Cannon miniPV-X User Manual
CONTENTS
i
1
INTRODUCTION/INSTALLATION 1
The miniPV®-X Automatic Viscometer .................................................................................. 1
Measuring kinematic viscosity ............................................................................................... 2
Safety cautions ..................................................................................................................... 3
Installation ............................................................................................................................ 5
Required installation components............................................................................... 5
V acuum Pump unit connections ................................................................................. 5
Bath unit connections ................................................................................................ 5
®
VISCPRO
Installing VISCPRO
Running the software............................................................................................................. 7
Checking configuration.......................................................................................................... 9
Manually changing tube calibration constants ....................................................................... 12
Checking W ash and Advanced Settings ............................................................................... 13
Preparing the miniPV -X for testing ...................................................................................... 15
for W indows® XP®............................................................................................ 6
®
software.............................................................................................. 6
Computer requirements............................................................................................. 6
Windows® XP® installation ........................................................................................ 6
Installation actions..................................................................................................... 6
Inital Configuration.................................................................................................... 9
Logging in ................................................................................................................. 9
Checking Instrument Settings .................................................................................... 9
V iewing/editing setup information ............................................................................. 11
Inserting the miniPV -X temperature probes/reference thermometer .......................... 15
Adjusting V acuum/Pressure settings ......................................................................... 16
Setting bath temperature ......................................................................................... 16
Training tube sensors............................................................................................... 18
Checking wash functions ......................................................................................... 17
Calibrating the miniA V ............................................................................................ 18
Notes on computer-directed miniAV operation ........................................................ 18
2
TESTING SAMPLES WITH THE miniPV-X
AUTOMATIC VISCOMETER 19
Turning on the miniPV -X ......................................................................................... 19
T esting samples....................................................................................................... 19
Pausing a test.......................................................................................................... 24
Resuming a test....................................................................................................... 24
Aborting a test ........................................................................................................ 25
CANNON
®
miniPV-X Automatic Viscometer with VISCPRO® Instruction & Operation Manual
Version 1.0a— January, 2011; CANNON
2139 High Tech Road • State College, PA 16803 • USA
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ii
Concluding a test .................................................................................................... 25
W orking with Instrument Groups ......................................................................................... 25
Group configuration ................................................................................................ 26
Configuring the Machine Status window to correspond with multiple-instrument place-
ment ....................................................................................................................... 27
V iewing test results ............................................................................................................. 27
Creating an analysis ............................................................................................................ 28
Configuring the VI Matcher (optional) ................................................................................. 28
3
4
CALIBRATING THE miniPV-X 29
Calibrating temperature ....................................................................................................... 29
Calibration procedure ............................................................................................. 29
Training sensors .................................................................................................................. 30
Standard tube calibration .................................................................................................... 31
Calibration procedure ............................................................................................. 32
Saving a calibration ................................................................................................. 34
miniPV -X calibration equations ............................................................................... 35
USING THE miniPV-X SOFTWARE 37
VISCPRO® generic instrument interface .............................................................................. 37
Main options .......................................................................................................... 38
Security options ...................................................................................................... 39
Initial security setup................................................................................................. 39
Adjusting Security Settings ...................................................................................... 41
Print/Print setup options .......................................................................................... 42
Analyses options................................................................................................................. 42
Analysis types......................................................................................................... 42
Analyses menu options............................................................................................ 42
Window options ................................................................................................................. 44
miniPV -X module menu options .......................................................................................... 45
Configure options ................................................................................................... 45
Print Instrument and Tray Settings ........................................................................... 45
Instrument Settings.................................................................................................. 47
Tray Settings: T ube and Bath ................................................................................... 49
Tray Settings: Test................................................................................................... 51
Tray Settings: W ash ................................................................................................ 53
Tray Settings: Advanced.......................................................................................... 56
Saving a configuration ............................................................................................. 58
Calibration.............................................................................................................. 58
Service menu options .......................................................................................................... 60
CANNON
®
miniPV-X Automatic Viscometer with VISCPRO® Instruction & Operation Manual
Version 1.0a—January, 2011; CANNON
2139 High Tech Road • State College, PA 16803 • USA
®
Instrument Company
T esting samples—software options...................................................................................... 64
Entering sample ID information................................................................................ 64
Selecting sample actions.......................................................................................... 64
V iscosity Action for viscosity standards ................................................................... 66
Copy & Paste Sample ID data entry options ........................................................... 67
Inserting/deleting a sample ID in the test sequence ................................................... 67
Saving Sample ID information ................................................................................. 68
miniPV -X analysis modules ..................................................................................... 68
Configuring the VI Matcher................................................................................................. 69
Turning off the VI Matcher...................................................................................... 72
Handling errors ................................................................................................................... 71
iii
5
OPERATING, MAINTAINING
AND SERVICING THE miniPV-X 73
miniPV -X components ........................................................................................................ 73
Bath Unit ................................................................................................................ 73
Solvent Dispensing System...................................................................................... 74
Maintaining the solvent system............................................................................................. 74
Filling the solvent container(s).................................................................................. 75
Emptying the W aste Receiver .................................................................................. 75
Dual-solvent washing .............................................................................................. 76
V iscometer tubes ................................................................................................................ 76
Thermistor operation............................................................................................... 76
Timing bulb determination........................................................................................ 76
Carousel Adjustments ......................................................................................................... 77
Homing the Carousel .............................................................................................. 77
Adjusting sample tray height .................................................................................... 77
Adjusting sample tray force ..................................................................................... 77
T emperature bath................................................................................................................ 79
Filling the bath ........................................................................................................ 79
Draining the bath..................................................................................................... 80
Bath heaters ........................................................................................................... 80
Bath fluid safety features ......................................................................................... 80
Checking solvent levels ........................................................................................... 80
Solvent/drain lines ................................................................................................... 80
Ventilation ........................................................................................................................... 81
Checking bath temperature ................................................................................................. 81
Dual-solvent washing .......................................................................................................... 81
Solvent wash by computer .................................................................................................. 81
Setting wash parameters ......................................................................................... 82
Preventive maintenance ....................................................................................................... 82
miniPV -X repair/replacement components ........................................................................... 83
6
CANNON
®
miniPV-X Automatic Viscometer with VISCPRO® Instruction & Operation Manual
Version 1.0a— January, 2011; CANNON
2139 High Tech Road • State College, PA 16803 • USA
®
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iv
ANALYSIS CONFIGURATION OPTIONS 85
Creating an analysis ............................................................................................................ 85
Sorting analysis data ........................................................................................................... 86
Using the date filter ............................................................................................................. 87
Using the sample filter ......................................................................................................... 88
Using the report/port output filter......................................................................................... 89
Reconfiguring a displayed analysis ....................................................................................... 89
Resizing table columns ........................................................................................................ 89
Saving a current analysis ..................................................................................................... 90
Deleting an analysis configuration......................................................................................... 90
Printing an analysis .............................................................................................................. 90
Keystrokes for selecting data for printing ................................................................. 91
Exporting analysis data........................................................................................................ 91
7
8
9
10
11
CAV DATA TABLE 93
Configuring the CA V Data T able ............................................................................. 95
STANDARD VI TABLE ANALYSIS 99
Configuring the standard VI table ............................................................................ 99
ERROR DATA EXPORT ANALYSIS 105
Configuring the Error Data Export analysis ............................................................ 105
ERROR LOG TABLE ANALYSIS 111
Configuring the Error Log Analysis .........................................................................111
USING THE DATABASE MANAGER 115
Archiving old data................................................................................................. 116
Changing the database directory............................................................................ 116
Importing archived data ........................................................................................ 117
Repairing/compacting the database........................................................................ 117
Exit ...................................................................................................................... 117
12
REPLACEMENT PARTS LIST 119
CANNON
®
miniPV-X Automatic Viscometer with VISCPRO® Instruction & Operation Manual
Version 1.0a—January, 2011; CANNON
2139 High Tech Road • State College, PA 16803 • USA
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v
A
I
APPENDIX A–MULTIPLE UNIT CONFIGURATION 121
Introduction ...................................................................................................................... 121
Kit components ................................................................................................................ 121
Procedure ........................................................................................................................ 121
Connecting components ........................................................................................ 121
Completing RS-485 connections ........................................................................... 121
INDEX 123
CANNON
®
miniPV-X Automatic Viscometer with VISCPRO® Instruction & Operation Manual
Version 1.0a— January, 2011; CANNON
2139 High Tech Road • State College, PA 16803 • USA
®
Instrument Company
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CANNON
®
miniPV-X Automatic Viscometer with VISCPRO® Instruction & Operation Manual
Version 1.0a—January, 2011; CANNON
®
Instrument Company
2139 High Tech Road • State College, PA 16803 • USA
CHAPTER
1
1
INTRODUCTION/INSTALLATION
The miniPV®- Series Automatic Viscometers
The miniPV®-Series Automatic Viscometers are specially designed to
handle the unique needs of polymer analysis laboratories for viscosity
determination of polymer solutions. The operator places the test
sample(s) in small vials in the sample holder(s), enters sample identification information from the computer keyboard, and initiates testing with
software keypad commands. Without any further operator involvement,
the miniPV-Series determines the viscosity and cleans the capillary
tube(s) in preparation for the next test. All pertinent test data can be
saved to a computer database for future retrieval and reporting.
Manual
This manual is designed to provide the operator with information about:
VISCPRO
miniPV
and operation
®
software installation and operation
®
equipment, installation
Applications
Calibration, service and mainte-
nance procedures
miniPV instruments are appropriate
for determining relative, inherent,
and reduced viscosity of polymers.
Viscosity and Instrinsic values can
also be reported. Instrinsic viscosity
can be dtermined by two single point
methods or by the rigorous HugginsKraemer analysis.
CANNON
®
miniAV®-HX Automatic Viscometer with VISCPRO® Instruction & Operation Manual
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2
Measuring Viscosity
Relative viscosity (Þr), a primary concern in the polymer industry ,
is determined from kinematic viscosity by factoring in the density
of the solvent and materials in solution and comparing the resulting absolute viscosity of the solution with the absolute viscosity of
pure solvent. ASTM D 2857 states that relative
viscosity is “the ratio of the viscosity of the solution, Þ, to the
viscosity of the solvent, Þs, that is, Þr = Þ/Þs .”
Units of measure
Methodology
NOTES
Inherent viscosity
Reduced viscosity
As a ratio, relative viscosity is a unitless measurement.
ASTM Method D2857 describes the appropraite test methodology for
determination of relative viscosity .
ASTM D 2857 states that “the kinetic energy correction constant is
negligible for the recommended viscometers and efflux times.” For this
reason, a default value of zero is assigned for E if the MiniPV viscometer
tube/bulb has not been calibrated.
Calibration is strongly recommended to ensure the highest precision when
measuring relative viscosity . Calibration is required for accurate determination of absolute viscosity . However , it is not necessary to calibrate if
measuring dilute solutions in the same bulb in which the solvent “blank”
has been analyzed.
Inherent viscosity (Þinh) is the ratio of the natural logarithm (ln) of the
relative viscosity (hr) to the mass concentration of the polymer (c) in g/
cm3, g/dl or g/ml , as expressed by the equation: Þinh = ln Þr/c.
Calculation of reduced viscosity is accomplished by first obtaining the
relative viscosity increment, Þi, (the ratio of the difference between the
viscosities of solution and solvent to the viscosity of the solvent alone, as
determined by the formula Þi = (Þ- Þs)/ Þs) and then relating that value
to the mass concentration of the polymer (c) using the formula Þ = Þi/c.
Instrinic viscosity
Adjusted Relative viscosity
CANNON
®
miniPV-Series Automatic Viscometer with VISCPRO® Instruction & Operation Manual
Intrinsic viscosity is the limiting value of the reduced viscosity or the
inherent viscosity at infinite dilution of the polymer. This value is calculated per ASTM D 2857 by extrapolation of viscosity versus concentration for several solution concentrations. Intrinsic viscosity calculations
performed by VISCPRO yield a value in dl/g (deciliters per gram). The
Billmeyer and Solomon-Ciuta equations for single-point intrinsic viscosity
calculation may also be used.
The adjusted relative viscosity (AR V) is only applicable to Solution
Relative Viscosity samples. The ARV Factor is simply a constant that is
stipulated in the viscosity action window .
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Manual viscometers
3
Sections 9-11 of ASTM D445 provide detailed instructions for using
manual viscometers. ASTM D 446 suggests a minimum flow time of 200
seconds for nearly all the glass capillary viscometers (see tables in ASTM
D 446).
Automatic viscometers
For automatic viscometers, ASTM D445 Section 6.1.2 states, “Automated apparatus may be used as long as they mimic the physical conditions, operations or processes of the manual apparatus they replace ...
The automated apparatus shall be capable of determining kinematic
viscosity of a certified viscosity reference standard within the limits stated
...”
Thus, automated viscometers can be used with flow times less than 200
seconds, as long as the kinetic energy correction and precision requirements are met.
miniPV Series tube characteristics
Each standard miniPV Series viscometer tube has two bulbs, each of
which has its own calibration. The normal flow times for each bulb are
40-400 seconds. Each tube has a hundredfold measurement range (for
example, range from 2-200 cSt or 20-2000 cSt for each tube).
NOTE
CANNON® Instrument Company has not recommended the use of longer
flow times with the miniPV Series, as shorter flow times allow greater
productivity . With longer flow times, the sample throughput would be
significantly reduced. However, the viscometer and sof tware design does
permit longer efflux times (up to 600 seconds) as desired by the user.
Safety cautions
Please observe the following safety procedures and notices for proper
operation of the miniPV Series:
Do NOT lift the unit by the side panel “ears”. Always support the
unit from the base when moving or lifting.
Make sure that your unit is operated only by qualified personnel.
Make sure that you read and understand all operating instructions and
safety precautions listed in this manual before installing or operating
your unit. If you have questions regarding instrument operation or
documentation, contact CANNON
®
Instrument Company.
Do not deviate from the installation, operation or maintenance
procedures described in this manual. Improper use of the miniPV
Series instrument may result in a hazardous situation and may void
the manufacturer’s warranty.
Handle and transport the unit with care. Sudden jolts or impacts may
cause damage to components.
Observe all warning labels.
Never remove warning labels.
Never operate damaged or leaking equipment.
CANNON
®
miniPV-Series Automatic Viscometer with VISCPRO® Instruction & Operation Manual
Version 1.a— January, 2011; CANNON
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®
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4
Never operate the unit without appropriate levels of approved bath
fluid in the bath.
Do not fill the bath vessel higher than the cold fill level.
( O )
Supply OFF Symbol
Unless procedures specify otherwise, always turn off the unit and
disconnect the mains cable from the power source before performing
service or maintenance procedures, or before moving the unit.
Never operate the equipment with damaged mains power cables.
Refer all service and repairs to qualified personnel.
In addition to the cautionary statements listed previously , additional
General Caution
cautions may be posted throughout this manual. These cautions, identified
by the caution symbol (see left) indicate important operational procedures. Read and follow these important instructions. Failure to observe
these instructions may void warranties, compromise operator safety , and/
or result in damage to the miniPV Series unit.
Hot Surface Caution
Protective Conductor
WARNING
MAINS
~
AC Power Input Symbol
Hot surface cautions may be attached on or near hot surfaces of the
miniPV Series. A void touching hot surfaces, particularly when operating
the miniPV Series at bath temperatures exceeding 50°C.
The Protective Conductor T erminal symbol is used to indicate required
ground connections for your instrument electrical supply.
When supplying power to this instrument, ensure that the protective
ground (earth) terminals of the instrument are connected to the protective
conductor of the (supplied) line (MAINS) power cord. Use only the
manufacturer-supplied power cord, which should be inserted in a socket
outlet (receptacle) which is also provided with a protective ground (earth)
contact.
conductor (grounding).
The ~MAINS symbol indicates instructions or connections for the AC
power supply. The AC Power input must match the electrical specifications listed on the label on the rear panel of the instrument. The supplied
AC Mains power cord must be attached to the connector labelled
~MAINS. This connection serves as a means of disconnect and should be
readily accessible.
Do not use an extension cord (power cable) without a protective
Hazardous materials
CANNON
The (O) symbol indicates the OFF position for the electrical switches for
your unit (AC Mains or accessories).
Routine miniPV Series operation may require the use and handling of
hazardous chemicals and solutions. CANNON
strongly urges the operators and technicians working with the miniPV
®
Instrument Company
2
®
miniPV-Series Automatic Viscometer with VISCPRO® Instruction & Operation Manual
Version 1.a— January, 2011; CANNON
2139 High Tech Road • State College, PA 16803 • USA
®
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Installation
Required installation components
Series to take proper safety precautions when working with these
materials. These safety procedures can be found in the Material Safety
Data Sheets which accompany the solutions.
miniPV Series setup can be accomplished in just a few minutes by
following the diagrams included with the manual. Fill the miniPV Series
bath per the instructions in Chapter 5.
User-supplied solvent container w/ G38 threads for lid
CANNON
®
-supplied Nalgene® waste bottle with lid
Waste Receiver Assembly
Blue transparent Vacuum line (6 mm FEP)
Pressure and Solvent lines (1/8” FEP) CAUTION
When moving or positioning the miniPV Series unit, do not lift it by the
side panel units (“ears”). Hinges on these modular components are
designed for easy removal. Always support the miniPV Series unit from the
base.
5
Vacuum Pump unit connections
Use the 1/4” blue opaque polyethylene tubing to vent exhaust from the
Waste Receiver Assembly Exhaust port to the user ventilation system.
Use the 6 mm FEP tubing to connect the Vacuum Port to the bath unit
V acuum connector .
Use the Waste Receiver Assembly power cable to provide AC power to the
V acuum Pump from the female Power Supply V acuum Pump AC connector .
Bath unit connections
Use the 1/8” FEP line to connect from the Solvent A fitting to the user-
supplied solvent container. Insert the end of the solvent tube through the
bottle cap (see NOTE below) and screw the 20-micron filter onto the tube
end. If using two solvents, do the same for the (optional) Solvent B fitting.
NOTE CANNON provides two G-38 reagent bottle caps for user solvent contain-
ers.
Use the 6 mm FEP tubing to connect the 6 mm Waste V ac port to the 6 mm
Waste/Vacuum fitting on the waste bottle lid.
Use the 1/8” FEP to connect the Pres[sure] barbed fitting to the Air Out
barbed fitting on the Power Supply unit.
Use the RS-232 cable to connect from the RS-232 port to the computer
connection. For multi-unit RS-485 connections, see APPENDIX A.
CANNON
®
miniPV-Series Automatic Viscometer with VISCPRO® Instruction & Operation Manual
Version 1.a— January, 2011; CANNON
2139 High Tech Road • State College, PA 16803 • USA
®
Instrument Company
6
Use the 6 mm FEP union to connect the protruding 6 mm FEP waste tube
from the bath unit to the 6 mm FEP tubing. Then connect the other end of
the 6 mm FEP tubing to the 6 mm fitting on the Waste Receiver lid.
Use the DC power cable to connect the bath unit DC IN to the DC OUT on
the power supply.
Use the MAINS power cord to connect the Power Supply to the MAINS
power outlet matching the voltage specifications on the Power Supply rear
panel.
VISCPRO® for Windows® XP
®
VISCPRO® is a powerful software product designed to provide a generic
instrument interface for controlling and operating your CANNON
instrument(s) via computer. All instrument functions necessary for testing
are controlled via computer. VISCPRO® also includes reporting/analysis
modules for processing and displaying sample data.Installing VISCPRO
software
Installing VISCPRO® software
T o install the VISCPRO® software, follow the instructions below in the
sequence presented. Make certain that you complete the sections on
checking instrument settings and initial calibration data. If you encounter
difficulties at any stage in the installation process, call CANNON
service at 814-353-8000.
Computer requirements
Consult CANNON® Instrument Company at 814-353-8000 for current
computer specifications. The computer should be a PC with a working
version of the Windows® XP® operating system installed.
®
®
®
Windows® XP
®
installation
Installation actions
CANNON
®
miniPV-Series Automatic Viscometer with VISCPRO® Instruction & Operation Manual
Version 1.a— January, 2011; CANNON
1. Turn on your computer. Wait for the Windows® software to load.
2. Insert the VISCPRO
®
installation CD-ROM into the disk drive. If the
installation program does not begin automatically , click the Control
Panel option from the W indows® Start Bar . Then double-click the
Add/Remove Programs icon and follow the Windows® prompts to
complete the installation procedure. The executable file for
VISCPRO® software installation is SETUP.EXE.
The installation program will:
create a directory for your program files. The default directory is
C:\Program Files\Cannon Instrument\VISCPRO.
write SETUP information to the W indows
®
Instrument Company
2139 High Tech Road • State College, PA 16803 • USA
®
registry.
copy the software executable file and other necessary files to the
.
.
directory you specify.
update other files in your W indows
compatible with the current VISCPRO
place a shortcut icon for the VISCPRO
Windows
®
place a copy of the VISCPRO database in the appropriate directory
for your operating system (see table below). The installation CDROM copy of the SAMPLES.MDB file contains initial factory
calibration data unique to that instrument.
metsySgnitarepO )dednemmocer(yrotceriDataDtluafeD
desktop.
®
directories to versions fully
®
software.
®
executable file on your
7
PX,0002swodniW \0.2\orPcsiV\tnemurtsnInonnaC\noitacilppA\sresUllA\sgn
TNswodniW \0.2\orPcsiV\tnemurtsnInonnaC\ataDnoitacilppA\sresUllA\seliforP\TNniW\:C
EM,89swodniW \0.2\orPcsiV\tnemurtsnInonnaC\ataDnoitacilppA\sresUllA\swodniW\:C
Running the software
the VISCPRO II icon
Title Bar
Menu Bar
itteSdnastnemucoD\:C
ehtrofhcraesoslanacuoY:ETON bdm.selpmas
elif
otevird\:Cehtno
etacol
retupmoccificepsruoyrofnoitamrofnisiht
reweivruoyrofdetcelessinoitpo"sredlofdnaselifneddihwohS"ehtniatrecekam,elbisivtoneraseirotceridfI
Provide power to the miniPV Series instrument, and verify serial connections to the computer. To load your newly-installed VISCPRO® software,
double-click on the VISCPRO® icon on your W indows® desktop (Windows® NT® users can click Start/All Programs/VISCPRO/VISCPRO
2.0).
Sample
Input
window
Status bar
Analysis
window
Status bar
CANNON
®
miniPV-Series Automatic Viscometer with VISCPRO® Instruction & Operation Manual
Version 1.a— January, 2011; CANNON
2139 High Tech Road • State College, PA 16803 • USA
®
Instrument Company
8
If you received a configuration disk with your installation package, the
software may have already been preconfigured with instrument settings
unique to your laboratory , including instrument type(s), tube range and
serial #, and calibration constants. In a moment, we will verify these
settings. The image below demonstrates a typical screen configuration:
®
The VISCPRO
primary display
®
The VISCPRO
VISCPRO
primary display window is framed on the top by the
®
title bar and menu bar, and on the bottom by the VISCPRO
status bar. The application window can be user -configured to include child
windows (Sample Input or Machine Status windows, Analyses) which can
be opened and closed independently . The Sample Input window describes
your CANNON
®
instrument and provides controls for running tests. The
Analysis window presents data from miniPV Series tests.
®
The Sample Input window
NOTE
The Data Table analysis/report window (displays data from completed tests)
CANNON
®
miniPV-Series Automatic Viscometer with VISCPRO® Instruction & Operation Manual
If the Sample Input window does not appear when the software loads, click
View Instrument from the Main menu, then click the desired instrument group
(type of instrument, e.g. miniPV Series, CCS, CAV -2100) from the list of
available instruments and click OK. If the Available Instruments list box is
blank, your miniPV Series instrument may not be on-line. Check cable
connections and make certain the unit power switch is ON.
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Checking configuration
Initial configuration
The installation CD-ROM copy of the SAMPLES.MDB file contains
initial factory calibration data unique to that instrument.NOTE
If you wish to restore the original configuration, archive your sample data
before doing so (see Chapter 13 for information on using the Database
Manager software). Then copy the original SAMPLES.MDB file from the
CD-ROM to the database directory corresponding to your operating system
(see table, previous page).
Follow the procedures in the next several sections of this chapter to
verify/edit the instrument and calibration settings to ensure that they
conform to the actual characteristics of your CANNON
®
instrument.
9
Configuration protection
Logging in
It is not necessary to log in to view current instrument settings. However,
to change the configuration settings, you must log in to the security
system as a manager. The software is installed with a default Manager
account. This account has no password, allowing any operator access to
manager-level software functions as long as the password is not activated/changed. If you would like to engage the full-release security
options, see Security Options in Chapter 4 for instructions.
1. Use your mouse to click Main from the VISCPRO® menu bar.
2. Click Log In from the Main menu options.
3. Click on the (arrow) on the right side of the User Name: list box
to display the list of registered users.
4. Click Manager. Do NOT enter a password unless you have previ-
ously set up the Manager account with a password.
5. Click OK. The Log In window will close automatically and you will
be logged in as management personnel.
Checking Instrument Settings
1. Use your mouse to click (select) Configure from the VISCPRO
menu bar.
CANNON
®
miniPV-Series Automatic Viscometer with VISCPRO® Instruction & Operation Manual
Version 1.a— January, 2011; CANNON
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®
Instrument Company
®
10
2. Select your instrument from the list of available instruments (there
may be only one instrument in the list).
3. Select Instrument Settings from the list of configuration options.
The Instrument Settings window will appear .
You will use the Instrument Settings window (see below) to describe
and control miniPV Series instrument operational features. These settings
affect the instrument as a whole. Check the instrument settings for your
instrument per the instructions below , and make any necessary changes:
Prompt options
CANNON
The Instrument Settings window
Use the ID field to input instrument identification information using up to
16 alphanumeric characters.
The S/N: field (non-editable) indicates the serial number from the label on
the miniPV Series rear service panel.
The Prompt for Check Standards options permit you to set a computer-
ized “alarm clock” which will pop up a message reminder to run a check
standard based on the schedule you set with the control. Notice that you
can specify a reminder after “x” number of days and/or “x” number of
samples. Click the check box(es) to enable/disable each reminder.
When you have verified all settings, click OK.
®
miniPV-Series Automatic Viscometer with VISCPRO® Instruction & Operation Manual
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Viewing/editing setup information
11
NOTE
For first-time installation, make certain that the factory-prepared Configuration file has been copied to the Default Data directory per instructions on
page 7 of manual. If your instrument has already been configured, you can
use the instructions in this section of the manual to check or, if necessary,
change the instrument settings.
1. Click Configure from the VISCPRO® menu bar.
2. Select your instrument group and instrument from the list of available
instruments.
3. Select Tray Settings: T ube and Bath from the list of configuration
options. The T ray Settings: Tube and Bath window will appear.
CANNON
The Tray Settings: Tube and Bath window
The T ray Settings: T ube and Bath window contains setup information
for each tube associated with your instrument. On multiple-tube CANNON instruments, you can click on the tube tabs to see the setup information for different tubes.
4. Verify that the tube serial number ( Tube S/N) is correct. If it is not,
input the correct serial number in the text box.
Each tube should have
a unique serial number!
5. Verify the presence of calibration
values (C and E) for each bulb. If
calibration data is not available, the
default values are C=1 and E=0.
Sample calibration constants
®
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Manually changing tube calibration constants
If you discovered any errors in the values of the calibration constants
(see previous section), follow the directions in this section to manually
correct them using calibration information previously obtained for your
unit. If the calibration values are correct, instrument setup is complete.
Procedure
NOTE
This procedure for manually entering/changing calibration constants
bypasses the normal calibration procedure. T o ensure the most accurate
viscosity readings, CANNON® Instrument Company recommends that the
instrument be calibrated per the calibration procedure outlined in Chapter 3.
1. Log in as a Manager and click Configure from the VISCPRO
®
menu bar.
2. Select your instrument from the list of available instruments.
3. Select Calibration from the list of configuration options. The Cali-
bration window will appear (see next page).
The Calibration window provides controls for calibrating each bulb of
any viscometer associated with your instrument. You can click on the bulb
spin controls
to display current constants and valid check standard
data available for calibration of each bulb.
1. Make sure that the spin controls
for Bulb are set to “1”:
CANNON
This corresponds to the bottom bulb in the tube.
2. Check the values for the calibration constant(s) as they appear at the
bottom of the window:
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miniPV-Series Automatic Viscometer with VISCPRO® Instruction & Operation Manual
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The Calibration window
Compare this value to your archive of the calibration constant data (if
available) for bulb 1. The values should be identical.
3. If they are not, place your cursor in the appropriate field, delete the
entry, then type the correct values for the constant in the text box.
13
4. Click Update tube
5. Use the bulb spin controls
to select the other bulb(s) for which
you noted calibration constant errors. Input the correct values for
Make certain to click Update Tube after you have corrected
each.
C and E calibration values for each bulb BEFORE selecting the next
bulb.
6. When you have entered corrected constant values for each bulb on
both tubes, click
to exit the Calibration window.
You have verified the software configuration of VISCPRO
samples with your instrument, follow the instructions in Chapter 2. For
additional details regarding operating procedures for your instrument or
software, consult the appropriate section of this manual.
Checking Wash and Advanced Settings
T o check Wash Settings for your miniPV Series instrument, click Configure from the VISCPRO menu options and select the desired instrument.
Then click Tray Settings: Wash. The Tray Settings: Wash window
will appear.
.
®
. To test
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Compare the values in the Tray Settings: W ash window with your
archived values and make any necessary changes; then click OK.
T o check Advanced Settings for your miniPV Series instrument, click
Configure from the VISCPRO menu options and select the desired
instrument. Then click Tray Settings: Advanced. The Tray Settings:
Advanced window will appear .
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miniPV-Series Automatic Viscometer with VISCPRO® Instruction & Operation Manual
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Compare the values in the Tray Settings: Advanced window with your
archived values and make any necessary changes; then click OK.
Preparing the miniPV Series for testing
Inserting the miniPV Series temperature probes/reference thermometer
15
Inserting the probes
miniPV Series top bath flange
The temperature probe and thermal fuse probe are semi-permanently
installed. Initial installation or replacement requires removal of the top
cover of the bath unit. The probes are inserted through the narrow
aperture on the top bath flange and held in place with a sliding metal plate
(friction fitting) secured with a thumbscrew .
Inserting the thermometer
CAUTION
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miniPV-Series Automatic Viscometer with VISCPRO® Instruction & Operation Manual
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The ASTM reference thermometer/adapter assembly can be inserted
through the grommet in the bath top cover and through the larger circular
aperture on the top bath flange (see photo image above). The assembly
includes a stop collar with set screw that can be adjusted to vary the
thermometer height.
Do NOT insert a reference thermometer while the miniPV Series bath
impeller is operating, as damage to the thermometer and/or viscometer
tube may result. Make certain to insert the appropriate reference thermometer for the current bath temperature! Use appropriate safety procedures
when handling the thermometer, as it contains mercury .
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Adjusting Vacuum/Pressure settings
T o adjust the vacuum setting for the miniPV Series, click Service from
the VISCPRO menu options and select the desired instrument group and
instrument. Then click Adjust Vacuum/Pressure to open the Adjust
Vacuum/Pressure window.
Select the desired adjustment (vacuum or pressure) and then follow the
screen prompts to complete the adjustment procedure, using the appropriate controls on the instrument side (“ear”) panel. The prompts will display
recommended vacuum/pressure settings and will also indicate how
adjustments may be made to alter the settings.
Setting bath temperature
WARNING
Prior to setting the bath temperature, ensure that the reference thermometer in the bath is suitable for the desired temperature range. If not,
remove thermometer from the bath. If the bath temperature rises above
the range of the thermometer, it may be damaged. Mercury thermo-meters
pose particular problems, since mercury from a damaged thermo-meter
may circulate with bath fluid.
To set the temperature:
1. Load the VISCPRO® software and click Configuration.
2. Select the miniPV Series from the list of available instruments and
click T ray Settings: T ube and Bath.
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3. Select the desired unit of temperature measurement (°C or °F).
4. Type the desired temperature in the Bath Temp: field. Acceptable
NOTES
The miniPV Series will not allow sample testing until the instrument has
equilibrated temperature at the test temperature.
T o cancel temperature selection before completing the procedure, click
Cancel.
After the target temperature has been set, the miniPV Series bath
temperature will be adjusted to the target temperature and the bath will
equilibrate at the test temperature. The VISCPRO II software always
displays the current and target bath temperature in the Sample Input
window.
Checking wash functions
T o ensure function of the solvent wash system, follow the procedure
below:
1. Place an empty vial in the sample tray position 1.
values are any numbers between 20°C and 100°C. If necessary, you
may use the decimal point key to input temperature to the nearest
0.01°C. Press OK to save the temperature setting.
CANNON
2. Select Wash viscometer tube to open the Wash viscometer tube
window .
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3. Click Begin Wash to initiate the wash cycle. The Status: indicator
will display and update current actions.
Bypass .... option
NOTES
Training tube sensors
NOTES
CAUTION
T o begin washing an evacuated sample cup, click the option box to make
certain that the Bypass initial cup evacuation option is selected. Do not
use this option with a filled cup or the cup will overflow.
4. When the Wash cycle has been completed, click Done to exit the
Wash viscometer tube window.
The Wash operation cannot be executed if the tube is currently running a
sample. To terminate the Wash cycle at any time, click Abort W ash.
The Wash viscometer tube function overrides automatic miniPV Series
software operations. Verify that the tubes are clean and dry before initiating computer-controlled sample testing.
miniPV Series tube sensors must be trained in order for the instrument to
properly perform test functions. To train miniPV Series sensors, follow
the instructions in Chapter 3.
The temperature should be calibrated prior to training the miniPV Series
tube sensors.
Calibrating the miniPV Series
Notes on computer-directed miniPV Series operation
Reporting data
CANNON
To ensure accurate test results, your instrument may need to be calibrated. If necessary , follow the instructions in Chapter 3 to calibrate your
miniPV Series temperature probe and viscometer tube.
A computer is required for miniPV Series operation. The computer
provides for automatic control of miniPV Series functions using the
VISCPRO® controlling software. Computer control permits data entry of
up to ten different sample IDs. Each of the identified samples can then be
tested with the miniPV Series instrument.
Test data for the samples is automatically saved to the VISCPRO
database for future reporting/data collection. Additionally , several reports
(analyses) may be used to calculate and display kinematic viscosity and
viscosity index (VI) values. See the chapters on VISCPRO® analyses for
further information.
All analyses provide a dynamic reporting option which can dynamically
display and transmit test results as testing is completed. Data can be sent
to your computer screen, printer, and/or serial port for in-house data
collection. See Chapter 6 for more information on configuring analyses.
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CHAPTER
19
2
Turning on the miniPV Series
Testing samples
Loading software
TESTING SAMPLES WITH THE
miniPV Series
This chapter of the manual will provide information on testing samples
using the miniPV Series. Observe the safety cautions noted in the
introductory chapter when operating equipment. The miniPV Series
should only be operated by qualified personnel.
Turn on the miniPV Series Bath Unit using the power switch on the
power supply unit.
1. Turn on the computer and load the miniPV Series software by
double-clicking the VISCPRO
®
II icon on the Desktop.
NOTES
NOTES
If the software is already loaded, use your computer mouse to click Main
from the menu bar and click Poll for Instruments from the Main menu
options. This will establish communications between the computer and the
on-line instrument.
Permit the bath to stabilize at test temperature before testing samples.
2. Pour sample material into the glass vial(s). For 20 mL vials, fill only
half full, as the viscometer tube will displace sample in the vial.
Approximately 10 mL of sample should be sufficient for testing in
either bulb of the viscometer.
Do not overfill the vials. Sample overflow may create problems for the tube
cleaning cycle.
You should periodically test calibration check st andards per your estab-
lished laboratory procedures. Recalibrate the miniPV Series (see
Chapter 3, Calibration) if result variance warrants.
3. Place the sample vials in the carousel.
4 Check the thermometer in the temperature bath to
make sure the bath is holding the proper temperature. If necessary, calibrate the miniPV Series
temperature control probe using the temperature
calibration procedure in Chapter 3.
CANNON
Filled
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5. Open the View Instrument Group window (if it is not already open)
by clicking View Instrument from the Main menu and selecting the
desired instrument group from the list box (see Chapter 4 for more
information).
The View Instrument Group window
6. Select the desired group ID and click OK to display the Sample
Input View .
The Samle Input window (miniPV Series four--bath system)
Then click the Tray tab corresponding with the desired miniPV Series.
7. Double-click on Sample ID (1) with the left mouse button to access
the sample ID data entry field (or press 2).
8. Enter sample ID information in the sample list box using your computer keyboard. After you have typed the sample ID, press the T
key to complete the entry and move the cursor to the next Sample ID
field. Or press R to complete the entry.
NOTE
CANNON
Once sample information is entered, the software automatically assigns a
sample action, Measure Sample Viscosity, for the sample. If you do not
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miniPV®-HX Automatic Viscometer with VISCPRO® Instruction & Operation Manual
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enter a sample ID, the sample is automatically labeled Unknown.
T o select or change a sample action, highlight the appropriate Sample
ID(s) using the mouse or arrow keys, then click the RIGHT mouse button
to access sample action options:
No action
Determine Solution Relative V iscosity
Determine Blank (Solvent) V iscosity
Determine Solvent V iscosity
Verify Known RV
Measure Kinematic Viscosity
Verify Known KV
No action: If No action is selected, all information for that sample
position will be cleared and that carousel position will not be tested.
Determine Solution RV If Determine Solution Relative Viscosity is
selected as the test option for a sample, the Polymer Sample Measurement Options window will open, permitting data entry of relevant parameters for the determination of RV. For information on data entry options,
21
Determine Solvent Viscosity If Determine Solvent Viscosity is selected as the test option for a sample, the Polymer Sample Measurement
Options window will open,
Verify Known KV/RV If Verify Known RV (relative viscosity) or Verify
Known KV (kinematic viscosity) are selected as the test option for a
sample, the Polymer Sample Measurement Options window will include a
new data entry field, RV or Check Standard Viscosity, which permits the
user to enter the known RV or KV of the sample: This information will
permit the VISCPRO software to compare calculated RV or KV values
with known values to determine the accuracy of current calibration and
machine performance. Measure Kinematic Viscosity If Measure Kinematic Viscosity is selected as the test option for a sample, the VISCPRO
software will calculate kinematic viscosity for the sample using the
sample drop time and ASTM D 445 formulas.
Defining and using a solvent blank for RV analysis
Using a solvent blank Relative viscosity by definition is a ratio between
the absolute viscosity* of a solution containing a solvent and sample
material, and the absolute viscosity* of the pure solvent . VISCPRO
calculates this ratio by comparing sample drop times for the solution and
the solvent “blank”. The significance of the resultant value is enhanced as
two additional variables are taken into account—sample/solvent density
and (with drop times under 200 seconds) an empirically-determined
kinetic energy correction constant.
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*The term absolute viscosity , as used in this manual, is also known as
dynamic viscosity . For the purpose of VISCPRO® software viscosity
calculations, and per ASTM D 2857 specifications, the absolute viscosity
is defined by the equation ç = Ctñ - Eñ/t 2 where C is a constant, t is the
drop time, ñ is the solution or solvent density and E is the kinetic energy
correction constant.
Relative viscosity calculation
The relative viscosity (RV) ratio (solute to solvent blank) is therefore defined
by the equation:
Software selection of blank
Since determination of a relative viscosity involves a comparison of solution
and blank, the VISCPRO controlling software requires the identification of a
blank for any samples tested using the Determine Solution Relative Viscosity
sample action. The blank is ordinarily selected from a list of solvents maintained by the VISCPRO database. This list is accessible from the Polymer
Measurement Sample Options window by using the drop-down list feature:
To display the list, click on the arrow. If the correct blank has not yet been
defined, the user may create a new blank by typing an ID for the blank into the
open field in the Polymer Measurement Sample Options window:
Procedure for blank definition
New blanks are created by testing the solvent in the miniPV using the
Determine Solvent V iscosity sample action. Follow the procedure for
testing samples
1. Select Determine Solvent Viscosity as the sample action for the
desired sample.
2. Enter an ID for each blank that includes both a description of the
blank and also the temperature at which that blank is to be tested in
the miniPV. The blank must be tested at the same temperature
intended for the solution
NOTE
CANNON
In some MiniPV applications involving dilute solutions, it may not be
necessary to input the density for the solvent blank and/or solution. If you
choose not to input solvent density for either the blank or for the sample,
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the density of both will not be included in relative viscosity calculations.
Unity Reference blank
A preexistent blank, Unity Reference, is hard-coded in the VISCPRO®
software with a value of “1”. Users selecting this blank when running an
RV
sample are effectively calculating the kinematic viscosity of the solution in
a
manner which permits them to use VISCPRO® polymer report options.
Testing volatile samples
The environment for viscosity measurement using the MiniPV
AIRBATH and compound viscometer is much different than it would be
with a conventional liquid bath and a U-shaped viscometer. Because of
the continuous downward flow of air in the AIRBATH, evaporation of
23
NOTES
sample components have the potential to adversely affect the analysis.
This
is because evaporation changes the composition of the sample and may
also affect temperature stability).
If you are testing at higher temperatures and/or with samples containing
components which may evaporate during the analysis, cover the sample
with aluminum foil or other easily penetrable membrane and secure with
the “O” ring and cap supplied for that purpose with the MiniPV. This
will seal the sample until the viscosity measurement is performed. Then
the
viscometer tip penetrates the aluminum foil/membrane and performs the
entire analysis without withdrawing completely from the sample vial.
If the aluminum foil has been penetrated and the sample has remained
in the analysis chamber for more than a few minutes, do not attempt to
reuse the sample. A new sample should be prepared.
CANNON
It is especially important to cover the samples when performing solution
viscosity analysis of polymers. Even a slight change of composition
caused by solvent evaporation may cause significant error.
Even samples that are high in viscosity may still contain volatile compo-
nents;
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24
these samples should also be covered before analysis. Most lubricating
oils, because they are manufactured at high temperatures and low pressures, do not contain significant volatile components and can be analyzed
without being covered.
The PolyVISC SPS Solution Preparation System from Cannon Instrument
Company is a semi-automated solution preparation system that can be
used with the minPV instruments. Contact Cannon for more information.
NOTE
Running check standards
NOTE
For additional information on software data entry features, including
multiple sample selection and cut & paste options, see Testing samples—
software options in Chapter 4.
If Verify Known KV is selected as the test option for a sample, the
Viscosity Action window will open automatically. Enter the neces-
sary check standard data, including the Check St andard viscosity
from the standard bottle, and click OK to complete data entry. To
revise or confirm standard data, right-click on the desired sample ID
from the list box and select Configure from the popup menu choices.
See Chapter 4 for additional information on the Viscosity Action window .
9. Continue entering sample information for all desired trays. When
sample ID data entry is complete, check the Tray Status window to
verify that all trays are ready for testing.
10. Click on the RUN button at the bottom of the Sample Input window.
The Select Trays window will open if more than one miniPV Series
instrument is online.
11. If necessary, click on the check box(es) to select the desired prepared “tray” (sample sequence) for automatic testing. For the
miniPV Series, a tray corresponds to the miniPV Series instrument.
Then click OK to begin the miniPV Series test(s).
Pausing a test
NOTE
Resuming a test
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miniPV-Series Automatic Viscometer with VISCPRO® Instruction & Operation Manual
T o temporarily halt testing for a given tube/sample, click the Pause
button from the Sample Input window. Then select the desired tray
(miniPV Series instrument) and pause action(s) from the Select Trays
window (Pause Now will immediately pause test actions; Pause after
current sample will pause testing after the current test is complete).
Click OK to pause testing for the selected tray(s).
If the test was paused prior to the initiation of the Wash cycle, drop time
data for that sample will be discarded.
To resume test actions for paused trays, click the Resume button from
the Sample Input window. Then select the desired trays from the Select
Trays window. Click OK to resume sample testing (see note above).
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