TriStar 3000
Operator’s Manual
V6.08(For serial number 1001 and higher)

300-42832-01
June 2007

Windows is a registered trademark of Microsoft Corporation© Micromeritics Instrument Corporation 2005-2007. All rights reserved.
The software described in this manual is furnished under a license agreement and may be used or copied only inaccordance with the terms of the agreement.

WARRANTYMICROMERITICS 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 andservice 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, failureof 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 theirreliability and durability. However, these materials cannot be totally guaranteed against wear and/or decomposition bychemical 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 theirrespective 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 discretionof 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 manufacturesa 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 DESCRIPTION
Organization of the Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
Conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-2
Equipment Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
SmartPrep Degasser . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
Vacuum Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4
Analysis Program . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
Report System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
Online Help . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-6

2. INSTALLATION
Unpacking and Inspecting the Equipment . . . . . . . . . . . . . . . . . . . . . . . 2-1
Equipment Damage or Loss During Shipment . . . . . . . . . . . . . . . . . . 2-1
Equipment Return . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
Installing the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Connecting the Computer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Connecting the Vacuum Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-4
Connecting Peripheral Equipment to the Computer . . . . . . . . . . . . . . . 2-6
Connecting the Gas Supply . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-7
Installing the SmartPrep Degasser . . . . . . . . . . . . . . . . . . . . . . . . . 2-9
Installing the Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-10
Initial Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-10
Using the Setup Program for Other Functions . . . . . . . . . . . . . . . . . . 2-13
Installing Subsequent Software Versions . . . . . . . . . . . . . . . . . . . 2-15
Adding an Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-16
Moving an Analyzer from one PC to another PC . . . . . . . . . . . . . . 2-17
Removing an Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-20
Changing an Analyzer Setup . . . . . . . . . . . . . . . . . . . . . . . . . 2-21
Reinstalling the Calibration Files . . . . . . . . . . . . . . . . . . . . . . . 2-22
Uninstalling the Analysis Program . . . . . . . . . . . . . . . . . . . . . . 2-23
Specifying Gas Ports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-25

3. USER INTERFACE
Turning the Analyzer On and Off . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
Turning the Analyzer On . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
Turning the Analyzer Off . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
Using the Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2
Shortcut Menus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2
Shortcut Keys . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2

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Dialog Boxes and Subdialog Boxes . . . . . . . . . . . . . . . . . . . . . . . . 3-4
Selecting Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-6
File Name Conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-8
Menu Structure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-9
Main Menu Bar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-9
Windows Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-10
Help Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-11

4. OPERATIONAL PROCEDURES
Specifying Sample Defaults . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1
Basic Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-1
Advanced Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-3
Defining Parameter Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-5
Sample Tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-5
Degas Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-7
Analysis Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-8
Adsorptive Properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-9
Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-10
Creating a Sample File . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-12
Basic and Restricted Formats . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-12
Advanced Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-14
Cleaning and Labeling Sample Tubes . . . . . . . . . . . . . . . . . . . . . . . . . 4-16
Calibrating Sample Tubes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-19
Preparing the Sample for Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-21
Weighing the Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-21
Degassing the Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-22
Installing the Sample Tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-23
Installing the Analysis Dewar . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-24
Performing an Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-26
Standard Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-26
QuickStart Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-27
Printing File Contents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-29
Generating a List . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-30
Exporting Isotherm Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-32
Generating Graph Overlays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-33
Multiple Graph Overlays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-33
Multiple Sample Overlays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-35

5. FILE MENU
Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-1
Open . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . 5-3
Sample Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4
Basic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-5
Advanced . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-8

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Sample Tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-11
Degas Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-13
Analysis Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-15
Adsorptive Properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-27
Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-29
Isotherm Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-32
BET/Langmuir Surface Area Report Options . . . . . . . . . . . . . . . . 5-34
t-Plot Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-37
Alpha-S Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-42
f-Ratio Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-44
BJH Adsorption/Desorption Report Options . . . . . . . . . . . . . . . . . 5-46
Tabular Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-49
Plot Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-51
Dubinin Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-53
Tabular Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . 5-55
Transformed Isotherm Plot Options . . . . . . . . . . . . . . . . . . . 5-56
Pore Volume Options . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-57
MP-Method Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . 5-58
Tabular Report Options . . . . . . . . . . . . . . . . . . . . . . . . . 5-60
Plot Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-61
Summary Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-63
Options Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-64
Sample Log Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-64
Collected/Entered Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-65
Save . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . 5-68
Save As . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 5-68
Save All . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 5-70
Close . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . 5-70
Close All . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 5-70
Print . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . 5-71
List . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . 5-73
Export . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . 5-75
Exit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . 5-77

6. UNIT MENU
Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-1
Sample Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-3
QuickStart . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-7
Enable Manual Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-11
Show Instrument Schematic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-13
Show Status . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-14
Show Instrument Log . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-15
Unit Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-17
Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-18
Temperature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-18
Pressure Scale . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-19
Zero Pressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-19

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Reset Pressure Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-20
Servo Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-20
Volume . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-21
Save to File . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-23
Load from File . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-23

7. REPORTS MENU
Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-1
Start Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-2
Close Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-5
DFT Plus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 7-5
Printed Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-6
Header . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-6
Onscreen Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-6
Tool Bar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-7
Shortcut Menus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-10
Tabular Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-10
Graphs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-11
Zoom Feature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-14
Axis Cross Hair . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-14
Report Examples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-15
Analysis Log . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-16
Isotherm Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-17
BET Surface Area Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-18
BET Surface Area Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-19
Langmuir Surface Area Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-20
t-Plot Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-21
t-Plot Graph . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-22
Alpha-S Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-23
f-Ratio Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-24
BJH Adsorption: Pore Distribution Report . . . . . . . . . . . . . . . . . . . . 7-25
BJH Adsorption: Cumulative Pore Volume Plot . . . . . . . . . . . . . . . . . 7-26
BJH Adsorption: dV/dD Pore Volume . . . . . . . . . . . . . . . . . . . . . . . 7-27
BJH Adsorption: dV/dlog(D) Pore Volume . . . . . . . . . . . . . . . . . . . . 7-28
BJH Adsorption: Cumulative Pore Area Plot . . . . . . . . . . . . . . . . . . . 7-29
BJH Adsorption: dA/dD Pore Area Plot . . . . . . . . . . . . . . . . . . . . . . 7-30
Summary Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-31
Sample Log Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-32

8. OPTIONS MENU
Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8-1
Option Presentation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8-3
Advanced . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8-4
Basic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 8-5
Restricted . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8-6

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Data Presentaton . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-7
Sample Defaults . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-8
Basic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 8-8
Advanced . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-11
System Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-14
Parameter Files Directory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-15
Service Test Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-16

9. TROUBLESHOOTING AND MAINTENANCE
Cleaning the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-1
Replacing Port Frit and O-ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-2
Calibrating the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-3
Zero pressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-3
Pressure scale . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-4
Servo valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-5
Temperature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-5
Volume . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-7

10. ORDERING INFORMATIONAPPENDICES
Appendix A: Forms
Appendix B: Error Messages
Appendix C: Calculations
Saturation Pressure (Po) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-1
Relative Pressure Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . C-1
Volume Adsorbed Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . C-3
Free Space . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-3
Measured, Calculated, and Entered . . . . . . . . . . . . . . . . . . . . C-3
Quasi Gemini . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-6
Equilibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-7
BET Surface Area Calculations2 . . . . . . . . . . . . . . . . . . . . . . . . . . C-8
Langmuir Surface Area Calculations . . . . . . . . . . . . . . . . . . . . . . . C-9
t-Plot Calculations4 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-11
BJH Pore Volume and Area Distribution Calculations . . . . . . . . . . . . . . C-13
Explanation of Terms . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-13
Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-14
Compendium of Variables . . . . . . . . . . . . . . . . . . . . . . . . . . . C-22
Dubinin-Radushkevich Calculations . . . . . . . . . . . . . . . . . . . . . . . . C-23
Dubinin-Astakhov Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . C-25
MP-Method Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-29
Summary Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-32
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-33

Feb 03v

Table of Contents

TriStar 3000

Appendix D: Free-space Correction . . . . . . . . . . . . . . . . . . . . . . . . . D-1
Measure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .D-2
Quasi-Gemini . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .D-2
Calculate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .D-3
Enter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. D-3
Appendix E: Maintaining High Purity Gases . . . . . . . . . . . . . . . . . . . . E-1
Using Metal Gas Lines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-1
Removing Trapped Air . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-1
Purge Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .E-2
Evacuation Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-4
Purging the System After Non-use . . . . . . . . . . . . . . . . . . . . . . . . E-6

INDEX

vi

Feb 03

CHAPTER 1
GENERAL DESCRIPTION•

Organization of the Manual•

Equipment Description•

Specifications

TriStar 3000

Organization of the Manual

GENERAL DESCRIPTIONThis manual describes how to install and operate the TriStar 3000.

Organization of the ManualThis operator’s manual is organized so that all operating procedures are located in
Chapter 4. Chapters 5, 6, 7, and 8 are reference chapters should you need additional information while performing these procedures.
This manual is divided as follows:

Feb 03

Chapter 1

General Description. Provides a general description of the
TriStar 3000 and its features and specifications.

Chapter 2

Installation. Describes how to unpack, inspect, install, and verify operation of the TriStar 3000.

Chapter 3User Interface. Provides instrument and software interface.

Chapter 4

Operating Procedures. Provides step-by-step procedures forthe operations performed with the TriStar 3000.

Chapter 5File Menu. Provides a description of the choices available on
the File menu.

Chapter 6

Unit [n] Menu. Provides a description of the choices available
on the Unit menu.

Chapter 7

Reports. Provides a description of the choices available on
the Reports menu.

Chapter 8

Options Menu. Provides a description of the choices available
on the Options menu.

Chapter 9

Troubleshooting and Maintenance. Provides user maintenance and service information.

Chapter 10

Ordering Information. Provides ordering information
for TriStar system components.

Appendix A

Forms. Contains forms you may use to record information
prior to entering it into the system.

1-1

Organization of the Manual

TriStar 3000

Appendix B

Error Messages. Lists the error messages that may be displayed by the software and includes a cause and action for
each.

Appendix C

Calculations. Provides the calculations used by the TriStar program.

Appendix D

Free-space Correction. Provides a discussion of the freespace measurements available with TriStar.

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.

1-2

Feb 03

TriStar 3000

Equipment Description

Equipment Description
The TriStar 3000 is an automated gas adsorption analyzer which contains threeports, allowing you to analyze up to three samples simultaneously. Or you can use
port 2 for measuring the free space using the Quasi-Gemini method and/or port 3
to measure the saturation pressure (Po) on a continuous basis. You can operate up
to four TriStar analyzers with one control module (computer). The TriStar 3000
system consists of the TriStar analyzer, a SmartPrep degasser (optional) for preparing samples, a vacuum pump, and a control module for entering analysis and report options.

Figure 1-1. TriStar Analyzer

SmartPrep Degasser
The SmartPrep is a flowing-gas, degassing unit which removes adsorbed contaminants from the surface and pores of your sample in preparation for analysis. It contains six sample ports, each one independently controlled for greater flexibility. It
contains two serial ports, one for connecting to the control module and the otheravailable for connecting an additional SmartPrep. In fact, you can connect up to 4
SmartPreps, one to the other, allowing the capability of up to 24 preparation ports
at one time! The SmartPrep is the recommended degassing unit for the TriStar
3000; however, you may furnish your own degassing method if desired. Chapter
10 provides ordering information for the SmartPrep.

Feb 031-3

Equipment Description

TriStar 3000

Vacuum Pump
A vacuum pump is required for sample analysis with the TriStar analyzer. A recessed cavity is provided at the rear of the instrument for its placement.
Vacuum pumps used with the TriStar must meet the following criteria. They must:•

be able to achieve vacuums better than 20 µmHg at the instrument inlet•

contain an anti-suckback valve to prevent vacuum pump oil from backing up
into the analyzer in the event of a vacuum pump failure•contain an NW16 inlet port for connection to the TriStar

An appropriate vacuum pump is available from Micromeritics. (Refer to Chapter
10 for ordering information.)

1-4

Feb 03

TriStar 3000

Equipment Description

Analysis Program®

The TriStar 3000 analysis program is designed to operate in the Windows environment. This makes operation of the TriStar 3000 easier and allows you to run
other applications while an automatic operation is in progress. If you are new toWindows, you should learn some basic Windows skills, such as using the mouseand choosing commands. Brief operating instructions are provided in Using theSoftware in Chapter 3. For more specific instructions, refer to the Windows operating manual or to the online tutorial.

Report System
The TriStar software includes a report system which allows you to manipulate andcustomize reports. You can zoom in on portions of the graphs or shift the axes to
examine fine details. Scalable graphs can be copied to the clipboard and pasted
into other applications. Reports can be customized with your choice of fonts and acompany logo added to the report header for an impressive presentation. Refer to
Chapter 7 for the options available for reports.

Online Help
An extensive online help system is provided for quick-and-easy access to a subject matter. The TriStar help system functions in the same manner as most otherhelp systems. You can choose a subject from the Contents window where topics
are organized in “books,” locate your topic using the Index window where topics
are listed alphabetically by key words, or search for information on a specifictopic using the Find window.

Feb 03

1-5

Specifications

TriStar 3000

Specifications
The TriStar 3000 has been designed and tested to meet the specifications provided
below.

Characteristic

Specification——————— PRESSURE MEASUREMENT ———————

Range:

0 to 999 mmHg

Resolution:

Within 0.05 mmHg

Accuracy:

Within 0.5% of full scale

Linearity:

Within 0.25% of full scale (transducer
manufacturer’s specification)——————— MANIFOLD TEMPERATURE ———————

Accuracy:± 0.25°C

Resolution:

Within 0.1°C—————— VACUUM SYSTEM ———————

Vacuum Pump:

One required; 20 µmHg (maximum) with antisuckback valve (May be purchased fromMicromeritics or supplied by user.)—————— ENVIRONMENT ———————

Temperature:

10 to 35°C, operating; 0 to 50°C, nonoperating

Humidity:

20 to 80% relative, noncondensing——————— ELECTRICAL ———————

Voltage:85 to 265 VAC

Frequency:

50/60 HzPower:

300 VA, maximum (110 VA for TriStar plus 190 VA
for vacuum pump)——————— PHYSICAL ———————

1-6

Height:76 cm (30 in.)

Width:

64 cm (25 in.)

Depth:

53 cm (21 in.)

Weight:45 kg (100 lbs)

Feb 03

CHAPTER 2INSTALLATION•

Unpacking and Inspecting the Equipment•

Installing the Analyzer•

Installing the Software•

Specifying Gas Ports

TriStar 3000

Unpacking and Inspecting the Equipment

INSTALLATIONThis chapter describes how to:•••

Unpack and inspect the equipment
Install the TriStar system
Verify operation of the system

Initially, your TriStar 3000 will be installed and verified for operation by anauthorized Micromeritics service representative or a representative of a
Micromeritics distributor. Installation instructions are provided in this manual incase the TriStar has to be relocated or reinstalled after a factory repair.

Unpacking and Inspecting the Equipment
When you unpack the shipping cartons, carefully compare the packing list withthe equipment actually received and check the equipment for any damage during
shipment. Be sure to sift through all packing materials before declaring equipment
missing.
If you need to declare equipment as damaged or lost, save the shipping cartons.
The claims investigator must examine the cartons in order to complete the inspection report.

Equipment Damage or Loss During Shipment
If equipment is damaged or lost in transit, you are required to make note of thedamage or loss on the freight bill. The freight carrier, not Micromeritics, is responsible for all damage or loss occurring during shipment. If you discover damage orloss of equipment during shipment, report the condition to the carrier immediately.

Equipment Return
Micromeritics strives to ensure that all items arrive safely and in working order.
Occasionally, due to circumstances beyond our control, a customer may receive
equipment which is not in working order. When equipment has been damaged(either during shipment or in use) and you wish to return the equipment to Micromeritics for repair or replacement, follow the steps below:1.

Feb 03

Pack the instrument in its original shipping carton if possible. If the original
carton is unavailable, for a nominal fee, Micromeritics can provide anothercarton for your use.

2-1

Unpacking and Inspecting the Equipment

TriStar 3000

Failure to package your instrument properly may result in shipping damage.

2-2

2.

Tag or otherwise identify the defective equipment, noting the defect and circumstances, if any, the circumstances under which the defect occurred.

3.

Reference the sales order or purchase order for the equipment, and provide
the date the equipment was received.

4.

Notify the Micromeritics Service Department of the defect and request shipping instructions. The Service Department will assign a Returned Materials
Authorization (RMA) number. Write the RMA number on the outside of the
carton.

Feb 03

TriStar 3000

Installing the Analyzer

Installing the Analyzer
Place the TriStar on an appropriately sized work table. Be sure to place the TriStar close enough to the control module so that cables may be connected adequately.

Connecting the Computer
Perform the following steps to connect the computer to the analyzer:
1.

Plug the female end of the RS-232 cable into the computer.

2.

Plug the other end into the connector labeled RS232 on the back panel of theanalyzer.

RS-232 Cable

Figure 2-1. RS232 Connections
3.

Tighten the retaining screws.

If you plan to install more than two instruments per computer, you must haveadditional serial I/O hardware. This hardware is available from Micromeritics;
refer to Chapter 10 for ordering information. Instructions for installing the hardware are given in Appendix E; they also are included with the hardware.
4.

Feb 03Connect the female end of the power cord into the power connector on theback panel of the analyzer. Insert the other end into an appropriate powersource.

2-3Installing the Analyzer

TriStar 3000

Connecting the Vacuum Pump
The TriStar requires a vacuum pump for operation. The instructions provided here
are for installation of the vacuum pump available from Micromeritics (refer to
Chapter 10 for ordering information). These instructions may vary slightly if you
are providing your own vacuum pump. Perform the following steps to install thevacuum pump:1.

Prepare the vacuum pump (check oil, install exhaust filter, etc.) following the
instructions provided in the vacuum pump manual. DO NOT connect the vacuum pump hose to the analyzer at this time.

2.

Prepare the oil vapor trap included in the TriStar accessories kit following the
instructions provided in its manual.

3.

Install the oil vapor trap onto the vacuum pump following the instructions provided in the oil vapor trap manual.

4.

Verify that the pump voltage (located on the pump motor) matches the voltage of the power outlet to which the pump will be connected.

Do not connect the pump power cord to a power source until the proper voltage
has been verified. Doing so could result in electrical shock and/or damage to the
pump.

2-4

5.

Slide the vacuum drip tray provided in the accessories kit partially into thecavity at the rear of the analyzer.

6.

Place the vacuum pump (with installed oil vapor trap) onto the tray.

7.

Plug the power cord provided for the vacuum pump (to the left just inside
the cavity) into the power outlet on the rear of the vacuum pump.

8.

Place the vacuum pump ON/OFF switch in the ON position.

Feb 03

TriStar 3000

Installing the Analyzer

9.

Slide the tray completely into the analyzer.

Oil Vapor Trap
(installed on vacuum
pump)

Vacuum Pump

Vacuum Pump Power Cord

Vacuum Pump Tray

Figure 2-2. Vacuum Pump Connection
10. Connect the vacuum hose from the analyzer to the vapor trap.

Feb 032-5

Installing the Analyzer

TriStar 3000

Connecting Peripheral Equipment to the Computer
Follow the instructions provided below to connect the monitor, keyboard, printer, andmouse. The following illustration shows typical connections.
Refer to the instruction manuals supplied with the computer, video monitor, andprinter for voltage requirements for these units.

Figure 2-3. Typical Computer Connections

2-6

1.

Plug the keyboard cable into the keyboard connector on the rear panel of thecomputer.

2.

Plug the monitor cable into the monitor connector on the rear panel of thecomputer.

3.

Plug the mouse cable into the mouse connector on the rear panel of the computer.

4.

Plug one end of the printer cable into the connector on the rear panel of theprinter. Plug the other end of the printer cable into the connector labeled
LPT1 (may be labeled PARALLEL) on the rear panel of the computer.

5.

Plug all power cords into the appropriate power source.

Feb 03

TriStar 3000

Installing the Analyzer

Connecting the Gas Supply
Compressed gases with a purity of 99.99% are required for analyses performed using the TriStar 3000. Gas bottles or an outlet from a central source should be located near the analyzer. Refer to Appendix F for tips on maintaining gas purity.
Appropriate regulators which have been leak-checked and specially cleaned are required. Gas regulators are available from Micromeritics (refer to Chapter 10 for ordering information).
1.

Attach an appropriate regulator to the gas bottle. Leave the gas bottle shut-off
valve closed until instructed otherwise.

Gas Bottle
Shut-Off Valve

Gas Bottle Pressure
Gauge
Outlet Pressure
Gauge

Shut-Off Valve Nut
Brass Reducer Fitting
Regulator
Shut-Off Valve

Gas Bottle

Copper Tubing
Pressure Control Knob

Figure 2-4. Connecting Two-Stage Regulator to Gas Supply
2.

If the regulator has a 1/8-in. outlet, proceed to the next step. If the regulator
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.

4.

Attach the copper tubing to the regulator or reducer fitting.

Do not over-tighten the fittings. Doing so could collapse the copper tubing andcause a leak.

5.

Purge the regulator as follows:a. Close the regulator shut-off valve by turning it fully clockwise.
b. Turn the pressure regulator control knob fully counterclockwise.

Feb 032-7

Installing the Analyzer

TriStar 3000

c. Open the gas bottle valve by turning it counterclockwise, then close the gas
bottle valve.
d. Observe the outlet 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 pressuregauge indicates 15 psig (1.0 bar). Open each regulator shut-off valve by turning it counterclockwise briefly. Then close each valve.
f.
6.

Make sure the gas bottle valve is completely closed.

Attach the other end of the copper tubing to the appropriate fitting on theback of the analyzer.

To Gas Supply

Figure 2-5. Gas Connections

2-8

7.

Repeat steps 1 through 6 for an additional analysis gas (if desired) and forhelium.

8.

After installing the software, access the Unit Configuration dialog from theUnit menu to specify ports for gas attachment(s). (Refer to Specifying Gas
Ports later in this chapter.)

Feb 03

TriStar 3000

Installing the Analyzer

Installing the SmartPrep Degasser
Refer to the SmartPrep operator’s manual for installation instructions. When you
install the SmartPrep, a menu item entitled “SmartPrep” is added to the main
menu bar of the TriStar, allowing you complete control of the SmartPrep throughthe TriStar program.

Feb 032-9

Installing the Software

TriStar 3000

Installing the SoftwareYour system must meet or exceed the following requirements before you can
install the TriStar 3000 analysis program:
•
•
•
•
•
•

Pentium 333MHz computer (or equivalent)
CD-ROM drive
128 megabytes of main memory
1-gigabyte hard drive
SVGA monitor (800 x 600 minimum resolution)
Windows 2000 or Windows XP Professional

The TriStar analysis program is also available as a standalone option so that you
can install it on a computer other than the one controlling the analyzer. This allows you to:••create or edit sample and parameter files
generate reports on completed sample files

Review the Micromeritics PROGRAM License Agreement for restrictions on theuse of another copy.

Initial Installation
The TriStar analysis program is supplied on a CD. Perform the following steps toinstall the program:
1.

Turn on the analyzer.

2.

Insert the program CD into your CD-ROM drive.

3.

Select Start from the Status bar, then Run from the Start menu.

4.

Enter the name of the drive designator, followed by setup. For example:
e:setup

5.

2-10

Click

OK

; the New Installation dialog is displayed.

Feb 03

TriStar 3000

Installing the Software

Displays the amount of current
disk space and the amountrequired for installation of theapplication. Also displays the
directory into which theapplication will be installed.

Select this option to add the
TriStar 3000 icon to yourdesktop for quick access tothe application.

You may cancel the installation at any time by selecting Exit . If you do so,
you must start the installation program from the beginning to install the analysis
program.
The Destination Folder group box displays the amount of current disk space,
the amount of disk space required for the analysis program, and the directory
into which the application will be installed. If you wish to install the application into a different directory, click Browse to choose the directory.

Feb 03

6.

If you want to run the application from the desktop, select the checkbox justbelow the Destination Folder group box to add an icon to the desktop.

7.

The TriStar 3000 icon is added to the Micromeritics folder by default. If you
prefer a different folder, enter or select one from the drop-down list.

2-11

Installing the Software

TriStar 3000

8.

Click

9.

In the Step 1 group box, click the radio button for the number of analyzers
to be attached to this computer. If you are attaching multiple analyzers, makesure your computer has sufficient serial ports. Additional hardware may be required (refer to Chapter 10 for ordering information).

Next; the Analyzer Configuration dialog is displayed.

Choose 0 (zero) if you are installing this program for data reduction on a computer other than the one controlling the analyzer.
10. In the Step 2 group box, enter the serial number(s) for the analyzer(s) you
are attaching to this computer.
11. Click Next ; the Calibration File Installation dialog is displayed. Read theinformation in the dialog(s) and proceed accordingly.
If you selected zero (0) as the number of instruments to install, the Calibration
dialog is not displayed.
12. After the calibration files are installed, the Installation Complete dialog box
containing the Readme file is displayed.
13. Use the scroll bar if you wish to read the contents of the file, then click
Finishto close the dialog.
14. Remove the Setup CD and store in a safe place. The original Setup CD contains the calibration files specific to your instrument. Upgrade CDs do notcontain calibration files. Therefore, it is important that you maintain youroriginal Setup CD in a secure location in the event calibration files need tobe reinstalled.

2-12

Mar 03

TriStar 3000

Installing the Software

Using the Setup Program for Other Functions
After initial installation of the TriStar analysis program, the application setup program is used to:
•
•
•
•
•
•
•

Upgrade software
Add an analyzer
Move an analyzer from one computer to another computer
Remove an analyzer from the computer
Change the analyzer setup
Reinstall calibration files
Uninstall the analysis program

To start the application setup program:
1.

Ensure that the analysis program is not operating.

2.

Insert the program CD into your CD-ROM drive.

3.

Select Start from the Status bar.

4.

Select Run from the start menu.

5.

Enter the drive designator of the CD-ROM drive, followed by setup. For example: e:setup.
Alternatively, you can click
lect setup.exe.

6.

Feb 03

OK
Clickdisplayed.

Browse, navigate to your CD-ROM drive, and se -; the setup Welcome screen showing the options available is2-13

Installing the Software

7.

TriStar 3000

Select the operation you wish to perform. Procedures for performing each operation are in subsequent sections.
After the requested operation is completed, the setup Welcome screen is again
displayed. A confirmation message indicating completion of the operation isshown in the lower section of the dialog.

Indicates status oflast operation.

8.

2-14

After you have completed all desired operations, click
dialog.

Exit

to close the

Feb 03

TriStar 3000

Installing the Software

Installing Subsequent Software Versions
When you install a software upgrade, the system installs all of the application
files and any status files that do not already exist on the computer. Existing analyzer status files are not affected and default and data files are not overwritten.
There are three types of subsequent installation; the software version controlled by
the setup program is:•••a later version than the version installed on the computer
the same version as the version installed on the computeran earlier version than the version installed on the computer

The setup program automatically detects which type of installation applies and customizes the selection in the Setup dialog accordingly.
1.

Start the Setup program. Choose the software option; remember, only the applicable option will display; it will be one of the following:•••

Feb 03Upgrade software to version (number) from version (number)
Reinstall software version (number)
Downgrade software to version (number) from version (number)2.

Click Start file installation ; the application installs the software and redisplays the
setup Welcome dialog.

3.

If no other operations are desired using this dialog, click
dialog.

Exit

to close the

2-15

Installing the Software

TriStar 3000

Adding an Analyzer
Add an analyzer to the existing application as follows:

2-16

1.

Start the Setup program. Select Add an analyzer, then click
Setup analyzer dialog is displayed:

2.

Enter the serial number of the analyzer being added, then the communications
port to which it is to be connected.

3.

Click Next ; the Calibration Installation dialog is displayed. Read theinformation in the dialog and proceed accordingly.

4.

After the calibration files are installed, the setup Welcome dialog is redisplayed.

5.

If no other operations are desired using this dialog, click
dialog.

Exit

Next

; the

to close the

Feb 03

TriStar 3000

Installing the Software

Moving an Analyzer from one PC to another PC
You can move an analyzer, along with its status and calibration files, from one computer (Source PC) to another computer (Destination PC).
This operation does not move sample or parameter files. To move these files, usea file management program such as Explorer or a backup/restore utility.
1.

Install the analysis program on the destination computer. Refer to Initial Installation earlier in this chapter. Be sure to select 0 as the number of instruments; all related instrument information will be transferred in the Move
operation.
If the analysis program is already installed on the destination computer, proceed to Step 2.

Feb 032.

Start the application setup program on the source computer. Refer to Using
the Setup Program for Other Functions earlier in this chapter.

3.

In the Setup dialog, select Move an analyzer from one PC to another PC,
then click Next ; the Move analyzer operation dialog is displayed.

4.

Select Source PC, then click

Next; the following dialog is displayed.

2-17Installing the Software

TriStar 3000

5.

In the Step 1 group box, select the analyzer that is to be moved.

6.

In the Step 2 group box, choose a location in which the moved files will be
stored. If possible, choose a floppy drive or a shared network drive. If this is
not possible, select a local folder. After the files are placed there, use a foldertransfer utility to copy this folder from the Source PC to the Destination PC.
Calibration files are not included in the moved files. These files must be copied and moved separately to the destination computer. The calibration files
are located in a subdirectory (folder) of the Hardware directory. The subdirectory is named 300-(serial number).

7.

Click Finish ; the files are moved and the setup Welcome screen is displayed.

8.

Start the application setup program on the destination computer.

9.

In the Setup dialog, select Move an analyzer from one PC to another PC;
the Move analyzer operation dialog is displayed (shown on previous page).

10. Select Destination PC, then click

2-18

Next

; the following dialog is displayed.

Feb 03

TriStar 3000

Installing the Software

11. In the Step 1 group box, enter the serial number of the analyzer being moved
and the communications port to which it will be attached.
12. In the Step 2 group box, click
files.
13. ClickFeb 03FinishBrowseand choose the location of the moved; the files are moved and the setup Welcome dialog is displayed.

2-19Installing the Software

TriStar 3000

Removing an Analyzer
You can remove an analyzer from the computer as follows. When you remove ananalyzer, the status files are removed as well.

2-20

1.

Start the Setup program. Refer to Using the Setup Program for Other Functions earlier in this chapter.

2.

From the Setup dialog, select Remove an analyzer, then click
Remove an analyzer dialog is displayed.

3.

From the drop-down list, choose the serial number of the analyzer you want
to remove.

4.

Click Remove ; the analyzer is removed and the Welcome screen is again displayed.

5.

Click

Exit

Next

; the

to close the dialog.

Feb 03

TriStar 3000

Installing the Software

Changing an Analyzer Setup
Change the analyzer setup as follows:

Feb 03

1.

Start the Setup program. Refer to Using the Setup Program for Other Functions earlier in this chapter.

2.

From the Setup dialog, select Change analyzer setup, then click
the Change analyzer setup dialog is displayed.

3.

From the drop-down list, choose the analyzer you want to change.

4.

Enter the new port number in the space provided.

5.

Click Finish ; the change is completed and the Welcome dialog is again
displayed.

6.

Click

Exit

Next

;

to close the dialog.

2-21

Installing the Software

TriStar 3000

Reinstalling the Calibration Files
You can reinstall the files containing an analyzer’s factory calibration data as follows:

2-22

1.

Start the Setup program. Refer to Using the Setup Program for Other Functions earlier in this chapter.

2.

From the Setup dialog, select Re-install calibration files for an analyzer,
then click Next ; the Re-install calibration files dialog is displayed.

3.

Select the analyzer whose calibration files you wish to reinstall from the dropdown list. If you have only one analyzer installed, a drop-down list is not included.

4.

Insert the CD containing the calibration files; ensure that the CD drive is displayed as the calibration file source location. If not, click Browse and choose
the CD drive.

5.

Click Finish ; the calibration files are reinstalled and the Welcome dialog isagain displayed.

6.

Click

Exit

to close the dialog.

Feb 03

TriStar 3000

Installing the Software

Uninstalling the Analysis Program
When you uninstall the ASAP 2020 analysis program, the application removes theanalysis program, status files, analyzer setup files, and resulting empty directories.
It does not remove data files. Perform the following steps to uninstall the program:Feb 03

1.

Start the Setup program. Refer to Using the Setup Program for Other Functions earlier in this chapter.

2.

From the Setup dialog, select Uninstall, then click
dialog is displayed.

3.

Click Uninstall ; the Select Uninstall Method dialog is displayed.

Next; the Uninstall

2-23

Installing the Software

4.

5.

2-24

TriStar 3000

Choose one of the following:•

Automatic: click Next ; the system uninstalls the analysis program automatically and the setup Welcome dialog redisplays.

•

Custom: click Next ; a series of dialogs is displayed, allowing you tochoose the files you wish to uninstall. After all files are selected and uninstalled, the setup Welcome dialog redisplays.

Click

Exit

to close the Welcome dialog.

Feb 03

TriStar 3000

Specifying Gas Ports

Specifying Gas Ports
After you have connected your analysis gas(es) to the analyzer, you must specify
which gas is connected to each port.
••

Valve 7 carries the free-space gas (He) and cannot be changed
Valves 8 and 9 are designated for the analysis gas(es)Specify gas connections as follows:

Feb 03

1.

From the Unit menu, select Unit configuration; the Unit Configuration dialog box is displayed.

2.

In the Gas Selections group box, enter the mnemonic name for the gas
OKinstalled for valve(s) 8 and 9; then click
to close the dialog box.

2-25

CHAPTER 3
USER INTERFACE•

Turning the Analyzer On and Off•

Using the Software•

Menu Structure•

Windows Menu•

Help Menu

TriStar 3000

Turning the Analyzer On and Off

USER INTERFACE
Turning the Analyzer On and Off
Turning the Analyzer On
1.

Place the computer, monitor, and printer ON/OFF switches in the ON position.

2.

Place the TriStar analyzer ON/OFF switch in the ON ( | ) position.

3.

Place the vacuum pump ON/OFF switch in the ON position. This step is notnecessary if your vacuum pump is connected to the TriStar’s internal vacuum
pump cable.

Turning the Analyzer Off
Always exit the analysis program and Windows before turning off the computer. Failure to do so could result in loss of data.

1.

Select Close from the System menu or Exit from the File menu.
If an analysis is in progress, the following message is displayed:
Instrument is busy. Continue program exit?
Yes

No

Even if you select Yes and the analysis program closes, the analysis continues and data continue to be collected. Reports that are queued under the
Print Manager will print. If, however, a power failure occurs and an uninterruptible power supply (UPS) is not attached to the analyzer, the data collected after exiting the analysis program are lost.

Feb 03

2.

Place the computer, monitor, and printer ON/OFF switches in the OFF position.

3.

Place the TriStar analyzer ON/OFF switch in the OFF position.

4.

Place the vacuum pump ON/OFF switch in the OFF position. This step is notnecessary if your vacuum pump is connected to the TriStar’s internal vacuum
pump cable.

3-1

Using the Software

TriStar 3000

Using the Software
The TriStar 3000 analysis program operates in the Windows environment and requires familiarity with standard Windows operations such as using the mouse,menus, and dialog boxes. While this manual provides brief instructions for suchstandard operations, you may have to refer to your Windows documentation or toits online help system to clarify functions which are specific to Windows.

Shortcut Menus
Shortcut menus (sometimes referred to as context-sensitive menus or pop-up
menus) are available for certain components on the instrument schematic when in
manual mode, and for onscreen graphs and tabular reports. These menus are accessed by selecting the item for which you want to display its menu and clicking
the right mouse button. For example, right-click in a column of an onscreen report
and the following menu is displayed.

Shortcut Keys
Shortcut keys can be used to activate some menu commands. Shortcut keys or key
combinations (if assigned) are listed to the right of the menu item. Instead of
opening the menu and choosing the command, simply press the key combination.
For example, to open a sample information file, press F2 ; the Open Sample Information dialog is displayed.
You can also use shortcut keys to access a menu or any function that contains anunderlined letter by pressing Alt plus the underlined letter in the command. For
example, to access the File menu, press Alt , then F .
Table 3-1 provides a list of the keys available in the TriStar 3000 analysis program.

3-2

Feb 03

TriStar 3000

Using the Software

Table 3-1. Shortcut Keys
Key(s)

Feb 03Function

F1

Access online help

F2Open a sample information file

F3

Open an analysis conditions file

F4

Open an adsorptive properties file

F5

Open a report options file

F6

Tile windows

F7

Cascade windows

F8

Start report

F9

Close all open reports

F11

Start the DFT Plus program (if installed)

Alt

F4

Exit the analysis program↑ Shift

F2

List sample information files↑ Shift

F3

List analysis conditions files↑ Shift

F4

List adsorptive properties files↑ Shift

F5

List report options files

3-3

Using the Software

TriStar 3000

Dialog Boxes and Subdialog Boxes
Dialog boxes are displayed when an item followed by an ellipsis (...) is selected.
Subdialog boxes are displayed when a push button on a dialog box is selected.
Both types of boxes may contain one or more of the following:
Data entry field

These fields may be either numeric (numbers only) or alphanumeric (numbers, letters, or printable characters). If
you make an invalid entry in either of these fields, an error message occurs.

Information bar

Some dialog boxes contain information pertinent to theselected field in an information bar across the bottom of
the dialog. For example, a range is shown for fields inwhich numeric entries are required.

Displays range forselected field.

List

A list contains selections from which you may choose
one or more items. To select an item on the list, position
the mouse pointer on the desired selection, then doubleclick. An item is selected if it is preceded with a checkmark.

Indicates item
is selected.

3-4

Feb 03

TriStar 3000

Using the Software

Push Button

A push button is used to display subdialog boxes inwhich to enter additional information about the subject
matter. For example, this push button displays a dialog
for specifying a range of dates (explained later in thischapter).

Push buttons also may be used to invoke an action. For
example, Cancel closes the open dialog box, discarding
any information you may have entered.
Radio Button

Radio buttons are contained within a group box. Thesebuttons are used to select options; you may choose only
one item.

Check Box

Check boxes also are used to select options. You may
make as many selections as you wish.

Drop-down List

A drop-down list is indicated by a down arrow to theright of the field. Drop-down lists contain a list of options from which you may choose one.

Down Arrow

Feb 03

3-5

Using the Software

TriStar 3000

Some dialog boxes contain one or both of the following push buttons:
Browse...

Displays a dialog box which allows you to select a filefor the subject matter.

Replace...

Allows you to copy file values from an existing file into
the one you are creating. You then can edit the values in
the new file without changing the ones in the original
file.

Selecting Files
Sample information is stored in files and saved under file names. Certain dialog
boxes contain a Files list box, which displays a list of files available for that particular operation. For example, the Open Sample Information dialog box:
Specify a new Status category
to limit the files displayed in
the Files: list box.

Click to specify arange of dates.

Choose thedrive/directory.
Choose the file
you wish to open.

From the list of files in the Files list box, move the mouse pointer to the file you
wish to open and double-click. If you do not see the desired file, it may be in another directory. Go to the Directories list box and choose the correct drive and/or
directory.
You may limit the list of files displayed in the Files: list box by choosing one of
the following:•

Use wildcard characters in the path name you enter in the File name field.
Wildcard characters such as * and ? can be used to filter file names. For
example, you can limit the list of files displayed to those beginning with
01 as by entering 01*.smp.

3-6

Feb 03

TriStar 3000

Using the Software•Enter a range of dates. SelectDates...

; the Select Dates dialog is displayed.

Select the Show Date Range radio button. This enables the From and To
fields allowing you to enter a beginning and ending date. Alternatively, you
may double-click in each field to display a calendar to set a date. The
range of dates remains the default until you change the dates or selectShow All Dates.
For convenience, the following function keys are available when the SelectDates dialog box is displayed:
F2
F3
F4

Clears the field
Inserts the current date
Displays a calendar from which you may select a date

You may change the date format by using the International Date Format function on the Windows Control Panel.

•

Select a file status from the Status drop-down list. Table 3-2 describes eachfile status.
Table 3-2. File Status and Description
StatusAll
Analyzing
CompleteEnteredNo analysis
Prepared
Preparing

Feb 03

Description

All sample information files in the specified
directory and within the specified range of dates.
Sample information files that are currently being
used for analysis or are in the degassing process.
Sample information files that were used in ananalysis that has been completed.
Sample information files that contain manuallyentered data.
Sample information files that have not been used toperform an analysis.
Sample information files that have been used in an
automatic degas operation, but not for an analysis.
Sample information files currently being used in an
automatic degas operation.

3-7

Using the Software

TriStar 3000

File Name Conventions
For sample information files, a default file name (the next available sequence number) and a default extension display. For Sample tube, Degas conditions, Analysis
conditions, Adsorptive properties, and Report options, only a default extension displays.
The following table shows the file name extensions for the TriStar 3000 analysis
program.
Table 3-3. Default File Name Extensions
File Type

Extension

Sample information

SMP

Sample tube

STP

Degas conditions

DEG

Analysis conditions

ANC

Adsorptive properties

ADP

Report options

RPO

Export to disk (ASCII)

EXP

Report to disk

RPT

List to disk

LST

Thickness curve

THK

Alpha-s curve

ALS

The following types are available for reports saved from theReport window:

3-8

ReportREP

Spreadsheet

XLS

ASCII

TXT

Feb 03

TriStar 3000

Menu Structure

Menu Structure

SmartPrep drop-downmenu displays here if a
SmartPrep unit is being
used with the TriStar.

Main Menu Bar
All functions for TriStar 3000 are accessed from the main menu bar. Brief descriptions are provided below; refer to the chapter given in parentheses for a detailed
description of the options contained on that menu.

Feb 03File

Allows you to manage sample and parameter files.
(Chapter 5)

Unit [n]Enables you to perform analyses, calibrations, and other
instrument operations. (Chapter 6)

SmartPrep

Displays only if you have a SmartPrep degassing unit installed on the TriStar. The options contained on thismenu are explained in the SmartPrep operator’s manual.

Reports

Enables you to generate, close, and customize reports.
(Chapter 7)

Options

Allows you to edit sample defaults, specify your system
configuration, and select data presentation formats.
(Chapter 8)

Windows

Enables you to arrange the windows and icons on yourscreen. It also displays the names of all open windows.
(this chapter)

Help

Displays Help information. (this chapter)

3-9

Menu Structure

TriStar 3000

Windows Menu

The choices on this menu allow you to arrange your open windows and icons.
Tile

Resizes all open windows and arranges them side by side
so that the contents of all open windows are visible.

CascadeResizes all open windows and arranges them in a stacked
fashion. The active window is positioned on top of thestack. Each window’s title remains visible, making it
easy to select other windows.

Arrange Icons

Arranges the symbols for all minimized windows in anorderly manner.

The Windows menu also displays all open files; the active window is precededwith a check mark.

3-10

Feb 03

TriStar 3000

Menu Structure

Help Menu

Feb 03

Help

Lists help topics for the TriStar 3000 analysis program.

About TriStar 3000

Displays information about the TriStar 3000 analysis program.

3-11

CHAPTER 4
OPERATIONAL PROCEDURES•

Specifying Sample Defaults•

Defining Parameter Files•

Creating a Sample File•

Cleaning and Labeling Sample Tubes•

Calibrating Sample Tubes•

Preparing the Sample for Analysis•

Performing an Analysis•

Printing File Contents•

Generating a List of File Statistics•

Exporting Isotherm Data•

Generating Graph Overlays

TriStar 3000

Specifying Sample Defaults

OPERATIONAL PROCEDURES
This chapter contains step-by-step procedures for operating the TriStar 3000. It
does not provide detailed descriptions of the fields in the dialogs used to performthese procedures. Refer to Chapters 5 through 8 for field descriptions.

Specifying Sample Defaults
Sample information files include the information required by the TriStar to perform an analysis and collect data. The TriStar automatically generates sample information file names and assigns the default values which you specify.
The sample information presentation can be presented in a basic or advanced format. Accordingly, sample defaults also are specified in the basic and advanced formats. If desired, you may define parameter files before entering sample defaults(refer to Defining Parameter Files in this chapter).

Basic Format
Perform the following steps to define defaults for a sample information file in the
Basic format.
Select Option Presentation on the Options menu and ensure that Basic is selected as the format.

1.

Feb 03

From the Options menu, select Sample Defaults; the Sample DeFaults dialog
is displayed.

4-1

Specifying Sample Defaults

TriStar 3000

2.

In the Sequence field, specify a default string. This is the number that is incrementally sequenced and displays in the File name field when you selectFile, Open, Sample information.

3.

In the field on the right of the Sample line, enter a format for the identification. Be sure to include the $ symbol if you wish to have the sample filenumber included as part of the identification.

You also can edit the word Sample. For example, you may prefer to use Test.

4.

Enter a default value in the Mass field. You can edit this value at the time ofanalysis.

5.

In the Density field, enter a value for the material to be analyzed. This information is required only for the Quasi-Gemini and computed free-spacemethods.

6.

Select the down arrow to the right of the following fields to specify default
parameter files:
Sample Tube
• Degas Conditions• Analysis Conditions• Adsorptive Properties• Report Options
•

7.

4-2

Click

Save

, thenClose.

Feb 03

TriStar 3000

Specifying Sample Defaults

Advanced Format
Perform the following steps to define defaults for a sample information file in the
Advanced format.
Select Option Presentation on the Options menu and ensure that Advanced is
selected as the format.

1.

From the Options menu, select Sample Defaults; the Default Advanced Sample Information dialog is displayed.

2.

In the Sequence field, specify a default string. This is the number that is incrementally sequenced and displays in the File name field when you selectFile, Open, Sample information.

3.

In the field on the right of the Sample line, enter a format for the identification. Be sure to include the $ symbol if you wish to have the sample filenumber included as part of the identification.

You also can edit the word Sample. For example, you may prefer to use Test.

Feb 03

4.

Edit the Operator and Submitter lines as desired. Or you may have either(or both) of these lines omitted entirely by selecting Omit.

5.

Enter default values for the sample’s mass and density. Both of these values
may be edited at the time of analysis.

4-3

Specifying Sample Defaults

TriStar 3000

6.

In the Type of Data group box, choose whether you wish to collect data automatically or enter it manually.

7.

After you complete the Sample Information dialog, click on the parametertabs to open associated dialogs; specify defaults as desired.
The defaults you specify for parameters serve as defaults for new parameter
files. For example, the values you specify in the Analysis conditions portionof the sample file display as the default values for newly created stand-alone
Analysis conditions files.

8.

4-4

Click

Save

, thenClose.

Feb 03

TriStar 3000

Defining Parameter Files

Defining Parameter Files
The following file types can exist as part of the sample information file, as wellas individual parameter files:
Sample tube
Degas conditions• Analysis conditions• Adsorptive properties• Report options••

Having these files exist independently allows you to use them over and overagain.
Several predefined parameter files (located in the PARAMS directory) are included with the TriStar 3000 analysis program. Although these files may comeclose to the needs of your laboratory, you may wish to define additional ones. Or
you can use a predefined file as a starting point. You can do this by creating a
new file and then selecting Replace . A dialog is displayed so that you can selectthe existing parameter file. Then you can make any changes you need to makeand the original file remains unchanged.
Make sure you save these files to the directory specified as the Parameter File directory (refer to Chapter 8 for additional information). If you do not save thesefiles to the specified directory, they will not display in the drop-down lists on the
Basic sample file editor.
Parameter files may be defined using either the Basic or Advanced format. The
following sections provide instructions for using the Basic format; the dialogs for
the Advanced format are the same as the ones on the Basic format.

Sample Tube
Sample tube files are used only for the Quasi-Gemini or Calculated free-spacemethods.
Perform the following steps to define a sample tube file:Feb 03

1.

From the File menu, select Open, Sample tube; the Open Sample Tube dialog is displayed.

2.

Enter a name in the File name field, then click

OK

.

4-5

Defining Parameter Files

TriStar 3000

3.

Click

4.

Enter a description in the Sample Tube field. Be sure to use an intuitive description so that you can recognize it easily.

5.

Select the stem diameter of the sample tube you plan to use.

6.

Enter the volume of the sample tube below the red line on the sample tube
stem. This value is obtained by calibrating the sample tube. (Refer to Calibrating Sample Tubes in this chapter.)Yes

to create the file; the Sample Tube dialog is displayed:This value is required only if you plan to use the quasi-Gemini or calculated
method for free-space measurement.

4-6

7.

Select whether you plan to use a filler rod and/or an isothermal jacket.

8.

Click

Save

, thenClose.

Feb 03

TriStar 3000

Defining Parameter Files

Degas Conditions
Degas Conditions files contain degassing information for sample preparation.
These files are used only if you are using the SmartPrep Degasser.
Perform the following steps to define a degas conditions file:Feb 03

1.

From the File menu, select Open, Degas conditions; the Degas Conditions
dialog is displayed.

2.

Enter a name in the File name field, then click

3.

Click

4.

Enter a description in the Description field. Be sure to use an intuitive description so that you can recognize it easily.

5.

Enter up to five stages of degassing (soak temperature, ramp rate, and soaktime).

6.

Click

Yes

Save

OK

.

to create the file; the Degas Conditions dialog is displayed:, then

Close

.

4-7

Defining Parameter Files

TriStar 3000

Analysis Conditions
Analysis conditions specify the data used to guide an analysis.
Perform the following steps to define an analysis conditions file:1.

From the File menu, select Open, Analysis conditions; the Analysis Conditions dialog is displayed.

2.

Enter a name in the File name field, then click

3.

Click

4.

Enter a description in the Description field. Be sure to use an intuitive description so that you can recognize it easily.

5.

Choose whether you wish to have the isotherm collected by target pressuresor dose increments. Then specify the options required for your choice.

6.

Click Preparation... to specify evacuation and leak test values.

7.

Click

8.

Click Po and T... to specify how the saturation pressure (Po) is to be measured and the analysis bath temperature.

9.

Click Equilibration... to specify the equilibration interval and its delay time.

10. Click

4-8

Yes

.

to create the file; the Analysis Conditions dialog is displayed:

Free space...

Save

OK

to specify how the free space is to be measured.

, thenClose.

Feb 03

TriStar 3000

Defining Parameter Files

Adsorptive Properties
Adsorptive properties provide the adsorptive characteristics for the analysis.
Perform the following steps to create an adsorptive properties file:1.

From the File menu, select Open, Adsorptive properties; the Open Adsorptive Properties dialog is displayed.

2.

Enter a name in the File name field, then click

3.

Click

4.

Verify that Nitrogen is displayed as the adsorptive. Nitrogen is the appropriate adsorptive in most analyses.

5.

Enter information (or accept the defaults) in the following fields (refer to Adsorptive Properties in Chapter 5):

Yes

OK

.

to create the file; the Adsorptive Properties dialog is displayed:

Maximum manifold pressure
Non-ideality factor
Density conversion factor
Molecular cross-sectional area6.

Feb 03

Click

Save

, thenClose

4-9

Defining Parameter Files

TriStar 3000

Report Options
Report options files specify the type of reports which can be generated from ananalysis or from manually entered data. They also contain report details such asaxis scale, axis range, and column headings. These report options files may be
used to generate reports automatically at any time during or after the analysis. Of
course, reports generated during analysis can only report on data collected up to
the time of the report.
Report options files may contain tabular reports only, plots only, or both tabular reports and plots. They may also contain user-defined report tables.
Report options files also may be defined to include overlay options. The TriStar
program enables you to overlay up to eight plots of different samples onto a ninth
plot of the same type. Or you can overlay one plot type onto a different plot typefrom the same analysis. Refer to Generating Overlays in this chapter.
Perform the following steps to define a report options file:

4-10

1.

From the File menu, select Open, Report options; the Open Report Options
File dialog is displayed.

2.

Enter a name in the File name field, then click

3.

Click

4.

Enter a description (up to 42 characters) in the Description field. Enter an
identifier that gives a more intuitive description of the file’s contents. For example, BJH Adsorption Report Options.

Yes

OK

.

to create the file; the Report Options dialog is displayed:

Feb 03

TriStar 3000

Defining Parameter Files

5.

Select Show report title and enter the title you wish to appear at the top of
the report. Or deselect this option if you prefer not to have a report title.

If your company logo exists as a bitmap (bmp) or enhanced metafile (emf),
you can have it display in the report header by selecting Show graphic. Click
Browse... to select the file; use the Height and Width fields to specify the size.
6.

If you wish to compare the same type of graph from multiple files, click
Overlays and choose the files. Then be sure you edit the graph from theSelected Reports window and choose Samples from the Overlay drop-down
list.

7.

The reports that may be generated are listed in the Selected Reports list.
Select reports by double-clicking on the desired report. Reports are deselectedin the same manner. A report is selected when it is preceded by a check mark.
You can edit some reports by highlighting the desired report and clicking
Edit...
.

8.

Feb 03

Click

Save

, thenClose

to save the information and close the dialog.

4-11

Creating a Sample File

TriStar 3000

Creating a Sample File
Whether you choose to create your sample file in advance or at the time of analysis, a sample information file must be created for each analysis. The sample information file consists of information groups which, collectively, identify the sample,
guide the analysis, and specify report options.
A sample file may be created in any of the sample presentation formats:•

Advanced. This format provides complete access to all parts of the sample
file, allowing you to edit parameters quickly and conveniently.

•

Basic. This format presents a single window from which you select predefined parameter files. You can also switch to the Advanced format if editing isrequired.

•

Restricted. This format presents a single window from which you select predefined parameter files. You cannot, however, switch to the Advanced format
for editing.

Basic and Restricted Formats
The Basic and Restricted formats are the easiest and simplest way to create a sample file. You simply create your sample information file using predefined parameter files (explained in this chapter). If more detailed conditions or custom files are
required, you must use the Advanced format (discussed next).
•

If you are using the Basic format, you can switch to the Advanced format if
editing is required.

•If you are using the Restricted format, you cannot edit parameter files.

Perform the following steps to create a sample information file using the basic or
restricted format.

4-12

1.

From the File menu, select Open, Sample Information; the Open Sample Information File dialog is displayed.

2.

Accept the next sequenced file number or enter a new name in the File namefield.

Feb 03

TriStar 3000

Creating a Sample File

3.

OK
Click
; thendialog is displayed.

4.

Enter the sample’s mass in the Mass field.

5.

Enter the material’s density in the Density field. This value is used for the
Quasi-Gemini or Calculated free-space methods.

6.

Click on the down arrow to the right of each of the following fields tochoose parameter files:

to create the file; the Basic Sample Information

Yes

Sample Tube
Degas Conditions (if using the SmartPrep degasser)• Analysis Conditions• Adsorptive Properties• Report Options••

If you have an existing sample file containing the options you wish to use forthis file, click Replace All... to choose the file and copy the options.

7.

Feb 03

Click

Save

, then

Close

.

4-13

Creating a Sample File

TriStar 3000

Advanced Format
The Advanced format presents all parts of the sample file in an index card manner. This format lets you customize your sample file, allowing you quick access toall parameters.
Perform the following steps to create a sample information file using the advanced format.
1.

From the File menu, select Open, Sample Information; the Open Sample Information File dialog is displayed.

2.

Accept the next sequenced file number or enter a new name in the File namefield.

3.

OK
Click
, thenis displayed.

Yes

to create the file; the Sample Information dialog

These fields may notdisplay if omitted insample defaults.

4-14

4.

In the Operator field, enter the name of the person who will be performing
the analysis.

5.

In the Submitter field, enter the name of the department, company, etc. submitting the sample for analysis.

6.

Enter the sample’s mass and density. The density is only relevant if you aremeasuring the free space using the Quasi-Gemini or Calculated method.

Feb 03

TriStar 3000

Feb 03Creating a Sample File7.

Choose whether you are going to use manually entered data or have it automatically collected.

8.

After you complete the Sample Information dialog, click on the parametertabs to open associated dialogs and edit as desired. Instructions for completing these dialogs are explained in Defining Parameter Files in this chapter.

9.

After you have completed all parameters, click

Save, then

Close

.

4-15

Cleaning and Labeling Sample Tubes

TriStar 3000

Cleaning and Labeling Sample Tubes
Sample tubes and filler rods must be clean and dry before samples are added andweighed. The following procedures are recommended. Refer to Table 4-1 for a listof materials needed to clean and weigh samples.
Table 4-1. Materials Required to Clean and Weigh Sample Tubes
Supplied by Micromeritics

Sample tube
Filler rod (if used)
Sample tube brush
Stopper for sample tube
Sample tube rack
Sample weighing support
Sample data worksheet (copiedfrom Appendix A of this manual)

4-16

Supplied by User

Drying oven
Ultrasonic cleaning unit
DetergentRubber gloves or lint-free cloth
Acetone or isopropyl alcohol
Safety glasses
Waste container
Balance
Pipe cleaners

1.

Turn on the drying oven used for heating the sample tubes and filler rods andset the temperature to 110 oC.

2.

Check the reservoir of the ultrasonic cleaning unit to make sure it is clean.

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 dissolved before placing the sample tubes and filler rods into the water. If too much detergent isused, 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 theultrasonic cleaning unit. Place the filler rods in the bowl also. Turn on the ultrasonic cleaning unit for approximately fifteen minutes.

Feb 03

TriStar 3000

Cleaning and Labeling Sample Tubes

Figure 4-1. Cleaning Sample Tubes

5.

Using rubber gloves, remove the sample tubes and filler rods from thereservoir.

6.

Clean the interior of the sample tubes with the brush supplied with the TriStar System.

7.

Rinse the sample tubes and filler rods thoroughly with hot water. Then rinsethem with isopropyl alcohol or acetone using a waste container to collectused solvent.

If isopropyl alcohol or acetone is not available, deionized water may be used
to rinse the sample tubes.

Figure 4-2. Rinsing Sample Tubes

Feb 034-17

Cleaning and Labeling Sample Tubes

8.

TriStar 3000

Using nitrogen, dry the interior of the sample tubes and filler rods under avent hood. Use a tubing extension long enough and small enough in diameterto fit inside the tubes.

Figure 4-3. Drying Sample Tubes

9.

Stand the sample tubes on the sample tube rack and place the filler rods in abasket or in the rack. Bake in a vacuum oven for two hours.

10. Remove the sample tubes and filler rods from the oven and allow them tocool.
Do not insert the filler rods at this time. Filler rods are inserted just before
the sample tube is installed on the analysis port.

11. Wipe a rubber stopper with a lint-free cloth.
12. Label the sample tube and stopper for identification.

4-18

Feb 03

TriStar 3000

Calibrating Sample Tubes

Calibrating Sample Tubes
You must calibrate sample tubes if you wish to use them to perform Quasi-Gemini analyses or to calculate free space. The calibrated volume is entered in thesample tube parameter file.
Make a copy of the Sample Tube Calibration Worksheet provided in Appendix
A, then proceed with the instructions provided below.
1.

Write the Sample Tube Identification on the worksheet.

2.

Place the sample weighing support on the balance. Tare the balance and allow
it to stabilize at zero (0).

3.

Place a clean, empty sample tube (without stopper) on the sample weighing
support. Record the stabilized weight on the worksheet as Empty sample tube
weight. .

Figure 4-4. Weighing Sample Tube

4.

Fill the sample tube with deionized water to the red line on the stem; the meniscus should be even with the line.

Meniscus

Red Line

Figure 4-5. Level of Deionized Water

Feb 034-19

Calibrating Sample Tubes

TriStar 3000

5.

Place the sample tube containing water on the sample weighing support. Record this weight on the worksheet as Sample tube plus water.

6.

Subtract the empty sample weight (step 3) from the weight of the sample
tube containing water (step 5). Record this value on the worksheet as Weightof the water.

7.

Insert a thermometer into the water to obtain its temperature, then refer to Table 4-2 to determine the water’s density. Record the density on the worksheet.
Table 4-2. Water Density

8.

Temperature(°C)

Density(g/cm3)Temperature(°C)

Density(g/cm3)15

0.9991016

23

0.9975412

16

0.9989450

24

0.9972994

17

0.9987769

25

0.9970480

18

0.9985976

26

0.9967870

190.9984073

27

0.9965166

20

0.9982063

28

0.9962371

210.9979948

29

0.9959486

22

0.9977730

30

0.9956511

Divide the weight of the water (step 6) by the density of water (step 7) to obtain the physical volume below the red line on the sample tube.
a. Record this value on the worksheet.
b. Enter this value in the Physical volume below mark field in the Sample
Tube dialog box.

4-20

Feb 03

TriStar 3000

Preparing the Sample for Analysis

Preparing the Sample for Analysis
A sample must be properly weighed and degassed before installing it on the sample port for analysis.
Make a copy of the Sample Data Worksheet provided in Appendix A, then proceed with the instructions provided below.

Weighing the Sample
Analysis results are expressed in units of surface area per gram of sample; therefore, the true sample mass must be known. Carefully weigh each sample tube set(sample tube and stopper) and sample as described below.
1.

Write the Sample Tube Identification on the Sample Data Worksheet.

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 on the sample weighing support. Record the stabilized weight on the Sample Data Worksheet as Empty sample tube mass. Remove the sample weighing support and sample tube set from the balance.

Figure 4-6. Weighing Sample Tube Set

4.

Place a sample weighing container onto the balance. Tare the balance and allow it to stabilize at zero (0).

Do not touch the sample with bare hands while performing the next six steps.
Doing so could affect the accuracy of results.

Feb 034-21

Preparing the Sample for Analysis

TriStar 3000

5.

Slowly add the desired amount of sample to the container.

6.

Weigh the stabilized sample and record the value on the Sample Data Worksheet as Sample mass (Before Degas).

7.

Remove the rubber stopper from the sample tube.

8.

Pour sample from the weighing container into the sample tube using the funnel provided.
If some sample clings to the inside of the sample tube above the red line, remove it using a pipe cleaner or lint-free wipe.

Figure 4-7. Placing Sample in Sample Tube

9.

Replace the rubber stopper.

10. Weigh the sample tube set containing the sample and record the value on the
Sample Data Worksheet as Sample tube set plus sample mass (Before Degas).

Degassing the Sample
After the sample has been weighed, use a degassing unit to remove any contaminants which may have adsorbed to the surface or pores of your sample. Appropriate degassing units are available from Micromeritics. Refer to Chapter 10 for
ordering information.
After degassing is complete, weigh the sample tube set containing the sample andrecord the weight on the Sample Data Worksheet as Sample tube set plus sample
mass (After Degas).

4-22

Feb 03

TriStar 3000

Preparing the Sample for Analysis

Installing the Sample Tube
You may use the three analysis ports as follows:•

Port 1 for a sample analysis•

Port 2 for a sample analysis or a Quasi-Gemini (blank sample tube)
measurement•

Port 3 for a sample analysis or continuous Po measurement

To attach a sample tube to a port, follow the steps below.
1.

Remove the sample tube stopper.

2.

If using an isothermal jacket: slide the jacket down over the stem of the sample tube until it touches the bulb of the sample tube.

3.

Install the dewar cover by inserting the sample tube through one of the holes
in the cover. Make sure the tapered side of the cover is toward the bulb of
the sample tube.

O-ringFerruleConnector Nut

Dewar Cover

Figure 4-8. Attaching a Sample Tube to an Analysis PortFeb 03

4.

Place the connector nut, ferrule, and O-ring onto the sample tube stem.

5.

Carefully insert a filler rod (if used) into the sample tube.

6.

Attach the sample tube to the analysis port. Make sure it is fully in theport. Secure it in place by screwing the connector nut onto the analysis port.
Hand-tighten the connector nut.

7.

Slide the dewar cover upward until it stops.

4-23

Preparing the Sample for Analysis

TriStar 3000

Installing the Analysis Dewar
Prepare the analysis Dewar after you have installed the sample tube(s),Always handle Dewars with care. Any product incorporating a vacuum is apotential safety hazard and should be treated with caution. Always observe
the precautions listed below.
We recommend the following be observed when handling Dewars containing liquefied gases:•

Protect yourself by wearing 1) goggles (or a face shield), 2) an insulated or
rubber apron, and 3) insulated gloves.

•

When pouring liquefied gases from one container to another: 1) cool the receiving container gradually to minimize thermal shock, 2) pour the liquefied
gas slowly to prevent splashing, and 3) vent the receiving container to the atmosphere.

•

Use a plastic stirring rod when stirring substances in a Dewar containing liquefied gases (or other materials of extremely low temperature). Do not use aglass or metal stirring rod unless it is coated with some type of protective coating.

•Do not remove the mesh covering from the Dewar flask. This covering is inplace to minimize the risk of flying particles if the Dewar is accidentallyknocked over or dropped and broken.

•

Do not handle heavy objects above the Dewar. If unavoidable, place a protective cover over the Dewar’s opening. If an object of sufficient weight is accidentally dropped into the Dewar, shattering may occur.

Install the analysis Dewar as follows:1.

Fill the dewar with the analysis bath liquid (liquid nitrogen) to about 5 cm (2in.) from the top.

Incorrect fluid levels can lead to measurement errors. You should check thelevel of the bath liquid before each analysis.

2.

4-24

Insert the dipstick into the dewar and check the level of the analysis bath liquid.

Feb 03

TriStar 3000

Preparing the Sample for Analysis

Level Indicator Mark
Wetness or Frozen
Condensation Indicates
Bath Liquid Level

Figure 4-9. Analysis Bath Fluid Dipstick3.

Allow approximately 30 minutes (for best results) for the temperature of thedewar to stabilize with that of the bath liquid. Then recheck the level of thebath liquid; add additional liquid if necessary.

It is unnecessary to allow time for stabilization unless the dewar has not beenin use for a while.

Feb 03

4.

Place the analysis dewar onto the elevator.

5.

Close the analysis compartment doors.

4-25

Performing an Analysis

TriStar 3000

Performing an Analysis
Once a sample has been degassed and transferred to an analysis port, you may begin analysis. The TriStar provides two types of analyses from which you may
choose:•Standard - allows you to perform up to three analyses using different analysis
conditions.

•

QuickStart - allows you to perform multiple sample analyses using the same
analysis conditions.

Refer to chapter 6 for a detailed description of the dialog boxes shown in this seciton.

Standard Analysis
1.

From the Unit menu, select Sample Analysis; the following dialog box is displayed.

Indicates Freespace Measurement and shows only
the Sample Tube Filefield and the Browse pushbutton when this port is being used for the Quasi
Gemini Method.

Indicates Po Measurement(no other fields are shown
when this port is being used
to measure the Po on a continuous basis.

4-26

2.

Click Browse... to choose a sample information file to be used for each port.

3.

The sample identification, sample weight, and sample density contained in thesample information file are displayed. Verify the sample weight and density.
The density value is irrelevant unless you are using the Quasi-Gemini or Calculate method for the free-space determination.

Feb 03

TriStar 3000

Performing an Analysis

4.

The Po and bath temperature are displayed; these may be edited if desired.

5.

Select Report after analysis to have a report generated automatically when
the analysis completes.

6.

Click Start to start the analysis; an analyzing view of the window is displayed so that you can view data as it is collected. A short delay is encountered before the port status changes from the Idle state.

QuickStart Analysis
It is not necessary to prepare sample files in advance when using the QuickStart
method. The information in the sample files is inserted automatically from the parameter files you choose.

Feb 03

1.

From the Unit menu, select QuickStart; the following dialog box is displayed.

2.

Select the Analysis Conditions, Adsorptive Properties, and Report Options
files to be used for the analyses.

3.

Select Report After Analysis and enter the number of reports and report destination, if desired.

4-27

Performing an Analysis

4.

Click

TriStar 3000

Next>>; the following dialog is displayed.

Indicates Freespace Measurement; shows only the
Sample Tube File field
and the Browse push button when this port is being
used for the Quasi Gemini
Method.

Indicates Po Measurement(no other fields are shown
when this port is being used
to measure the Po on a continuous basis)

5.

Assign a sample information file to each port:
a. Click Browse... , thenb. Click

Yes

OK

.

to create the file.

The analysis conditions, adsorptive properties, and report options selected on
the previous screen are inserted automatically into the newly created files.
6.

Select a sample tube file for the sample tube you plan to use.

7.

Enter the sample’s mass and density. The density is used only for the QuasiGemini or Calculated free-space method.

8.

Ensure that the Po value and bath temperature are correct; edit if needed.

9.

Click

Start

to start the analysis; the following actions occur:•

A view of the data collection as it progresses is displayed. A short delay is encountered before the port status changes from the Downloading state. If desired, you can obtain a report on the data collected so far by selecting theappropriate Report Port [n] push button; the report is printed to the screen.

•

When the analysis finishes, the QuickStart dialog shown in Step 4 again is displayed.

10. Repeat steps 5 through 9 to perform additional analyses or click
close the QuickStart dialog.

4-28

Close

to

Feb 03

TriStar 3000

Printing File Contents

Printing File Contents
You can print the contents of one or more of the following file types to thescreen, a printer, or to a file on disk.
Sample information
Sample tube
• Degas conditions• Analysis conditions• Adsorptive properties• Report options••

1.

From the File menu, select Print. A drop-down list containing file types isdisplayed.

2.

Choose the file type; a dialog similar to this one is displayed.

Choose thedestination.

Choose the file
you wish to print.

Click to complete
the printing process.

Feb 03

3.

From the Files list box, select the file you wish to print. If you plan to print
multiple files, hold down Ctrl while clicking on the desired files.

4.

From the Settings group box, choose a Destination for your file. If you
choose File as the destination, enter a name in the File name field, or accept
the default. If you have selected multiple files, individual files are exported
as their file name with the extension .RPT.

5.

Click

OK

; the file is printed to the specified destination.

4-29

Generating a List

TriStar 3000

Generating a List
You can generate a list of the following information on one or more files to thescreen, a printer, or to a file on disk.
File nameDate the file was created (or last edited)• Time the file was created (or last edited)• File identification• Status••

1.

From the File menu, select List. A drop-down list containing the following
file types is displayed.
Sample information• Sample tube
• Degas conditions• Analysis conditions• Adsorptive properties• Report options•

2.

Choose the file type; a dialog similar to this one is displayed.

Choose thedestination.

Choose the file(s)on which you wish
to generate a list.

Click to complete theprocess.

3.

4-30

From the Files list box, select the file from which you wish to have a list
generated. If you plan to list information for multiple files, hold down Ctrl
while clicking on the desired files.

Feb 03

TriStar 3000

Feb 03Generating a List

4.

From the Settings group box, choose a Destination for your list. If you
choose File as the destination, enter a name in the File name field, or accept
the default. If you have selected multiple files, individual files are exported
as their file name with the extension .LST.

5.

Click

OK

; the list is printed to the specified destination.

4-31

Exporting Isotherm Data

TriStar 3000

Exporting Isotherm Data
Export allows you to copy the isotherm data in a sample information file and export it in a format it in ASCII text. If saved to a File, the data can be imported
into applications such as spreadhseets. The output file consists of four columns
containing the absolute pressure, relative pressure, specific volume adsorbed, andthe elapsed time.
1.

From the File menu, select Export; the Export Sample File dialog is displayed.

Choose the type.
Choose thedestination.

Choose the file
you wish to export.

Click to complete
the export process.

2.

From the Files list box, select the file you wish to export. If you plan to export multiple files, hold down Ctrl while clicking on the desired files.

3.

From the Settings group box, choose a Destination for your exported file.
If you choose File as the destination, enter a name in the File name field, or
accept the default. If you have selected multiple files, individual files are exported as their file name with the extension .ISO (isotherm).

4.

4-32

Click

OK

; the file is exported to the specified destination.

Feb 03

TriStar 3000

Generating Graph Overlays

Generating Graph Overlays
Use the graph overlay function when you wish to compare graphically multiple
graph options. Overlays may be generated in two ways:•

Multiple Graph Overlays
Overlaying two different types of graphs from the same sample on top ofeach other. This type of overlay is available for BJH Adsorption/ Desorption reports only.

•

Multiple Sample Overlays
Overlaying the same type of graph for up to eight samples on top of apreviously selected sample.

Varying symbols are used to differentiate the graphical lines and reported in a legend at the top of the output. If color output is available, different colors are usedinstead.

Multiple Graph Overlays
To overlay two different types of graphs from the same sample file:Feb 03

1.

From the File menu, select Open, Sample Information. Double-click on thedesired file. If your window is presented in the Basic format, click Advanced .

2.

Select the Report Options tab.

3.

Select the type of report on which you wish to have overlays generated. Remember, only BJH Adsorption/Desorption reports can be chosen for this typeof overlay.

4-33

Generating Graph Overlays

4.

Click

TriStar 3000

Edit...

; the BJH Adsorption/Desorption dialog is displayed.

Select the reportvariable

Click to choose thesecond reportvariable.

5.

From the Selected Reports window, choose the report variable on which you
wish to have another variable overlaid, then click Edit... . A dialog similar
to this one is displayed.

Displays the firstreport variable.

Choose the second
variable from thisdrop-down list.

6.

From the Overlay drop-down list, choose the report variable you wish toOKoverlay, then click.

You do not have to save these options before generating overlay reports. If
you do save, the report options for your original sample file will be replacedwith the new ones.

4-34

Feb 03

TriStar 3000

Generating Graph Overlays

7.

From the Reports menu, select Start report; the Start Report dialog is displayed. In most cases, your file name will be highlighted and displayed in theFile name: field. If it is not, simply navigate to the appropriate directory andchoose the file.

8.

OK
Click
; the Select Reports dialog is displayed. Clickclose the dialog and generate the overlays.

OKagain toMultiple Sample Overlays
To overlay the same type of graph on multiple samples:
1.

From the File menu, select Open, Sample Information. Double-click on thedesired file. If your window is presented in the Basic format, click Advanced .

2.

Select the Report Options tab.

3.

Choose the type of report from the Selected Reports window; then click
Edit...
.

4.

Choose one:
If you are overlaying
these types of reports....

Then....

Isotherm
BET Surface Area
Langmuir Surface Areat-PlotSelect the Overlay Samples checkbox.

BJH Adsorption
BJH Desorption

Choose the report variable from the Selected
Reports window, then click Edit... .

Click

OK

.

Click on the down arrow in the Overlay: fieldOKand choose Samples; then click
.
OK
Click
again to close the BJH
Adsorption/Desorption dialog and display theReport Options dialog.

5.

Feb 03

From the Report Options dialog, click
ples dialog is displayed.

Overlays...

; the Graph Overlays Sam-

4-35

Generating Graph Overlays

TriStar 3000

6.

Click Browse... to the right of the Sample [n] field; the Open Sample Information dialog is displayed.

7.

Choose the file containing the graph you wish to overlay, then click
You may choose up to eight files in this manner.

OK.

You do not have to save these options before generating overlay reports. If
you do save, the report options for your original sample file will be replacedwith the new ones.

4-36

8.

From the Reports menu, select Start report; the Start Report dialog is displayed. Your primary file should be highlighted and in the File name: field.
If it is not, simply navigate to the appropriate directory and choose the file.

9.

OK
Click
; the Select Reports dialog is displayed. Clickclose the dialog and generate the overlays.

OKagain toFeb 03

CHAPTER 5
FILE MENU•

Description

•

Open

•

Save

•

Save As•

Save All

•

Close

•

Close All

•

Print

•

List

•

Export•Exit

TriStar 3000

Description

FILE MENUThe File menu contains options which allow you to manage sample and parameter
files.

Description

Listed below are brief descriptions of the File menu options. Detailed descriptions
follow this section.
Open

Opens an existing file or creates a new one. When you
select this item, a drop-down menu containing the following file types is displayed:•

Sample information
Sample tube
• Degas conditions• Analysis conditions• Adsorptive properties• Report options•

Feb 03

Save

Saves the file in the active window.

Save As

Saves the file in the active window as a different name.
You also can use this option to save a subset of the sample file as a parameter file.

Save All

Saves all open files.

5-1

Description

5-2

TriStar 3000

Close

Closes the file in the active window.

Close All

Closes all open files.

Print

Prints the contents of a sample or parameter file.

List

Generates a list of certain information for sample or parameter files.

ExportExports the isotherm data contained in a sample file.

Exit

Exits the analysis program.

Feb 03

TriStar 3000

Open

Open
Open allows you to create or edit a sample or parameter file.
Regardless of which file type you select, a dialog box similar to the one shown
here is displayed.

File nameFor sample information files, this field contains the next
sequenced file name generated by the analysis program.
For parameter files, the file name displayed includes thewild card (*) and a default extension as follows:*.STB for sample tubes*.DEG for degas conditions*.ANC for analysis conditions*.ADP for adsorptive properties*.RPO for report options
If you are creating a new file, enter a name in the Filename field. If you are editing an existing file, select afile from the list.

Refer to Selecting Files in Chapter 3 for a description of the other fields on this
dialog box.

Feb 035-3

Open

TriStar 3000

Sample Information
Sample information files contain information used to control the analysis. Therefore, every analysis must be linked with a sample information file before theanalysis can proceed. A sample information file is comprised of the following:
sample identification
sample tube parameters• degas conditions (if using automatic degassing)• analysis conditions• adsorptive properties• report options• collected/entered data (when an analysis has been completed)••

Parts of the sample information file can also exist as parameter files which areseparate from the sample information file itself. Having these files exist independently allows you to use them as many times as you wish. For example, if
you typically use the same analysis conditions for many of your analyses, you cancreate an analysis conditions file containing those conditions. Then when you create your sample file, select that file for your analysis conditions. Once it becomespart of the new sample file, you can edit it in any way you wish without changing the file from which it was copied.
Sample information files are presented in three formats: Advanced, Basic and
Restricted.
Specify or change your format by selecting Option presentation from the Options menu.

5-4

•

Basic
Presents the entire sample information file in a single dialog. With this format, you can quickly create a sample information file using previously defined parameter files. This format also allows you to switch to the
Advanced format to view or edit parameters.

•

Advanced
Presents all parts of the sample information file in a single, index card
tabbed dialog. Each tab opens its associated dialog. Use this format to create customized files.

•

Restricted
Presents the sample information file in a single dialog similar to the Basic
format. With the Restricted format, however, you cannot switch to the Advanced format to edit parameters. Some menu items also are unavilable.

Feb 03

TriStar 3000

Open

Basic
When you open an existing sample information file or create a new one using the
Basic format, all parts of that file are contained on a single dialog. With the Basic format, you can quickly create a sample information file using previously defined parameter files. This format also allows you to switch to the Advanced
format to view or edit parameters. Chapter 4 provides step-by-step instructions forcreating a Basic sample information file.

If you are creating a new file, this dialog displays the defaults you specified
in Sample defaults. Chapter 8 explains how to establish sample defaults.

SampleDisplays the next sequenced file description or the nameof the file you are opening. You may enter a new description or add to the existing one.
Range:

Mass

50 alphanumeric charactersEnter the mass of the sample to be analyzed.
Use 1.0000 when performing a blank analysis.

Density

Enter the density of the sample to be analyzed. Thisvalue is used only for the Quasi-Gemini or Calculated
free-space method.
Use 0.000 when performing a blank analysis.

Feb 035-5

Open

TriStar 3000

Add Log Entry

Displays the Add Log Entry dialog.

Enter information pertinent to the sample file. For example, if you are not using the SmartPrep for automatic degassing, you may wish to enter external degassing
information. Any information you enter here is printed aspart of the sample log report. You may make multiple entries by selecting this push button as many times as you
wish.
Sample Tube

Click the down arrow to display a list of previously defined sample tube files supplied with the analysis program, as well as any you may have created. Choose thesample tube file you wish to use.

Degas Conditions

Click the down arrow to display a list of previously defined degas conditions files supplied with the analysis
program, as well as any you may have created. Choose
the degas conditions file you wish to use.
These files are pertinent only if using the SmartPrep fordegassing samples.

Analysis Conditions

5-6

Click the down arrow to display a list of previously defined analysis conditions files supplied with the analysis
program, as well as any you may have created. Choose
the Analysis Conditions file you wish to use.

Feb 03

TriStar 3000

Open

Adsorptive
Properties

Click the down arrow to display a list of previously defined adsorptive properties files supplied with the analysis program, as well as any you may have created.
Choose the adsorptive properties file you wish to use.

Report Options

Click the down arrow to display a list of previously defined report options files supplied with the analysis program, as well as any you may have created. Choose theReport options file you wish to use.

Replace All...

Feb 03

Allows you to copy all parameters of an existing sample
file’s values into the sample information file you are creating. An “open file” dialog is displayed so that you may
OKselect the desired file. Click; the values are copied into the new file automatically. You may edit the values in the new file; the file from which they were copied
remains unchanged.

Save

Saves the information you have specified for this sample
file.

Close

Closes the dialog box. If a file containing unsavedchanges is open, you are prompted to save before the dialog box closes.

Advanced

Displays the sample information file in the advanced format, allowing you to view or edit parameters.

5-7

Open

TriStar 3000

Advanced
When you open an existing sample information file or create a new one using theAdvanced format, all parts of the sample file are displayed in a tabbed dialog.
The Advanced format allows you to customize sample files. Chapter 4 provides
step-by-step instructions for creating an Advanced sample information file.

The prompts for the Sample, Operator, and Submitter fields may be customized
by selecting Options, Sample defaults. Refer to Chapter 8 for instructions on customizing these prompts.
SampleDisplays the next sequenced file description or the nameof the file you are opening. You may enter a new description or add to the existing one.
Range:

Operator
Submitter

Enter the name of the operator who will be performing
the analysis and the name of the person (or department)
submitting the sample for analysis. Either or both ofthese fields may be omitted from this dialog by choosing
to do so when establishing defaults (Chapter 8).
Range:

5-8

50 alphanumeric characters

40 characters

Feb 03

TriStar 3000

Open

Mass

Enter the sample’s mass.
Use 1.000 when performing a blank analysis.

Density

This value is used only for the Quasi-Gemini or Calculated free-space method.
Use 0.000 when performing a blank analysis.

Type of Data

Choose whether data are to be collected automatically by
the analysis program or manually entered.
If you choose Manually entered, an “Entered” tab isadded so that you may enter the desired data.

Add Log Entry

Displays a dialog box so that you may enter pertinent information relating to the sample file. For example, if you
are not using automatic degassing, you may wish to enter external degassing information. Any information you
enter here is printed as part of the sample log report.
You may make multiple entries by selecting this push button as many times as you wish.

Replace All...

Allows you to copy an existing sample file’s values into
the sample information file you are creating. An “openfile” dialog is displayed so that you may select the deOK
sired file. Click; the values are copied into the
new file automatically. You may edit the values in the
new file; the file from which they were copied remains
unchanged. This replaces all parameters of the entire sample information file, excluding any collected data fromthe other file.

Each of the individual tabbed dialogs contains a Replace... push button if you
wish only to replace specific parameters and not the entire contents.

Comments

Save

Feb 03Enter comments about the sample or its analysis conditions. Comments entered here are printed in the headerof the reports.
Saves the information you have specified for this sample
file.

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Close

Closes the dialog box. If changes have been made in the
dialog and have not been saved, you will be prompted tosave before the dialog box closes.

Basic

Displays the sample information file in the basic format.

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Sample Tube
This dialog allows you to enter the specifics for a sample tube. A sample tube
file can be created as an independent parameter file or as part of the sample information file.
Be sure to save this file to the directory you specified as the Parameter Files
directory if it is to be included in the drop-down list of the Basic Sample Information dialog (see Parameter Files Directory in Chapter 8).

Sample Tube

Enter a description for the file.
Range:

Feb 0340 alphanumeric characters (at least one
character is required)

Replace...

Allows you to replace the values in the current sample
tube file with those from an existing file. An “open file”
dialog is displayed so that you may select the desiredOK
file. Click; the values are copied into the new
file automatically. You may edit the values in the newfile; the file from which they were copied remains unchanged

Stem Diameter

Select the diameter of the sample tube you are using forthis analysis.

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Physical volume
below markEnter the volume below the red line on the sample tube.
Refer to Calibrating the Sample Tube in Chapter 2.
This value is used only when using the Quasi-Gemini or
Calculated method for measuring the free space.

If you plan to use a calculated free space or the Quasi-Gemini method, it is agood idea to set up these files for your sample tubes.

Use isothermal jacket
Use filler rod

Select whether you are using an isothermal jacket and/or
a filler rod.
A filler rod is used to reduce the stem free-spacevolume, resulting in reduction of free-space error.
An isothermal jacket is used to maintain a constant temperature profile along the sample tube stem during an extended analysis (more than 1 or 2 hours).

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Degas Conditions
This dialog is used only if you are using the SmartPrep Degasser for degassing
your sample.
Be sure to save this file to the directory you specified as the Parameter Files
directory if it is to be included in the drop-down list of the Basic Sample Information dialog (see Parameter Files Directory in Chapter 8).

Description

If you are opening an existing file, this field contains thedescription.
If this is a new file, enter a description.
Range:

Feb 0340 alphanumeric characters (at least one
character is required)

Replace...

Allows you to copy the values of an existing degas conditions file into the file you have open. An “open file” dialog is displayed so that you may select the desired file.
OK
Click; the values are copied into the new fileautomatically. You may edit the values in the new file;the file from which they were copied remains unchanged.

Conditions Table

Allows you to enter up to five stages of degas conditions.

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Soak TemperatureEnter the temperature at which the sample is to soak
while flowing gas.

Ramp Rate

Enter the rate at which the temperature is to change
when advancing to the soak temperature.

Soak TimeEnter the amount of time to soak the sample.

InsertInserts a row into the conditions table. A row is inserted
above the selected line; the cursor moves to the new line.

DeleteDeletes the selected row from the conditions table.

Clear

Clears all entries contained in the conditions table. The
rows do not have to be selected.

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Analysis Conditions
This dialog allows you to specify the analysis conditions for your sample. An
analysis conditions file can be created as an independent parameter file or as partof the sample information file.
Be sure to save this file to the directory you specified as the Parameter Files
directory if it is to be included in the drop-down list of the Basic Sample Information dialog (see Parameter Files Directory in Chapter 8).

Description

If you are opening an existing file, this field contains thedescription.
If you are creating a new file, enter a description.
Range:

Replace...

Feb 0340 alphanumeric characters (at least one
character is required)

Allows you to replace the values in the current analysis
conditions file with those from an existing file. An “openfile” dialog is displayed so that you may select the deOK
sired file. Click; the values are copied into the
new file automatically. You may edit the values in the
new file; the file from which they were copied remains
unchanged.

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Isotherm Collection

The choices in this group box allow you to specify how
you wish to have isotherms collected.

Target Pressures

Select this option to have isotherms collected by specifying target pressures. When you select this option,
Pressures andOptions(directly to the right of thisfield) become enabled. Select each push button to verify
or edit data.

Pressures

Displays the Entered Pressures dialog.

Edit the existing pressure table or clear the table and enter a new pressure table.
A pressure table is a table of relative pressure points(and possibly calculation assignments) at which data (isotherms) are to be collected. The relative pressures may
span the entire range of 0.00000001 to 0.995 P/Po. There
must be one adsorption branch followed optionally by
one desorption branch.
Several analysis conditions files containing complete pressure tables are included with the TriStar software; they
are located in the PARAMS subdirectory. These files(and all other parameter files) can be changed. If you
want to use any of these files, it is recommended thatyou use the Save As option on the File menu to save thefile as a different name; then make your changes.

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Pressures(continued)

The pressure table for automatically collected data includes the pressure points for data collection and (whenUse calculation assignments is selected) identifies calculations through which the data are processed. The systemprocesses data for the following reports:•

BET surface area
Langmuir surface area
• t-Plot• BJH Adsorption• BJH Desorption• Total pore volume•

Insert range...

Displays the Insert Pressure Range dialog.

This dialog allows you to specify the starting pressure,the ending pressure, the number of points to insert
within the specified range, and whether you wish to havelinear or geometric progression.
Choose Linear to insert evenly spaced points into your table.
Choose Geometric from low pressure to insert geometrically spaced points from the low pressure range. For example, if you wish to insert 5 points with a 0.01 startingpressure and a 0.16 ending pressure, the following points
are inserted into the table:
0.01
0.02
0.04
0.08
0.16

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Pressures(continued)

Choose Geometric from saturation to insert geometricallyspaced points from the saturation pressure. For example,
if you wish to insert 5 points with a 0.99 starting pressure and a 0.84 ending pressure, the following points areinserted into the table:
0.99
0.98
0.96
0.92
0.84
Insert predefined

Displays the Insert Predefined Pressures dialog.

Choose predefined pressure points for surface area, t-Plotmicropore and/or BJH adsorption/desorption.
Click on the down arrow of each field to choose the desired set of points. You can also specify Adsorption/desorption total pore volume and saturation.
InsertInserts a row into the pressure table. A row is inserted
above the selected line; the cursor moves to the new line.
DeleteDeletes the selected row.
Clear

Clears all entries from the table. The rows do not haveto be selected.

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Options

Allows you to specify target pressure options; the Target
Pressure Options dialog box is displayed.

First Pressure Fixed Dose
Select this option to have the sample dosed with a specified amount of gas until the first pressure point isreached. This initial dosing quickly meets the adsorptive
demand of the sample.
The first point on the pressure table is the thresholdvalue. Once this first pressure point is reached, points
are equilibrated and recorded in accordance with thespecified pressure table.
You may wish to use this mode if you are performing astandard nitrogen analysis of microporous or highly
mesoporous materials such as catalysts. If the first pressure table point is low, and you expect the gas uptake ofthe sample to be high, choosing this mode can shorten
the time required to reach the first point on the pressuretable.
Maximum volume increment
Select this option to specify when additional data points
are to be collected between target pressures in regions ofhigh adsorption. When the maximum increment has beenadsorbed since the last collected data point, another point
is equilibrated and collected.
When using this option, reaching pressure points exactly
is not important; therefore, the tolerances should be set
relatively large (10 mmHg and 10% or so) for proper
functioning of the algorithm. The pressure table should
also have several points scattered over the region of interest.

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Options(continued)

During desorption, this field is treated as a maximum volume “decrement” value.
Absolute pressure tolerance
Relative pressure tolerance
These values are used to determine how close the actualpressure must be to each target pressure from the pressure table. At lower pressures the relative tolerance
value is lower, and at higher pressures the absolute tolerance value is lower. For example:
Experiment 1: you have an absolute tolerance of 5mmHg, a relative tolerance of 5%, and a target pressureof 40 mmHg; 5% of 40 mmHg is 2 mmHg. Since 2
mmHg (relative tolerance) is lower than 5 mmHg (absolute tolerance), 2 mmHg is used. Therefore a minimumpressure of 38 mmHg (40 - 2) must be attained to collect data for a target pressure of 40 mmHg.
Experiment 2: you have an absolute tolerance of 5mmHg, a relative tolerance of 5%, and a target pressureof 200 mmHg; 5% of 200 mmHg is 10 mmHg. Since 5
mmHg (absolute tolerance) is lower than 10 mmHg (relative tolerance), 5 mmHg is used. Therefore a minimumpressure of 195 mmHg (200 - 5) must be attained to collect data for a target pressure of 200 mmHg.
Normally, surface area measurement points are widely
spaced, and the resulting measurement is not very sensitive to the precise location of points so wider tolerances
may be used. Unnecessarily tight tolerances lengthen theanalysis.

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Dose Increments

Options

In this form of dosing, there is no predefined pressure table. The sample is dosed repeatedly with a fixed amountof gas and isotherm points are collected after equilibrating each dose. Each entry in the table defines how muchto dose for a segement of the isotherm.
Displays the Dose Increments dialog.

Insert or edit target ranges for up to 10 dose increments.
The current specified dose increments are displayed. The
ending relative pressure and the dose amount (entered oras the fraction of the previous volume adsorbed) for eachtarget range are shown.
InsertDisplays the Dose Increment Edit dialog.

Edit

Ending pressure:Enter the desired ending pressure of this segment.

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InsertEdit(continued)

Dose increment
Select this option to have the sample dosed with a specified amount of gas for each isotherm point taken.
Percent of previous
Select this option to have the sample dosed with a percentage of the volume adsorbed during the previous
interval of the table. For example if in the previous segment 5 cm3 STP of gas was adsorbed and you enter 40%
in this field, this segment will dose 2 cm3 STP for each
isotherm point taken.
This feature is disabled for the first entry of the dose increment table.

DeleteDeletes the selected range.

Clear

Clears the table of all entries except one; one entry is required.

Preparation...

Displays the Analysis Preparation dialog.

Select Fast evacuation when analyzing samples (such aspellets) that do not fluidize or shed particles under evacuation.
If you deselect Fast evacuation; Evacuation rate andUnrestricted evac from become enabled. Enter the desired evacuation rate and the pressure value at which unrestricted sample evacuation should begin.

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Preparation...

(continued)

In the Evacuation time field, enter the time you wish toallow for preliminary evacuation which takes place prior
to free-space measurement.
Select Leak test to check for system leaks or sample outgassing before the analysis. The leak test seals the sample tube and monitors the pressure. If the pressure rises
more than 0.15 mmHg, the analysis does not proceedand you are notified with a message. While leak testingslightly increases analysis time, it prevents the continuation of analysis and collection of erroneous data if aleak exists.
If you select Leak Test, enter the amount of time youwant the pressure monitored.

Free Space...

Displays the Free Space dialog.

Specify the type of free-space measurement you wish tohave performed. Refer to Appendix F for a discussion of
free-space methods.
MeasureMeasures the free space automatically over the sample
prior to data collection.
Lower Dewar for evacuation
Lowers the dewar during evacuation.
Evacuation time
Enter the time you wish to allow for evacuation after thefree-space measurement.

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Measure(continued)

Outgas test
Checks the system for sample outgassing after the freespace measurement. The outgas test seals the sample
tube and monitors the pressure. If the pressure rises
more than 0.025 mmHg within the time specified for theoutgas test duration, outgassing is present. If outgassing
is found, the test repeats up to nine times with a 30-minute evacuation time between each test. If the 10th test
fails, the analysis does not proceed and you are notified
of its cancellation. Outgas testing slightly increases analysis time, but it prevents continuation of analysis and collection of erroneous data if outgassing is present.
Enter the outgas test duration.

Quasi-Gemini

Select this option to have the free space of the sample
tube continuously balanced against an identical empty
sample tube. For each data point taken on the isotherm,a corresponding measurement is taken with the empty
sample tube (must be connected on
port 2) and that gas quantity subtracted from the gas
quantity in the actual sample tube.

Calculate

Select this option to have the free-space measurement calculated using the sample and tube parameters.

Enter

Enables the Warm free space and Cold free space
fields so that you may enter the free space manually.
The warm free space is the sample tube gas capacity
measured at room temperature.
The cold free space is the sample tube gas capacity measured with the Dewar raised.

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Po and T...

Displays the Po and Temperature Options dialog.

This dialog provides four options for obtaining the saturation pressure (Po) and analysis bath temperature. Clicking on each option prompts you for the entry of relatedparameters in the lower portion of the dialog box.
Option1

Prompts for...

a measurement interval (how often during
analysis the Po is to be measured) and theanalysis bath temperatureThis method may slow analysis time slightly
since the sample port and the Po tube both
require interaction with the manifold
plumbing system.

2

a Po and analysis bath temperatureThis methoid uses the values you enter in
the Po and temperature fields.

3

an analysis bath temperature and an estimate
for the initial Po.
This method measures the Po over the
sample. After the Po is measured, the value
is reapplied to all data points.

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Option4

Prompts for...

an analysis bath temperature.
This method measures the PO on acontinuour basis; enabling you to measure
every data point without slowing down theanalysis. It does, however, require thededicated use of one of the sample ports.

Equilibration...

Displays the Equilibration dialog box.

Enter an equilibration interval.
The equilibration interval is the number of seconds between successive pressure readings during equilibration.
At least 11 pressure readings for each equilibration are
required to obtain an accurate reading of the pressurechanges.
•Long equilibration intervals (15 - 100 seconds) tend tolengthen analyses but improve data integrity.

•

Short equilibration intervals (1 - 14 seconds) produce
faster analyses. For some samples, however, shortequilibration intervals may result in less accurate data.

Enter a minimum time for equilibration in the Minimum
equilibration delay at P/Po > = 0.995 field. This prevents premature equilibration which may be caused bysaturation.

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Adsorptive Properties
This dialog allows you to specify the characteristics of the gases used in the
TriStar system. An adsorptive properties file can be created as an independent
parameter file or as part of the sample information file.
If this is a new file, be sure to save it to the directory you specified as the Parameter Files directory to include it in the drop-down list of the Basic Sample Information dialog (see Parameter Files Directory in Chapter 8).

Adsorptive

If this is a new file, this field contains either the nameof the default adsorptive gas or blanks. Enter the nameof the adsorptive gas.
Maximum number of characters: 40 (alphanumeric)Feb 03

Mnemonic

The mnemonic name for the adsorptive gas; for example,
N2 for nitrogen, CO2 for carbon dioxide, etc.

Maximum manifoldpressure

The maximum gas pressure allowed in the manifold.

Non-ideality factor

Enter a factor to compensate for the forces of attraction
between molecules in a real gas.

Density conversion
factorEnter the density conversion factor. The density conversion factor is determined by obtaining the ratio of thegas volume (STP) to the liquid volume.

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Molecular crosssectional area

The molecular cross-sectional area.

Replace...

Allows you to replace the values in the current adsorptive properties file with those from another file. An“open file” dialog box is displayed so that you may seOKlect the desired file. Click; the values are copied into the new file automatically. You may edit thevalues in the new file; the file from which they were copied remains unchanged.

Psat vs t...

Displays the Psat vs. Temperature dialog for the adsorptive gas.

This table contains saturation pressures and their corresponding temperatures. The table may include as manyas ten entries; at least two are required.
Edit the table by moving the cursor to the desired saturation pressure or temperature and entering a different
value. Points always have to be in an ascending order. If
you try to add a point which is less than the previous
one, you will receive an error message.
InsertInserts a new row. A row is inserted above the selectedline; the cursor moves to the new line.
DeleteDeletes the selected row.

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Report Options
This dialog box allows you to specify report options for a new file or to edit anexisting one. A report options file can be created as an independent parameter fileor as part of the sample information file.
If this is a new file, be sure to save it to the directory you specified as theParameter Files directory to include it in the drop-down list of the Basic
Sample Information dialog (see Parameter Files Directory in Chapter 8).

Description

If you are editing an existing file, this field displays a description of the report options file. You may change thename if you wish.
If this is a new file, the default report options description
is displayed. Enter a name for this file.
Maximum number of characters: 40

Show report title

This option allows you to enter a title for your report.
If this is a new file, the title you specified as the default
is displayed. You can accept the default title or enter a
new one.
Maximum number of characters: 50
If you deselect this option, a title will not display on thereport.

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Show graphic

Select this option to have a graphic display above the report title. The graphic can be in a bitmap (bmp) or an enhanced metafile (emf) format. For example, you may
wish to display your company logo.
Click Browse... to choose the graphic, then enter theheight and width in the appropriate fields. This image
can also be edited from the report window.

Replace...

Allows you to replace the values in the current report options file with those from an existing file. An “open file”
dialog box is displayed so that you may select the deOK
sired file. Click; the values are copied into the
new file automatically. You may edit the values in the
new file; the file from which they were copied remains
unchanged.

Overlays

Displays the Graph Overlay Samples dialog.

Choose the sample files you wish to overlay onto
selected plots.
Click Browse... to the right of the sample [n] field tochoose a file. You may select up to eight files. Afterchoosing your file(s), be sure to select the “Overlay samples” option for each report type you plan to overlay. Refer to Chapter 4 for instructions on generating overlays.

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Selected Reports

Contains a list of available reports:•

Isotherm
BET Surface Area
• Langmuir Surface Area
• t-Plot• Alpha-S Method• f-Ratio Method• BJH Adsorption• BJH Desorption• Dubinin• MP-Method• Options Report• Summary Report• Sample Log Report•

You can find examples of these reports in Chapter 7.
Using the mouse pointer or the arrow keys, move to thedesired report and double-click the left mouse button, orpress Spacebar . A report is selected when it is precededwith a check mark. You may deselect it in the same manner.
Edit

Displays an associated dialog for the selected report. Editing options for available reports are shown in the following sections.
This button is disabled for some reports, such as the Options and Sample Log reports, since they do not containparameters which may be edited.

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Isotherm Report Options
The isotherm report indicates adsorption (up to saturation pressure) and desorption(down from saturation pressure) of a gas by a solid held at constant temperature.
Click Edit for Isotherm report options; the Isotherm Report Options dialog box
is displayed.

Select Reports

Allows you to choose the type of report you wish to generate. You may choose as many as you wish.
Choices: Tabular Report, Linear plot,
Logarithmic plot
If calculation assignments are not used, any outlier
points are included and marked in the analysis log report, but are not included in plots.

Plot Options

Choose which branch(es) of the isotherm you wish toplot.
Choices: Plot adsorption, Plot desorption

Linear/Logarithmic
Plot Options

Choose options for linear and logarithmic plots.
Choices: Plot curve, Plot points, Overlay samples
Autoscale x-axis, Autoscale y-axis

Overlay samples

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Select this option to overlay this plot with data fromother samples. The other samples are specified by selecting Overlays on the main Report Otions screen.

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Autoscale x-axis
Autoscale y-axis

Choose this option to have the x- and/or y-axes scaled
automatically. The lowest and highest values collectedduring analysis are used as the beginning and ending
points.
Deselect the autoscale options to specify beginning andending ranges; the corresponding From and To fields become enabled.
The X-axis shows the relative pressure.
The Y-axis shows the volume of gas adsorbed.

From/To fields

Feb 03Specify beginning and ending values for the x- and yaxes ranges when you choose not to autoscale data. Data
collected outside these ranges are not included in the plot.

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BET/Langmuir Surface Area Report Options•

The BET calculation obtains the sample surface area value by determining
the monolayer volume of adsorbed gas from the isotherm data.

•

The Langmuir calculation determines the surface area of a sample by relating the surface area to the volume of gas adsorbed as a monolayer.

Click Edit for BET (or Langmuir) surface area report options; the BET (orLangmuir) Surface Area Report Options dialog box is displayed.

Displays as Langmuir
Surface Area Report
Options if the Langmuirreport is being edited.

The Langmuir and BET Surface Area dialogs include the same fields; theoperating instructions for both are the same.

5-34

Tabular report

Select this option to have a tabular report of the plotteddata.

BET (or Langmuir)
Transform plot

Generates a traditional BET (Langmuir) surface area plotthat is used to determine monolayer volume and BET C
constant.

BET (or Langmuir)
Isotherm plot

Uses the BET (Langmuir) monolayer volume and constant to produce an isotherm.

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Overlay samples

Allows you to overlay data of the selected type from thecurrent plot with data from other samples. The other samples are selected by clicking Overlays on the main Report Options screen.

Autoscale x-axis
Autoscale y-axis

Select these options to have the X- and/or Y-axes scaled
automatically.
Both X- and Y-axes begin at zero; the system uses thehighest values collected during analysis as the ending
points. If you choose not to autoscale data, the Fromand To fields are enabled, allowing you to enter theranges.
The X-Axis Range fields show the relative pressure.
The Y-Axis Range fields show the quantity of gas
adsorbed.

From/To fields

Pressures

Feb 03

Enabled when you choose not to autoscale data (deselectthe Autoscale option), allowing you to specify the beginning and ending ranges of the X- and/or Y-axis. Data collected outside these ranges are not included in the plot.
The valus entered in the To field must be greater thanthe value entered in the From field.
Displays the Report Relative Pressure Table dialog sothat you may edit or enter relative pressure points.

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Pressures•

If Use calculation assignments is not selected on thecollected/Entered dialog, the isotherm is interpolated tothese pressure points, and those interpolated values areused in the BET calculations.

•

If Use calculation assignments is selected, collected
data are used.

(continued)

Insert predefined

Displays the Surface Area Report Pressure Selection dialog, allowing you to select predefined points.
Choices: None, 1 Point, 3 Point, 5 Point,
5 Point Low Pressure

5-36

InsertInserts a row into the table above the selected line; thecursor moves to the new line.

DeleteDeletes the selected row.

Clear

Removes all but the one required entry from the table.
The rows do not have to be selected. A warning message
requesting confirmation is displayed before the table iscleared.

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t-Plot Report Options
The t-Plot calculation allows quantitative analysis of the area and total volume ascribed to micropores. Matrix area, the area external to micropores, is directly determined and often proves to be a valuable way of chacterizing complex mixedmaterials. Click Edit for t-Plot report options; the t-Plot Report Options dialog
is displayed.

Thickness Curve

Presents the type of thickness curves available.
•

HalseyHarkins-Jura• Carbon Black STSA
• Broekhoff-de Boer
• User-Defined•

You can also apply the Frenkel-Halsey-Hill thickness
curve using the Halsey option, and entering the appropriate values in the equation. Use Edit to edit the values
in the equation.
Edit

Feb 03

Displays the equation for the type of thickness curve
selected so that you may view or edit the values.

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Halsey

Displays the Halsey Thickness Equation dialog.

You can edit the values for the multiplier, numerator, andexponent.
Refer to Appendix C, Calculations, for more information.
Harkins-Jura

Displays the Harkins-Jura Thickness Equation dialog.

You can edit the values for the numerator, first elementof the denominator, and exponent.
Refer to Appendix C, Calculations, for more information.
Carbon Black
STSA

Displays the STSA Thickness Equation dialog.

All coefficients can be edited.

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Broekhoff-de Boer Displays the Broekhoff-de Boer equation dialog.

You can edit the values for the multiplier, numerator, andexponent.
Refer to Appendix C, Calculations, for more information.
User-Defined

Displays the Entered t-Curve dialog allowing you to define a t-curve by entering the relative pressure and thickness values.

This table can also be created in another application if
desired and imported into this dialog using Open .
When creating the table in another application, the file
must be saved as ASCII text with a. THK extension.
Use a two-column format with the relative pressures in
the first column and the thickness values in the second
column. Columns must be separated by a space (or a tab).

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Open

Allows you to import the values from an existing thickness curve (THK) into this table. One predefined curveis shipped with the analysis program and is found in the
Referenc directory. The Referenc directory is defaulted
when you select this push button.
After the values are copied into the table, you may edit
them if desired. Editing these values will not affect thefile from which they were copied.

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Save asEnables you to save the current table of values under afile name.

Clear

Clears the table of all but one entry; one entry is required.

Surface Area
group box

Allows you to choose the surface area value used forthickness calculations. You can use BET (most commonlyused), Langmuir, or enter one of preference.

Pressure range

Displays the Report Relative Pressure Range dialog sothat you may specify minimum and maximum relative
pressures to use with this report.

•

If Use calculation assignments is not selected on theCollected/Entered dialog, all of the nonoutlier pointsof the collected data within the specified range areused for calculating the data for this report..

•

If Use calculation assignments is selected, collected
data points which are assigned to this report type areused.

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Fitted Thickness
Range

Provides two fields, allowing you to enter the minimum
and maximum thicknesses you wish to include in the
thickness curve.

The values entered for the thicknesses can be expressed in angstroms or
nanometers. Select Data presentation from the Options menu to specify desired units.
Surface area
correction factor

This value corrects for surface areas that are not smoothand brings the values for BET surface area and micropore surface area into accordance. For most samples, thedefault value of 1.000 is adequate.

Tabular report

Select this option to have a tabular report generated.

t-PlotSelect this option to have a graphical representation ofdata.

Overlay samples

Allows you to overlay data from the current sample filewith data from other sample file(s). The other sample
file(s) are chosen by clicking Overlays on the main Report Options screen.

Autoscale x-axis
Autoscale y-axis

Select these options to have the X- and/or Y-axes scaled
automatically.
Both X- and Y-axes begin at zero; the system uses thehighest values collected during analysis as the ending
points.
If you choose not to autoscale data, the From and To
fields are enabled, allowing you to enter the ranges.

From/To fields

Enabled when you choose not to autoscale data (deselectthe Autoscale option), allowing you to specify the beginning and ending ranges of the X- and/or Y-axis. Data collected outside these ranges are not included in the plot.
The value entered in the To field must be greater thanthe value entered in the From field.
••

Feb 03

The X-Axis Range fields show the relative pressure
The Y-Axis Range fields show the quantity of gas
adsorbed.

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Alpha-S Plot

The Alpha-S plot converts the standard adsorption isotherm into a dimensionless
isotherm using the quantity adsorbed at a relative pressure of 0.4.
Table

Provides two columns for entering the relative pressure(first column) and the alpha-s values (second column).
This table can also be created in another application if
desired and imported into this dialog using Open .
When creating the table in another application, the file
must be saved as ASCII text with an ALS extension. Use
a two-column format with the relative pressures in thefirst column and the alpha-s values in the second column. Columns must be separated by a space (or a tab).

Open

5-42

Allows you to import the values from an existing alpha-s
curve (ALS) into the table. One predefined curve isshipped with the analysis program and is located in the
Referenc directory. The Referenc directory is defaulted
when you click this push button. After the values are copied into the table, you may edit them if desired. Editingthese values will not affect the file from which they
were copied.

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TriStar 3000

Open

Save asEnables you to save the current table of values under afile name.

Clear

Clears the table of all entries.

Fitted alpha-S Range

Provides two fields for entering the minimum and maximum relative pressures from which the fit will be determined.

Relative pressure
range

Provides two fields for entering a pressure range whencalculation assignments are not used.

Tabular report

Choose this option to have a tabular report generated

Alpha-S Plot

Choose this option to have the data plotted as a graph.

Overlay samples

Allows you to overlay data from the current sample filewith data from other sample file(s). The other sample
file(s1 are chosen by clicking Overlays on the main Report Options screen.

Autoscale x-axis
Autoscale y-axis

Select these options to have the X- and/or Y-axes scaled
automatically.
Both X- and Y-axes begin at zero; the system uses thehighest values collected during analysis as the ending
points.
If you choose not to autoscale data, the From and To
fields are enabled, allowing you to enter the ranges.

From/To fields

Enabled when you choose not to autoscale data (deselectthe Autoscale option), allowing you to specify the beginning and ending ranges of the X- and/or Y-axis. Data collected outside these ranges are not included in the plot.
The valus entered in the To field must be greater thanthe value entered in the From field.
••

Feb 03

The X-Axis Range fields show the relative pressure.
The Y-Axis Range fields show the quantity of gas
adsorbed.

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f-Ratio Plot

The f-Ratio report allows you to take the measured isotherm and normalize it using a reference isotherm.

5-44

Reference Isotherm

Displays the sample file you choose as a reference. You
should always choose a file containing an isotherm measured from a non-porous sample of the same material as
the current sample.

Browse...

Click to choose the sample file you wish to use as areference for the isotherm.

Relative pressure
range

Allows you to enter a pressure range when calculations
assignments are not used.

Tabular report

Choose this option to have a tabular report generated
The tabular report contains four columns: relative pressure, quantity adsorbed for the isotherm of interest, quantity adsorbed for the reference isotherm, and the ratio of
the quantities adsorbed.

t-PlotChoose this option to have the data plotted as a graph.

Overlay samples

Allows you to overlay data from the current sample filewith data from other sample file(s). The other sample
file(s) are chosen by clicking Overlays on the main Report Options screen.

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Autoscale x-axis
Autoscale y-axis

Select these options to have the X- and/or Y-axes scaled
automatically.
Both X- and Y-axes begin at zero; the system uses thehighest values collected during analysis as the ending
points.
If you choose not to autoscale data, the From and To
fields are enabled, allowing you to enter the ranges.

From/To fields

Feb 03

Enabled when you choose not to autoscale the axis, allowing you to enter a range.

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BJH Adsorption/Desorption Report Options
Or BJH Desorption
Report Options

Not available on the
Desorption dialog.

The BJH Adsorption and Desorption dialog boxes include the same fields; theoperating instructions for both are the same.

The BJH calculation determines the mesopore volume/area distribution which accounts for both the change in adsorbate layer thickness and the liquid condensed
in pore cores. You can generate BJH reports from both adsorption and desorption
data.
Thickness Curve

The choices in this group box allow you to choose thetype of thickness curve you wish to use and change values of the equation, if desired.
Choices: Halsey, Harkins-Jura, Carbon Black STSA,
Broekhoff de Boer, and User-Defined
You must choose an equation for the type of thickness
curve to be used.

An incomplete pore distribution may be generated if you select a thickness
curve which is not a good match for the sample being analyzed.

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Edit

Displays the equation for the type of thickness curve selected. Refer to the previous section, t-Plot Report Options, for an explanation of this push button.

Minimum BJH(diameter, radius,or width)

Enter the minimum diameter (or radius) of pores you
wish to have included in the BJH reports. The value entered in this field must be less than the value entered in
the Maximum BJH field.

Maximum BJH(diameter, radius,or width)

Enter the maximum diameter (or radius) of pores you
wish to have included in the BJH reports. The value entered in this field must be greater than the value enteredin the Minimum BJH field.

Fraction of pores
open at both ends

During adsorption calculations, the software assumes thatall pores are closed at one end. Sometimes a percentage
of pores may be open at both ends, causing disagreementin the adsorption and desorption data or in the values for
total volume and total BJH pore volume. In this field,
you may enter the fraction of pores open at both ends tocompensate for this error.
•

Adsorptive

This field is not shown on the BJH Desorption Report
Options dialog.

Displays the BJH Adsorptive Options dialog.

The recommended adsorptives and their values areshown. You may specify up to six additional adsorptive/adsorbate property factor combinations.

Feb 03

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Adsorptive(continued)

The adsorbate property factor is the combination of constants in the numerator of the BJH equation which is specific to the type of gas used. Adsorbate property factors
may be specified in angstroms or nanometers. SelectOptions, Data presentation from the main menu to specify units.

Smooth differentials

Smooths all differential calculations, eliminating variations in the differential computation caused by noise in
the input data.

Pressure range

Displays the Report Relative Pressure Range dialog sothat you may enter the range of pressures to use withthis report.

Selected Reports•

If Use calculation assignments is not selected on theCollected/Entered dialog, all of the non-outlier pointsof the collected data within the specified range areused for calculating the data for this report•

If Use calculation assignments is selected, collected
data points which are assigned to this report type areused.

Contains a list of available BJH reports:•

Tabular Report
Cumulative Pore volume• dV/dW, dV/dD, or dV/dR Pore Volume• dV/dlog(W), dV/dlog(D) ,or dV/dlog(R) Pore volume• Cumulative Pore Area
• dA/dW, dA/dD,or dA/dR Pore Area
• dA/dlog(W), dA/dlog(D), or dA/dlog(R) Pore Area•

You can measure pore width (w), pore radius (R), or pore diameter (D) for
BJH reports. Select Options, Data presentation from the Main Menu to choose
the desired measurement

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Selected Reports(continued)

Edit

Choose a report by double-clicking on the report nameor highlight the report name and press the Spacebar . A
report is selected when it is preceded with a check mark.
Reports are deselected in the same manner.
Allows you to edit the selected report. Editing options
for available reports are shown in the following sections.

Tabular Report
Select Edit for the BJH Adsorption/Desorption tabular report to specify themethod of data reduction; the BJH Adsorption (or Desorption) Tabular Report
Options dialog box is displayed.

Feb 03Fixed poresize table

Specify exact pore sizes for which volume or area data
are reported. Only the pore sizes within the specified
range are reported. Select to enter or edit a fixed poresize table.

Collected points

Includes all relative pressure points collected by thesystem.

Columns...

Displays the BJH Adsorption (or Desorption) Tabular Report Column Options dialog.

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Columns...

(continued)

Table...

The default column title appears next to the column number. Each column includes a pull-down list of the datatypes available for inclusion in the report. You can measure pore width, pore radius, or pore diameter.
Enabled when you choose Fixed pore size table. Displays the BJH Adsorption (or Desorption) Fixed Pore
Size Table dialog so that you may enter or edit a fixedpore size table.

The fixed pore size table must contain a minimum of
two points and may include as many as 1000. The points
must be strictly decreasing.

5-50

InsertInserts a row into the pressure table. The row is inserted
above the selected row and the cursor moves to the newrow.

DeleteDeletes the selected row from the pressure table.

Clear

Clears all points from the pressure table; none have to be
selected.

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Plot Options
Click Edit for BJH Adsorption/Desorption plots to specify plotting methods
and to customize plots. The following plots are available:
A dialog box similar to the following is displayed when you select a BJH plot.

Valid ranges display here.

Plot Options

Lists the data presentation styles available for BJH plots.
You may choose to plot as a curve, points, or both.

X-axisLists the scale options for the x-axis.

Linear/Logarithmic

Choose whether you wish to have the X-axis on a logarithmic or linear scale.

Autoscale

Select this option to have the x-axis scaled automatically.
The lowest and highest values collected during analysis
are used as the beginning and ending points.
When you deselect this option, the adjacent fields are enabled so that you can specify beginning and ending
values.
Data ranges are displayed in the information bar acrossthe bottom of the dialog box when a cursor is in a numerical data field.

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Y-axisLists the options for the y-axis.

Variable

Choose the desired variable for the Y-axis.

Overlay

Displays a list of overlay choices. You may choose tooverlay the current plot with data from other samples orwith other plots from this sample.

Autoscale

Select this option if you wish to have the y-axis scaled
automatically. The lowest and highest values collectedduring analysis are used as the beginning and ending
points.
When you deselect this option, the adjacent fields are enabled so that you can specify beginning and ending
values.
Data ranges are displayed in the information bar acrossthe bottom of the dialog box when the cursor is in a numerical data field..

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Dubinin Report Options

Report Type

Allows you to specify the type of report you wish to generate. At least one type of report must be selected.
Select Radushkevich to generate the Radushkevich
report.
Select Astakhov to generate the Astakhov report. With
this choice, you may select Optimize exponent. If you
do not select this option, the Exponent value field is enabled so that you can enter a value.
Refer to Appendix C, Calculations, for additional
information.

Fitted relative
pressure range

Allows you to specify minimum and maximum limits on
relative pressures included in the line fit. Data collected
outside these limits are not included in the line fit.

Selected Reports

Lists the available Dubinin reports. Choose a report by
double-clicking on the report name or highlight the report name and press the spacebar. A report is selected
when it is preceded with a check mark ().
The following reports are available:•

Tabular Report
Transformed Isotherm• dV/dW Pore Volume (Astakhov only)•

Feb 03

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TriStar 3000

Adsorptive

Allows you to specify up to ten adsorptive/affinity coefficient (beta) combinations. The Dubinin Adsorptive Options dialog is displayed.

Pressure range

Displays the Report Relative Pressure Range dialog sothat you may specify minimum and maximum relative
pressures to use with this report.
•

If Use calculation assignments is not selected on theCollected/Entered dialog, all of the nonoutlier pointsof the collected data within the specified range areused for calculating the data for this report..

•

If Use calculation assignments is selected, collected
data points which are assigned to this report type areused.

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Tabular Report Options
Selecting Tabular Report from the Dubinin Report Options dialog box enables
you to customize your report with one to six columns of data for Astakhov reports and one to five columns of data for Radushkevich reports. The Dubinin
Tabular Report Column Options dialog is displayed.

The default column title appears next to the column number. Each column includes a drop-down list of the data types to include in the report.
*The value for n (shown in Column 5) is the optimized exponent if Optimized
Astakhov exponent is selected on the Dubinin Report Options dialog box. If not,then the value for n is the entered exponent value.

Oct 99

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Transformed Isotherm Plot Options
Selecting Transformed Isotherm from the Dubinin Plot Option dialog enables you
to restrict the line fit to a portion of the isotherm. The Dubinin Transformed Isotherm Plot Options dialog box is displayed.

Overlay Samples

Select this option to overlay the current plot with datafrom other samples. Then click Overlays on the Report
Options dialog to choose the sample files.

Autoscale x-axis
Autoscale y-axis

Select these options to have the X- and/or Y-axes automatically scaled. Both anes begin at zero; the system
uses the highest values collected during analysis as theending points for anes ranges.
If you choose not to autoscale data for either (or both)axis, the corresponding fields are enabled so that you
may enter a beginning and ending value.
•

The X-axis shows the quantity of gas adsorbed atstandard temperature and pressure.
• The Y-axis shows the log of relative pressure.
Data ranges are displayed in the information bar acrossthe bottom of the dialog when the cursor is in a numerical data entry field.

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Pore Volume Options
When you select dV/dW Pore Volume from the Dubinin Report Options dialog
box, the Dubinin dV/dw Pore Volume Options dialog is displayed.

Plot options

Choose to plot curve, points, or both.

Overlay Samples

Select this option to overlay data from other samples.
Then click Overlays on the Report Options dialog tochoose the files.

Autoscale x-axis
Autoscale y-axis

Select these options to have the X- and/or Y-axes automatically scaled. Both axes begin at zero; the system
uses the highest values collected during analysis as theending points.
If you choose not to autoscale data for either (or both)axis, the corresponding fields are enabled so that you
may enter a beginning and ending value. Data collected
outside these ranges are not included in the plot.
Data ranges are displaye din the information bar acrossthe bottom of the dialog when the cursor is in a numerical data entry field.

Feb 03

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MP-Method Report Options

Pore size can be expressed in Angstroms or nanometers. Select Data Presentation, Units from the Options menu to secify desired unit.

Thickness Curve

Equation

Harkins-Jura

Select the thickness curve type from this group box. You
must choose either the Halsey equation or the HarkinsJura equation. Use Equation to edit the values in theequation.
Displays the equation for the type of thickness curve
selected.
Displays the Harkins-Jura Thickness Equation dialog box.

You can edit the values for the numerator, first elementof the denominator, and exponent.

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Halsey

Displays the Halsey Thickness Equation dialog box.

You can edit the values for the multiplier, numerator, andexponent.
Refer to Appendix C, Calculations, for more information
Selected Reports

Lists the available MP-Method reports. Choose a reportby double-clicking on the report name or highlight the report name and press the spacebar. A report is selected
when it is preceded with a check mark ().
The following reports are available:•

Tabular Report
Cumulative Pore Volume• dV/dW Pore Volume• Cumulative Pore Area
• dA/dW Pore Area•

The data for these reports are measured in pore width
only.

Feb 03

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Tabular Report Options
Selecting Tabular Report from the MP-Method Report Options dialog box enables you to customize your report with one to six columns of data. (The datatypes in the first and second columns cannot be changed.) The MP-Method Tabular Report Column Options dialog box is displayed.

The default column title appears next to the column number for columns three
through six. Each of these columns includes a pull-down list of the data types toinclude in the report. The following data types are available:
Columns 1 and 2 are fixed and cannot be edited.
The MP-Method reports hydraulic radius only. If you select Pore size in diameter from the Data presentation menu, the MP-Method still reports poresize in radius.

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Plot Options
Selecting an MP-Method plot option from the MP-Method Report Options dialog
boxes enables you to specify the plotting method used for your report and to customize the plot. The following plots are available:
Cumulative Pore Volume
dV/dw Pore Volume• Cumulative Pore Area
• dA/dw Pore Area••

When you select any of these plots from the MP-Method Report Options dialog
box, a dialog box similar to the following one is displayed. The fields on all dialog boxes are the same.

Plot options

Choose to plot a curve, points, or both.

X-AxisChoose Autoscale x-axis to have the x-axis scaled automatically. The X-axis begins at zero and the system uses
the highest values collected during analysis as the ending
point.
If you deselect Autoscale, the corresponding fields areenabled so that you may enter a beginning and ending
value. Data collected outside these ranges are not included in the plot.
Data ranges are displaye din the information bar acrossthe bottom of the dialog when the cursor is in a numerical data entry field.

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Y-AxisVariable

Click on the down-arrow to choose a variable for the
Y-axis.

Overlay

You can use the choices in this drop-down list to overlay
plots. You can choose a different type of plot for the current sample to overlay with the listed Variable, or you
can choose Samples to overlay the variable plot with thesame type of plot from other samples. Click Overlays on
the Reports Options dialog box to choose the samples.

Autoscale

Choose this option to have the y-axis scaled automatically. Y-axes begin at zero. The system uses the highest
values collected during analysis as the ending points foraxes ranges.
If you deselect this option, the corresponding fields areenabled so that you may enter a beginning and ending
value. Data collected outside these ranges are not included in the plot.
Y-axis range fields show the volume of gas adsorbed.
Data ranges are displaye din the information bar acrossthe bottom of the dialog when the cursor is in a numerical data entry field.

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Summary Report
The summary report provides a condensed listing of data results. Click Edit
for Summary report options; the Summary Report Options dialog box is displayed.

The choices on this dialog box allow you to choose the types of data to include
in the Summary report.
If you choose Adsorption or Desorption total for Pore Volume data the P/Po
field is enabled so that you can enter the relative pressure at which to calculate
the total pore volume. If Use calculation assignments (Collected Data screen) is
not selected, the isotherm is interpolated to this value and that point used for the
Total pore volume calculation. Otherwise, the point selected with calculation assignment is used.

Feb 03

Select all

Selects all choices on the dialog box.

Deselect all

Deselects all choices on the dialog box..

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Options Report
The Options report is a subset of the contents report; it provides pertinent information for the following:
Sample tube
Degas conditions• Adsorptive properties• Analysis conditions• Free space• Po and temperature• Equilibration• Isotherm collection••

Sample Log Report
The Sample Log report displays the following:
Manual control operations performed during analysis
Information entered using Add Log Entry on the sample file editor• Warnings and/or errors which occurred during analysis
•
•

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Collected/Entered Data
This dialog is displayed only in the Advanced mode of the sample file presentation, and only after an analysis has been completed.

Pressure table

For collected data, columns for the following are displayed:•absolute pressure
relative pressure• quantity adsorbed• outliers (if Use calculation assignments is not selected)• calculation assignments for each requested report option (if Use calculation assignments is selected)•

For entered data, columns for the following aredisplayed:•absolute or relative pressure, depending on theselection in the Pressures group box• quantity adsorbed
InsertFeb 03

Enabled only for entered data. Inserts a row into the pressure table.

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DeleteEnabled only for entered data. Deletes the selected row.

Clear

Enabled only for entered data. Clears the entire table;rows do not have to be selected.

Use calculation
assignments

If selected, allows you to assign the points to be collected for each report type.
If deselected, each report (with the exception of Langmuir and BET) uses a range of pressures as selected in
the report options. The Langmuir and BET reports interpolate to entered relative pressures on the report options.
The outlier points can be selected so that they will not
be reported.

Po and T...

Displays the Po and T dialog.

This dialog box allows you to edit the Po measurement
and analysis bath temperature.

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OpenFree Space...

Displays the Free Space dialog, allowing you to edit freespace values.

This dialog also shows the isotherm for the analysis. The
isotherm is redrawn each time values are edited.
MeasureQuasi-Gemini

Either of these choices is enabled only if selected as themethod used in the original analysis.
If Quasi-Gemini was selected, Sample Tube... is enabled sothat you may edit the parameters of the sample tube usedas the balance in the Quasi-Gemini method.

Calculated

Select this option to have the free-space measurement calculated using the sample conditions and sample tube parameters.

Enter

Enables the Warm free space and Cold free space
fields so that you may enter the free space manually.
The warm free space is the sample tube gas capacity
measured at room temperature.
Range:
Default:

1.0000 to 999.0000 cm3
16.000 cm3

The cold free space is the sample tube gas capacity measured with the Dewar raised.
Range:
Default:

Feb 031.0000 to 999.0000 cm345.0000 cm3

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Save AsTriStar 3000

Save
Save enables you to save any changes you have made to the file in the active window. The file is saved under its current name.

Save As
Save As enables you to:

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•

save a sample or parameter file in the active window under a different
name. This option is useful for making a duplicate copy of a file that you
can modify as desired without changing the original one. The original fileremains open when you use this function, so be sure to open the new file
before making any changes.

•

save a subset (parameter) of the sample file in the active window as astandalone parameter file. For example, select Analysis Conditions from theSave As menu to create a standalone parameter file of the analysis conditions portion of the active sample file.

•save as an ASCII file the relative pressures and corresponding thicknesses.
These data are derived by dividing the condensed volume of adsorptive by
the selected surface area. The density conversion factor in the adsorptive
properties file is used to convert quantity adsorbed to volume of condensed
adsoptive.

•

save as an ASCII file the relative pressures and resulting quantities adsorbed. These data are derived by taking the isotherm and dividing it by
the quantity adsorbed at 0.4 relative pressure.

Feb 03

TriStar 3000

Save As

A dialog similar to the one shown below is displayed when you select the Save
As command.

Enter a file name (up to eight characters) in the File name field; the appropriateOKextension is appended automatically when you click. The new file issaved as specified, but does not remain in the active window. Be sure to open the
new file before making any changes to the file.
When saving Alpha-S files, the Save As t-Curve dialog box is shown first, allowing you to select the type of curve.

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TriStar 3000

Save All
Save All enables you to save all open files under their current names. This option
provides a faster way to save all open files at one time and avoids having to perform a Save operation on each individual file.

Close
Close enables you to close the file in the active window. The following message
is displayed if changes have been made to the file:(File name) has been changed.
Save changes before closing?
Yes

No

CancelYes saves any changes and closes the active window.
No discards any changes and closes the active window;.
• Cancel returns you to the open file.
••

Close All
Close All enables you to close all open files under their current names. The following message is displayed for each file in which changes have been made:(File name) has been changed.
Save changes before closing?
Yes

No

CancelYes saves any changes and closes the active window.
• No discards any changes and closes the active window.
• Cancel returns you to the open file.
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TriStar 3000

Print

Print
Print enables you to print the entire contents of a file. When you select File,
Print from the main menu, the following choices are presented:
Sample information• Sample tube
• Degas conditions• Analysis conditions• Adsorptive properties• Report options•

Regardless of which file type you select, a dialog box similar to the one shown
below is displayed.

File nameDates...

Files
Directories
Destination:

The name of the file you select from the Files: list box
is copied to this field.
This push button and the contents of these list boxes are
explained in Selecting Files in Chapter 3.

Contains a drop-down list of the available print destinations.
If you select Screen, Printer, or Printer/Plotter, the requested file is sent to that specified destination.

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Destination:(continued)

Settings, File name

5-72

If you select File, the requested file is converted to atext file which can be viewed with a text editor or othertext file manipulation tools. You also must enter a namein the File name field of the Settings group box (or accept the default).
Enabled only if you select File as the destination. A default name is displayed in the field, but you may enter a
new one if you wish.

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TriStar 3000

List

List
List enables you to generate a listing of the following information on a selected
sample or parameter file.
File name• Date the file was created• Time the file was created• File identification• File status•

The List dialog is common to all file types. The title bar displays the type of fileon which you have requested a list.

File name

If you select only one file from the Files: list box, thename is copied to this field. If multiple files are selected,
the last one selected displays in this field.

You may request a list of multiple files by holding down Ctrl
files. If no files are selected, a list is generated for all files.

Dates...

Files
Directories

Feb 03

while selectingThis push button and the contents of these list boxes are
explained in Selecting Files in Chapter 3.

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Destination

Contains a drop-down list of the available print destinations.
Choices: Screen, Printer, Printer/Plotter, FileIf you select File, enter a name in the File name field of
the Settings group box.

Settings, File name

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Enabled only if you select File as the destination. Entera name in the File name field.

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TriStar 3000

ExportExportExport allows you to copy the isotherm data in a sample information file and reformat it in an ASCII format acceptable to other programs, such as spreadsheets.
The output file consists of four columns containing the absolute pressure, relative
pressure, specific quantity absorbed, and the elapsed time.
You may select multiple files by holding downmouse button once on each file.

Ctrl

and clicking the left

Select File, Export from the main menu; the Export Sample File dialog box isdisplayed.

File nameDates...

Files
Directories

Feb 03The name of the file you select from the Files list box iscopied to this field.
This push button and the contents of these list boxes are
explained in Selecting Files in Chapter 3.

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Settings
Export Type
Destination

Fixed at Isotherm.
Contains a drop-down list of the available print destinations.
Choices: Screen, Printer, Printer/Plotter, FileIf you select File, the File name field is enabled.

File name

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Allows you to specify a name for your exported file, or
you may accept the default.

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TriStar 3000

Exit

Exit
Exit enables you to exit the TriStar analysis program. Select File, Exit from themain menu. Even if an analysis is in progress, it will continue until completion;
analysis data are collected and stored in an embedded controller.
•

If a window containing a modified file is open, the following message isdisplayed:
Modifications have been made to (file name).
do you want to save the modifications?
Yes

No

CancelYes saves any changes and exits the analysis program; No abandons any
changes and exits the analysis program; and Cancel returns you to theopen file.
•

If an analysis is in progress, the following message is displayed:
CAUTION: Sample analysis is in progress. If you exit
the program analysis will continue to completion, but thedata are not saved to disk until the program is restarted.
Do you want to exit the program?
YesNo

Yes exits the analysis program; No leaves the analysis program active andallows the analysis to finish
Although data are stored in an embedded controller when you exit the
program, data are not saved to disk in the control module until you reenter
the program and save the data. If a power failure occurs and the analyzer
does not have an Uninterruptible Power Supply (UPS), any unsaved data
are lost.
•

If a report is in progress, the following message is displayed:
CAUTION: Reports are being generated. If you exit the
program these reports will be canceled.
Do you want to cancel reports and exit the program?
YesNo

Yes cancels the reports and exits the analysis program; No leaves theanalysis program active and allows the reports to finish.

Feb 035-77

CHAPTER 6
UNIT MENU•

Description•

Sample Analysis•

QuickStart•

Enable Manual Control•

Show Instrument Schematic•Show Status•

Show Instrument Log•

Unit configuration•

Calibration

TriStar 3000

Description

UNIT MENUThe Unit menu contains the options for the operations which can be performed
with the TriStar 3000. The main menu will contain a Unit menu for each attachedanalyzer. For example, if you have two attached analyzers, the main menu contains two Unit menus. For easy differentiation, the status displays associated witheach unit are displayed in different colors. The unit number and the serial number
also are displayed in the title bar of the operational windows. This is especiallyconvenient if you have more than one analyzer attached to the same control module.
This menu does not appear on the menu bar if the analysis program is being
used for offline data operations on a computer other than the one controllingthe analyzer.

Description

Listed below are brief descriptions of the Unit menu options. Detailed descriptions are found later in this chapter.

Feb 03Sample Analysis

Allows you to perform up to three analyses using different analysis conditions.

QuickStart

Allows you to perform multiple sample analyses using
the same analysis conditions, allowing you to create sample files at the time of analysis.

Enable ManualControl

Allows you to control the system manually.

6-1

Description

6-2

TriStar 3000

Show Instrument
Schematic

Displays the analyzer’s schematic.

Show Status

Displays the status window.

Show Instrument
Log

Displays a log of recent analyses, calibrations, and error
messages.

Unit Configuration

Displays software version, hardware configuration, andcalibration information. Also allows you to enter mnemonic names for port gases.

Calibrate

Allows you to calibrate the manifold temperature, thepressure scale, pressure offset, manifold volume, andservo valve. It also allows you to save calibration files aswell as load previously saved files.

Service Test

Enables you to perform certain troubleshooting procedures. This option is enabled only with the direction of a
Micromeritics service representative.

Feb 03

TriStar 3000

Sample Analysis

Sample Analysis
Use this mode of operation to schedule analyses which have different analysis conditions or report options. You may schedule up to three analyses at a time, depending on the number of ports you have available. All three ports are available forsample analyses if you are not using:••port 2 for a Quasi-Gemini measurement
port 3 for a continuous Po measurement

You can continue to schedule analyses by clicking Next>> (appears after the firstseries of analyses are finished) on the analyzing view of the Analysis dialog.
Select Sample Analysis from the Unit menu to display this view of the Analysis
dialog box.

View

Allows you to choose the view you wish to display inthe window.
Choices:

Operation, Instrument Schematic,
Instrument Log

Operation displays the current mode of operation.
Instrument Schematic displays a schematic of the TriStar
system. Refer to Show Instrument Schematic later inthis chapter for additional information.
Instrument Log displays a list of recent analyses, calibrations, and errors or messages. Refer to Show Instrument
Log later in this chapter for additional information.

Feb 036-3

Sample Analysis

Port [n]TriStar 3000

This field is blank until you choose a file to use for theoperation on this port.
•

If port 2 is being used for a Quasi-Gemini free-spacemeasurement, a message stating so is displayed.

•

If port 3 is being used to measure the Po, a message
stating so is displayed.

SampleDisplays an identification of the sample file.

Mass

Enter a value for the sample mass.
This field is not shown for ports 2 and 3 when:••

Density

Port 2 is being used for a Quasi-Gemini measurement.
Port 3 is being used for a Po measurement.

Displays the density of the sample specified in the sample information file.
This field is not shown for ports 2 and 3 when:••

Browse...

Port 2 is being used for a Quasi-Gemini measurement.
Port 3 is being used for a Po measurement.

Click to:•Select a sample information file when using the port
for an analysis; the Open Sample Information dialog isdisplayed.

•

Select a sample tube file when using the port for a
Quasi-Gemini measurement; the Open Sample Tube dialog is displayed.

The file name you select is copied to the Port [n] field.
Clear

6-4

Clears the information displayed for this port.

Po

Enabled if you have selected Entered for the Po measurement for at least one file. Enter the Po value, or edit thecurrent one.

Bath temperatureEnter the temperature for the analysis bath.

Feb 03

TriStar 3000

Sample Analysis

Report after analysis...

Start

Allows you to have a report generated automatically after
the analysis; displays the Report Settings dialog so thatyou may specify output options.

Starts the analysis; displays an analyzing view of theAnalysis dialog box.

Port Activity

Status Window

This view also displays port activity as well as the statuswindow.

Feb 036-5

Sample Analysis

6-6

TriStar 3000

Skip

Skips an analysis; visible only when an analysis is in progress. The Skip dialog is displayed so that you may
choose the port(s) containing the analysis you wish to
skip.

Suspend

Suspends an analysis; visible only when an analysis is inprogress. A dialog similar to the one shown above is displayed so that you may choose the port(s) containing theanalysis you wish to suspend.

ResumeResumes a suspended analysis; visible only when an
analysis is suspended. A dialog similar to the one shown
above is displayed so that you may choose the port(s)containing the analysis you wish to resume.

Report Port [n]These push buttons allow you to generate reports ondata collected at that time for the sample in the respective port. The reports are printed to the screen only.

Close Valves

Enabled when analysis is complete, allowing you toclose all sample port valves immediately; otherwise thevalves close in approximately five minutes.

CancelCancels an analysis; enabled only when an analysis is inprogress. A dialog similar to the one shown above is displayed so that you may choose the port(s) containing theanalysis you wish to cancel.

Start

On this view of the Analysis dialog box, this push buttonchanges to Next>> when analyses are finished.

Next>>

Returns you to the first view of the Analysis dialog box
so that you may schedule additional analyses.

Close

Closes the Analysis dialog.

Feb 03

TriStar 3000

QuickStart

QuickStart
Use this mode of operation to analyze samples of the same type using the same
analysis conditions, adsorptive properties, and report options. You may schedule
up to three analyses at a time, depending on the number of ports you have available. All three ports are available if you are not using:••port 2 for a Quasi-Gemini measurement
port 3 for a continuous Po measurement

You can continue to schedule analyses by clicking Next>> (appears after the firstseries of analyses are finished) on the analyzing view of the Analysis dialog.
When you select this option from the Unit menu, the QuickStart dialog box is displayed.

View

Click the down arrow to choose the view you wish tohave displayed in the window.
Choices:

Operation, Instrument Schematic,
Instrument Log

Operation displays the current mode of operation.
Instrument Schematic displays a schematic of the TriStar
system. Refer to Show Instrument Schematic later inthis chapter for additional information.
Instrument Log displays a list of recent analyses, calibrations, and errors or messages. Refer to Show Instrument
Log later in this chapter for additional information.

Feb 03

6-7

QuickStart

TriStar 3000

Sample Options

This group box provides drop-down lists of previously defined files (including any you may have created) foranalysis conditions, adsorptive properties, and report options. Choose a file from each list to be used in the sample files for this series of analyses.

Report Options

This group box allows you to have a report generated after each analysis. You may also specify the number of reports you want and a destination. If you choose File as adestination, the File name field is enabled. You can accept the default name or enter a new one.

Next>>

Advances you to the second view of the QuickStart dialog.

The second view of the QuickStart dialog allows you to specify sample information for this set of samples.

Port [n]6-8This field is blank until you choose a file to use for theoperation on this port.
•

If port 2 is being used for a Quasi-Gemini free-spacemeasurement, a message stating so is displayed. No
other fields are available for this port.

•

If port 3 is being used to measure the Po, a message
stating so is displayed. The Sample Tube field andBrowse... are shown so that you can select a file.

Feb 03

TriStar 3000

QuickStart

SampleDisplays the identification of the sample file.

Sample Tube

Select the sample tube file you wish to use with thisanalysis.

Mass

Enter a value for the sample mass.
This field is not shown for ports 2 and 3 when:••

Density

Port 2 is being used for a Quasi-Gemini measurement.
Port 3 is being used for a Po measurement.

Displays the density of the sample specified in the Analysis conditions file.
This field is not shown for ports 2 and 3 when:••

Browse...

Clear

Feb 03

Port 2 is being used for a Quasi-Gemini measurement.
Port 3 is being used for a Po measurement.

Click to display:•

The Open Sample Information File dialog (if using theport for an analysis), allowing you to create a file forthe analysis on the current port. The analysis conditions, adsorptive properties, and report options selectedon the previous screen are used.

•

The Open Sample Tube dialog (if using the port for a
Quasi-Gemini measurement), allowing you to select asample tube file.

Clears the information displayed for this port.

Po

Enabled if you have selected Entered for the Po measurement. Enter the Po value you wish to use if it has not already been entered, or if you wish to change it.

Bath temperatureEnter the temperature of the analysis bath.

6-9

QuickStart

TriStar 3000

Start

Starts the analysis; displays an analyzing view of theAnalysis dialog box.

Port Activity

Status Window

This view contains data collection for each analysis, aswell as port information. Refer to the previous section
for an explanation of the push buttons contained on this
dialog.
When analyses are complete, the second view of the dialog again is displayed, allowing you to quickly start thenext set of samples.

6-10

Feb 03

TriStar 3000

Enable Manual Control

Enable Manual Control
Select this option to control certain components of your system manually. The instrument schematic must be visible to use this option. If it is not visible, selectShow Instrument Schematic.

Servo Valve
Elevator

When manual control is enabled, the valve symbols change color on the monitor
screen to indicate their status.
••

Green = open
Yellow = closed

Use the mouse to move to the desired component and click the left mouse button
once to select it.
Each component that can be actuated has a shortcut menu displaying the operations available for that particular component. These menus may be accessed by selecting the desired component, then clicking the right mouse button once, orpressing ↑ Shift F9 .
The options available for the components on the instrument schematic are:Valves 1 through 13

Open, Close, Pulse
Open and Close open and close the valves. You may also
open and close the valves by double-clicking on thevalve or by pressing Spacebar while the valve is selected.

Feb 03

6-11

Enable Manual Control

Valves 1 through 13(continued)

Servo Valve

TriStar 3000

Pulse quickly turns the valve on and off, allowing the operation to proceed in small increments. You may also
pulse the valve by pressing P while the valve is selected.
Set, Close
Set displays the Servo Valve Settings dialog so that you
may choose to dose or evacuate and specify a target pressure. You may also display this dialog by pressing
Spacebar while the servo valve is selected.

Close closes the servo valve. You may also close theservo valve by pressing Spacebar while the servo valve
is selected.
Elevator

Raise, Lower, Stop
Raise and Lower raise and lower the elevator. You may
also raise and lower the elevator by double-clicking in
the elevator area or pressing Spacebar while the elevatorarea is selected.
Stop stops the elevator at its current position. You may
also stop the elevator by double-clicking in the elevatorarea or pressing Spacebar while the elevator area is selected.

6-12

Feb 03

TriStar 3000

Show Instrument SchematicShow Instrument Schematic
Select this option to display a schematic of the analyzer. Refer to the previous section for an explanation of the components contained on the instrument schematic.
Even if manual control is not enabled, you still can determine the state of thevalves by their color.
••

Green = open
White = closed

If you wish to change the state of a valve, you must enable manual control.

Feb 03

6-13

Show Status

TriStar 3000

Show Status
Select this option to show only the status window of the analyzer.
If you have multiple instruments attached to your control module, the statusbar for each instrument is displayed in a different color.

The status window shows the current status for each port.
You may wish to use this option if:

6-14

•

You have an automatic operation in progress and you wish to edit a sample
file. This way, you can keep up with the status of your operation while performing another task.

•

You have multiple units attached to your control module. You can selectShow Status on each unit menu and have the status for all units displayed
at one time.

Feb 03

TriStar 3000

Show Instrument Log

Show Instrument Log
Displays a log of recent analyses, calibrations, and errors or messages. By default,
this information is logged for a 7-day period for analyses and a 30-day period formessages and calibrations. You may change the time for which this information isretained in the Unit section of the WIN3000.INI file.

You can choose the type of information to display in the window by selecting
only the desired item(s). For example, select only the Calibration option to display calibration information:

Feb 03

6-15

Show Instrument Log

TriStar 3000

AnalysisCalibration
Message

These options allow you to choose which entries are displayed in the window.

Report...

Displays the Log Report Settings dialog so that you canspecify report output options.

Use the Start Date field to specify a date at which tostart the printout. You can specify a date using one of
the following methods:•

Highlight the field (or press F2 to clear the field) andtype in the desired date•

Double-click in the field (or press F4 ) to display acalendar to choose a date•Press F2 to clear the field, then F3 to insert the current date

Select the number of reports desired in the Number ofReports field; you may print up to 4. This field is disabled if you are printing to a File or to the Screen.
Choose the report destination in the Destination field. If
you choose File as the destination, the File name field isenabled, allowing you to enter a name for the printed
file (or you may accept the default).

6-16

Feb 03

TriStar 3000

Unit Configuration

Unit Configuration
Select this option to display hardware/software configurations, calibrations, andgas selections of the connected analyzer. When you select this option from theUnit menu, the Unit Configuration dialog box is displayed.

Feb 03

Configuration

Displays the number of the port being used to control
the analyzer and the serial number of the selected analyzer.

Software Versions

Displays the software versions of the MICBIOS, controller, and TriStar 3000 analysis program.

Gas Selections

Allows you to specify the mnemonic names for the analysis gas(es). Valves 8 and 9 are designated for the analysis gas. Valve 7 displays the free-space gas; this fieldcannot be edited.

Servo Valve

Displays the date the servo valve was last calibrated.

Calibrationgroup boxes

The remaining group boxes display calibration information for their respective component.

6-17

Calibration

TriStar 3000

Calibration
This option allows you to calibrate the manifold temperature, pressure scale, zeropressure, servo valve, and system volume. You can also save the current calibrations to a file or load a different calibration file. Refer to Chapter 9 for step-bystep instructions for each calibration procedure.

Temperature
Use this option to adjust the offset of the manifold temperature sensor to agreewith a value obtained using a calibration device. The Calibrate Manifold Temperature dialog is displayed so that you may enter the measured value.

6-18

Feb 03

TriStar 3000

Calibration

Pressure Scale
Use this option to adjust the scale of the pressure transducers. The Calibrate
Pressure Scale dialog is displayed.

This dialog allows you to adjust the scale by entering a value obtained using apressure gauge, as well as specifying which transducer(s) are at that pressure.

Zero Pressure
Use this option to evacuate the manifold and zero the selected transducers. The
Calibrate Pressure Offset dialog is displayed.

Choose the transducer(s) you wish to have offset to zero. Click Start and a dialog indicating evacuation is in progress is displayed. When evacuation is complete, the dialog closes automatically.

Feb 036-19

Calibration

TriStar 3000

Reset Pressure Calibration
Use this option to restore factory calibration settings for all transducers; a warning dialog is displayed.

Click
Cancelto restore the values; current values will be overwritten. Clickto retain current values.
OK

Servo Valve
Use this option to calibrate the servo valve to the manifold pressure transducer.
The servo valve should always be recalibrated after a pressure calibration has
been performed. The Calibrate Servo Valve dialog is displayed.

The only action required here is to click Start . The servo valve is then used tofill and equilibrate the manifold, first to 100 mmHg and then to 760 mmHg. The
pressure transducer readings (previously calibrated) at these points are used to calibrate the servo set point. Status messages are displayed during this procedure,then the dialog closes automatically.

6-20

Feb 03

TriStar 3000

Calibration

VolumeUse this option to calibrate the system volume. The Calibrate Volume dialog is displayed so that you may specify how you want the volume calibrated.

Displays as Next>> if
you choose Measured.

Previous

Retains the current system volume which is displayed to
the left of this choice.

EnteredEnter a value to use for the system volume.

Measured

Allows you to measure the system volume using an entered reference volume.

Done

Closes the dialog; displays for the Previous and Enteredselections.

Next>>

Advances you to the next view of the Calibrate Volume
dialog; displays for the Measured selection.
This view of the Calibrate Volume dialog allows you toenter the parameters required when using a reference volume to calibrate the system volume.

Feb 036-21

Calibration

TriStar 3000

Reference Volume

Enter the volume of the reference device.

Reference Volume
Temp.

Enter the temperature of the reference volume.

Perform
measurement

Enter the number of measurements you wish to make.

Thermalequilibration time

Enter the amount of time you wish to have the gas
equilibrate in the reference volume before taking the pressure measurement.

Start

Begins the calibration; a status view is displayed. Afterthe calibration has finished, a confirmation view is displayed.

This dialog allows you to confirm the calculated volume.
The Measured field contains the value of the last measurement; for example, the value for the third measurement is shown if you selected three measurements. The
Average field contains an average of the number of selected measurements. This dialog also gives you the opportunity to return to the Previous or Entered value.
Click

6-22

Done

to close this dialog.

Feb 03

TriStar 3000

Calibration

Save to FileUse this dialog to save the current calibration settings to a file. The Select Calibration File dialog is displayed.

File nameDefaults to the current date. You can enter a different
name if you wish.

Load from File
Displays the Select Calibration File dialog (shown above) so that you can load adifferent calibration file.

Feb 036-23

CHAPTER 7
REPORTS MENU•

Description•

Start Report•

Cancel Reports•

DFT Plus•

Printed Reports•

Sample Reports

TriStar 3000

Description

REPORTS MENUThis chapter describes the commands on the Reports menu; it also contains examples of reports.
Reports can be generated for data:•collected on a sample that has completed analysis
collected on a sample that is currently being analyzed (includes only the information collected up to the time of the report)• that is manually entered•

Description

Listed below are brief descriptions of the commands contained on the Reports
menu. Detailed descriptions follow this section.
Start report

Allows you to generate a report on a completed sample
analysis or on the data collected thus far for an analysis
in progress.

Close reports

Closes all open report window(s).

DFT Plus

Invokes the DFT Plus program, allowing you to generate
DFT Plus reports.
This option is functional only if the DFT Plus programis installed.

Feb 03

7-1

Start Report

TriStar 3000

Start Report
Select this option to generate a report on a sample analysis. Select Start reportfrom the Reports menu to display the Start Report dialog.

File name

7-2

The name of the sample file you select from the Files
list window is copied to this field. If you select multiple
files, the last one selected is displayed. If you have asample file open, its name defaults to this field.
•

If you select multiple files on which to have reports generated, the reports specified in each sample file areprinted to the output destination.

•

If you choose a single file, the Select Reports dialog containing the available reports is displayed. This dialog allows you to choose the reports you wish to generate.
Refer to Chapter 5 for information on available reports.

Feb 03

TriStar 3000

Start Report

File name(continued)

StatusSelect (or deselect) reports by double-clicking on the desired report (reports are selected when they are precededwith a check mark). Alternatively, you can hightlight thereport and press the Spacebar .
This drop-down list determines what type of sample files
are displayed in the Files list window in the specified directory for all dates, or within the specified range ofdates (using Dates... push button).
Choices:All, Analyzing, Complete, Entered

All displays all types of samples files (Analyzing, Complete, and Entered).
Analyzing displays sample files that are currently being
used in an analysis.
Complete displays sample files that have been used in ananalysis.
Entered displays sample files that contain maually entered data.
Dates...

Displays the Select Dates dialog so that you may specify
a range of dates. Refer to Selecting Files in Chapter 3
for a description of this push button.

CopiesEnabled when the Printer or Printer/Plotter destinationis chosen. This option allows you to print up to four copies of the selected report(s).

Destination

Displays a drop-down list of output destinations.
Choices:File, Printer, Printer/Plotter, Screen

If you select Printer or Printer/Plotter, requested reports
are printed to the selected printer and/or plotter. This option also enables the Copies field allowing you to print
up to four copies of each report.
If you select Screen, reports are displayed onscreen. Using this option allows flexibility for manipulating and customizing reports. Refer to Printed Reports later in thischapter.

Feb 037-3

Start Report

TriStar 3000

Destination(continued)

7-4

If you select File, the tabular reports of the requested
file are converted to a text file which can be viewed witha text editor or other text file manipulation tool.

File nameEnabled when you select File as the destination. Allows
you to enter a name, or you may accept the default.

Files list box

Displays a list of the available sample files for the
choice shown in the Status field and within the range ofdates specified in the Dates dialog..

Directories

Displays a list of available drives and directories. The
drive and directory last accessed is displayed immediately above the Directories list box.

Feb 03

TriStar 3000

DFT Plus

Close Reports
This option enables you to close all open report windows at one time. This avoids
having to select close on each report window. This option is unavailable if reports
are being generated.

DFT Plus
DFT Plus® is an enhanced data reduction application. This program allows you to
calculate pore volume, surface energy, and surface area distribution from the adsorption isotherm of materials which have been previously analyzed on a
Micromeritics physisorption analyzer.
This option is nonfunctional if the DFT Plus program is not installed. See Chapter 10 for ordering information.

Feb 037-5

Printed Reports

TriStar 3000

Printed Reports
HeaderAll printed reports (either to the screen or to a printer) contain a header displaying file statistics.
•

Tabular and graphical reports contain sample and instrument statistics suchas date and time of analysis, analysis conditions, and so forth.
The headers for these reports also contain notes of any changes to the sample file that occur after analysis.

•

Summary report headers contain the same type of information displayed intabular and graphical reports with the exception of notes.

Onscreen Reports
The report window containing onscreen reports provides many options for customizing and manipulating reports:•

a tool bar
shortcut menus• zoom feature• axis cross hairs•

When reports are printed to the screen, they are printed in a window like the one
shown below. Each requested report is listed in the Reports window on the tool
bar; they are also indicated by selectable tabs across the top of the report header.
To view a specific report, select its tab or select the report in the Reports window
and click Show .

7-6

Feb 03

TriStar 3000

Printed Reports

Tabs display for each type of report you choose to generate.

HeaderList of reports
requested.

Options on
Tool Bar

Displays graphical(or tabular) data.

Tool Bar

Reports
Show

Feb 03

Contains a list of all requested reports.
Shows the selected report in the report window. If the report has been hidden, it and its associated tab will become visible.

7-7Printed Reports

TriStar 3000

DeleteDeletes the selected report. A deletion confirmation dialog is displayed since this function cannot be undone.
The deleted report(s) will have to be regenerated if deleted in error.

Hide

Hides (removes) the selected report from the report window. The report’s associated tab is also removed.

Open

Allows you to open a previously saved report file.

Print

Displays a print dialog so that you can choose an appropriate printer for report output. A list of available reports
is displayed in the window on the right side of the dialog.

For convenience in selecting which reports to print, pushbuttons are provided beneath the report window. Or, you
can make your selection by clicking on the desired
reports.
Current

selects the report displayed in the report window.

Shown

selects only the shown reports; any nonhighlighted reports indicate they are hidden. You can still select hidden reports from this window to print.
Allselects all reports, including those that may havebeen hidden.
Clear

7-8

clears all selections.

Feb 03

TriStar 3000

Printed Reports

Save

Saves all reports of the currently open file in a report format using the same name as the sample file, only withan rep extension. If you wish to specify a name and/or
specific reports to save, use the Save as push button.

Save asSaves all or specified reports from the currently open
file. The push buttons displayed on this dialog performin the same manner as the print dialog (explained above).
Reports can be saved in three different formats:
Report system (*.rep): Saved in a format which allows
you to reopen the file using the Open push button on
the Report window tool bar.
Spreadsheet (*.xls): Saved in a format which can be imported into most spreadsheet programs.
Ascii Text (*.txt): Saved in ASCII text which can be imported into programs accepting this type of file.

Default Fonts

Displays the Default Fonts dialog so that you can edit
report fonts.

The window on the left lists the items for which the font
can be edited.
Click Edit to edit the font of a selected item; a fontdialog is displayed so that you can specify the desired
font and attributes.
Click Save to save the changes as the default. If you
do not click Save , the changes will apply to the current report set only. The next reports will revert to thedefault font.

Feb 037-9

Printed Reports

Default Fonts

TriStar 3000

Click

Load

to load the default font of a selected item.

Click

Close

to close the dialog.

(continued)

Shortcut Menus
Shortcut menus are accessed when you right-click on the tabular or graphical portion of a report.

Tabular Reports

7-10

Resize column

Displays a dialog so that you can specify the width of
the selected column (in inches).

Rename column

Displays a dialog so that you can edit the name of theselected column. Use to insert line feeds.

Move column

Allows you to move the location of the selected column
to the left or to the right.

Align column

Enables you to right-align, left-align, or center the datain the selected column.

Hide column

Displays a list of all columns, enabling you to select the
one you wish to hide.

Show column

Displays a list of all hidden columns, enabling you toselect the one you wish to have shown again.

Feb 03

TriStar 3000

Printed Reports

Column font

Displays a Font dialog, allowing you to change font attributes for the tabular data in the current report.

Header font

Displays a Font dialog, allowing you to change font attributes for column headers in the current report.

Edit title

Allows you to edit the table title and font.

Copy table as text

Enables you to copy the entire table (column headers anddata) and then insert it into another program. Colums aretab-delimited, allowing easy alignment.

Graphs

Feb 03

Autoscale

Autoscales all axes of the graph. This function is usefulfor returning to a full view after having zoomed in.

Show curve

Shows any curve(s) that has been hidden. This option isdisabled (greyed) if no curves have been hidden.

Hide curve

Hides (removes from view) any unwanted curve(s).

7-11Printed Reports

TriStar 3000

Edit curve

Displays the Curve Properties dialog, allowing you toedit curve properties.

Title

Displays the title of the curve you are editing.

Style

Drop-down list containing styles in which collected data
can be displayed.
Choices:

7-12

Curve, Histogram, Points, Curve and Points

Curvegroup box

Contains options for curves and points. You can edit the
curve interpolation, the style of curve and/or points, aswell as the pen color. The options in this group box are
disabled if Histogram is chosen in the Style drop-down
list.

Histogramgroup box

Allows you to specify the type of fill as well as thecolor if Histogram is chosen as the style for collected
data.

Feb 03

TriStar 3000

Feb 03

Printed Reports

Edit axis

Displays the Axis Properties dialog, allowing you to edit
axis properties.

Edit legend

Displays the Legend Properties dialog, allowing you toedit the placement of the legend.

Edit title

Displays the Title Properties dialog, allowing you to edit
the current graph’s title and font.

Copy as metafile

Copies the graph and places it on the clipboard, allowing
you to paste it into other applications accepting Windows
metafiles.

Copy as text

Copies the data used to generate the graph as a series oftab-delimited columns of text.

7-13

Printed Reports

TriStar 3000

Zoom Feature
A zoom feature is included with the report system so that you can zoom in to examine fine details. To use this feature, simply hold down the left mouse buttonand drag the mouse cursor (drawing a box) across the area you wish to view;
then release the button. The enlarged area immediately fills the graph area. Rightclick in the graph area and choose Autoscale from the shortcut menu to return tothe normal view

Axis Cross Hair
A cross-hair function is available so that you can view axis coordinates. To use
this feature, simply left-click in the desired area of the graph.

X-axis position

Point of Coordination

Y-axis position

Right-click in the graph area and choose Autoscale form the shortcut menu to remove cross-hair lines and return to the normal view. Alternatively, you can clickoutside of the graph area.

7-14

Feb 03

TriStar 3000

Report Examples

Report Examples
The remainder of this section contains samples of some of the reports which may
be generated by the TriStar 3000 Analysis Program. Most of the reports can bevaried through entries on the report options screens.

Feb 037-15

Report Examples

TriStar 3000

Analysis Log

7-16

Feb 03

TriStar 3000

Report Examples

Isotherm Plot

Feb 037-17

Report Examples

TriStar 3000

BET Surface Area Report

7-18

Feb 03

TriStar 3000

Report Examples

BET Surface Area Plot

Feb 037-19

Report Examples

TriStar 3000

Langmuir Surface Area Plot

7-20

Feb 03

TriStar 3000

Report Examples

t-Plot Report

Feb 037-21

Report Examples

TriStar 3000

t-Plot Graph

7-22

Feb 03

TriStar 3000

Report Examples

Alpha-S Method

Feb 037-23

Report Examples

TriStar 3000

f-Ratio Method

7-24

Feb 03

TriStar 3000

Report Examples

BJH Adsorption: Pore Distribution Report

Feb 037-25

Report Examples

TriStar 3000

BJH Adsorption: Cumulative Pore Volume Plot
The vertical dashed lines on this report indicate selected minimum and maximum
BJH pore sizes.

7-26

Feb 03

TriStar 3000

Report Examples

BJH Adsorption: dV/dD Pore Volume
The vertical dashed lines on this report indicate selected minimum and maximum
BJH pore sizes.

Feb 037-27

Report Examples

TriStar 3000

BJH Adsorption: dV/dlog(D) Pore Volume
The vertical dashed lines on this report indicate selected minimum and maximum
BJH pore sizes.

7-28

Feb 03

TriStar 3000

Report Examples

BJH Adsorption: Cumulative Pore Area Plot
The vertical dashed lines on this report indicate selected minimum and maximum
BJH pore sizes.

Feb 037-29

Report Examples

TriStar 3000

BJH Adsorption: dA/dD Pore Area Plot
The vertical dashed lines on this report indicate selected minimum and maximum
BJH pore sizes.

7-30

Feb 03

TriStar 3000

Report Examples

Summary Report

Feb 037-31

Report Examples

TriStar 3000

Sample Log Report

7-32

Feb 03

CHAPTER 8OPTIONS MENU•

Description•

Option Presentation•

Data Presentation•

Sample Defaults•

System Configuration•

Parameter Files Directory•

Service Test Mode

TriStar 3000

Description

OPTIONS MENUThe Options menu contains options which allow you to configure the system toyour laboratory’s requirements. With the options on this menu, you can:•Choose between basic, advanced, or restricted mode
Edit program defaults• Specify data presentation modes• Specify printer/plotter options• Specify a directory for predefined parameter files•

Description

Listed below are brief descriptions of the options contained on the Options menu.
Detailed descriptions follow this section.

Feb 03

Option presentation

Allows you to display the sample file dialog in either Basic, Advanced, or Restricted format.

Data presentaton

Allows you to choose the way in which data are presented on the screen and in printed reports.

Sample defaults

Allows you to specify defaults for the parameters contained in the sample information and parameter files.

Tube characteristics

Enabled only when in Service Test Mode.

System configuration

Allows you to specify the printer and/or plotter to which
you wish to have reports sent.

8-1

Description

8-2

TriStar 3000

Parameter files
diretory

Allows you to specify a location for the predefined parameter files used by the Basic format.

Service Test Mode

Enables you to perform certain troubleshooting procedures. This option is available only under the direction of
a Micromeritics service representative.

Feb 03

TriStar 3000

Option Presentation

Option Presentation
The sample editing dialogs for the TriStar 3000 analysis program may be presented in three different formats: Advanced, Basic, or Restricted.

Each format displays sample information and menu options differently.
•

Advanced: displays all parts of the sample information file in a tabbed dialog as in an index card file. Clicking on each tab opens an associated dialog. Use this format to edit parameter files or create customized sample files.

•

Basic: displays the sample file and parameter files in a single dialog. Use
this format to create sample files using previously created parameter files.

Basic and Advanced formats contain a toggle push button so that you may
switch from one format to the other. The push button displays as Advanced in
Basic format and as Basic in Advanced format.
•

Feb 03

Restricted: displays in the same manner as the Basic format. This format
also is used to create sample files using previously created parameter files.
However, you cannot switch to the Advanced format to edit parameters. You
must also use a password for entering and exiting this format.

8-3

Option Presentation

TriStar 3000

Advanced
The Advanced format presents all parts of the sample information file in a tabbed
dialog. For example, if you wish to open or create a sample file using the Advanced format, the following dialog is displayed.

If you are opening an existing
file, this dialog
also contains atab for Collected
or Entered Data.

The Advanced format is used to create customized sample files — easily andquickly. You can also switch to the Basic format, if desired, by clicking Basic
Chapter 5 provides a detailed description of this dialog.

8-4.

Feb 03

TriStar 3000

Option Presentation

Basic
The Basic format presents the sample information file and its parameter files in asingle dialog. For example, if you wish to open or create a sample information
file using the Basic format, the dialog box is displayed in this manner.

This pushbutton does
not display
when in the
Restricted
format.

The Basic format is used to create sample information files using previously defined parameter files. You can easily switch to Advanced format, if desired, by
clicking Advanced . Chapter 5 provides a detailed description of this dialog.

Feb 038-5

Option Presentation

TriStar 3000

Restricted
The Restricted format is identical to the Basic format, except that certain menu
options are disabled, and you cannot switch to the Advanced format. This format
is password-protected and is typically used in laboratories where analysis conditions must remain constant, for example, in the pharmaceutical industry.
When you select Restricted, a dialog requesting a password is displayed:

Any password (up to 31 characters) can be used to enable the Restricted format.
The same password, however, must be used to exit the Restricted format. For example, if you enter “password” to enable the Restricted format, then you must use“password” to exit. If you forget the password, open the system INI file and navigate to the Private section. The current password will be shown immediately following “OptionPresentationPassword.” Make a note of the password, exit the INI
file, and enter the password where requested. Do not attempt to delete the password in the INI file.

8-6

Feb 03

TriStar 3000

Data Presentaton

Data Presentaton
The options on the Data presentation drop-down menu allow you to specify how
you wish tabular and graphical data to display on screen and in printed reports.

Units

Displays the Unit Selections dialog box allowing you tochoose the way in which certain criteria are to display.

Solid graph grid lines
Allows you to choose whether to use solid or dotted lines
Dotted graph grid lines when you choose to show graph grid lines.
When you choose dotted graph grid lines, the screen output actually displays as solid; however, dotted lines display when printed to a printer.
Show graph grid lines

The options on this cascading menu allow you to choose
what type of lines to display on graphs, or you canchoose to have none displayed.
Choices:

Feb 03None, Horizontal, Vertical, Both

8-7

Sample Defaults

TriStar 3000

Sample Defaults
This option allows you to specify default parameters for sample information files.
This option is presented in two formats: Advanced and Basic. Select Option presentation from the Options menu to choose the format you wish to use. Alternatively, you can switch between the two formats using the Advanced / Basic toggle
push button displayed on the lower right side of the screen.

Basic
When you select Sample Defaults while using the Basic format, the Default Basic
Sample Information dialog box is displayed.

Sequence

8-8Specify a default sequence for the sample file name. The
number you specify is sequenced incrementally each time
you create a sample file. It is the number that appears in
the File name: field when you select File, Open, Sample
information.
•

Use numbers, letters, or other printable characters,such as dashes. At least three numbers must be included.

•

Use up to eight characters.

•

DOS prohibits using such characters as * or ?. Referto your DOS manual for more information.

Feb 03

TriStar 3000

Sample Defaults

SampleAllows you to enter an additional identification that provides more information than the sample file name alone.
In the field on the left, edit the prompt for Sample if you
wish. For example, you may prefer to use Test or Material. The maximum number of characters is 20.
In the field on the right, specify a format for the sample
identification.
•

Use numbers, letters, or other printable characters,such as dashes.

•

Maximum number of characters is 42, plus the $ symbol.

•

Include the automatically generated file name as partof the identification by using the $ symbol where
you want the sequence number to appear.
For example, if the sequence number is 000-001, enter the sample identification as follows:
Lab #25 - $The resulting sample identification for the first sample information file would be:
Lab #25 - 000-001
and the second:
Lab #25 - 000-002, and so on.

Feb 03

Mass

Enter a default value for the sample mass. Regardless ofwhat weight you enter as the default, the value can be edited in the sample information file.

Density

Enter the density of the material you are analyzing.

8-9

Sample Defaults

Sample Tube
Degas Conditions
Analysis Conditions
Adsorptive Properties
Report Options

8-10

TriStar 3000

Each parameter contains a drop-down list containing filesof that type which were included with the software, as
well as any you may have created. Choose the file you
wish to use as the default.

Replace all...

Allows you to replace all parameters of the default sample file you are creating with parameters from an existing
sample file. For example, you may have an existing sample file that contains most (or all) of the parameters thatyou wish to use. You can click this push button, chooseOK
the file, and then
. All parameters of the file you
choose are copied into the sample defaults dialog. You
can even change the values in these files (if needed) without affecting the file from which they were copied.

Save

Saves the specified defaults.

Close

Closes the dialog.

Feb 03

TriStar 3000

Sample Defaults

Advanced
When you select Sample Defaults while in the Advanced format, the Sample
Defaults dialog box with the Sample Information dialog is displayed.

Sequence

SampleAllows you to specify a default sequence for the sample
file name. The number you specify is sequenced incrementally each time you create a sample file. It is the numberthat appears in the File name: field when you select File,
Open, Sample information.
•

Use numbers, letters, or other printable characters,such as dashes. At least three numbers must be included.

•

Use up to eight characters.

•

DOS prohibits using such characters as * or ?. Referto your DOS manual for more information.

Allows you to enter an additional identification that provides more information than the sample file name alone.
In the field on the left, you can edit the prompt for Sample if you wish. For example, you may prefer to use Test
or Material. The maximum number of characters is 20.
In the field on the right, specify a format for the sample
identification.

Feb 038-11

Sample Defaults

SampleTriStar 3000•

Use numbers, letters, or other printable characters,such as dashes.

•

Maximum number of characters is 42, plus the $ symbol.

•

Include the automatically generated file name as partof the identification by using the $ symbol where
you want the sequence number to appear.

(continued)

For example, if the sequence number is 000-001, enter the sample identification as follows:
Lab #25 - $The resulting sample identification for the first sample information file would be:
Lab #25 - 000-001
and the second:
Lab #25 - 000-002, and so on.
Operator
Submitter

Allow you to enter the name (or other identification) of
the operator performing the analysis and the name of theperson, department, customer, etc. that submitted the sample for analysis.
The fields on the left can be edited to display somethingother than Operator and Submitter if you like.
The fields on the right allow you to specify default names
or titles.

8-12

•

Include the automatically generated file name as partof the identification by using the symbol $ where
you want the sequence number to appear. Refer tothe example in the previous section.

•

Maximum number of characters for the prompt is 20.

•

Maximum number of characters for the identification
is 42, including the $ symbol.

•

Omit this item entirely from the sample information
file by selecting Omit.

Feb 03

TriStar 3000

Sample Defaults

Mass

Enter a default value for the sample’s mass. Regardless ofthe value you enter in this field, the value can be edited
in the sample file.

Density

Enter a default density. If there is a material you analyze
quite often, you may wish to use its default in this field.
This value can be edited in the sample information file.

Comments

Allows you to enter comments about the sample or its
analysis conditions. Anything you ener in this window isprinted in the report header.

Add Log Entry

Allows you to enter comments about the sample or its
analysis conditions. Anything you enter using this option
appears in the Instrument Log Report; it does not display
in the report header.

Replace all...

Allows you to replace the contents of all parameter files
contained in the current default sample file with thosefrom an existing sample file. For example, you may havean existing sample file that contains most (or all) of theparameters that you wish to use. You can select this pushOK
button, choose the file, and then
. All parameter
files of the file you choose are copied into the sample defaults dialog. You can even change the values in thesefiles (if needed) without affecting the file from which
they were copied.

Click on each remaining tab of the Advanced Sample dialog to establish parameter defaults. Refer to Chapter 5 if you need assistance on the fields of these dialogs.

Feb 038-13

System Configuration

TriStar 3000

System Configuration
This option allows you to specify printer and plotter destinations for report output;
the System Configuration dialog box is displayed.

Printer namePlotter name

The printer and plotter names are shown exactly as they
appear in the Operating System Print Manager.
Select Default if you wish to use the default printer andplotter as designated in the Print Manager.
If you wish to change the default printer, deselectDefault. Then choose another printer (or plotter) from thedrop-down list.

8-14

Feb 03

TriStar 3000

Parameter Files Directory

Parameter Files DirectoryThis option allows you to select the location for the predefined parameter files displayed in the drop-down lists on the Basic Sample Information dialog box.
When you select this option, the Parameter File Directory Selection dialog is displayed.

The directory specified here is the one you should use when creating parameter
files to be included in the drop-down lists on the Basic sample information dialog.
It is where the software goes to obtain the files for the drop-down lists. If parameter files are not saved to this directory, they are not included in the lists.

Feb 03

8-15

Service Test Mode

TriStar 3000

Service Test Mode
Certain service tests are included in the TriStar operating program. These tests,
however, can be performed only with the assistance of a trained Micromeritics
service representative. When you select Service Test Mode from the Options
menu, a dialog box prompting you to enter a password is displayed. This password is coded to change on a regular basis and, therefore, is known only by yourservice representative. You will be unable to perform these tests without his guidance.
After Service Test Mode has been enabled, the tests are accessible from the Unit
menu.

8-16

Feb 03

CHAPTER 9
TROUBLESHOOTING AND
MAINTENANCE•

Cleaning the Analyzer•

Replacing Port Frit and O-ring•

Calibrating the System

TriStar 3000

Cleaning the Analyzer

TROUBLESHOOTING AND MAINTENANCE
The TriStar 3000 system has been designed to provide efficient and continuous
service. However, certain maintenance procedures should be followed to obtain thebest results over the longest period of time. This chapter includes maintenanceprocedures and calibration procedures.

Cleaning the Analyzer
The exterior casing of the analyzer may be cleaned using a clean cloth, dampened
with isopropyl alcohol (IPA), a mild detergent, or a 3% hydrogen peroxide solution.
Do not allow liquid to penetrate the casing of the analyzer. Doing so could result in damage to the unit.

Feb 039-1

Replacing Port Frit and O-ring

TriStar 3000

Replacing Port Frit and O-ring
A 40-µm frit is located in the analysis port of the analyzer. If the frit is contaminated, the contaminant may adsorb or desorb during analysis, affecting the resutls.
A contaminated frit on the analysis port may be indicated by a leak or by a freespace reading much lower than normal.
A contaminated frit should be replaced as follows:
1.

Remove the sample tube fitting from the analyzer using a wrench. Pry out thefrit and O-ring.

40-µm Frit
O-ringSample Tube Fitting

Figure 9-1. Analysis Port Frit and O-ring
To avoid degassing problems, the frit andO-ring should be clean and should
not be touched with bare hands.

2.

9-2

Replace the frit and O-ring. Carefully reassemble the sample tube fitting andtighten by hand. Then tighten with a wrench to prevent leaks.

Feb 03

TriStar 3000

Calibrating the System

Calibrating the System
A calibration file was created specifically for your analyzer and included withyour accessories. Chapter 2 describes how to install this file. It is unnecessary torecalibrate your system unless you suspect that it may be out of calibration.
You may wish to recalibrate your system if:•analysis on a known reference material or a blank tube gives unexpected
results•

the transducers have been serviced

You can review calibration details of your analyzer by selecting Unit configuration on the Unit menu.
If it becomes necessary to recalibrate your system, the following order isrecommended:•

Zero pressure
Pressure scale• Servo valve• Temperature• Volume•

Zero pressure

Feb 031.

Install a blank sample tube on each port.

2.

From the Unit menu, select Calibration, Zero pressure; the Calibrate Pressure
Offset dialog is displayed.

3.

Ensure that all transducers are selected,then click
automatically when calibration is complete.

Start. The dialog closes

9-3

Calibrating the System

TriStar 3000

Pressure scale
1.

Install a pressure reference on one port and sample tubes on the other two ports.

2.

From the Unit menu, select Enable manual control (if the instrument schematicis not displayed, select Show instrument schematic).

3.

Ensure that valves 1, 2, and 3 are open and the system is at a stable pressurenear atmosphere.

In rare cases, calibrations may become corrupt so that manual control of the
instrument is inoperative. If this occurs, select Reset pressure calibration fromthe Unit menu to restore factory defaults. Then proceed with the calibration.

9-4

4.

From the Unit menu, select Calibration, Pressure scale; the Calibrate Pressure
Scale dialog is displayed.

5.

Enter the pressure obtained from the reference gauge in the Actual manifoldpressure field.

Feb 03

TriStar 3000

Calibrating the System

Servo valve
Make sure the pressure transducer has been calibrated before performing thisprocedure.

1.

From the Unit menu, select Calibration, Servo valve; the Calibrate Servo Valvedialog is displayed.

2.

Click

Start

; the dialog closes when calibration is complete.

Temperature
1.

Remove the retaining screws and remove the top cover from the analyzer.

Figure 9-1. Removing the Top Cover

Feb 039-5

Calibrating the System

2.

TriStar 3000

Locate the dosing manifold and insert the calibration device into the hole next to
the RTD (resistance thermal device).
RTD

Dosing Manifold
Calibration Device
Calibration Device

RTD

Figure 9-2. Inserting the Calibration Device

9-6

3.

Wait until the temperature stabilizes (approximately 1 to 2 minutes).

4.

From the Unit menu, select Calibration, Temperature; the Calibrate Manifold
Temperature dialog is displayed.

5.

Enter the temperature obtained using the calibration device, then clickOK.

Feb 03

TriStar 3000

Calibrating the System

VolumeIf you wish to use the previous volume or enter one manually, skip steps 1
and 2 and and begin at step 3.

1.

Install the calibration volume onto ports 1 and 2.

Figure 9-3. Installing the Calibration Volume
2.

Insert the volume portion into an ice bath.

3.

From the Unit menu, select Calibration, Volume; the Calibrate Volume dialog
is displayed.

Displays as Next>> if
you choose Measured
as the method.

Feb 039-7

Calibrating the System

4.

TriStar 3000

Choose the method you wish to use for calibrating the volume.
•

Previous: simply click
ume is used.

•Entered: enter the volume you wish to use, then click
dialog box.

•

Measured: click
displayed.

Next >>

Done

to close the dialog box; the previous vol-to close the; a second view of the Calibrate Volume dialog is

5.

Enter the volume of the calibration volume device.

6.

Ensure that the temperature is 0.00 ± 0.10 °C.

7.

Select (or enter) the number of measurements you wish to make; generally, 3 issufficient.

8.

Select (or enter) an equilibration time; generally, 10 minutes are sufficient.

9.

Click Start to begin calibration; an informational dialog displaying calibration
status is displayed. After calibration is complete, a final view of the Calibration
Volume dialog is displayed.

10. Confirm that the value is acceptable and click

9-8

Done

Done

to close the dialog.

Feb 03

CHAPTER 10
ORDERING INFORMATIONTriStar 3000

Ordering Information

ORDERING INFORMATIONThe TriStar 3000 Analysis System components and accessories can be orderedthrough our Customer Order Entry Department - (770) 662-3636. When ordering,please use the information provided in the following table.
Table 10-1. TriStar 3000 System Components and Accessories
Part Number

Mar 03Item and Description

065-00000-00

SmartPrep 065, Windows interface allowing programmableramp and soak rates; degasses up to six samples with flowing
gas060-00030-00

FlowPrep 060, degasses up to six samples at up to
400 °C with flowing gas

061-00030-00

VacPrep 061, degasses up to six samples at up to
400 °C; uses flowing gas or evacuation by vacuum(evacuation requires a vacuum pump and a regulator)

062-00000-11

Vacuum pump with built-in anti-suckback valve, 100/120
VAC, includes hose kit

062-00000-23

Vacuum pump with built-in anti-suckback valve, 220/240
VAC, includes hose kit

062-33002-00

Activated alumina oil vapor trap004-16830-00

Activated alumina, 500 grams; for oil vapor trap003-22617-00

Valve, solenoid 24 VDC 10-32 Mt, 0.025-in. orifice, forstandard evacuation (Valves 1 through 10)003-22626-00

Valve, solenoid 24 VDC 10-32 Mt, 0.060-in. orifice, for fastevacuation (Valves 11, 12, and 13)004-62230-58

CGA 580 fitting, 30 psig (He, N2)004-62230-32

CGA 320, 30 psig (CO2)004-33601-00

Expansion Kit; adds an additional outlet to the gas regulator

004-33602-00

Pressure Relief Kit; prevents excessive gas pressure in theevent of regulator failure (not to be used with toxic gases)

004-16833-00

Reference Material, Carbon black, SA~23.8 m2/g

004-16821-00

Reference Material, Silica alumina, SA~215 m2/g,
PV~0.6 cc/g003-20665-00

Cable, M/F 9-pin D 6 ft. straight thru

10-1Ordering Information

TriStar 3000

Part Number

10-2

Item and Description

004-25549-00

Reducer, 1/8-in. tube x 1/4-in. tube

230-02001-00

Gas inlet line

240-14855-00

Rack, sample tube

240-25853-00

Funnel, sample tube

240-25901-00

Dip stick

300-33601-00

Sample Tube Kit, 1/4-in; includes sample tubes,
isothermal jackets, filler rods, ferrules, O-rings, caps, anddewar cover300-33602-00

Sample Tube Kit, 3/8-in; includes sample tubes, brush (forcleaning sample tubes), isothermal jackets, filler rods,
ferrules, O-rings, stoppers, and dewar cover300-33603-00

Sample Tube Kit, 1/2-in; includes sample tubes, brush (forcleaning sample tubes), isothermal jackets, filler rods,
ferrules, O-rings, stoppers, and dewar cover

300-61001-00

Sample tube, 1/4-in. stem OD; for analyzing powderedsamples where free-space management (with a filler rod
inserted) is critical

300-61002-00

Sample tube, 3/8-in. stem OD; for analyzing any type ofsample300-61003-00

Sample tube, 1/2-in. stem OD; for analyzing larger piecesof granular or pelleted samples

300-25901-00

Isothermal jacket, for sample tube

300-25902-00

Isothermal jacket, for 3/8-in. sample tube

300-25903-00

Isothermal jacket, for 1/2-in. sample tube

300-25904-00

Filler rod assembly, for 1/4-in. sample tube

300-25905-00

Filler rod assembly, for 3/8-in. sample tube

300-25906-00

Filler rod assembly, for 1/2-in. sample tube

004-25466-00

O-Ring, for sample port and 1/4-in. sample tube

004-25022-00

O-Ring, for 3/8-in. sample tube

004-25469-00

O-Ring, for 1/2-in. sample tube

300-31802-02

Dewar cover, for 1/4-in. and 3/8-in. sample tubes

300-31802-03

Dewar cover, for 1/2-in. sample tube

004-54104-00

Brush, for cleaning 3/8-in. sample tubes

004-54609-00

Brush, for cleaning 1/2-in. sample tubes

Dec 06

TriStar 3000

Ordering Information

Part Number

Mar 03Item and Description

300-25825-00

Ferrule, for 1/4-in. sample tube

300-25826-00

Ferrule, for 3/8-in. sample tube

260-25843-00

Ferrule, for 1/2-in. sample tube

004-27046-00

Frit, 40 µm, for sample port

240-32004-00

Stopper, rubber, for 3/8- and 1/2-in sample tubes

004-32604-08

Cap, plastic, for 1/4-in sample tube

300-32800-00

Support, sample weighing

300-34008-00

Vacuum pump tray

300-25861-20

Dewar

300-42832-00

Operator’s manual, TriStar 3000

003-20690-00

USB Expander kit, for connecting multiple instruments toa single computer

202-33023-00

DFT Plus Program; allows you to use the total
experimental isotherm to determine microporosity andmesoporosity as a continuous distribution of pore volume
with respect to pore size202-33024-00

DataMaster Program; allows you to generate classical or
micropore data reductions

10-3

APPENDIX A
FORMSSample Data Worksheet
TriStar 3000

Use this worksheet to record the values necessary to calculate the sample mass (refer to Weighing the Sample in Chapter 4).

Sample Tube Identification:_________________________________

Sample Mass
Note: Record all values in grams.
Before Degas

After Degas

After Analysis

A. Mass for empty sample tube set:______________ _______________ _______________

B. Sample tube plus sample mass:______________ _______________ _______________

C. Sample mass (B - A):______________ _______________ _______________

Degas Information
Degas apparatus:________________________________________________

Temperature (°C):________________________________________________

Time (hours):________________________________________________

Actual time started:________________________________________________

Actual time finished:________________________________________________

Degas notes: _____________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________

Page 1 of 1

Sample Tube Calibration Worksheet
TriStar 3000

Use this worksheet to record the values necessary to calibrate a sample tube which is to be usedin an analysis where the free space is to be determined by the quasi-Gemini or calculated method.

Sample Tube Identification:_________________________________

Water Weight
Note: Record all weights in grams.
A. Empty sample tube weight:______________________________________

B. Sample tube plus water:______________________________________

C. Weight of the water (B - A):______________________________________

Physical Volume
D. Water temperature:______________________________________

E. Water density (refer to table):______________________________________

Temperature(°C)

Density(g/cm3)Temperature(°C)

Density(g/cm3)15

0.9991016

23

0.9975412

16

0.9989450

24

0.9972994

17

0.9987769

25

0.9970480

18

0.9985976

26

0.9967870

190.9984073

27

0.9965166

20

0.9982063

28

0.9962371

210.9979948

29

0.9959486

22

0.9977730

30

0.9956511

Physical volume below the red line (C ÷ E):______________________________________

Page 1 of 1

APPENDIX B
ERROR MESSAGESTriStar 3000

Appendix B

ERROR MESSAGES
Error messages for the are listed numerically. If the Action response instructs you to
contact your service representative, record the error message and make backup copies
of any files involved in the operation.
The 1000 series error messages, used primarily for software testing, are not included in this appendix. These errors should not occur during normal operation. If you receive a 1000 series error message, contact your service
representative after making backup copies of any files involved in the operation.
24012402240324042405240624072408240924102411241224132414241524162417241824192420242124222423242424252426242724282429-

Jan 05FATAL ERROR: (error message)
MMDevice- Invalid state seen in T/O table.
MMDevice- Invalid state seen in ERR table.
MMDevice- Invalid state seen in DONE table.
MMDevice- Invalid CmdType in DONE table.
MMDevice- Invalid I/O State returned.
MMDevice- CommandManager failed.
MMDevice- XModem failed.
MMDevice- SerialComm failed.
MMDevice- Invalid UserID returned.
MMDevice- Invalid state reached. cannot continue.
MMDevice- Time-out. Canceling operation.
MMDevice- Time-out during block receive. Retrying.
MMDevice- Error. State was (number).
CommandMgr- Invalid state reached. cannot continue.
CommandMgr- Time-out. State was (number).
CommandMgr- Parity or overrun error in receive.
CommandMgr- Bad ACK received.
CommandMgr- MICIC reports a command receive error: (number).
CommandMgr- Unknown ACK (number number number) vs(number number number).
CommandMgr- ’Last ACK’ received from MICIC.
XModem- Invalid state reached. cannot continue.
XModemSender- Invalid state reached. cannot continue.
XModemRcvr- Invalid state (number). cannot continue.
XModemRcvr- Time-out. State was (number).
XModemRcvr- Error. State was (number).
XModemRcvr- Packet received out of sequence.
XModemRcvr- Packet failed CRC validate.
XModemRcvr- Duplicate packet received.

Cause:

An internal processing and/or hardware error has occurred duringcommunication with the analyzer.

Action:Contact your service representative if you continue to receive thismessage.

B-1

Appendix B

TriStar

2430- Error accessing file (file name), error code = (number).

Cause A:

Diskette may be damaged.

Action A: Clean the diskette drive. If this does not eliminate the problem, attempt operation using a backup copy of the file.
Cause B:

Hard disk may be damaged.

Action B: Contact your service representative.
Cause C:A software error occurred when the file was accessed.

Action C: Contact your service representative.
Cause D: The name specified contains one or more invalid characters.
Action D: Enter a valid DOS filename (refer to your operating systems manual).

2431- Error writing file (file name), error code = (number).

Cause:The hard disk does not have enough space left to perform the operation.

Action:Copy files not used regularly from the hard disk to diskette, deletethem from the hard disk, and then try the operation again.

2432- Invalid response from MMI ’FILE_READ’ request.

B-2

Cause:

An internal processing and/or hardware error has occurred.

Action:Contact your service representative if you continue to receive this error message.

Jan 05TriStar 3000

Appendix B

2433- New entries have been found in this directory. Refresh the directory
information?

Cause:

Several TriStar 3000 files (sample information, analysis conditions,adsorptive properties, or report options) have been added to this directory by some function other than the TriStar 3000 program.

Action:Select Yes to update the directory information with data from each
new file. This operation may take a minute.
Select No if you do not want to spend the time updating the directory information. This option may be feasible if a large number offiles have been copied into the directory and you know the name of
the file you wish to access.

2434- File (file name) — Subset # (number) wrote wrong amount of data.

Cause:

An internal processing and/or hardware error has occurred.

Action:Contact your service representative if you continue to receive this error message.

2435- SerialComm Rcv Time-out — Expected (number) | Rcv’d (number).

Cause:

An internal processing and/or hardware error has occurred duringcommunication with the interface controller.

Action:Contact your service representative if you continue to receive this error message.

2436- Path specification (path name) is invalid.

Cause:

You entered an invalid path name and/or extension.

Action:Type a valid path name (including the proper extension) and press↵ Enter .

2437- File (file name) does not exist.

Jan 05

Cause:

You entered a file specification that does not exist.

Action:Enter an existing file specification or select a file name from thelist box.

B-3

Appendix B

TriStar

2438243924402441244224432444244524462447-

Disk drive (letter): is inaccessible.
Could not register file.
Subset not found.
Seek within file failed.
Bad header in subset file.
Subset owner denied access.
Not a valid file format.
Subset wrote the wrong amount of data.
Error reading data.
Error writing data.

Cause:An unexpected error occurred when you tried to access a data file.

Action:Contact your service representative.

2448- File directory (path name) is invalid. Resetting to the installation directory.

Cause:

A working directory specified in the .INI file is invalid. The directory may have been deleted or moved to a different location.

Action:The installation directory will be substituted. The next time you
open a file, use the Directories: list to move to the correct directory.

2449- This field does not contain a valid file specification.

Cause:

You entered an invalid file name.

Action:See the description of file naming conventions in your DOS or Windows manual and re-enter the name.

2458- An instrument is performing a critical operation. Wait a few moments
before exiting the application.

B-4

Cause:

You are attempting to exit the application while the instrument isperforming a critical operation. This operation must be completed
before the application can be stopped.

Action:Wait a short time and attempt to stop the application again.

Jan 05TriStar 3000

Appendix B

2459- An instrument is busy. A delay in restarting this application could result inloss of new data. Continue with program Exit? (Yes, No)

Cause:

You are attempting to exit the application while an analysis is inprogress. While this is possible, the data collected while the application is inactive will not be permanently recorded until the application is re-started. A power failure to the instrument could causesome data to be lost.

Action:If you are not concerned with the potential for loss of data should apower failure occur, select Yes to continue; otherwise select No.

2460- Fatal Communications error on (Unit n - S/N: nnnn)

Cause:

There was a fatal error in the serial communications between the application and the software in the instrument. All displays for that instrument will be closed.

Action:Ensure that the analyzer is connected to the computer on the communications port configured in the Setup program. Stop the TriStar
3000 software and then restart it. If this error persists, contact yourservice representative.

2461- No instruments are in operation. This application will unconditionally terminate.

Cause:At least one instrument must be active for the application to operate. The initialization of all of the instruments configured with the
Setup program has failed. The application stops.

Action A:

Usually this message is preceded by another message giving the reason for the instrument’s failure to initialize. See the instructions forthat message.

Action B: Ensure that the instrument is attached to the computer on the communications port configured with the Setup program. Verify that the
instrument has the power switch in the ON position and that thelight on the front panel is illuminated. If the application continues
to fail in its attempts to initialize the instrument, contact your service representative.

Jan 05B-5

Appendix B

TriStar2462- Non-Fatal timer error on Unit n - S/N: nnnn.

Cause:The software has detected a non-fatal error in the timer.

Action:One of the instrument’s internal components has failed. Contact
your service representative.

2463- Non-Fatal DMA error on Unit n - S/N: nnnn.

Cause:The software has detected a non-fatal error in the analyzer’s Direct
Memory Access component.

Action:One of the instrument’s internal components has failed. Contact
your service representative.

2464- Non-Fatal memory bank 3 error on Unit n - S/N: nnnn.

Cause:The software has detected a non-fatal error in the analyzer’s memory bank 3.

Action:One of the instrument’s internal components has failed. Contact
your service representative.

2465- Non-Fatal memory bank 4 error on Unit n - S/N: nnnn.

Cause:The software has detected a non-fatal error in the analyzer’s memory bank 4.

Action:One of the instrument’s internal components has failed. Contact
your service representative.

2466- Unit n - S/N: nnnn has no interface card and cannot be initialized.

B-6

Cause:The software has detected that the analyzer’s electronic components
cannot support the software.

Action:Contact your Mircromeritics Service Representative.

Jan 05TriStar 3000

Appendix B

2467- Not enough memory error on Unit n - S/N: nnnn

Cause:The software has detected insufficient memory in the instrument forthe software to execute properly.

Action:One of the instrument’s internal components has failed. Contact
your service representative.

2468- The instrument contains a different software version. Do you want toreset it?

Cause:

The application has discovered that a different version of softwareis already running on the instrument.

Action:If there is no chance that some instrument other than the TriStar
3000 is connected to the instrument, select Yes to reset the instrument and download the proper software. Otherwise, select No toleave the instrument unchanged.

2469- The instrument software did not initialize properly on Unit n - S/N: nnnn.

Cause:The software in the instrument failed to execute properly.

Action:Reinstall the TriStar 3000 software, then restart it. If the problem
persists, contact your service representative.

2470- Unable to read instrument software file for Unit n - S/N: nnnn.

Cause:

The application tried to read the instrument software file to download it to the instrument. It was unable to do so.

Action:Reinstall the TriStar 3000 software, then restart it.

2471- Unit n - S/N: nnnn has an invalid communications port specified.
It cannot be initialized.
2472- Unit n - S/N: nnnn communications port specified in the program
control files is not a valid device. Unit cannot initialize.
2473- Unit n - S/N: nnnn communications port specified in the program
control files is not physically installed in the Control Module. Unitcannot initialize.

Jan 05

Cause:

The communications port associated with this unit was not valid.

Action:

Run the Setup program, specifying a valid port for this unit, when
you are prompted to do so.

B-7

Appendix B

TriStar2474- Unit n - S/N: nnnn communications port specified in the program control
files is already in use. Unit cannot initialize.

Cause A:The communications port associated with this instrument is in use
by some other program in the system.

Action A:

Close the other program to release the port. Restart the TriStar 3000
software.

Cause B:The component associated with this unit is also being used by the
SmartPrep.

Action B: Run the Setup program and specify different communication ports
for each TriStar and the SmartPrep.
2475- Unit n - S/N: nnnn communications port specified in the program
control files cannot be accessed. Unit cannot initialize.
2476- Unit n - S/N: nnnn startup failed. Could not initialize thecommunications port.

Cause:

The communications port associated with this unit was not valid.

Action:

Run the Setup program, specifying a valid port for this unit, when
you are prompted to do so.

2477- Unit n - S/N: nnnn did not properly initialize.

Cause:The software was unable to initialize this instrument; this is usuallycaused by one of the conditions listed in the error messages above.

Action:Correct the problem as described above, then restart the application.

2480- File <name> cannot be analyzed. It is currently being edited.

Cause:

You are trying to start an analysis using a file that is open for editing.

Action:Finish editing the file, save and close it, then start the analysis.

2481- Error accessing the sample information file <name>.

B-8

Cause:An unexplained error prevents you from accessing this file.

Action:The hard disk drive may be corrupt. Run diagnositics.

Jan 05TriStar 3000

Appendix B

2484- The edit session for <name> must be saved before the analysis. Savechanges and continue with the analysis? (yes, no)

Cause:

You are trying to start an analysis using a file that contains unsavedchanges and is open for editing.

Action:Select Yes to save the changes and proceed with the analysis; select No to cancel the analysis and continue editing the Sample Information file.

2486- Could not construct (name) report type. Program will terminate.

Cause A:You may not have full rights to the application’s folders and files.

Action A: Contact your system administrator to have full rights granted.
Cause B:An internal processing and/or hardware error has occurred.

Action B: Contact your service representative if you continue to receive this error message.

2487- Could not start report generator. Error code (number). Program willterminate.

Cause:

An internal processing and/or hardware error has occurred.

Action:Contact your service representative if you continue to receive this error message.

2488- File (file name) cannot be opened for editing. It is already in use.

Cause:

The file you specified is being used in another edit operation.

Action:Check the Windows list to locate the other edit session.

2489- File (file name) cannot be opened for writing. It is already in use.

Jan 05

Cause:

The file you specified in a Save As operation is already open for
edit.

Action:Select a different file for the Save As operation.

B-9

Appendix B

TriStar2490- No ’.INI’ file present. Application will terminate.

Cause:The ASCII file containing initialization information and system options information used during program startup does not exist.

Action:

Run the TriStar 3000 Setup program, select Change analyzer
setup, and create the control file used by the TriStar 3000.

2492- This field’s entry is invalid.

Cause:The highlighted field contains an invalid entry.

Action:Check the entry and correct the error.

2493- An entry is required for this field.

Cause:

This field requires a valid entry for you to proceed.

Action:Enter or select an appropriate value.

2494- Value is out of the valid range.

Cause:The value you entered in the highlighted field is outside the valid
range of values.

Action:Check the entry and enter or select an appropriate value.

2495- Value is out of the valid range. Enter a value between (value) and (value).

Cause:The value you entered in the highlighted field is outside the valid
range of values.

Action:Check the entry and enter or select a value within the indicatedrange.

2496- Invalid number.

B-10

Cause:The number you entered in the highlighted field is invalid.

Action:Check the entry and enter or select a valid number.

Jan 05TriStar 3000

Appendix B

2497- This field contains an invalid character.

Cause:

You entered an invalid character in the highlighted field.

Action:Check the entry and enter valid characters.

2498- The requested change to the Sample’s status is invalid at this time.

Cause:A request to change the file’s status (for example, from automatically collected to manually entered) could not be done.

Action:Contact your service representative if you continue to receive this error message. Record the name of the sample file in which the problem occurred.

2499- Sequence number must contain at least 3 digits.

Jan 05

Cause:

You tried to enter a sequence number that did not contain at least
three digits.

Action:Enter a sequence number that contains at least three digits.

B-11

Appendix B

TriStar2500- All sample file names that can be created using the sequence number pattern already exist. You may want to modify the next sequence number.

Cause:

No more sample information files can be created using the currently
entered file name sequence number.

Action:Select Sample defaults from Options on the Main Menu and enter
another sequence number.

2501- System resources have reached a dangerously low level. Please close
some windows to avoid the loss of data.

Cause:

A large number of windows are open and consuming the system resources available to all applications.

Action:Close one or more windows on the screen. Contact your service representative if you continue to receive this error message.

2505- Error Logger cannot be initialized! Error code (number). Program will exit.

Cause:

An internal processing and/or hardware error has occurred.

Action:Contact your service representative.

2506- (sample file) Output device (name) is not installed. Printing cannot be accomplished.

Cause:The selected output device is not installed in Windows.

Action:Select a different output device in the System Configuration dialog
box. Install the device using the Control Panel - Printers operation.

2508- (sample file) Overlay file (name) was not found. It will not be included in
the reports.

B-12

Cause:The specified overlay file could not be found.

Action:Ensure that the file specified as an overlay does exist.

Jan 05TriStar 3000

Appendix B

2509- (sample file) Error opening file (name): (error). Reports cannot be produced.

Cause:

An error occurred while the program was opening a file necessary
to the report operation.

Action:Use the name given in the error message to investigate. Contact
your service representative if you continue to receive this error message.

2510- (sample file) Error parsing reports from file (name). Reports cannot be produced.

Cause A:One or more data entry fields in the sample file may contain an invalid character (such as a single quote or double quotes).

Action A: Review the data entry fields (for example, the Sample field) and remove the invalid character.
Cause B:The system was unable to create the usual temporary files during
the report, possibly due to insufficient disk space.

Action B: Check the space available on the hard disk.
Cause C:An internal processing error occurred.

Action C: Contact your service representative.

2511- Print job (name) has been cancelled due to insufficient disk space. Delete
unnecessary files and restart the report.

Cause:The disk drive does not have enough space for the temporary file required by the Windows Print Manager. Therefore, printing of the requested report has been canceled.

Action:Delete unnecessary files from the disk. You will require at least fivemegabytes of free space for normal operation.

2512- Print job (name) cancelled.

Jan 05

Cause:The requested print job was canceled at your request.

Action:None required.

B-13

Appendix B

TriStar4000- Memory Allocation Error.
4001- Error Smoothing Data.

Cause:

An internal processing and/or hardware error occurred during report
generation.

Action:Contact your service representative if you continue to receive this error message.

4002- Thermal Transpiration correction had no effect.

Cause:The Thermal transpiration correction option was selected on theReport Options dialog box. However, the correction did not change
any pressure by more than one percent.

Action:Deselect this option to disable this message. This correction is only
meaningful for very low pressures.

4003- Error Converting Pressures.
4004- Error Computing Volume Adsorbed.

Cause:

An internal processing and/or hardware error occurred during report
generation.

Action:Contact your service representative if you continue to receive this error message.

4005- Pressures were not smoothed. Not enough pressures below 0.10 P/Po.

Cause:The Smooth pressures below 0.10 P/Po option was selected on theReport Options dialog box. There must be at least 10 pressures
within this range for smoothing to occur.

Action:Deselect this option to disable this message.

4006- Report Type Not Found.
4007- Error Processing Report.

B-14

Cause:

An internal processing and/or hardware error occurred during report
generation.

Action:Contact your service representative if you continue to receive this error message.

Jan 05TriStar 3000

Appendix B

4008- Report requested on sample file with no data points.

Cause:You selected a file for reporting which contains no collected data.

Action:Select another file which contains collective data and restart the report.

4010- Summary Report was not included in the Selected Reports.

Cause:You did not select a plot or a table for any of the Selected Reports
in the Report Options dialog; you selected the reports only to generate an entry in the summary. However, the Summary was not included in the Selected Reports.

Action:Select a plot or table in one or more of the Selected Reports, and/or
add the Summary to the Selected Reports.

4015- Error creating export file for sample <sample file name>.

Cause:

A file error occurred during creation of an export output file.

Action:The output file name may be invalid. Ensure that the target directory exists. Ensure that the target diskette is not full or write protected. The target disk drive may be damaged or inoperative. Verify
that other files may be created on the same drive. Contact your service representative if you continue to receive this error message.

4016- Sample <sample file name> has no data for export to ISO/DFT.

Cause:

The file selected for export has a status of No Analysis. No export
file will be created.

Action:Select a file which contains analysis data.

4023- The file <name> cannot be prepared for analysis. It is open for editing andcontains errors.

Jan 05

Cause:

You are trying to start an analysis using a file that contains errors
and is open for editing.

Action:Finish editing this file, save and close it, then start the analysis.

B-15

Appendix B

TriStar

4400- The communications port specified for the SmartPrep(s) is not physicallyinstalled in the Control Module. Cannot initialize.

Cause:

The communications port associated with this unit was not valid.

Action:

Run the setup program and set up the unit on a valid port.

4401- The communications port specified for the SmartPrep(s) is already in use.
Cannot initialize.

Cause:

The communications port associated with this instrument is in use
by some other program in the system.

Action:Close the other program to release the port. Restart the TriStar 3000
application.

4402- The communications port specified for the SmartPrep(s) cannot be
accessed. Cannot initialize.
4403- Cannot communicate with SmartPrep Unit %d - S/N: %s.

Cause:

The communications port associated with this unit was not valid.

Action:

Run the setup program and set up the unit on a valid port.

4404- The application version of the SmartPrep Unit n - S/N: nn is invalid.

Cause:

The controller software running on the designated instrument is invalid.

Action:Use the SmartPrep setup program to download the proper controller
software to the instrument, or contact a service representative if unavailable.

4405- Fatal communications error with SmartPrep Unit n - S/N: nn.

B-16

Cause:

There was a fatal error in the serial communications between the application and the SmartPrep Instrument Controller. All displays forthat SmartPrep will be closed.

Action:Ensure that the SmartPrep is properly chained to the computer on
the communications port configured in the Setup program. Stopand re-start the application. If this error persists, contact your service representative.

Jan 05TriStar 3000

Appendix B

6000- An error occurred while loading the application control information. Data
entry cannot be performed. (Code number)Cause:

An error occurred accessing the control information disk file required by this application.

Action:The disk drive may have failed or be corrupt. Run diagnostics onthe disk drive.

6003- Unable to read the calibration file (number).

Cause:Your attempt to load a previously saved calibration file was unsuccessful.

Action:Make sure the file exists, and that you have entered the file namecorrectly, then try again.

6004- Unable to write the calibration file (number).

Cause:Your attempt to save the calibration to a separate file was unsuccessful.

Action:Make sure that the disk is neither full nor write-protected, then try
again.

6005- The sample has an invalid status and cannot be used for this analysis.

Cause:You selected a sample file with a status other than No Analysis orPrepared.

Action:Select a sample file with a status of No Analysis or Prepared.

6006- Cannot do quasi-gemini freespace with sample selected on port 2.

Jan 05

Cause:

You attempted to select a file requesting Quasi-Gemini free space
for analysis, but have already selected a sample for port 2. In QuasiGemini free space, port 2 is used for the balance tube and cannot
have a sample selected.

Action:Select a file that does not request Quasi-Gemini free space or clear
the sample file on port 2 and reselect the file.

B-17

Appendix B

TriStar6007- Cannot do Po measurement in sample tube with sample selected on port 3.

Cause:

You attempted to select a file requesting Po in Port 3 measurement,
but have already selected a sample for port 3.

Action:Select a file that does not request Po in port 3 measurement orclear the sample file on port 3 and reselect the file.

6008- At least one sample must be selected to proceed.

Cause:

You attempted to start an analysis without selecting any sample files.

Action:Select at least one file, then start the analysis.

6009- You must select a sample tube on port 2 to do a Quasi-Gemini analysis.

Cause:

You attempted to start an analysis requesting Quasi-Gemini
freespace, but have not selected the sample tube file for the balance
tube on port 2.

Action:Select a sample tube file for port 2 describing the balance tube used.

6010- This sample requires a different adsorptive and cannot be analyzed at thesame time as the other samples.

Cause:You selected a sample file for analysis that requires a different adsorptive gas than the sample file already selected.

Action:Select only sample files to be analyzed with the same adsorptive
and perform the analysis. Then perform the analysis with the otheradsorptive.

6011- The adsorptive required by this analysis is not available on this instrument.

Cause:

You attempted to start an analysis with an adsorptive that is not connected to the instrument.

Action A:

Make sure that the adsorptive is connected to the instrument, andthen select the unit configuration item of this unit’s menu to tell theapplication that the gas is connected.

Action B: Select only sample files for which the analysis gas is available.

B-18

Jan 05TriStar 3000

Appendix B

6012601360146015-

Cannot read the analysis conditions parameter file.
Cannot read the adsorptive properties parameter file.
Cannot read the report options parameter file.
Cannot read the sample tube properties parameter file.

Cause:The parameter set you selected on the QuickStart opening screen
cannot be read.

Action:Close ands restart QuickStart analysis and reselect the parametersfrom the available set.

6016- Dosing manifold from valve (number) failed.

Cause A:The maximum time was exceeded before the target pressure point
was reached. The nitrogen regulator may be set too low or turned
off.

Action A:

Set the analysis gas regulator to 10 psig (0.7 bar), then resume theanalysis.

Cause B:

The analysis gas bottle is empty.

Action B: Connect a new analysis gas bottle, then resume the analysis.

6017- Leak test failed on port (number).

Jan 05

Cause:

With the sample port valve closed, the sample pressure increased by
0.15 mmHg before the leak test duration was completed.

Action:Check sample tube fitting and ensure that it is securely attached tothe port, then restart the analysis.

B-19

Appendix B

TriStar6019- Elevator failed to reach upper/lower limit switch.

Cause A:The maximum time for the analysis was exceeded before the elevator reached the UP position. Ice may be present in the bottom or
the neck of the dewar.

Action A:

Check the dewar and remove ice if necessary. Then restart the analysis.

Cause B:The Psat tube is interfering with elevator movement.

Action B: Make sure the Psat tube is close to the sample tube and the dewar
cover is over both the sample and Psat tubes. Then restart the analysis.

6020- Warning, servo valve performance is out of specification.

Cause:The servo valve tried to dose to a pressure but was unable to reach
it within specification. The analysis will continue.

Action:At the next appropriate time, calibrate the servo valve to bring itback within specification (refer to Chapter 9).

6021- Servo calibration failed.

Cause A:The maximum time was exceeded before the target pressure point
was reached. The nitrogen regulator may be set too low or turned
off.

Action A:

Set the analysis gas regulator to 10 psig (0.7 bar), then resume theanalysis.

Cause B:

The analysis gas bottle is empty.

Action B: Connect a new analysis gas bottle, then resume the analysis.

6022- This file already selected for the analysis.

B-20

Cause:

You tried to choose a file for this analysis which has been selected
for another analysis.

Action:Choose a different file.

Jan 05TriStar 3000

Appendix B

6023- The instrument (number) is not calibrated.

Cause:The TriStar application is in the process of initializing the instrument and has noticed that no calibration information is available forthat unit.

Action:Click OK . When the instrument has initialized, open the calibration screen and calibrate the instrument.

6024- Evacuation failed.

Cause:

While attempting to zero the pressure transducers, the instrument
was unable to evacuate to a pressure of less than 1 mmHg. Thismay be due to a leak or a bad calibration.

Action A:

Check the sample tube fitting and ensure that it is securely attachedto the port.

Action B: Calibrate the pressure offsset. If this calibration fails because thesystem cannot be evacuated, select Reset pressure calibration fromthe Calibration menu to restore the factory calibration settings. This
will overwrite the current calibration settings.

6026- Psat gas is not condensing.

Cause A:The working Dewar does not contain enough bath liquid.

Action A:

Refill the Dewar and try the operation again.

Cause B:The Psat gas is contaminated.

Action B: Replace the Psat gas supply.
Cause C:The Psat tubing from the regulator to the instrument is contaminated.

Action C: Pump out the tubing.

Jan 05

B-21

APPENDIX CCALCULATIONSTriStar 3000

Appendix C

CALCULATIONSThis appendix contains the calculations used in the TriStar program.

Saturation Pressure (Po)Po method is selected by the user on the Po and Temperature Options dialog box. It
may be entered or measured in the Po tube or on port 3.
•

If entered, Po = user-entered value•

If measured, Po = equilibrated pressure reading after saturating Po tube or the
sample tube

Relative Pressure Calculations
If Po was measured at intervals in the Po tube and several data points were collectedin the interval:•

For points taken before the previous Po measurement,
PoI = Po1 +•(Po2 − Po1) x (TI − To1)
(To 2 − To 1)

For points taken after the previous Po, use the previous Po:
Po I = Po1

If Po was entered, use the entered Po:
PoI = PoE
Calculate relative pressure for the Ith data point:
PRELI =

Feb 03

PI
PoI

C-1

Appendix C

TriStar 3000

where:
PoI
Po1
Po2
PoE
TI
To1
To2
PRELI
PI

C-2

= saturation pressure for the Ith data point (mmHg)= most previous measured saturation pressure before Ith data
point (mmHg)= first measured saturation pressure after the Ith data point (mmHg)= entered saturation pressure (mmHg)= time when the Ith data point was taken (minutes)= time when Po1 was measured (minutes)= time when Po2 was measured (minutes)= relative pressure for the Ith data point (mmHg)= absolute pressure for the Ith data point, taken at equilibrium (mmHg)

Feb 03

TriStar 3000

Appendix C

Volume Adsorbed Calculations
Free Space
The free space can be measured, calculated, entered, or obtained using the QuasiGemini method. The quantities used for the data reduction are the warm free space(VFW), the cold free space (VFC), and the analysis bath temperature.

Measured, Calculated, and Entered
For measured free space, the cold and warm free space volumes are calculated as follows:
VFW =

 P1

VMAN
− 1 x TSTD
x 
T1
 P2


VFC =

 P1

VMAN
x 
− 1 x TSTD
T2
 P3


For calculated free space, the cold and warm free space volumes are calculated inthree steps.
First, the sample volume is determined:
VSAMP =

WSAMP
DSAMP

Second, the warm and cold portions of the free space are determined:•

With a filler rod:
VFWP = (VPORT + VSTEMWARM ) x

TSTD
TMAN

VFCP = (VBELOW + VSTEMCOLD − VSAM) x

Feb 03

TSTD
TANLS

C-3

Appendix C

TriStar 3000•

Without a filler rod:
VFWP = (VPORT + VSTEMWARM + VRODWARM ) x

TSTD
TMAN

VFCP = (VBELOW + VSTEMCOLD − VSAMP + VRODCOLD) x

TSTD
TANLS

Third, the warm and cold free space volumes are calculated:
VFC = VFWP + VFCP
VFW = VFWP + VFCP x

TANLS
TROOM

The volume of the analysis bath temperature is calculated as follows:
VABT =

VFC − VFW
TABT
1−
TRM

where:

C-4

DSAMP
P1
P2
P3

=
=
=
=

T1
T2

=
=

TABT

=

TANLS
TRM
TSTD
VABT

=
=
=
=

VBELOW
VFC
VFCP
VFW
VFWP
VMAN
VPORT

=
=
=
=
=
=
=

sample density (g/cm3)
system manifold pressure before dosing helium onto sample (mmHg)
system manifold pressure after dosing helium onto sample (mmHg)
sample pressure after raising Dewar and equilibrating withhelium (mmHg)
system manifold temperature before dosing helium onto sample (K)system manifold temperature after raising Dewar andequilibrating with helium (K)analysis bath temperature (K), from the Po and Temperature
Options dialog box
analysis temperature (K)approximate room temperature (298 K)
standard temperature (273.13 K)
portion of cold free space at analysis bath temperature:used in non-ideality correction (cm3 at standard temperature)
volume of the sample tube below the red line
volume of cold free space (cm3 at standard temperature)cold portion of free space (cm3 at standard temperature)
volume of warm free space (cm3 at standard temperature)warm portion of free space (cm3 at standard temperature)
manifold volume (cm3)sample port volume (cm3)

Feb 03

TriStar 3000

Appendix C

VRODCOLD = filler rod cold portion volume (cm3)
VRODWARM = filler rod warm portion volume (cm3)= sample volume
VSAMP
VSTEMCOLD = Sample tube cold portion above the red line
VSTEMWARM = sample tube warm portion volume (cm3)= sample weight (g)WSAMP
For the Ith dose: PSYS1I PSYS2I  TSTD−NGASI = NGASI−1 + VMAN x x TSYS1I TSYS2I  PSTDNADSI = NGASI - PSAMPI ÷ PSTD x (VFC + PSAMPI x VABT x C)
VI =

NADSI
WSAMP

where:
C
NADSI
NGASI
PSTD
PSYS1IPSYS2IPSAMPI
TSTD
TSYS1ITSYS2I
VABT
VFC
VMAN
WSAMP
VI

Feb 03= nonideality correction factor, user-entered on Adsorptive
Properties dialog box= amount of gas adsorbed after equilibrating Ith dose (cm3 STP)
= total amount of gas dosed into sample tube after Ith dose (cm3 STP)
= standard pressure (760 mmHg)= system manifold pressure before Ith dose of gas onto
sample (mmHg)= system manifold pressure after Ith dose of gas onto
sample (mmHg)= sample pressure after equilibrating Ith dose of gas onto
sample (mmHg)= standard temperature (273.13 K)= system manifold temperature before Ith dose of gas onto
sample (K)= system manifold temperature after Ith dose of gas onto
sample (K)= portion of cold free space at analysis bath temperature:used in non-ideality correction (cm3 at standard temperature)= volume of cold free space (cm3 at standard temperature)= manifold volume (cm3)= weight of sample (g)= amount of gas adsorbed per gram of sample (cm3/g STP)

C-5

Appendix C

TriStar 3000

Quasi Gemini
The quantity adsorbed, NADSi, is calculated as follows:
NADSI = NDOSEDI - ComputedColdSampleGas - BlankPressureCorrection x(NBLANKI - ComputedColdBlankGas)
where:
ComputedColdSampleGas = PsamI
 RSTD 
x VFCPSAMP x ]x (1 + PSAMPI x C)
 PSTD TANLS 
BlankPressureCorrection =PSAMPI x (1 + PSAMPI x C)
PBLANKI x (1 + PBLANKI x C)

ComputedColdBlankGas = PBLANKI
TSTD 
x VFCPBLANK x
 x (1 + PBLANKI x C)
TANLS 
 PSTDNDOSEDINBLANKI
PBLANK
PSAMPI
PSTD
TANLS
TSTD
VFCPBLANKVFCPSAMP
VSAMP

C-6

total quantity dosed for the Ith point
volume dosed into the blank tube
pressure of the blank tube
pressure at which the equilibrated sample point was taken
standard pressure (760 mmHg)
analysis temperature (K)standard temperature (273.13 K)
cold portion of free space for blank tube (see calculation for
calculated free space)= Cold portion of free space for sample tube (see calculation for
calculated free space)= sample volume
=
=
=
=
=
=
=
=

Feb 03

TriStar 3000

Appendix C

Equilibration
Equilibration is reached when the pressure change per equilibration time interval (first
derivative) is less than 0.01% of the average pressure during the interval. Both thefirst derivative and average pressure are calculated using the Savitzky-Golay1 convolution method for polynomial functions. The equations below are those used to compute weighted average and first derivative, respectively, for the 6th point of an
11-point window.
PAVG =−36(P1 + P11) + 9(P2 + P10) + 44(P3 + P9) + 69(P4 + P8) + 84(P5 + P7) + 89(P6)429

PCHG =

5(P1 − P11) + 4(P2 − P10) + 3(P3 − P9) + 2(P4 − P8) + (P5 − P7)
110

PPCPI = 100%

PCHG
PAVG

where the numerical constants are from the Savitzky-Golay convolution arrays, and
PAVG
PCHG
PPCPI
PI

=
=
=
=

average pressure (mmHg)
change in pressure (mmHg)
Percent change per interval
Ith pressure reading taken at equilibrium intervals (mmHg)

If the value you enter for the maximum equilibration time is too small, thepoints are collected before equilibration is reached.

If PAVG is greater than 0.995 times the current Po, equilibration will not takeplace until the Minimum equilibration delay for P/Po > 0.995 has expired, in addition to the standard equilibration criteria.

Feb 03C-7

Appendix C

TriStar 3000

BET Surface Area Calculations2
For each point designated for surface area calculations, the BET transformation is calculated as follows:
PrelI(1.0 − PrelI) x NadsI

BI =where BI is in units of g/cm3 STP.
A least-squares fit is performed on the (PrelI ,BI) designated pairs where PrelI is the independent variable and BI is the dependent variable. The following are calculated:
a. Slope (S g/cm3 STP)
b. Y-intercept (YINT g/cm3 STP)
c. Error of the slope (SERR g/cm3 STP)
d. Error of the y-intercept (YIERR g/cm3 STP)e. Correlation coefficient (Cc)
Using the results of the above calculations, the following can be calculated:
BET Surface Area (m2/g):

SABET =CSA x (6.023 x 1023)(22414 cm3 STP) x (1018 nm2⁄m2) x (S + YINT)

where= analysis gas molecular cross-sectional area (nm2), user-enteredon the Adsorptive Properties dialog box

CSA
BET C value:C =S + YINT
YINT

Volume of the Monolayer (cm3/g STP):

VM =

C-8

1
1
=
C x YINTS + YINT

Feb 03

TriStar 3000

Appendix C

Error of the BET Surface Area (m2/g):

BETERR =SABET x (SERR2 + YIERR2)0.5
YINT + S

Langmuir Surface Area Calculations
For each point designated for surface area calculations, the Langmuir3 transformation
is calculated as follows:

LI =

PrelI
NadsI

where LI is in units of g/cm3 STP
A least-squares fit is performed on the (PrelI ,LI) designated pairs where PrelI is the independent variable and LI is the dependent variable. The following are calculated:
a. Slope (S g/cm3 STP)
b. Y-intercept (YINT g/cm3 STP)
c. Error of the slope (SERR g/cm3 STP)
d. Error of the y-intercept (YIERR g/cm3 STP)e. Correlation coefficient (Cc)
Using the results of the above calculations, the following can be calculated:
Langmuir Surface Area (m2/g):

SALAN =CSA x (6.023 X 1023)(22414 cm3 STP) x (1018 nm2⁄m2) x S

where
CSA

Feb 03= analysis gas molecular cross-sectional area (nm2), user-enteredon the Adsorptive Properties dialog box

C-9

Appendix C

TriStar 3000

Volume of the Monolayer (cm3/g STP):

VM =

1
S

Langmuir b Value:b = (YINT) (VM)

Error of the Langmuir Surface Area (m2/g):

LANERR =C-10

SALAN x SERRS

Feb 03

TriStar 3000

Appendix C

t-Plot Calculations4
For each point designated for t-Plot calculations, the following calculations are done:
Thickness for the Ith point (Å):
HP3

 HP2 tI = HP1 x ln(PrelI) (Halsey5 )

or
HJP3

HJP1
tI = 
(Harkins and Jura6)
HJP2 − log(PrelI) ortI = STSA1(PrelI)2 + STSA2(PrelI) + STSA3
where:
tI
HP1
HP2
HP3
HJP1
HJP2
HJP3
PrelI
STSA1
STSA2
STSA3

=
=
=
=
=
=
=
=
=
=
=

thickness for Ith point
Halsey parameter #1
Halsey parameter #2
Halsey parameter #3
Harkins and Jura parameter #1
Harkins and Jura parameter #2
Harkins and Jura parameter #3
relative pressure for the Ith point (mmHg)
statistical thickness surface area parameter #1
statistical thickness surface area parameter #2
statistical thickness surface area parameter #3

A least-squares analysis fit is performed on the (tI, NadsI) data pairs where tI is the independent variable and NadsI is the dependent variable. Only the values of tI betweentMIN and tMAX, the minimum and maximum thickness, are used. The following are calculated:
a. Slope (S cm3/g-Å STP)
b. Y-intercept (YINT cm3/g STP)
c. Error of the slope (SERR cm3/g-Å STP)

Feb 03

C-11

Appendix C

TriStar 3000

d. Error of the Y-intercept (YIERR cm3/g STP)e. Correlation coefficient (Cc)
Using the results of the above calculations, the following can be calculated:
External Surface Area (m2/g):

SAEXT =

(S cm3 ⁄ g−Å STP) x (1010 Å ⁄ m) x (D cm3 liquid ⁄ cm3 STP)
F x (106 cm3 ⁄ m3 )

where
F
D

= surface area correction factor, user-entered on the t-Polot Report
Options dialog box= density conversion factor, user-entered on the Adsorptive
Properties dialog box

Micropore Surface Area (m2/g):

SAµP = SATOT − SAEXT
where SATOT is the BET surface area if the user enabled the BET report exclusively,or Langmuir surface area if the user enabled the Langmuir report exclusively. If neither report has been selected, SATOT is the BET surface area value calculated using a
set of default parameters.
Micropore Volume (cm3 liquid/g):

VµP = (YINT cm3 ⁄ g STP) x (D cm3 liquid ⁄ cm3 STP)

C-12

Feb 03

TriStar 3000

Appendix C

BJH Pore Volume and Area Distribution Calculations
For adsorption data, the relative pressure and volume adsorbed data point pairs collected during an analysis must be arranged in reverse order from which the points
were collected during analysis. All calculations are performed based on a desorption
model, regardless of whether adsorption or desorption data are being used.
The data used in these calculations must be in order of strictly decreasing numericalvalue. Points which do not meet this criterion are omitted. The remaining data set iscomposed of relative pressure (Pr), volume adsorbed (Va) pairs from (Pr1, Va1) to(PrN, VaN) where (PrN = 0, VaN = 0) is assumed as a final point. Each data pair represents an interval boundary (or desorption step boundary) for intervals i=1 to i=N-1
where N = total number of (Pr, Va) pairs.
Generally, the desorption branch of an isotherm is used to relate the amount of adsorbate lost in a desorption step to the average size of pores emptied in the step. A poreloses its condensed liquid adsorbate, known as the core of the pore, at a particular
relative pressure related to the core radius by the Kelvin7 equation. After the core has
evaporated, a layer of adsorbate remains on the wall of the pore. The thickness of
this layer is calculated for a particular relative pressure from the thickness equation.
This layer becomes thinner with successive decreases in pressure, so that the measured quantity of gas desorbed in a step is composed of a quantity equivalent to theliquid cores evaporated in that step plus the quantity desorbed from the pore walls ofpores whose cores have been evaporated in that and previous steps. Barrett, Joyner,and Halenda8 developed the method (known as the BJH method) which incorporates
these ideas. The algorithm used on the TriStar 3000 is an implementation of the BJH
method.

Explanation of Terms
A pore filled with condensed liquid nitrogen has three zones:

Feb 03a.

The core - evaporates all at once when the critical pressure for that radius isreached; the relationship between the core radius and the critical pressure isdefined by the Kelvin equation.

b.

The adsorbed layer - composed of adsorbed gas that is stripped off a bit ata time with each pressure step; the relationship between the thickness of thelayer and the relative pressure is defined by the thickness equation.

C-13

Appendix C

TriStar 3000

c.

The walls of the cylindrical pore - the diameter of the empty pore is required to determine the pore volume and pore area. End area is neglected.

pore
a
d
s
o
r
b
e
d

c
o
r
e

wall

l
a
y
e
r

Insignificant
compared tocore length

Calculations
The volumes adsorbed (Va) are converted to the liquid equivalent volumes (V1,
cm3/g):

VlI = (Va I)(D)
where D is the Density Conversion Factor from the Adsorptive Properties dialog box.
The relative pressure (Pr1) is assumed to be close to unity so that substantially all thepores in the sample are filled.
The corresponding Kelvin core radius is calculated. Only pores smaller than this size
will be included:

Rc1 =

−A
(1 + F)[ln(Pr1)]

where
A
F

= adsorbate property factor (the BJH Adsorptive Options dialog box)
= fraction of pores open at both ends (from the BJH Adsorption
Report Options dialog box or the BJH Desorption Report Options
dialog box); assumed to be zero for desorption

This radius will be adjusted for the thickness of the adsorbed layer during subsequentcalculation steps.

C-14

Feb 03

TriStar 3000

Appendix C

The thickness of the remaining adsorbed layer at this relative pressure is calculated:HP3

 HP2 Tw1 = HP1  ln(Pr1) 
where

HP1, HP2, and HP3 are Halsey Parameters 1, 2, and 3 (respectively) from the Halsey
Thickness Equation dialog box.
These calculations illustrate the use of the Halsey thickness equation. If the HarkinsJura equation was selected, substitute the following wherever the thickness equation
appears:
HJ3

HJ1


Tw1 = 

Pr
)
HJ2
−
log(
1


where

HJ1, HJ2, and HJ3 are Harkins-Jura Parameters 1, 2, and 3 (respectively) from theHarkins-Jura Thickness Equation dialog box.
The following calculations (a-c) are made for each relative pressure interval based on
the increment of volume desorbed during that interval. The variable I refers to the interval number, that is I=1 for the first interval from Pr1 to Pr2, and so on. J refers toeach previous interval during which new pores were found. K refers to the total number of intervals in which new pores have been found. K is also the number of lines
reported on the BJH table for collected data.
a.

The thickness of the adsorbed layer at the end of the interval is calculated asfollows:HP3

 HP2 Tw1+1 = HP1  ln(Pr1+1) (For the last pressure interval from the lowest PrI to zero relative pressure,
TwI+1 = 0.)
For the first pressure interval, there are no previously opened pores so thevolume desorbed from walls of previously opened pores is zero (Vd1 = 0),
and the remainder of Step a is skipped.
The change in thickness of the wall layer due to desorption from preivously
opened pores is calculated:∆Tw = Tw I − TwI+1

Feb 03

C-15

Appendix C

TriStar 3000

The annular cross-sectional area of the wall layer desorbed is calculated forall previously opened pores:
CSAJ = π [(Rcj + ∆Tw)2 − Rcj 2] (10−16 cm2 ⁄ A2)
The total volume of gas desorbed from walls of previously opened pores iscalculated:
VdI = ∑(LpJ)(CSAaJ) for all previously opened pores
where LPJ = length of previously opened pores as calculated in Step
b(2).
b.

The physical processes occurring for this pressure interval are determined asfollows:(1) If VdI is greater than the current increment of volume desorbed(VlI - VlI+1 ), desorption from walls only is occurring. Total surface ofwalls exposed thus far (cm2/g) is calculated as follows:
SAw = ∑ π (LpJ)(DavgJ)(10−8 cm ⁄ A) for all previously opened pores
where
DavgJ = weighted average pore diameter calculated below in
Step b(2).
A new layer thickness (∆Tw) that will not overcompensate for the actual volume desorbed in this interval is calculated:∆Tw =(VlI − VlI+1)(108 A ⁄ cm)
SAw I

Since no cores are evaporated in this pressure interval, no new poresare revealed. Thus no ending Kelvin radius and average pore diameterare calculated for this interval. Note that this means the report may
have fewer tabulated intervals on the collected data report than experimental pressure intervals.
(2) If VdI is less than the volume increment desorbed during this interval(VlI − VlI+1) the remaining volume is due to new pores with core evaporation taking place in this interval. K, the number of intervals with new
pores exposed, is increased by 1. (For the interval from the lowest PrI
to zero relative pressure, no new pore volume is calculated and the restof Step b is skipped.)

C-16

Feb 03

TriStar 3000

Appendix C

The volume desorbed from newly opened pores in this interval is calculated as follows:
VcI = (VlI − VlI+1) − VdI
The Kelvin radius for the end of the interval is calculated as follows:
RcK+1 =

−A
(1 + F)[ln(PrI+1)]

All new pores opened in this interval are represented by one pore having a length-weighted average pore diameter and a corresponding length
sufficient to account for the required volume of adsorbate. The weighted
average pore diameter is calculated as follows:
DavgK =

(2) (RcK + RcK+1) (RcK) (RcK+1)
RcK 2 + RcK+1 2

DavgK is the diameter of a pore which would have a surface area that is
the average of the areas for pores with radius RcK and RcK+1, if its
length was the mean of the lengths at those radii.
The relative pressure corresponding to DavgK is calculated as follows:−2A

PavgK = ln−1 (1 + F)(DavgK) The thickness of the adsorbed layer at this pressure is calculated as follows:HP3

 HP2 Tw avgK = HP1ln(PavgK) Feb 03C-17

Appendix C

TriStar 3000

The decrease in thickness of the wall layer by desorption from the wallsof new pores during the lower portion of the pressure interval is calculated as follows:∆Td = Tw avgK − Tw I+1
The cross-sectional area of the newly opened pores is calculated as follows:2 DavgK+ ∆Td (10−16 cm2 ⁄ A2)
CSAcK =  2The length of the newly opened pores is calculated as follows:
LpK =
c.

VcI
CSAcK

Pore diameters and radii are adjusted for the change in thickness of the adsorbed wall layer during this interval. If new pores were opened during thisinterval, the average diameter is adjusted by the change in layer thickness
during the second portion of the desorption interval as follows:
DavgK

new

= DavgKold+ 2(∆Td)

The layer thickness change during the whole interval is added to diametersof previously opened pores as follows:
DavgJ

new

= DavgJold+ 2(∆Tw )(not including DavgK)The layer thickness change desorbed during this interval also is added to theradii corresponding to the ends of the pressure intervals as follows:
RcJnew = RcJold + ∆Tw
for all except RcK+1.
Steps a to c are repeated for each pressure interval.

C-18

Feb 03

TriStar 3000

Appendix C

After the above calculations have been performed, the diameters corresponding to the ends of the intervals are calculated as follows:
DpJ = 2(RcJ)
for all RcJ including RcK+1.
The remaining calculations are based on Dp(I), Davg(I), and Lp(I). These calculations are only done for Davg(I) values that fall between the Minimum BJH
diameter and the Maximum BJH diameter specified by the operator on the
BJH Adsorption Report Options dialog box or the BJH Desorption Report
Options dialog box.
1)

Incremental Pore Volume (VpI,cm3 ⁄ g):2

 DavgI 
VpI = π (LpI)  1016 cm2 ⁄ A2
2


2)

Cumulative Pore Volume (VpCUM(I), cm3 ⁄ g):
VpCUM(I) = ∑ VpJ for J ≤ I

3)Incremental Surface Area (SAI, m2 ⁄ g):
SAI = π (LpI)(10−2 m ⁄ cm)(DavgI)(10−10 m ⁄ A)

4)

Cumulative Surface Area (SACUM(I), m2 ⁄ g):
SACUM(I) = ∑ SAJ for J ≤ I

5)dV/dD pore volume (dV ⁄ dDI, cm3 ⁄ g−A):dV ⁄ dDI =6)

VPI
DpI − DpI+1

dV/dlog(D) pore volume (dV ⁄ dlog(D)I, cm3 ⁄ g):dV ⁄ dlog(D)I = VpI ⁄ log(DpI ⁄ DpI+1)

Feb 03

C-19

Appendix C

TriStar 3000

7)dA/dD pore area (dA ⁄ dDI, m2 ⁄ g−A):
dA ⁄ dDI =8)

SAI
DpI − DpI+1

dA/dlog(D) pore area [dA ⁄ dlog(D)I, m2 ⁄ g]:dA ⁄ dlog(D)I = SAI ⁄ log(DPI ⁄ DpI+1)

For fixed pore size tables (if selected), the following calculations are performed:
1)

Average Fixed Pore Size (DFavgJ, A):
DFavgJ =DpFJ + DpFJ+1
2

calculated for all intervals in the fixed pore size table.
For the intervals with DFavgI between the Minimum BJH diameter and theMaximum BJH diameter.
2)

Cumulative Pore volume (VpFCUMI, cm3 ⁄ g):
VpFCUMI = INTERP(DpFI+1)
where INTERP(x) is the value interpolated from the function X = DpJ+1 andY = VpCUMJ, using an AKIMA semi-spline interpolation.

3)

Incremental Pore Volume (VpFI, cm3 ⁄ g):
VpFI = VpFCUMI − VpFCUMI−1
where VpFCUM0 = 0.

4)

Cumulative Surface Area (SAFCUMI, m2 ⁄ g):
SAFCUMI = INTERP(DpFI+1)
where INTERP(x) is the value interpolated from the function X = DpJ+1 andY = SACUMJ.

C-20

Feb 03

TriStar 3000

Appendix C

5)

Incremental Surface Area (SAFI, m2 ⁄ g):
SAFI = SAFCUMI − SAFCUMI−1
where SAFCUM0 = 0.

6)

dV/dD pore volume (dV ⁄ dDpFI, cm3 ⁄ g−A):dV ⁄ dDpFI = INTERP(DpFI+1)
where INTERP(x) is the value interpolated from the function X = DavgJ and
Y = dV ⁄ dDJ.

7)

dV/dlog(D) pore volume [dV ⁄ dlog(DpF)I, cm3 ⁄ g]:dV ⁄ dlog(DpFI = INTERP(DpFI+1)
where INTERP(x) is the value interpolated from the function X = DavgJ and
Y = dV ⁄ dlog(D)J.

8)

dA/dD pore area (dA ⁄ dDpFI, m2 ⁄ g−A):
dA ⁄ dDpFI = INTERP(DpFI+1).
where INTERP(x) is the value interpolated from the function X = DavgJ and
Y = dA ⁄ dDJ.

9)

dA/dlog(D) pore area [dA ⁄ dlog(DpFI ), m2 ⁄ g]:dA ⁄ dlog(DpFI = INTERP(DpFI+1)
where INTERP(x) is the value interpolated from the function X = DavgJ and
Y = dA ⁄ dlog(D)J.

Feb 03C-21

Appendix C

TriStar 3000

Compendium of Variables
Va
Vl
D
Pr
Dp
Rc
A
F
∆Tw
Tw

= quantity adsorbed expressed as a volume (cm3/g STP)
= liquid equivalent volume of volume adsorbed (cm3/g)= density conversion factor from the Adsorptive Properties dialog box(cm3/cm3 STP)
= relative pressure= pore (or core) diameter (A)= Kelvin radius (A) of core
= adsorbate property factor; from the BJH Adsorptive Options dialog box= fraction of pores open at both ends; from the BJH Adsorption Report
Options dialog box or the BJH Desorption Report Options dialog box= thickness of adsorbed layer desorbed during interval (A)= thickness of remaining adsorbed wall (A)HP1, HP2, and HP3 are Halsey parameters from the Halsey Thickness Equation dialog box.
HJ1, HJ2, and HJ3 are Harkins and Jura parameters from the Harkins-Jura Thickness
Equation dialog box.
STSA1, STSA2, and STSA3 are STSA parameters from the STSA Thickness Equation dialog box.
Vd
Davg
CSAa
CSAc
SAw
∆Td
Vc
Lp

C-22

=
=
=
=
=
=
=
=

volume of gas desorbed from walls of previously opened pores (cm3/g)
average pore diameter (A)annular cross-sectional area of the desorbed layer (cm2)cross-sectional area of opening of newly opened pores (cm2)total surface area of walls exposed (cm2/g)
thickness of layer desorbed from walls of newly opened pores (A)volume desorbed from cores of newly opened pores (cm3/g)
length of pore (cm/g)

Feb 03

TriStar 3000

Appendix C

Dubinin-Radushkevich Calculations9The Dubinin-Radushkevich equation is as follows:
2

B x T2 Po 
x log log (V) = log (Vo ) −βPwhere:
V
Vo
Po
P
B
β
T

volume adsorbed at equilibrium pressure (cm3/g STP)
the micropore capacity (cm3/g STP)
saturation vapor pressure of gas at temperature T (mmHg)
equilibrium pressure (mmHg)
a constant
the affinity coefficient of analysis gas relative to Po gas(for this application β is taken to be 1)= analysis bath temperature (K), from the Po and Temperature
Options dialog box

=
=
=
=
=
=

For each point designated for Dubinin-Radushkevich calculations, the following calculations are done:
LV = log (V)2 Po 
LP = log  PThe intercept, log(Vo) can be found by performing a least-squares fit on the (LP,LV)
designated pairs where LP is the independent variable and LV is the dependent variable. Assuming the adsorption of gas is restricted to a monolayer, Vo is the monolayer capacity. Based on this assumption, the following are calculated:
a. Slope (S cm3/g STP)
b. Y-intercept (YI cm3/g STP)
c. Error of the slope (SERR cm3/g STP)
d. Error of the y-intercept (YIERR cm3/g STP)e. Correlation coefficient (Cc)

Feb 03

C-23

Appendix C

TriStar 3000

Using the results of the above calculations, the following can be calculated:
Monolayer Capacity (cm3/g STP):
Vo = 10YI

Error of Monolayer Capacity (cm3/g STP):VoERR = Vo x (10YIERR - 1.0)
Micropore surface area (m2/g):
SDP =σ x Vo x (6.023 x 1023)
22414 cm3 x (1018 nm2 ⁄ m2)

where:σC-24= molecular cross sectional area of gas (nm2)from the Adsorptive Properties dialog box

Feb 03

TriStar 3000

Appendix C

Dubinin-Astakhov Calculations
The Dubinin-Astakhov equation is a follows:NN (R x T)   Po log (V) = log (Vo) −  x log P  βEo  
where:
V
Vo
Po
P
T
R
E0
N
β

volume adsorbed at equilibrium pressure (cm3/g STP)
the micropore capacity (cm3/g STP)
saturation vapor pressure of gas at temperature T (mmHg)
equilibrium pressure (mmHg)
analysis bath temperature (K)the gas constant (0.0083144 KJ/K-mole)characteristic energy (KJ/mole)
Astakhov exponent, may be optimized or user enteredfrom the Dubinin Report Options dialog box= the affinity coefficient of the analysis gas relative to the Po gas,from the Dubinin Adsorptive Options dialog box

=
=
=
=
=
=
=
=

For each point designated for Dubinin-Astakhov calculations, the following calculations are done:
LV = log(V)
N


Po 
LP = log PA least-squares fit is performed on the (LP,LV) designated pairs where LP is the independent variable and LV is the dependent variable. If the user selected yes for the Optimize Astakhov Exponent prompt, a systematic search for the optimum value of N is
conducted by recalculating the linear regression and selecting the value of N thatgives the smallest standard error of the y-intercept. The exponent N is optimized towithin 10-4. If the optimum value for N is not found in this range, an exponent of 2
is used. The following are calculated:
a. Slope (S cm3/g STP)
b. Y-intercept (YI cm3/g STP)
c. Error of the slope (SERR cm3/g STP)
d. Error of the y-intercept (YIERR cm3/g STP)e. Correlation coefficient (Cc)

Feb 03C-25

Appendix C

TriStar 3000f.

Optimized Astakhov exponent (N)Using the results of the above calculations, the following can be calculated:
Monolayer Capacity (cm3/g STP):
Vo = 10YI
Micropore Volume (cm3/g):
WI = (VI x D)
where
= density conversion factor (cm3 liquid/cm3 STP)
from the Adsorptive Properties dialog box

D

Limiting Micropore Volume (cm3/g):
Wo = (Vo x D)
where
= density conversion factor (cm3 liquid/cm3 STP)
from the Adsorptive Properties dialog box

D

Error of Limiting Micropore Volume (cm3/g):
WoERR = Wo x (10YIERR - 1.0)

Characteristic Energy (KJ/mole):
E =

C-26

2.303 x R x T
1(2.303 x S) ⁄N

Feb 03

TriStar 3000

Appendix C

Modal Equivalent Pore Diameter (Å):
1⁄N

1⁄3


  3N 
DMODE = 2 x  
3N + 1  103 nm3 ⁄ Å3  x  β ⋅ Eo  

where
β

= affinity coefficient of the analysis gas relative to the Po gas
from the Dubinin Adsorptive Options dialog box

Maximum Differential Pore Volume (cm3/g-Å):This value is also known as frequency of the mode12dV 3N + 1 
Max = 0.5 x (3N + 1) x Wo x dDmode 3N 

1⁄3N

1⁄3
 3N + 1 −β ⋅ E0 3N 
x 3
33  xe (10 nm ⁄ Å ) Mean Equivalent Pore Diameter (Å)
1⁄3 103 nm3 ⁄ Å3 

 β⋅E
o

DMEAN = 2 x  3N + 1 Γ 3N 

Micropore surface area (m2/g):
 3N + 1  β ⋅ E  ⁄3xΓ
SDA = 10000 x 2.0 x Wo x  3
33
 3N 
 10 nm ⁄ Å 1

Γ is calculated by a polynomial approximation11 over the domain 0 ≤ x ≤ 1 as follows:Γ(x+1) = 1+b1x + b2x2 + b3x3 + b4x4 + b5x5 + b6x6 + b7x7 + b8x8 + ε(x)| ε(x) | ≤ 3 x 10-7

Feb 03C-27

Appendix C

TriStar 3000

b1
b2
b3
b4
b5
b6
b7
b8

=
=
=
=
=
=
=
=

-0.57719 1652
0.98820 5891
-0.89705 6937
0.91820 6857
-0.75670 4078
0.48219 9394
-0.19352 7818
0.03586 8343

and where 3N +1 
x+1 = 
 3N 

Equivalent Pore diameter (Å):
N

1⁄3N

  3 3 3  − 10 nm ⁄ Å  β ⋅ E0  
DI = 2 x   ln(WI) − ln(Wo) 

dV/dD Pore Volume (cm3/g-Å): 103 nm3 ⁄ Å3 dV

= 0.5 x Wo x 3N x dDI β ⋅ E0 


N

−3N

  3
 10 nm3 ⁄ Å3   DI x e − x 2  β ⋅ E0
  


C-28

 DI x  2

−(3N+1)Feb 03

TriStar 3000

Appendix C

MP-Method Calculations10
For each point designated for MP-method calculations, the following calculations are
done:
Thickness for the Ith point (Å):
HP3

 HP2 tI = HP1 x ln(PrelI) (Halsey5 )

or
tI =

HJP3
HJP1
(Harkins and Jura6)
HJP2 − log(PrelI)

where:
tI
HP1
HP2
HP3
HJP1
HJP2
HJP3
PrelI

=
=
=
=
=
=
=
=

thickness for Ith point
Halsey parameter #1
Halsey parameter #2
Halsey parameter #3
Harkins and Jura parameter #1
Harkins and Jura parameter #2
Harkins and Jura parameter #3
relative pressure for the Ith point (mmHg)

With the (tI,VI) data pairs, the Akima semi-spline interpolation method is used to interpolate volume adsorbed values based on thickness values that are evenly spaced
0.2 Angstrom apart starting at the first outlier point. Outliers are defined as thosepoints have the maximum instantaneous slope within an iteratively shrinking subsetof all points. The remaining pore surface area calculation result is the slope of theline defined by two consecutive interpolated points. The slopes of each pair of consecutive points from the origin to the last point must be monotonically decreasing
and non-negative. With the interpolated points set the following can be calculated:

Feb 03C-29

Appendix C

TriStar 3000

Average pore hydraulic radius (Å):
RI =tI + tI−1
2

Remaining pore surface area for the Ith point (m2/g):
SI =(VI − VI−1) x (D x 10−6 m3 ⁄ cm3)
(tI − tI−1) x 10−10 m ⁄ Å

where
D

= density conversion factor (cm3 liquid/cm3 STP) on
the Adsorptive Properties dialog box

Incremental pore surface area occluded for the Ith point (m2/g):
SINCI = SI−1 − SI

Cumulative pore surface area occluded for the Ith point (m2/g):
SCUMI = SINCI + SINCI−1 + … + SINC1

dA/dR pore surface area for the Ith point (m2/g-Å):
SSINCIdA=tI − tI−1
dRI

Incremental pore volume occluded for the Ith point (cm3/g):
VINCI = (SINCI x 104 cm2 ⁄ m2 ) x (RI x 10−8 cm ⁄ Å)

C-30

Feb 03

TriStar 3000

Appendix C

Cumulative pore volume occluded for the Ith point (cm3/g):
VCUMI = VINCI + VINCI−1 + … + VINC1
dV/dR pore volume for the Ith point (cm3/g-Å):
VINCI
dV
=
tI − tI−1
dRI

Feb 03C-31

Appendix C

TriStar 3000

Summary Page
The following calculations and the results of previous calculations (as noted) are used
to generate the summary page:a. Single Point BET Surface Area (m2/g)
S1PT =[Va x (1−Pr)] x CSA x (6.023 x 1023 )
22414 cm3 STP x 1018 nm2 ⁄ m2

where
Pr
Va

= pressure closest to 0.3 of the relative pressure points designatedfor surface area calculations.
= volume corresponding to Pr

b. Multipoint BET Surface Area
See BET Surface Area Calculationsc. Langmuir Surface Area
See Langmuir Surface Area Calculations
d. t-Plot Micropore Surface Area
See t-Plot calculations.
e. t-Plot External Surface Area
See t-Plot calculations.
f.

BJH Cumulative Adsorption

g. BJH Cumulative Desorption
h. Adsorption Total Pore volumei.

Desorption Total Pore volumej.

t-Plot Micropore Pore Volume
See t-Plot calculations.

k. Average Pore Diameterl.

BJH Adsorption Average Pore Diameter

m. BJH Desorption Average Pore DiameterC-32

Feb 03

TriStar 3000

Appendix C

References
1.

Savitzky, A. and Golay, M.J.E., Anal. Chem. 36, 1627 (1964).

2.

Brunauer, S.; Emmett, P.H.; and Teller, E., J. Am. Chem. Soc. 60, 309 (1938).

3.

Langmuir, I., J. Am. Chem. Soc. 38, 2267 (1916); J. Am. Chem. Soc. 40,
1361 (1918); Phys. Rev 8, 149 (1916).

4.

deBoer, J.H., et al, J. Catalysis 3, 32, 38, 44, 268 (1964); J. Catalysis 4,319, 643, 649 (1965); Cranston, R. and Inkley, F., Adv. Catalysis 9, 143(1957).

5.

Halsey, G., J. Chem. Phys. 16, 931-937 (1948).

6.

Harkins, W.D. and Jura, G., J. Chem. Phys. 11, 431 (1943).

7.

Kelvin, J. (published under the name of Sir William Thomson), Phil. Mag.
42, 448-452 (1871).

8.

Barrett, E.P.; Joyner, L.S.; and Halenda, P.P., J. Am. Chem. Soc. 73, 373-380(1951).

9.

Dubinin, M., Carbon 21, 359 (1983); Dubinin, M., Progress in Surface andMembrane Science 9, 1, Academic Press, New York (1975); Dubinin, M. andAstakhov, V., Adv. Chem. Ser. 102, 69 (1971); Lamond, T. and Marsh, H.,
Carbon 1, 281, 293 (1964); Medek, J., Fuel 56, 131 (1977); Polanyi, M.,
Trans. Faraday Soc. 28, 316 (1932); Radushkevich, L., Zh. fiz. Kemi. 33,
2202 (1949); Stoeckli, H., et al, Carbon 27, 125 (1989).

10. Mikhail, R., Brunauer, S. and Bodor, E., J. Colloid and Interface Sci. 24, 45(1968).

Feb 03

C-33

APPENDIX D
FREE-SPACE CORRECTIONTriStar 3000

Appendix D

FREE-SPACE CORRECTION
Free space is that volume of the sample tube which is unoccupied by the sample.
The quantity of gas dosed into the sample tube is calculated from the differencein pressures in the manifold before and after the dose is delivered. The quantityof gas adsorbed by the sample is calculated by subtracting the quantity of gas remaining in the free space of the sample tube after equilibrium is established fromthe quantity of gas originally dosed into the sample tube. Free space must be determined accurately to obtain a precise value for quantity adsorbed.
Static-volumetric systems such as the TriStar 3000 consist basically of a gas manifold joined to a sample tube by an isolation valve. The manifold section has connections for an absolute pressure transducer, a temperature gauge, and a vacuum
system. It also has inlets for the adsorptive gas and helium. A Dewar flask containing a cryogenic liquid (usually LN2 at approximately 77 K) is situated so that it
can be raised to immerse most of the sample tube. Two temperature zones exist
within the sample tube when immersed in the cryogenic bath: a warm zone (thevolume above the liquid level and near ambient temperature) and a cold zone (thevolume below the liquid level at cryogenic temperature). Not only must the total
free-space volume be determined, but it also is necessary to determine the quantity of gas residing within the “cold” zone since a nonideality correction must be
applied to only that quantity of gas.
The total quantity of gas in the partly immersed sample holder cannot simply be
determined using n = PV/RT because temperature is not constant over the total
volume, but instead is distributed as two temperature zones with a steep temperature gradient between them. A convenient method for resolving this problem is toderive two factors which, for the existing temperature profile, can be multipliedby the prevailing pressure to reveal the molar volume of gas contained in the coldzone and the total quantity residing in the free volume of the immersed sample
holder (the cold free space).
The TriStar 3000 system provides four methods for free-space determination:••••

Feb 03

MeasureQuasi-Gemini
Calculate
Enter

D-1

Appendix D

TriStar 3000

MeasureGenerally, this method, although requiring a little more time (approximately 10
minutes) is the most preferred one for determining free space. It is simple, automatic, requires very little information, and essentially is error-proof. With thismethod, the instrument first evacuates the manifold and sample tube (containing
sample), then isolates the sample tube by closing the valve. Then the manifold ischarged with helium, the pressure measured, and the valve opened allowing thehelium to expand into the sample tube at ambient temperature. Again the pressure
is measured.
The dewar is raised and the sample tube is cooled to cryogenic temperature.
Again pressure drops; when pressure has equilibrated, the value is recorded. Warmand cold free spaces are calculated from (1) system volume, (2) system, ambient,and bath temperatures, and (3) measured pressures. From these, the value of the
portion of cold free space at cryogenic temperature which requires correction for
nonideality can be determined.
This method may be undesirable if:

D-2•

Helium is unavailable; free-space determination by the TriStar 3000 requires
the use of helium•

Analysis speed is a major factor; a helium free-space measurement of 10 to
15 minutes is required•Your sample tends to absorb and retain helium for a prolonged period of timeor if it adsorbs helium

Feb 03

TriStar 3000

Appendix D

Quasi-GeminiThis method requires the dedicated use of port 2, allowing concurrent free-spacecorrection. With this method, an empty sample tube (called the “balance” tube) is
installed on port 2 to run concurrently with one or two analyses on the otherport(s). You must enter the following information accurately for best results:
•
•
•
•
•

Sample tube stem nominal diameter (found on the Sample Tube dialog)
Indicate whether a filler rod is being used (found on the Sample Tube dialog)
Analysis bath temperature (found on the Po and Temperature dialog)
Sample tube volume below the index mark for the sample and balance tubes(refer to Calibrating the Sample Tube in Chapter 4)
Sample weight and density (found on the Sample Information dialog)

A separate pressure table is not required for the balance tube. Its pressure table isa composite of the pressure table(s) for the analysis. Therefore, each data pointcollected for the analysis has a corresponding pressure point on the balance tube
record from which a computed pressure/volume point may be interpolated to exactly the pressure obtained by the analysis.

CalculateThis method is the most rapid and efficient way of compensating for free space.
You must enter the following information accurately:
•
•
•
•
•

Sample tube stem diameter (found on the Sample Tube dialog)
Indicate whether a filler rod is being used (found on the Sample Tube dialog)
Sample tube volume below the index (red) markAnalysis bath temperature (found on the Po and Temperature dialog)
Sample’s weight and density (found on the Sample Information dialog)

The volume of the portion of the sample tube below the index mark is measured
by filling the sample tube to the index mark, weighing, and calculating the volume using the weight and density of the fluid. This value is used in calculating
the free space and should be engraved onto the sample tube for future use. Refer
to Calibrating the Sample Tube in Chapter 4.

Feb 03D-3

Appendix D

TriStar 3000

Enter
This method allows you to enter predetermined values for the warm and cold freespaces. The values to enter may be obtained in one of two ways:•

A pre-analysis free-space calibration of the sample tube containing sample•

The total free space of an empty sample tube is measured and the displacement of the sample calculated from its mass and density and subtracted fromthe total free space

In either procedure, ensure that the level (or, in cases where the Isothermal Jacket
is used, the effective level) of the cryogen bath on the sample tube is the same
when the analysis is performed as it was when gathering data for free-space calculations.

D-4

Feb 03

APPENDIX E
MAINTAINING HIGH PURITY GASESTriStar 3000

Appendix E

Maintaining High Purity Gases
The TriStar 3000 was designed to measure accurately the surface area of all typesof materials. It is important that the gases (nitrogen or helium) used for thesemeasurements be of highest purity, especially when analyzing low surface areasamples. Three ways to ensure high purity gases are to always maintain:•••

thoroughly purged gas pressure regulators
non-permeable gas lines
leak-free connections

Impure gas is strongly indicated, for example, if a series of measurements on a
low surface area material yields decreasing specific surface areas with decreasing
quantities of sample. The TriStar uses very small amounts of helium; therefore
any residual air in the regulator can distort results of subsequent analyses forquite some time.
Micromeritics offers the following suggestions to assist you in maintaining highpurity gases (particularly helium) for the TriStar.
•••

Use metal gas lines only
Remove trapped air from the regulator and gas lines
Purge the regulator and instrument lines after periods of non-use (this stepis unnecessary if you are using V2.00 or higher)

Using Metal Gas Lines
You should always use metal gas lines which have been carefully cleaned of any
oils and greases used in the manufacturing process. Do not use plastic or rubber
gas lines. When these types of permeable, nonmetallic gas lines are used with helium, contaminants accumulate at a much faster rate. This causes errors in analysis results and can also contaminate a clean sample.

Removing Trapped Air
When connecting the regulator to the gas bottle, air is unavoidably trapped on thehigh- and low-pressure sides of the regulator, as well as in the gas lines. You
should remove as much of this air as is possible before opening the gas bottle
valve. If this air is allowed to remain in the regulator, it will mix with the heliumand cause inaccurate results in subsequent analyses. Or if the valve is open for
any length of time, the air trapped on the high pressure side may diffuse backinto the gas bottle and contaminate its entire contents.

Feb 03E-1

E-2

Aug 01

There are two methods for removing trapped air from the regulator lines: thePurge Method and the Evacuation Method.

Purge Method
This is the preferred method for removing trapped air.
1.

From the Unit menu, select Enable manual control (if the instrument schematic is not displayed, select Show instrument schematic).

If you have multiple TriStars installed, make sure you choose the correct Unit
menu.

E-2

2.

Close all valves.

3.

Open the regulator Shut-off valve.

4.

Open the gas bottle valve briefly and allow the regulator to be charged withgas until the high pressure gauge reads just over half the tank pressure; thenquickly close the valve.

Feb 03

TriStar 3000

Appendix E

Gas Bottle Pressure Gauge(High Pressure Side)

Outlet Pressure Gauge(Low Pressure Side)

Gas Bottle ValveTo Analyzer
Shut-Off Valve
Pressure Control Knob

Feb 03

5.

Using the Pressure Control knob, set the output pressure (gas bottle pressuregauge) to 15 psig.

6.

Loosen the fitting at the helium inlet (on the rear panel of the TriStar) until
the low pressure side drops to approximatley 3 psig (0.02 MPa), then tighten
the fitting.

7.

Repeat steps 4, 5, and 6 three times.

8.

Briefly open the gas bottle valve; then, using the Pressure Control knob, reset
the regulator output pressure to 15 psig.

9.

After the pressure has stabilized (indicating there are no leaks), open the gas
bottle valve.

E-3

E-4

Aug 01

Evacuation Method
To use this method, your gas tank must be within 10 feet of the instrument.

1.

Do one of the following:
If...

Then...

The regulator has notbeen filled with gas
and the gas line is
attached to the
instrument:

Close the gas bottle valve.

The regulator is filledwith gas:

Close the gas bottle valve.

Open the regulator Shut-off valve.

Open the regulator Shut-off valve.
Loosen the helium inlet fitting (or nut) on therear panel of the instrument.
Allow all of the gas in the regulator to expel
from the line (pressure reading will be zero).
Retighten the helium inlet fitting (or nut).

2.

From the Unit menu, select Enable manual control (if the instrument schematic is not displayed, select Show instrument schematic).

If you have multiple TriStars installed, make sure you choose the correct Unit
menu.

3.

Close all valves; then open valves 6, 7, and 10.

Open valves 6,7, and 10.

E-4

Feb 03

TriStar 3000

Appendix E

4.

Allow evacuation to continue for 20 minutes. This pulls a vacuum on the helium line to the gas bottle. The manifold pressure transducer should fall close
to zero.

Be sure to allow evacuation for a full 20 minutes. If evacuation time is too short,
trapped air may remain in the lines.

5.

Feb 03

Close valves 6, 7, and 10.

E-5

E-6

Aug 01

Purging the System After Non-use
These steps are unnecessary if your analysis program is V2.00 or higher. V2.00(or higher) provides automatic purges before analysis if your system is idle formore than 24 hours.
You should always purge the regulator after periods of non-use. Even though theregulator and lines have been carefully cleaned, vapors sometimes permeate the Orings and seals in the TriStar system. These permeated vapors gradually increase
the level of contaminants in the helium line and regulator when the instrument isidle for more than hours. Use the following guidelines:•

Always purge the regulator and lines when the TriStar has been idle for
72 hours (3 days).

•

Purge the regulator and lines when the TriStar has been idle for morethan 24 hours if your sample has a total surface area of less than a few
meters squared and you plan to measure the free space.

Using an open sample port, purge the regulator and lines as follows:
1.

Remove the sample tube or plug from port 2 (in this example).

2.

From the Unit menu, select Enable manual control (if the instrument schematic is not displayed, select Show instrument schematic).

If you have multiple TriStars installed, make sure you choose the correct Unit
menu.

3.

Open Valves 2, 6, and 7, allowing the helium to flow through the system topurge the lines.
1. Open valve 2.

2. Open valve 6.

3. Open valve 7.

E-6

Feb 03

TriStar 3000

Appendix E

4.

After approximately 1 to 2 minutes, close valve 7.

5.

Open the nitrogen valve (8 or 9); allow the nitrogen to flow through the system for one minute. This allows the helium to be flushed from the system.

It is important that you flush the helium from the manifold after purging. If helium is allowed to remain in the manifold for a sufficient amount of time,transducer offset problems may be encountered.
6.

Feb 03

Close the nitrogen valve.

E-7

INDEXINDEX$ symbol, 8-9AAbsolute pressure tolerance, 5-20
Add log entry, 8-13
Add Log Entry push button, 5-6, 5-9Adding an analyzer, 2-16
Adsorbate property factor, 5-48
Adsorptive properties file, 5-27
defining, 4-9
printing contents, 5-71
Adsorptive push button
BJH report, 5-47
Dubinin report, 5-54
Advanced format, 5-4, 5-8, 8-3
sample defaults, 8-11
sample information file, 4-14, 8-4
Alpha-S reportexample of, 7-23
options, 5-42
Analyses
performing, 4-26, 6-3
QuickStart method, 4-27, 6-7
Analysis conditions file, 5-15
defining, 4-8
printing contents, 5-71
Analysis dewar
See Dewar
Analysis Log reportexample of, 7-16
Analysis Preparation dialog, 5-22
Analysis program
exiting, 5-77
installing, 2-10
installing upgrade, 2-15
uninstalling, 2-23
using, 3-2
Analyzer
adding another, 2-16
changing setup, 2-21
cleaning, 9-1
configurations, 6-17
installing, 2-3
moving to a different computer, 2-17
removing, 2-20
schematic, 6-11
turning on/off, 3-1

Feb 03Astakhov report, 5-53
calculations, C-25
Autoscale, 5-33, 5-52, 5-61, 5-62
Axis
coordinates, viewing, 7-14
properties, editing, 7-13
Axis Properties dialog, 7-13

B
Basic format, 5-4, 5-5, 8-3
sample file defaults, 8-8
sample information file, 4-12, 8-5
Bath temperature, 6-9
calculations, C-4
BET surface area report
calculations, C-8, C-9
example of, 7-18
options, 5-34
BJH Adsorption/Desorption report
calculations, C-13
examples of, 7-25
options, 5-46
BJH Adsorptive Property Factor dialog, 5-47
Broekhoff-de Boer thickness curve, 5-39
Browse push button, 3-6, 6-4, 6-9

C
Calibration
information, 6-17
manifold temperature, 6-18, 9-5
Pressure scale, 6-19, 9-4
sample tube, 4-19
servo valve, 6-20, 9-5system volume, 6-21, 9-7
zero pressure, 9-3
Calibration fileloading, 6-23
reinstalling, 2-22
saving, 6-23
Cancel push button, 6-6
Carbon Black STSA thickness curve, 5-38
Catalysts, 5-19
Cautions, 1-2
Check box, 3-5
Close All command, 5-70
Close command, 5-70

Index-3

IndexClose Reports command, 7-5
Cold free space, 5-24
calculations, C-4
Collected data, 5-65
Columns, editing on onscreen reports, 7-10
Comments window, 8-13
Computerconnecting analyzer, 2-3
connecting peripheral equipment, 2-6
Cross hair, axis, 7-14
Curve Properties dialog, 7-12D
Datacollected, 5-65
entered, 5-65
Data Presentation command, 8-7
Date format, changing, 3-7
Dates push button, 3-7
Default Basic Sample Information dialog box, 8-8
Degas conditions file, 5-13
defining, 4-7
printing contents, 5-71
Degassing unit, 1-3, 10-1
Density conversion factor, 5-27
Dewar
installing, 4-24
precautions, 4-24
DFT Plus command, 7-5
Dialog boxes, using, 3-4
Dose increment, 5-21, 5-22
Dose Increments dialog, 5-21
Dubinin Adsorptive Options dialog box, 5-54
Dubinin report
calculations, C-23
options, 5-53
types available, 5-53
Dubinin Report Options dialog box, 5-55
Dubinin Tabular Report Column Options dialog,
5-55
Dubinin-Radushkevich
calculations, C-24

E
Elevator options, 6-12
Enable Manual Control command, 6-11
Entered data, 5-65
Equation
Broekhoff-de Boer, 5-39
Halsey, 5-59

Index-4

TriStar 3000

Harkins-Jura, 5-58
STSA Carbon Black, 5-38
Equation push button, 5-37, 5-47, 5-58
Equilibration
calculations, C-7
push button, 5-26
Error messages, B-1
Evacuation options, 5-22
Exit command, 5-77
Exiting the analysis program, 5-77
Export command, 5-75
Exporting sample files, 4-32, 5-75

F
f-Ratio reportexample of, 7-24
options, 5-44
Fileprinting contents, 4-29
printing to, 7-4
selecting, 3-6
status, 3-7
File menu
Close All command, 5-70
Close command, 5-70
description, 5-1
Exit command, 5-77
Export command, 5-75
List command, 5-73
Open command, 5-3
Print command, 5-71
Save All command, 5-70
Save command, 5-68
File namedefault extensions, 3-8, 5-3
included as part of ID, 8-9
sequence, 8-8
Filler rod, 5-12
Fixed dose, 5-19
Forms, 1-1
Free Space, D-1
calculated method, 5-24, D-3
calculations, C-3
cold, 5-24
dialog, 5-23
entered method, 5-24, D-4
measured method, D-2
Quasi-Gemini method, 5-24, D-3
warm, 5-24
Function keys
See Shortcut keys

Feb 03

TriStar 3000

Index

G

L

Gas supply
connecting regulators, 2-7
specifying, 2-25
Gases
maintaining high purity, E-1
selecting, 6-17
Graphcopying as metafile, 7-13
editing onscreen, 7-11
grid lines, 8-7
legend, editing, 7-13
Graph overlay, 4-33
for multiple graphs, 4-33
for multiple samples, 4-35
Graph Overlay Samples dialog, 5-30
Graphic, appearing in report title, 5-30
Grid lines, 8-7

Langmuir surface area report
calculations, C-9
example of, 7-20
options, 5-34
Leak test, 5-23
Legend Properties dialog, 7-13
List command, 5-73
List, generating, 4-30, 5-73
Log entry, 5-6
Log Report settings, 6-16
Low surface area sample, analyzing, E-1

HHalsey equation, 5-59
Halsey thickness curve, 5-38
Halsey Thickness Equation dialog box, 5-59
Harkins and Jura thickness curve, 5-38
Harkins/Jura equation, 5-58
Help menu, 3-11
Help, online, 1-5

I
Increment, maximum volume, 5-19
Insert Pressure Range dialog, 5-17
Installation
analysis program, 2-10
sample tube, 4-23
Instrument log, 6-2, 6-15
Instrument Schematic dialog box, 6-11
Instrument schematic, showing, 6-13
Isothermcollecting, 5-16
data, exporting, 5-75
report options, 5-32
Isotherm collection
dose increments, 5-21
target pressures, 5-16
Isotherm reportexample of, 7-17
options, 5-32
Isothermal jacket, 5-12

Feb 03M
Maintenance, system, 9-1
Manifold temperature, 6-18
Manualconventions, 1-2organization, 1-1
Manual control, 6-11
accessing shortcut menu, 6-11
enabling, 6-11
Maximum BJH diameter (or radius), 5-47
Maximum volume increment, 5-19
Menu bar, 3-9
Menu structure, 3-9
Mesoporous materials, 5-19
Metafile, copying graphs as, 7-13
Minimum BJH diameter (or radius), 5-47
MP-Method Cumulative Pore Area Options dialog,
5-61
MP-Method Cumulative Pore Volume Options
dialog, 5-61
MP-Method dA/dR Pore Area Options dialog,
5-61
MP-Method dV/dR Pore Volume Options dialog,
5-61
MP-Method report, 5-58
calculation, C-29
options, 5-58
types available, 5-59
MP-Method Tabular Report Column Option dialog,
5-60

N
Next push button, 6-6
Non-ideality factor, 5-27
Notes, 1-2

Index-5

IndexTriStar 3000

Free Space, 5-23
Overlays, 5-30
Po and T, 5-25
Preparation, 5-22
Psat vs t, 5-28
Replace, 3-6
Skip, 6-6
Suspend, 6-6

O
O-ring, port
replacing, 9-2
Open command, 5-3
Operator, specifying, 8-12
Option Presentation command, 8-3
Options menu
Data Presentation command, 8-7
description, 8-1
Option presentation command, 8-3
Parameter Files Directory command, 8-15
Sample Defaults command, 8-8Service Test Mode command, 8-16
System configuration command, 8-14
Options report, 5-64
Outgas test, 5-24
Overlay samples, 5-35, 5-41, 5-43, 5-44
Overlays push button, 5-30

PParameter files, 5-4
defining, 4-5
specifying location, 8-15
Parameter Files Directory command, 8-15
Password, restricted format, 8-6
Physical volume below mark, 5-12
Po and T push button, 5-25
Po and Temperature Options dialog box, C-4, C-23
Po value, 6-4
Ports
Gas connection, 3-10Preparation push button, 5-22
Presentation options, 8-3
Pressure
relative, calculations, C-2
saturation, C-1
table, 5-16
target, 5-16
tolerance, 5-20
Pressure offset, 6-19
Pressure scale calibration, 6-19
Pressures push button, 5-48
Print command, 5-71
Printer/plotter, specifying default, 8-14
Printing to a Filedescription, 5-72
Psat vs t push button, 5-28
Push button, 3-5
Browse, 3-6
Dates, 3-7
Equilibration, 5-26

Index-6Q
Quasi-Gemini
calculations, C-6
free-space method, D-3
QuickStart command, 6-7
QuickStart dialog box, 6-7

RRadio button, 3-5
Radushkevich report, 5-53
calculations, C-23
Ramp rate, 5-14
Ranges, valid, 3-4
Relative pressure
calculations, C-1
See also Pressure
Relative pressure tolerance, 5-20
Removing an analyzer, 2-20
Replace All pushbutton, 5-7, 5-9
Replace push button, 3-6, 5-11, 5-13, 5-15, 5-28,
5-30
ReportAlpha-S method, 5-42
Analysis Log, 7-16
BET Surface Area, 5-34
BJH Adsorption/Desorption, 5-46
closing, 7-5
displaying company logo in title, 5-30
Dubinin, 5-53
examples, 7-15
f-Ratio method, 5-44
generating, 7-2graphs, editing onscreen, 7-11
header, 7-6
Isotherm, 5-32, 7-17
Langmuir surface area, 5-34
legend, editing, 7-13
onscreen, 7-6
onscreen, shortcut menus for, 7-10
Options, 5-64
Sample log, 5-64

Feb 03

TriStar 3000

saving in other formats, 7-9
Summary, 5-63
t-Plot, 5-37
Tabular, 5-49
Tabular, editing onscreen, 7-10
Tool bar, 7-7
types available, 5-31
zoom feature, 7-14
Report options file, 5-29
defining, 4-10
printing contents, 5-71
Reportsheader, 7-6
MP-Method, 5-58
Reports menu
Close Reports command, 7-5
description, 7-1
DFT Plus command, 7-5
Start Report command, 7-2
Restricted format, 8-3, 8-6
sample information file, 4-12
Resume push button, 6-6
Returning equipment, 2-1

S
Sampledegassing, 4-22
entering density, 8-9
low surface area, E-1
Sample Analysis command, 6-3
Sample defaults
Advanced format, 4-3, 8-11
Basic format, 4-1
specifying, 8-8
Sample file namespecifying default sequence, 8-11
Sample information file, 3-6, 5-4
Advanced format, 5-4, 5-8
Basic format, 5-4, 5-5
creating in Advanced format, 4-14
creating in Basic format, 4-12
exporting, 4-32, 5-75
generating a list, 5-73
printing contents, 5-71
Restricted format, 5-4
specifying defaults, 8-8
Sample Log report, 5-64
example of, 7-32
Sample tube
calibrating, 4-19
cleaning and labeling, 4-16
file, 5-11

Feb 03Index

installing, 4-23
Sample Tube file, 4-5
Saturation pressure, C-1
Save All command, 5-70
Save As command, 5-68
Save command, 5-68
Schematic, 6-11
Select Dates dialog, 3-7
Selectingfiles, 3-6
Service Test mode, 8-16
Servo valve
calibrating, 6-20
settings, 6-12
Setup program
adding an analyzer, 2-16
changing an analyzer setup, 2-21
moving an analyzer to a different computer, 2-17
reinstalling analysis program, 2-15
reinstalling calibration files, 2-22
removing an analyzer from the computer, 2-20
uninstalling the software, 2-23
using for other functions, 2-13
Shortcut keys, 3-2
for Select Dates dialog, 3-7
list of, 3-3
Shortcut menu, 3-2
for graphs, 7-11
for instrument schematic, 6-11
for tabular reports, 7-10
Show Instrument Log command, 6-15
Show Instrument Schematic command, 6-13
Show Status command, 6-14
Skip push button, 6-6
SmartPrep Degasser, 1-3
Soaktemperature, 5-14
time, 5-14
Softwareinstalling, 2-10
installing upgrade, 2-15
using, 3-2
Specifications, 1-6
Spreadsheet format
exporting isotherm data, 5-75
saving reports, 7-9
Start push button, 6-6
Start Report command, 7-2
Start Report dialog box, 7-2
Status list, 7-3
Status window, 6-14
STSA thickness curve, 5-38
Submitter, specifying, 8-12

Index-7

IndexSummary Report
calculations, C-32
example of, 7-31
options, 5-63
Surface area correction factor, 5-41
Suspend push button, 6-6
System configuration command, 8-14
System volume, calibrating, 6-21

T
t-Plot report
calculations, C-11
example of, 7-21
options, 5-37
Target pressure, 5-16
Temperaturebath, 6-9
manifold, 6-18
soak, 5-14
Text, copy graph data as, 7-13
Thickness curve, 5-37, 5-46, 5-58
Broekhoff-de Boer, 5-39
Carbon Black STSA, 5-38
Halsey, 5-38, 5-59
Harkins and Jura, 5-38
Harkins-Jura, 5-58
User-defined, 5-39
Title Properties dialog, 7-13
Tool bar, reports window, 7-7
Transducer offset, 6-19
TriStarSee also Analyzer
description, 1-3
specifications, 1-6
unpacking/inspection, 2-1

TriStar 3000

U
Unit configuration, 6-17
Unit Menu
description, 6-1
Enable Manual Control command, 6-11
QuickStart command, 6-7
Sample Analysis command, 6-3
Show Instrument Log command, 6-15
Show Instrument Schematic command, 6-13
Show Status command, 6-14
Unit Configuration command, 6-17
Units dialog box, 8-7
Use calculation assignments, 5-66
User-defined thickness curve, 5-39

V
Vacuum pump, 1-4
connecting to analyzer, 2-4
View, 6-7

W
Warm free space, 5-24
calculations, C-4
Warnings, 1-2
Weighing
sample, 4-21
Windowtile, 3-10
Windows menu, 3-10
Worksheet
See Forms

Z
Zero pressure calibration, 6-19
Zoom feature, 7-14

Index-8

Feb 03