Correction12 . . . . . . . . . . . . . . . . . . . . . C-27 Interaction Parameter . . . . . . . . . . . . . . . . . . . . . . . C-28
Additional Calculations . . . . . . . . . . . . . . . . . . C-28 Interaction Parameter Components . . . . . . . . . . . . . . . . C-30
Dubinin-Radushkevich Calculations14 . . . . . . . . . . . . . . . . . C-32 Dubinin-Astakhov Calculations . . . . . . . . . . . . . . . . . . . . . C-34 MP-Method Calculations15 . . . . . . . . . . . . . . . . . . . . . . . C-39 Summary Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-41 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-43
Appendix D: Default Files and System Files . . . . . . . . . . . . . . . . D-1 Appendix E: Testing for Leaks . . . . . . . . . . . . . . . . . . . . . . . E-1
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-2
Terms . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-2 Basic Activities . . . . . . . . . . . . . . . . . . . . . . . . . . E-3
Choosing the Appropriate Transducer . . . . . . . . . . . . . . . . . E-5 Preparing the Analyzer for Leak Testing . . . . . . . . . . . . . . . . E-6 Determining the Outgas Rate: General Instructions . . . . . . . . . . E-7 Determining the Leak Rate for a Valve: General Instructions . . . . E-8 What To Do If You Detect a Leaking Valve . . . . . . . . . . . . . . E-9
Removing Differential Pressure from a Leaking Valve . . . . . E-9 Repairing or Replacing a Leaking Valve . . . . . . . . . . . . . E-9
Testing Individual Valves . . . . . . . . . . . . . . . . . . . . . . . . E-11 Testing Valves 1 and 2 . . . . . . . . . . . . . . . . . . . . . . E-11 Testing Valve 3 . . . . . . . . . . . . . . . . . . . . . . . . . . E-16 Testing Valves 4 and 5 . . . . . . . . . . . . . . . . . . . . . . E-19 Testing Valve 6 . . . . . . . . . . . . . . . . . . . . . . . . . . E-22 Testing Valve 7 . . . . . . . . . . . . . . . . . . . . . . . . . . E-25 Testing Valve 8 . . . . . . . . . . . . . . . . . . . . . . . . . . E-28 Testing Valve 9 . . . . . . . . . . . . . . . . . . . . . . . . . . E-31 Testing Valve 10 . . . . . . . . . . . . . . . . . . . . . . . . . E-34 Testing Valve 11 . . . . . . . . . . . . . . . . . . . . . . . . . . E-37 Testing Valves 10 and 11 (Alternate Method) . . . . . . . . . . E-40
Valve Test Data Sheets . . . . . . . . . . . . . . . . . . . . . . . . . E-43 Valves # 1 and 2 (tested together) . . . . . . . . . . . . . . . . E-43 Valve # 3 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-44 Valves # 4 and 5 . . . . . . . . . . . . . . . . . . . . . . . . . . E-45 Valve # 6 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-46 Valve #7 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-47 Valve # 8 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-48 Valve # 9 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-49 Valve # 10 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-50 Valve # 11 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-51 Valves # 10 and 11 (tested together) . . . . . . . . . . . . . . . E-52
ASAP 2010 Table of Contents
Jan 01 vii
viii Jan 01
GENERAL INFORMATION
This manual describes how to install and operate the Accelerated Surface Area and Porosimetry (ASAP) 2010 System for Windows®. It includes instructions for the following ASAP 2010 systems:
• Standard System • Krypton System • Micropore System
Organization of the Manual
The manual is divided into the following chapters:
Chapter 1 - General Information. Describes the components of the ASAP 2010 and lists its specifications.
Chapter 2 - Installation and Calibration. Describes how to unpack, in- spect, install, and calibrate the ASAP 2010.
Chapter 3 - General Operating Instructions. Describes how to use the analyzer’s front and rear panel controls and the system menus and dialog boxes.
Chapter 4 - Defining Analysis Variables. Describes how to enter informa- tion used to control analyses and produce reports.
Chapter 5 - Performing Analyses. Provides instructions for preparing sam- ples and performing analyses.
Chapter 6 - File Maintenance. Provides instructions for creating and edit- ing files used by the system.
Chapter 7 - Reports. Describes how to print and cancel reports, and how to use the graph overlay capability. It also contains samples of reports.
Chapter 8 - System Options. Describes how to configure the system to meet your laboratory’s requirements. Some of the system options which you may select include report formats, default sample information, and pore size units. Also explains how to manually control the system.
Chapter 9 - Troubleshooting and Maintenance. Provides instructions for troubleshooting hardware problems and for performing routine mainte- nance procedures.
Chapter 10 - Ordering Information. Provides part numbers and descrip- tions of the ASAP 2010 System components and accessories that may be ordered from Micromeritics.
ASAP 2010 Organization of the Manual
Jan 01 1-1
Appendix A - Forms. Contains forms you may use to record information prior to entering it into the system.
Appendix B - Error Messages. Lists the error messages that may be dis- played by the software/hardware and includes a cause and action for each.
Appendix C - Calculations. Contains the calculations used by the system to produce reports.
Appendix D- Default Files and System Files. Describes the files shipped with or created by the ASAP 2010 software.
Appendix E - Testing for Leaks. Describes the procedure for testing each valve for leaks.
Conventions
This manual uses the symbols shown below to identify notes of importance, cautions, and warnings.
Notes contain a tip or important information pertinent to the subject matter.
Cautions contain information to help you prevent actions which could damage the instrument.
Warnings contain information to help you prevent actions which could cause personal injury.
Conventions ASAP 2010
1-2 Jan 01
Equipment Description
The ASAP 2010 System consists of an analyzer; a control module (com- puter), which enables you to enter analysis and report options; and an inter- face controller, which controls analyses.
Figure 1-1. ASAP 2010 System
The ASAP 2010 analyzer contains two sample preparation ports and one analysis port. Inline cold traps are located between the vacuum pump and the manifold in both the analysis and the degas systems. The sample saturation pressure (Psat) tube is located next to the sample analysis port.
The analysis bath fluid Dewar resides on an automatically operated elevator. Controls and indicators located on a control panel operate the vacuum sys- tems, degas valves, and heating mantles. A sliding shield can be lowered to provide safety or raised to provide access to the sample analysis port and preparation ports.
Analyzer
Gas Requirements
Compressed gases are required for analyses performed by the ASAP 2010 analyzer. Gas bottles or an outlet from a central source should be located near the analyzer.
Appropriate regulators which have been leak checked and specially cleaned are required. Pressure relief valves should be set to no more than 30 psig (200 kPag). Gas regulators are available from Micromeritics; refer to Chap- ter 10, Ordering Information.
Sliding Shield
Analysis Bath Dewar
Analysis Software
The ASAP 2010 System software for Windows monitors and controls the ana- lyzer. It enables you to perform automatic analyses with just a few keystrokes and collects and reports analysis data. You can choose from a variety of re- ports, which can be automatically printed after an analysis or stored and printed later. The following are some of the reports available:
• Summary report for area, volume, and average pore size • Elapsed-time analysis log showing recorded data • BET surface area • Langmuir surface area • Micropore analysis by t-Plot using the Halsey thickness equation • Micropore analysis by t-Plot using the Harkins and Jura (deBoer) thick-
ness equation • BJH adsorption pore distribution • BJH desorption pore distribution • Horvath-Kawazoe differential pore volume* • Dubinin analysis* • MP-Method analysis*
*Micropore systems only
• Isotherm of volume adsorbed vs. relative pressure • BET plot showing BET transformation vs. relative pressure • Langmuir plot showing Langmuir transformation vs. relative pressure • t-Plot by Halsey thickness equation • t-Plot by Harkins and Jura (deBoer) thickness equation • Cumulative adsorption (or desorption) pore volume • dV/dD adsorption (or desorption) pore volume • dV/dlog(D) adsorption (or desorption) pore volume • Cumulative adsorption (or desorption) pore area • dA/dD adsorption (or desorption) pore area • dA/dlog(D) adsorption (or desorption) pore area • Horvath-Kawazoe cumulative pore volume* • Horvath-Kawazoe dV/dD pore volume* • Dubinin transformed isotherm* • Dubinin dV/dR pore volume* • MP-Method cumulative pore volume* • MP-Method dV/dR pore volume* • MP-Method cumulative pore area* • MP-Method dA/dR pore area*
*Micropore systems only
Jan 01 1-5
For most reports and data entry, you can measure either the pore diameter or radius, and pore size can be expressed in either angstroms or nanometers.
For all plots, you can select the X- and Y-axis ranges to enhance the detail of any required section. Also, you can automatically scale the X- and Y-axis ranges to show all available information.
For micropore reports, t-Plots, and BJH reports, the parameters of the Halsey equation and the Harkins and Jura equation are variable.
For BJH, Horvath-Kawazoe, Dubinin, and MP-Method tabular reports, you may select multiple columns of data. Data can be reported at collected points or at pore sizes you select.
Analysis Software ASAP 2010
Specifications
The ASAP 2010 system has been designed and tested to meet the specifi- cations provided in Table 1-1.
Table 1-1. ASAP 2010 Specifications
Characteristic Specification
———— PRESSURE MEASUREMENT ————
Resolution: 1000-mmHg Transducer 10-mmHg Transducer* 1-mmHg Transducer* (optional for high stability)
0.001 mmHg 0.00001 mmHg 0.000001 mmHg
Accuracy: (Includes nonlinearity, hysteresis, and nonrepeatability. Transducer manufacturer’s specifications.)
1000-mmHg Range 10-mmHg Range (Krypton and micropore systems) 1-mmHg Range (optional for high stability)
Within 0.073% of full scale Within 0.15% of reading
Within 0.12% of reading (for long-term stability)
———— VACUUM SYSTEM ————
Vacuum Pumps: Two independent, 2-stage mechanical pumps; one for analysis and one for degas. Ultimate vacuum 5 x 10-3 mmHg.
High Vacuum Pump* (Analysis System):
Ultimate vacuum; less than 0.75 x 10-6
mmHg (Molecular Drag Pump) or less than 3.8 x 10-9 mmHg (Turbo Molecular Pump)
Ultimate vacuum measured by pump manufacturer according to Pneurop Standard 5608.
———— MANIFOLD TEMPERATURE TRANSDUCER ————
Accuracy: ± 0.02°C (by keyboard entry)
*Multigas and micropore systems
Characteristic Specification
———— DEGAS SYSTEM ————
Temperature Range: Ambient to 450°C
Selection: Digitally set, 1°C increments
Accuracy: Deviation less than ±10°C of set point at thermocouple
Backfill Gas: User-selectable, typically helium or nitrogen
———— SYSTEM CAPACITY ————
Analysis: 1 sample port and 1 saturation pressure tube
Total Operating Capacity: Up to four complete analysis units can be independently controlled by one control module
———— CRYOGEN SYSTEM ————
Special Features: Patented Isothermal Jackets effectively maintain cryogen level constant on sample tube and Po tube during analysis while evaporation of cryogen occurs
Capacity 1.9 Liter Dewar, which provides up to 60 hours of unattended analysis
Analysis Time: Unlimited. cryogen Dewars may be refilled without affecting the accuracy of results
———— SAMPLE SIZE ————
Sample tubes are available for various size pellets, cores and powders. Sam- ple tube stems are normally 1.27-cm (1/2-in.) OD with 9-cc bulbs. Also available are 0.635- (1/4-) or 0.953-cm (3/8-in.) OD with 9-cc bulbs. Mono- lithic samples up to 12 mm diameter x 25 mm long fit into a taper-sealed tube. Special tubes can be designed to accommodate unusual samples.
Specifications ASAP 2010
1-8 Jan 01
Characteristic Specification
———— ENVIRONMENT ————
Temperature: 10 to 30°C operating; -10 to 55°C storing or shipping
Humidity: 20 to 80% relative, noncondensing
———— ELECTRICAL ————
Frequency: 50/60 Hz
Normal: Argon, carbon dioxide, nitrogen, krypton (Krypton System), and other suitable gases
———— PHYSICAL ————
ASAP 2010 Specifications
Jan 01 1-9
This chapter contains instructions for the following:
• Unpacking and inspecting the equipment • Installing the analyzer • Installing the analysis program • Connecting gas bottles to the system • Verifying operation of the ASAP 2010 System • Calibrating the ASAP 2010 System
The procedures are provided in the sequence recommended for system instal- lation. Follow the procedures in the order presented to ensure proper system operation.
Unpacking and Inspection
When you receive the shipping cartons, carefully compare the packing list with the equipment actually received while checking for equipment damaged during shipment. Be sure to sift through all packing materials before declar- ing equipment missing.
Save the shipping cartons if equipment or parts have been damaged or lost. The inspector or claim investigator must examine the cartons prior to completion of the inspection report.
Equipment Damage or Loss During Shipment
When equipment is damaged or lost in transit, you are required to make note of the damage or loss on the freight bill. The carrier, not the shipper, is re- sponsible for all damage or loss. In the event of equipment damage or loss during shipment, contact the carrier of the equipment immediately.
Equipment Return
Micromeritics strives to ensure that all items arrive safely and in working or- der. Occasionally, due to circumstances beyond our control, equipment is re- ceived which is not in working condition. When it is necessary to return equipment (damaged either during shipment or while in use) to Micromeritics for repair or replacement, use the following procedure:
ASAP 2010 Unpacking and Inspection
Jan 01 2-1
1. Tag or identify the defective equipment, noting the defect and circum- stances, if any, under which the defect is observed.
2. Referencing the sales order or purchase order, identify the date that the equipment was received.
3. Notify the Micromeritics Service Department of the defect and request shipping instructions. The service department will assign a Returned Ma- terials Authorization (RMA) number. Write the RMA number on the out- side of the shipping carton.
Setting up the Analyzer
The ASAP 2010 System should be installed correctly and tested to make sure it is operating properly before actual analyses are attempted. Setup and check- out procedures are described in this section.
Installing the Vacuum Pumps
The dual vacuum pump assembly is installed at the factory, but it is not con- nected to the power or vacuum connections. This section describes the follow- ing procedures:
• Removing the rear panel • Connecting the vacuum pumps • Connecting the degas and analysis systems to the vacuum pump • Verifying line voltage selection
Refer to Chapter 9, Troubleshooting and Maintenance, for detailed instruc- tions on the following procedures:
• Installing the oil vapor traps on the vacuum pumps • Filling the vacuum pump with fluid • Installing the vacuum pump exhaust filters
Setting up the Analyzer ASAP 2010
2-2 Jan 01
Removing the Rear Panel
1. Place the main unit on a table with the rear panel exposed.
Figure 2-1. Main Unit (rear view)
2. Loosen (but do not remove) the screws along the bottom of the analyzer upper rear panel. Then remove the screws from the top of the upper rear panel. Remove the panel by pulling the upper edge away from the analyzer and then upward.
3. Remove the screws from the lower right rear panel.
4. Remove the cable ties that secured the vacuum hoses and cable for shipment. Slide the vacuum pump assembly out of the main unit.
5. Remove the vacuum pump drain hoses from their shipping location on top of the pumps. Attach the hoses to the handles so that they will be ready when needed for vacuum pump oil draining.
Preparing and Installing the Oil Vapor Traps
The oil vapor traps are attached to the intake port of the vacuum pump. They reduce the amount of oil vapor that collects in the hoses leading to the instru- ment. The traps contain alumina, which must be activated before using to re- move sorbed moisture. Refer to Replacing the Alumina in the Oil Vapor Traps in Chapter 9 for instructions on preparing the alumina and installing the oil vapor traps.
Upper Rear Panel
Jan 01 2-3
Adding Vacuum Pump Fluid
Refer to Inspecting and Changing Vacuum Pump Fluid in Chapter 9 for detailed instructions.
Connecting the Vacuum Pumps
1. Make sure the power cord of each vacuum pump is completely plugged into the socket on the side of the power module.
Figure 2-2. Vacuum Pump Power Cord Connection
2. Be sure the flat cable for the control panel passes through the slot at the front of the analyzer. Slide the dual vacuum pump assembly toward the analyzer.
Connecting the Degas and Analysis Systems to the Vacuum Pump
Connect the degas system to the oil vapor trap and vacuum pump as follows:
1. Locate the vacuum pump closest to the electrical power connector. Loosen the wing nut that secures the vacuum clamp on the intake port of the pump. Open the clamp and remove it from the intake port.
Power Cord Sockets
2-4 Jan 01
2. Remove the dust cover.
The dust cover must be removed from the vacuum pump intake port. Operation of the pump with the dust cover on the port could result in damage to the pump.
3. Remove the plastic cover from the hose labeled “Degas.”
4. Install the oil vapor trap on the intake port centering ring. The trap may be mounted with either end up. Open the clamp included with the oil va- por trap and place it around the flanges of the pump and trap. Close the clamp and secure it by turning the wing nut clockwise.
5. Use the centering ring and clamp removed in Step 1 to attach the hose to the trap or to the intake port.
Figure 2-3. Installing Oil Vapor Trap
6. Connect the analysis system to the vacuum pump by following the proce- dure described above.
Centering RingClamp
Jan 01 2-5
Installing the Vacuum Pump Exhaust Filters
Refer to Replacing the Vacuum Pump Exhaust Filter in Chapter 9.
Verifying Line Voltage Selection
Do not connect the ASAP 2010 to the power source until the proper volt- age selection is made. Doing so could result in electrical shock and/or damage to the assembly.
Verify the line voltage as follows:
1. Slide the safety gate to the right.
2. Slide the voltage selection switch to the voltage position to suit the avail- able power supply.
3. Slide the safety gate to the left.
Figure 2-4. Voltage Selection Switch
Safety Gate
2-6 Jan 01
Installing the Analyzer Control Panel
The analyzer control panel is packaged separately. Operation of the vacuum systems, degas valves, and heating devices for sample preparation is provided by the controls and indicators on the control panel. The control panel must be mounted and connected for proper operation.
1. Connect the ground wire to the analyzer:
a. Remove the screw located at the lower left of the ribbon cable con- nector.
b. Insert the screw into the ring connector on the end of the ground wire.
c. Replace the screw and tighten securely.
2. Insert the ribbon cable connector from the analyzer into the input connec- tor (striped side to the left) at the rear of the control panel. Secure the connection by clamping the locking tabs to the connector.
Make sure that the side of the control panel ribbon cable with the stripe is facing to the left when connected to the control panel. Improper con- nection could result in damage to the analyzer.
Ribbon Cable Connector (Striped Side to Left)
Ground Wire
Jan 01 2-7
3. Mount the right side of the control panel to the analyzer by inserting the pivot pin from the analyzer into the hole on the side of the control panel.
4. Mount the left side of the control panel by sliding the control panel in the direction of the pivot pin already in place (Step 3) while aligning the second pivot pin from the analyzer with the hole in the other side of the control panel.
Pivot Pin
Pivot Pin
2-8 Jan 01
Installing the Cold Trap Tubes
The glass cold trap tubes are supplied with the accessories. Install them as follows:
1. Loosen the nut and O-ring.
2. Slide the glass tube up around the metal tube and secure it with the O-ring and nut.
3. Repeat for the second cold trap port.
Installing Saturation Pressure (Psat) Tube
The saturation pressure tube is packaged separately. This tube must be mounted onto the front of the analyzer next to the sample analysis port as de- scribed below.
1. Remove the plastic protective cover from the saturation pressure port by turning it counterclockwise.
O-ring
Nut
Jan 01 2-9
2. Ensure that the O-ring is in place on the end of the saturation pressure tube. Rotate the tube so that the isothermal jacket is closest to the analy- sis port. Secure the tube in place by turning the connector nut clockwise. Tighten by hand.
Selecting the Control Module Power Input
The power input selection on the control module must be set to match the in- put power source. The control module operates with either 100-120 VAC or 200-240 VAC at 50 or 60 Hz. Refer to the instruction manual supplied with your control module for instructions on selecting power input.
Do not connect the control module power cord to a power source until the proper voltage selection is made. Doing so could result in electrical shock and/or damage to the control module
Inserting the Line Fuse
The appropriate line fuse must be installed before the interface controller can be operated. The fuse is inserted in the power connector as follows:
1. Make sure the power cord is not connected to the controller.
Failure to disconnect the power cord from the controller before removing the cover from the input power connector could result in electrical shock.
Sample Port Po Port
2-10 Jan 01
2. Using a pointed object, remove the cover from the power connector at the rear of the controller.
3. Fuse the power line according to local safety practices. Referring to the following figure, identify the position of the fuse block. In a single-fuse arrangement, the fuse block should be positioned so the side with the sin- gle fuse slot and the jumper bar is away from the cover. In a double- fuse arrangement, the fuse block should be positioned so the side with the double fuse slots is away from the cover.
If the fuse block is positioned properly for the desired fusing, proceed to Step 4.
If the fuse block is not positioned properly for the desired fusing, per- form the following procedure first:
a. Remove the fuse block retaining screw.
b. Lift the fuse block from the cover.
c. Rotate the fuse block.
d. Mount the fuse block to the cover.
e. Replace the retaining screw.
Figure 2-5. Fusing Arrangements
Jan 01 2-11
4. Insert a 0.5 A Slow-Blow fuse.
The fuse must be identical in type and rating to that specified. Use of another fuse could result in electrical shock and/or damage to the controller.
5. Replace the input power connector cover.
6. Attach the power cord to the controller and to an appropriate power source.
Installing the Board
Perform the following procedure if the circuit board is not installed in the in- terface controller:
1. Make sure the power switches for the analyzer, interface controller, and control module are in the OFF positions. Plug the power cords into elec- trical outlets to ensure a good ground connection.
2. Remove the cover from the interface controller.
3. Remove the screw from the expansion slot in the interface controller.
4. Remove any jewelry from your hands and wrists. Attach a ground strap to your wrist and to the interface controller. Keep the ground strap con- nected until instructed to remove it.
5. Remove the controller board from the anti-static bag.
6. Set the switch(es) as follows:
If.... Then....
Your board contains DIP switches:
1 OFF 4 ON 7 ON 2 OFF 5 ON 8 OFF 3 ON 6 ON
Your board contains a rotary switch:
Position 1
7. Holding the circuit board by the edges only, carefully insert it into the expansion slot. Make sure the board is fully seated in the slot.
Setting up the Analyzer ASAP 2010
2-12 Jan 01
8. Insert the screw removed from the expansion slot cover and tighten it.
9. Remove the ground strap from the interface controller.
10. Replace the interface controller cover.
Connecting the Analyzer and the Interface Controller
The interface controller communicates messages with tones from its resi- dent speaker. As with the standard visual messages, these tonal messages indicate processing status. The ASAP 2010 System should be set up in an environment which allows you to hear these messages. Refer to Appendix B, Error Messages, for additional information.
1. Attach the interface cable:
a. Connect one end to the output connector labeled COMPUTER on the rear of the analyzer.
b. Connect the other end to the input connector labeled Analyzer on the rear of the interface controller.
ASAP 2010 Setting up the Analyzer
Jan 01 2-13
2. Attach the communication cable:
a. Connect one end to the connector on the rear panel of the control module.
b. Connect the other end to the connector labeled RS232 on the back of the interface controller.
c. Tighten the retaining screws.
The RS-232 cable is used to connect the interface controller to the con- trol module. The standard cable has a 9-pin female connector for the in- terface controller and a 9-pin female connector for the control module and is configured as a null modem cable. If your control module has a different pin configuration, use the appropriate adapter to attach the in- terface controller to the control module.
You may attach an Uninterruptible Power Supply (UPS) to the interface controller to preserve ASAP 2010 data in the event of a power failure. In the event of a power failure during analysis, the data collected before the power failure will be preserved when power is restored. The UPS voltage must be greater than or equal to 100 VA for each interface controller.
Interface Controller
2-14 Jan 01
Connecting the Cables
The interface controller must be connected to the control module for the ASAP 2010 System to operate properly. The control module must be con- nected to the keyboard, the monitor, the printer, and the plotter (if used). Typi- cal cable connections are shown in the following illustration.
Figure 2-6. ASAP 2010 Cable Connections
1. Connect the keyboard to the control module by plugging the coiled cable into the connector at the rear of the control module.
Some monitors and printers shipped from the United States by Micromeritics must be connected to a 100-120 VAC power source. Connecting this equipment to a 200-240 VAC power source could result in electrical shock and/or damage to the equipment.
ASAP 2010
Control Module
Power Breaker Switch
Input Power Connector
Control Module On/Off
Jan 01 2-15
2. Connect the video monitor to the control module by plugging the moni- tor interface cord into the appropriate power source. Refer to the monitor manufacturer’s instruction manual for voltage requirements.
3. To install a peripheral device such as a printer or plotter, consult your Windows manual. Plotter cables are available from Micromeritics; refer to Chapter 10, Ordering Information, for part numbers.
4. Verify that one end of the control module power cord is inserted into the power input receptacle at the rear of the control module and the other end is inserted into the appropriate power source. Refer to the control module manufacturer’s instruction manual for voltage requirements.
5. Insert one end of the analyzer power cord into the input power connec- tor at the rear of the analyzer and the other end into the appropriate power source.
6. Plug the interface controller power cord into the appropriate power source.
Turning On the System
1. Place the ON/OFF switches for the control module, interface controller, monitor, and any peripheral devices in the ON position.
2. Place the analyzer Main Power switch in the ON position and verify that the red Power Supply indicators on the rear of the analyzer are illumi- nated.
3. If this is the first time you are using the system, install the Disk Operat- ing System (DOS) and Windows programs according to the instructions supplied with the program diskettes.
DOS version 6.0 is already installed if you purchased your control mod- ule from Micromeritics.
Setting up the Analyzer ASAP 2010
2-16 Jan 01
Turning Off the System
Always make sure you exit the program or Windows before turning off the control module. Failure to do so could result in loss of data.
1. Select Close from the System Menu or Exit from the File menu.
If you exit the ASAP 2010 System program with analyses in progress, the analyses continue and data are collected. Reports that are queued un- der the Print Manager will print. If, however, a power failure occurs and an uninterruptible power supply (UPS) is not attached to the interface controller, the data collected after exiting the ASAP 2010 System pro- gram are lost.
2. Place the control module, interface controller, monitor, printer, and plot- ter ON/OFF switches in the OFF position.
3. Place the analyzer Main Power switch in the OFF position.
Installing the Analysis Program
Your system must meet or exceed the following requirements before you can install the software:
• DOS version 5.0 or higher • Windows version 3.1 (enhanced mode) or Windows 95 • 386 control module with four megabytes memory and 20 megabytes
disk space
You can also install the 2010 analysis program on a computer other than the one controlling the analyzer, allowing you to:
• create or edit sample and parameter files • generate reports on completed sample files
Review the Micromeritics PROGRAM License Agreement for restrictions on the use of additional copies.
The ASAP 2010 System is designed to be used with the Windows Print Manager, which queues print jobs and helps the system operate more efficiently. If the Print Manager is not used, it may take longer to print reports.
ASAP 2010 Setting up the Analyzer
Jan 01 2-17
Power Management features should be disabled so that the Micromeritics application can communicate properly with the instrument during opera- tion. These features can be disabled in the Control Module Setup configu- ration; in some versions of Windows, including 95, 98, and NT; or through a utility supplied by the control module manufacturer.
If this is an update installation, all data files will be preserved. The default files for analysis conditions (*.anc), adsorptive properties (*.adp), and report options (*.rpo) will be updated. (Refer to Appendix D for de- fault values.) All previous versions will be saved as OLDxxxx.* files, where xxxx is the first four characters of the file name. For example, if the analysis conditions file 13XARLAR.ANC is updated, the previous ver- sion will be saved as OLD13XA.ANC. If you have created custom files, they will remain unchanged.
The ASAP 2010 System program is supplied on 3 1/2-in. diskettes. Perform the following steps to install the program:
1. Place diskette 1 into a diskette drive.
2. Choose one of the following:
• Windows 3.1 a. Select File from the Windows Program Manager. b. Select Run from the File menu.
• Windows 95 a. Select Start from the Status bar. b. Select Run from the Start menu.
3. Enter the name of the drive designator, followed by SETUP. For example:
A:SETUP
4. Click ; several instructional screens are displayed. Follow the in- structions appearing on the screens.
Enter 0 (zero) when prompted for the number of instruments to be at- tached if you are installing this program for data manipulation on a com- puter other than the one controlling the analyzer.
You may cancel the installation at any time by selecting . If you do so, you must start the installation program from the beginning to install the analysis program.
OK
Exit
Certain conditions such as the following may prevent installation:
• Installing the ASAP 2010 System program with insufficient disk space. • Running a version of Windows lower than version 3.1. • Operating Windows in a mode other than enhanced mode.
If you receive an error message during installation, refer to Appendix B, Error Messages, for corrective action.
5. When installation is complete, a message prompts you to select the ASAP 2010 System program from the Micromeritics group window. Click .
Changing Your Hardware Configuration
Perform the following steps to change the communications port used for con- necting the analyzer and control modul, or the number of analyzers connected to the control module,
1. Place the ASAP 2010 System program diskette #1 into a diskette drive.
2. Choose one of the following:
• Windows 3.1 a. Select File from the Windows Program Manager. b. Select Run from the File menu.
• Windows 95 a. Select Start from the Status bar. b. Select Run from the Start menu.
3. Enter the name of the drive designator, followed by SETUP. For example:
A:\SETUP
4. When the Micromeritics Application Update Setup dialog box appears, choose one of the following:
• Change communications port configuration Select the communications port and enter the serial number of the analyzer.
• Change the number of units Enter the number of ASAP 2010 System analyzers to be connected to the control module. Select the communication port and enter the serial number for each analyzer unit.
OK
Connecting Regulators and Delivery Tubes
Delivery tubes for connecting the gases used with the ASAP 2010 system are supplied with the instrument. Regulators are available from Micromeritics. Re- fer to Chapter 10, Ordering Information, for part numbers.
Nitrogen System
The nitrogen system requires two regulators. The helium gas bottle is con- nected to the analyzer for use in free-space measurements. The nitrogen gas bottle is connected to the analyzer for use in saturation pressure (Psat) meas- urement and can also be used as the analysis gas. Other gases can also be used as the analysis gas. Nitrogen or helium (or other suitable gas) can be used as the degas backfill gas.
Figure 2-7. Typical Gas Connections
2-20 Aug 98
Nitrogen (Saturation Pressure and Analysis)
Helium (Analysis Free Space)
Setting up the Analyzer ASAP 2010
Krypton System
The krypton system includes a mounting bracket on the rear panel of the ASAP 2010. Attach the gas select manifold bracket to the mounting bracket with the two screws provided.
Figure 2-8. Installing the Gas Select Manifold
The krypton system requires three regulators. The helium gas bottle is con- nected to the analyzer for use in free-space measurements, a gas bottle con- taining the analysis gas (krypton or a gas other than nitrogen) is connected for analyses, and a nitrogen gas bottle is connected for use in saturation pressure (Psat) measurements. If nitrogen is used as the analysis gas, the nitrogen bottle is connected for analysis and saturation pressure measurement. Nitrogen or helium (or other suitable gas) can be used as the degas backfill gas.
Analysis Gas Inlet
Mounting Bracket
Jan 01 2-21
Changing Analysis or Backfill Gas
Refer to Connecting the Gas Supply to the Analyzer, which follows this section, for instructions on changing the backfill gas,
Perform the following procedure to change the analysis gas:
1. Connect the gas supply to the analyzer and purge the gas lines. 2. Select the analysis gas in the Unit Configuration dialog box. 3. Select the Psat gas in the Unit Configuration dialog box. 4. Select the appropriate adsorptive properties and analysis conditions.
Instructions for each of these steps follow.
Helium (Analysis Free Space)
Krypton or Other (Analysis)
Krypton or Other (Analysis)
Setting up the Analyzer ASAP 2010
2-22 Jan 01
Connecting the Gas Supply to the Analyzer
1. Attach an appropriate regulator to the gas bottle. Leave the gas bottle shut-off valve closed until instructed otherwise.
2. If the regulator has a 1/8-in. outlet, proceed to the next step. If the regu- lator has a 1/4-in. outlet, attach the reducer fitting to the outlet of the regulator shut-off valve.
3. Tighten the regulator shut-off valve nut.
Do not over-tighten the fittings. Doing so could collapse the brass fitting and cause a leak.
4. Attach the copper tubing to the regulator or reducer fitting.
5. Purge the regulators as follows:
a. Close the regulator shut-off valve by turning it fully clockwise.
b. Turn the pressure regulator control knob fully counterclockwise.
c. Open the gas bottle valve by turning it counterclockwise, then close the gas bottle valve.
Shut-Off Valve Nut
Brass Reducer Fitting
Jan 01 2-23
d. Observe the high pressure gauge. If the pressure decreases, tighten the nut connecting the regulator to the gas bottle. If the pressure is stable, proceed to Step e.
e. Turn each pressure regulator control knob clockwise until the outlet pressure gauge indicates 10 psig (0.7 bar). Open each regulator shut- off valve by turning it counterclockwise briefly. Then close each valve.
f. Make sure the gas bottle valve is completely closed.
6. Attach the other end of the copper tubing to the gas port on the back of the analyzer.
7. Open the regulator shut-off valve to the helium port on the back of the analyzer.
8. Install a plug in the sample port and run the ASAP 2010 Program.
9. After the automatic backfill step, close all regulator shut-off valves.
10. Enable manual control. (Refer to Chapter 8 for instructions.) Open all analysis valves. Evacuate the system for several hours, overnight if possi- ble.
Selecting the Analysis Gas in the Unit Configuration Dialog Box
The Unit Configuration dialog box specifies the gas used for analysis. When you change analysis gas, select Calibrate from the Main Menu bar; then se- lect Unit configuration. If more than one unit is connected, select the appro- priate unit; then select Unit Configuration. Move the cursor to the Analysis gas prompt and select the appropriate gas. If the name of the analysis gas does not appear on the list, you must create an adsorptive properties file for the gas.
Selecting the Psat Gas in the Unit Configuration Dialog Box
The Unit Configuration dialog box specifies the saturation pressure (Psat) gas. When you change the Psat gas, select Calibrate from the Main Menu bar; then select Unit configuration. If more than one unit is connected, se- lect the appropriate unit; then select Unit configuration. Move the cursor to the Psat gas prompt and select the appropriate gas. If the name of the Psat gas does not appear on the list, you must create an adsorptive properties file for the gas.
2-24 Jan 98
Setting up the Analyzer ASAP 2010
Selecting Adsorptive Properties and Analysis Conditions
Adsorptive properties and analysis conditions information is included in sample information files. When you change analysis gas, you may wish to en- ter or select properties specific to that gas. Refer to Defining Analysis Condi- tions in Chapter 4 and Sample Information in Chapter 6 for more information.
ASAP 2010 Setting up the Analyzer
Jan 01 2-25
Verifying Operation
Installation of the ASAP 2010 system is now complete. It is important to per- form checkout procedures to verify proper operation. These procedures are de- signed to assist you in verifying that installation procedures were performed correctly and that the ASAP 2010 is in proper working order. These proce- dures should be performed following installation, and may be performed fol- lowing any subsequent equipment repairs, replacements, or relocation.
If the results obtained match the referenced information within the specified limits, verification of proper system operation is complete. However, if the re- sults do not match, refer to the troubleshooting procedures in Chapter 9, Troubleshooting and Maintenance. After corrective procedures have been performed, repeat the procedures for verifying operation. If the desired results are not obtained, service to the system or operational assistance may be re- quired.
The equipment and materials required for each procedure are listed in the following table.
Table 2-1. Procedures Required to Verify Operation
Procedure Items Supplied by
Calibrating manifold temperature sensor
None Temperature measurement device
Calibrating (zeroing) pressure gauge
Calibrating system volume
Reference volume (sphere)
Cleaning and labeling glassware
Sample tube Filler rod Sample tube brush Stopper or seal frit for sample tube Sample tube rack
Drying oven Ultrasonic cleaning unit Alconox® (or similar detergent) Rubber gloves or lint-free cloth Acetone Safety glasses Waste container
Verifying Operation ASAP 2010
Micromeritics Items Supplied by User
Weighing sample Sample data sheet (Appendix A) Sample weighing support Reference material
Balance (scale) Pipe cleaners Forceps
Degassing sample Sample tube set Degas heating mantle Clip for degas heating mantles
Sample
Sample tube set Isothermal jacket for sample tube
None
Liquid nitrogen Safety glasses Insulating gloves
Installing analysis dewar
1.9 Liter Dewar Dewar stopper/ insulator (analysis) Dipstick (Dewar depth gauge)
Liquid nitrogen Safety glasses Insulating gloves
Performing analysis of sample
None None
The control module, video monitor, keyboard, printer, and analysis program must have been installed as described earlier in this section of the manual.
Each procedure must be followed exactly as specified. Read each proce- dure carefully before attempting to complete it.
ASAP 2010 Verifying Operation
Jan 01 2-27
Calibrating the Analyzer
Calibration enables you to display system hardware and calibration informa- tion, and to calibrate the master pressure gauge, pressure scale, manifold tem- perature, and system volume. After you start a calibration, you cannot start another type of calibration or an analysis on the current unit nor on multiple units (if installed) until the operation is complete or canceled.
Calibrating the Manifold Temperature Sensor
Calibrate temperature enables you to correct for any changes in the manifold temperature sensor that occur with time. Annual calibration is recommended.
The manifold temperature sensor can be calibrated by two different methods.
• Method 1 (the simplest of the two methods) requires the use of a small diameter probe, such as a 1/16-in. (1.5-mm) thermocouple, on the reference temperature gauge.
• Method 2 should be used for probes larger than 1/16 in. (1.5 mm).
Method 1
1. Insert the thermocouple probe into the opening located to the left of the sample port connector.
2. Move the thermocouple back and forth until you locate the small open- ing on the underside of the manifold. Push the thermocouple through the white insulation into the opening until the thermocouple stops.
You may have to scrape the insulation to locate the opening on the under- side of the manifold.
Right Side Panel
Verifying Operation ASAP 2010
3. Allow the temperature gauge reading to stabilize.
4. Select Calibrate from the Main Menu; then select Calibrate tempera- ture... to display the Calibrate Manifold Temperature dialog box.
5. Enter the manifold temperature indicated on the temperature gauge. Click to store the new value.
Range: 10.000 to 100.000oC
You may use to exit the dialog box without entering or saving a new manifold temperature.
6. Remove the thermocouple probe.
Method 2
1. Remove the screws which fasten the top panel at the upper rear of the analyzer. Then remove the four screws (two on each side) at the top of the analyzer. Lift the top panel from the analyzer.
Figure 2-10. Removing Analyzer Top Panel
OK
Cancel
Jan 01 2-29
2. Locate the heat shield (a metal enclosure) above the analysis valves. To gain access to the manifold, remove the heat shield by lifting it upward.
3. Determine the temperature of the analysis manifold by inserting a cali- brated standard device (such as a thermocouple temperature meter or mercury thermometer) into the hole in the side of the manifold as shown in the following figure. Allow the temperature to stabilize.
4. Select Calibrate from the Main Menu; then select Calibrate tempera- ture to display the Calibrate Manifold Temperature dialog box.
Heat Shield
Analysis Manifold
2-30 Jan 01
5. Enter the manifold temperature indicated on the calibrated standard device. Click to store the new value.
Range: 10.000 to 100.000 oC
You may use to exit the dialog box without entering or saving a new manifold temperature.
6. Remove the calibrated standard device, replace the heat shield, and re- place the analyzer top panel. Insert and tighten the screws at the top of the analyzer and tighten those on the lower edge.
Calibrating the Pressure Gauge
Calibrate pressure gauge enables you to evacuate the manifold and zero all the transducers. Your system may contain from one to three of the following transducers:
• 1000 mmHg transducer (standard on all ASAP 2010 systems) • 10 mmHg transducer (standard on all Krypton and Micropore systems) • 1 mmHg transducer (optional)
The system automatically zeros the transducers before an analysis begins. Therefore, you do not need to use this feature unless you are operating the system in manual mode.
Perform the following steps to calibrate the pressure gauge:
1. Set the analysis vacuum level on the lower front panel of the analyzer to less than 25 µmHg for systems with a 1000 mmHg transducer only. If you have a 10-mmHg transducer (krypton or micropore system) or a 1-mmHg transducer, set the analysis vacuum level to 5 µmHg.
2. Select Calibrate from the Main Menu; then select Calibrate pressure gauge to display the Calibrate Pressure Gauge dialog box.
OK
Cancel
Jan 01 2-31
3. Select Start Calibration to evacuate the manifold and zero the pressure gauge(s).
4. When the calibration is complete, click to exit the dialog box.
You may cancel a calibration at any time by selecting . If you cancel a calibration, no new calibration data are saved.
Calibrating the Pressure Scale
Calibrate pressure scale allows the software to adjust the gain of the 1000- mmHg transducer to match a reference standard.
The pressure in the manifold must be between 500 and 900 mmHg to scale the 1000-mmHg transducer properly.
To calibrate the pressure scale:
1. Attach a reference pressure gauge to the sample port of the analyzer.
2. With manual control enabled:
a. Dose the manifold with helium to 760 mmHg.
b. Open the sample port to expose the reference pressure gauge to the same pressure as the analyzer’s 1000-mmHg transducer.
OK
Cancel
2-32 Jan 01
3. Select Calibrate from the main menu. Then select Calibrate pressure scale to display the Calibrate 1000 mmHg Transducer Scale dialog box.
4. Select Match to entered pressure.
5. Enter the pressure reported by the reference pressure gauge, then click .
6. Close the sample port and evacuate the manifold.
7. Remove the reference pressure gauge.
Calibrating the System Volume
Calibrate volume enables you to calibrate system volume after servicing valves, transducers, or any part of the analysis plumbing. The status of the ASAP 2010 must be idle to calibrate system volume. Before you calibrate system volume, calibrate the manifold temperature sensor and the master pres- sure gauge.
The reference volume (a sphere of known volume) should be at thermal equilibrium with the calibration chamber. You can easily achieve thermal equi- librium by storing the reference volume in the calibration chamber when the chamber is not in use. If the reference volume is not stored in the chamber, the calibration function allows up to 99 minutes for the reference volume to reach thermal equilibrium.
You can achieve an accurate determination of system volume by repeating the measurement process until you obtain four measurements with a standard de- viation of 0.05 cm3 or less. Set the vacuum thermocouple to a set point of 10 µmHg or less.
OK
To calibrate the system volume:
1. Make sure the reference volume is installed in the calibration chamber.
a. Open the door to the calibration chamber located on the left upper rear panel of the analyzer.
b. Remove the chamber cap by unscrewing it.
c. If the reference ball is in the chamber, replace the cap, close the door, and continue with the next step.
If the reference ball is not in the chamber, place it in the chamber, replace the cap, and close the door. Allow at least ten minutes for thermal equilibration; then continue with the next step.
2. Select Calibrate from the Main Menu; then select Calibrate volume to display the Calibrate System Volume dialog box.
3. The fields described below in the Measure System Volume group box en- able you to enter the reference volume, number of times to perform the measurement, and thermal equilibration time. Status messages and in- structions display during the calibration process.
Reference volume The volume of the reference volume sphere. This field is disabled during calibration and analysis.
Range: 10.0 to 99.9999 cm3
Perform measurement The number of times to perform the measure- ment. This field is disabled during calibration and analysis.
Range: 1 to 10
Verifying Operation ASAP 2010
2-34 Jan 01
Thermal equilibration time
The amount of time the program waits after you load the reference volume into the calibra- tion chamber before starting the calibration. For the first measurement only, the reference volume has been stored in the calibration chamber, enter 0. This field is disabled during calibration and analysis.
Range: 0 to 99 minutes
Measurement Status Displays status messages and instructions dur- ing calibration.
4. Click to begin calibration. Follow the instructions dis- played in the dialog box for removing and inserting the reference vol- ume. You may access other dialog boxes and perform other functions during calibration.
When calibration is complete, the following message displays:
Measurement (number) of (requested number): Calibration completed.
Once the calibration is started, is enabled. Select this push button if you decide to cancel the current calibration. If you cancel the current calibration, the dialog box remains open so that you may be- gin another one.
5. The system volume and lower manifold volume display in the Select Volumes group box. This group box enables you to select the system vol- ume stored. Choose one of the following:
Previous Stores the system volume and lower manifold volume in use before accessing the calibration function.
Entered Enables you to manually enter values for the system volume and lower manifold volume.
Range: 10.0000 to 99.9999 cm3
Measured Stores the last measured system volume and lower manifold volume. This field is disabled until all measurements are complete.
Average Stores the average of measured system vol- umes and lower manifold volumes. This field is disabled until all measurements are com- plete.
Start Measurements
Cancel Measurement
Jan 01 2-35
6. The Compute Average group box enables you to enter the number of cali- brations used to calculate the standard deviations and average.
Enter the number of calibrations used to calculate the average in the Average last (number) measured values field. This field becomes enabled after all measurements are complete.
The standard deviation for the average last (number) measured values dis- plays in the System Std dev and Lower Std dev fields.
Range: 1 to number of calibrations performed
7. Click to save the system volume calibration data and exit the dialog box. Click if you wish to disregard the values meas- ured with the current calibration.
Cleaning and Labeling Sample Tubes
Sample tubes and filler rods must be clean and dry before samples are added and weighed. The following procedures are recommended. Refer to Table 2-2 for a list of materials needed to clean and weigh samples.
Table 2-2. Materials Required to Clean and Weigh Sample Tubes
Supplied by Micromeritics Supplied by User
Sample tube Filler rod Sample tube brush Stopper or seal frit for sample tube Sample tube rack Sample weighing support Sample data worksheet (copied from Appendix A of this manual)
Drying oven Ultrasonic cleaning unit Detergent Rubber gloves or lint-free cloth Acetone or isopropyl alcohol Analysis bath fluid Safety glasses Waste container Balance Pipe cleaners
1. Turn on the drying oven used for heating the sample tubes and filler rods and set the temperature to 110 oC.
2. Check the reservoir of the ultrasonic cleaning unit to make sure it is clean.
OK
Cancel
2-36 Jan 01
3. Using 5 grams of Alconox (or other suitable detergent) per 500 mL of warm water, fill the reservoir of the ultrasonic unit with enough water to cover the sample tubes and filler rods. Make sure the detergent is dis- solved before placing the sample tubes and filler rods into the water. If too much detergent is used, it may be difficult to rinse from the sample tubes.
4. Fill the sample tubes with warm water and place them in the reservoir of the ultrasonic cleaning unit. Place the filler rods in the bowl also. Turn on the ultrasonic cleaning unit for approximately fifteen minutes.
5. Using rubber gloves, remove the sample tubes and filler rods from the reservoir.
6. Clean the interior of the sample tubes with the brush supplied with the ASAP 2010 System.
7. Rinse the sample tubes and filler rods thoroughly with hot water. Then rinse them with isopropyl alcohol or acetone using a waste container to collect used solvent.
If isopropyl alcohol or acetone is not available, deionized water may be used to rinse the sample tubes.
ASAP 2010 Verifying Operation
Jan 01 2-37
8. Using nitrogen, dry the interior of the sample tubes and filler rods under a vent hood. Use a tubing extension long enough and small enough in di- ameter to fit inside the tubes.
9. Stand the sample tubes on the sample tube rack and place the filler rods in a basket or in the rack. Bake for two hours.
Verifying Operation ASAP 2010
2-38 Jan 01
10. Remove the sample tubes from the oven and allow them to cool.
11. Using either rubber gloves or a lint-free cloth (but not bare hands), place a filler rod (if used) in each sample tube by holding the sample tube horizontally and sliding the filler rod into the sample tube slowly.
Do not hold the sample tube in a vertical position when inserting the filler rod. Dropping the rod directly into the sample tube can break the sample tube.
12. Wipe a rubber stopper (or seal frit, if used with 1.27-cm (1/2-in.) tubes) with a lint-free cloth.
If helium is used as the degas backfill gas, seal frits are recommended. Refer to Chapter 10, Ordering Information.
13. Label the sample tube and stopper or seal frit for identification.
14. Fill the tube with the selected backfill gas; then insert the stopper or seal frit quickly to avoid releasing the gas.
To obtain the accurate weight of a degassed sample, the gas in both the empty sample tube and in the tube with the sample must be the same.
ASAP 2010 Verifying Operation
Weighing Samples
Analysis results are expressed in units of surface area per gram of sample; therefore, the true weight of the sample must be known. Carefully weigh each sample tube set and sample as described below.
1. Write the Sample Tube ID on the Sample Data Worksheet. (A Sample Data Worksheet, which you may copy, is included in Appendix A.)
2. Place the sample weighing support on the balance. Tare the balance and allow it to stabilize at zero (0).
3. Place the sample tube set (sample tube, stopper or seal frit, and filler rod, if used) on the s