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BROOKFIELD DV-I PRIME

Digital Viscometer

Operating Instructions

Manual No. M/07-022-D0613

BROOKFIELD DV-I PRIME Digital Viscometer Operating Instructions Manual No. M/07-022-D0613

TABLE OF CONTENTS

I. INTRODUCTION

5

I.1

Components

6

I.2

Utilities

7

I.3

Components and Dimensions

8

I.4

Specifications

10

I.5

Setup

11

I.6

Safety Symbols and Precautions

11

I.7

Key Functions

12

I.8

Preventative Maintenance and Cleaning

13

II. GETTING STARTED

14

II.1

Auto Zero

14

II.2

Spindle Selection

15

II.2.1 Spindle Selection for Models WITHOUT Temperature Display

15

II.2.2

Spindle Section for Models WITH Temperature Display

16

II.3

Speed Selection & Setting

17

II.4 Autorange

18

II.5

CGS or SI Units Selection

19

II.6

Temperature Display in °F or °C

19

II.7 Out of Range

19

II.8 Operation

20

II.9

Timed Modes for Viscosity Measurement

21

II.9.1 Set Up

21

II.9.2

Timed Stop

21

II.9.3

II.9.4

Time to Torque

23

Temperature Offset

25

II.10

Print Modes

26

II.11 Communication with Wingather Software

27

II.12

Math Models

31

II.12.1 The Power Law (Ostwald) Model

31

II.12.2 The Herschel-Bulkley Model

32

II.12.3

The Bingham Model

34

II.12.4 The Casson Model

35

II.12.5 Other Common Rheological Models

37

III. MAKING VISCOSITY MEASUREMENTS

39

III.1 Quick Start

39

III.2

Preparations for Making Measurements

39

III.3 Selecting a Spindle/Speed

40

III.4 Multiple Data Points

40

Appendix A - Cone/Plate Viscometer Set-Up

42

Appendix B - Viscosity Ranges

47

Appendix C - Variables in Viscosity Measurement

51

Appendix D - Spindle and Model Codes

53

Appendix E - Calibration Check Procedures

55

Appendix F - The Brookfield Guardleg

62

Appendix G - Communications

64

Appendix H - Laboratory Stands with Parts Identification

65

Appendix I - DVE-50A Probe Clip

67

Appendix J - Fault Diagnosis and Troubleshooting

68

Appendix K - Online Help and Additional Resources

69

Appendix L - Warranty Repair and Service

70

Appendix M - Viscosity Test Report

71(tear out page)

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Manual No. M/07-022-D0613

I.

INTRODUCTION

The Brookfield DV-I PRIME Viscometer measures fluid viscosity at given shear rate. Viscosity is a measure of a fluid’s resistance to flow. You will find a detailed description of the science of viscosity in the Brookfield publication “More Solutions to Sticky Problems”, a copy of which was included with your DV-I PRIME.

The principle of operation of the DV-I PRIME is to drive a spindle (which is immersed in the test fluid) through a calibrated spring. The viscous drag of the fluid against the spindle is measured by the spring deflection. Spring deflection is measured with a rotary transducer. This system provides continuous sensing and display of the measurement during the entire test. The measurement range of a DV-I PRIME (in centipoise or milliPascal-seconds) is determined by the rotational speed of the spindle, the size and shape of the spindle, the container the spindle is rotating in, and the full-scale torque of the calibrated spring.

There are four basic spring torque series offered by Brookfield:

Model

Spring Torque milli Newton-m

dyne-cm

LVDV-I PRIME

673.7

0.0673

RVDV-I PRIME

7,187.0

0.7187

HADV-I PRIME

14,374.0

1.4374

HBDV-I PRIME

57,496.0

5.7496

The higher the torque calibration, the higher the measurement range. The viscosity measurement range for each torque calibration may be found in Appendix B.

Spring torque decals, on peel-off labels, are being supplied with your instrument. Please select the appropriate decal and attach to the viscometer.

The DV-I PRIME is available with a built-in temperature probe option, which allows temperature

readout over the range -100ºC to +300ºC (-148ºF to + 572ºF).

temperature measurement or temperature measurement of the sample during viscosity testing. Contact Brookfield or your local Brookfield agent for more information on this instrument option.

This option allows ambient

All units of measurement are displayed according to either the CGS system or the SI system.

1. Viscosity appears in units of centipoise (shown as “cP”) or milliPascal-seconds (shown as mPa•s) on the DV-I PRIME Viscometer display.

2. Torque appears in units of dyne-centimeters or Newton-meters (shown as percent “%”) in both cases) on the DV-I PRIME Viscometer display. Temperature appears in units of Celsius (shown as C) or Fahrenheit ( shown as F) on the DV-I PRIME Viscometer display.

( shown as F) on the DV-I PRIME Viscometer display. Tp 3. The following applies to

Tp 3.

The following applies to DV-I PRIME Viscometers with the temperature probe option. Look for the symbol Tp throughout this manual for instructions pertaining specifically to DV-I PRIME Viscometers with temperature probe option.

to DV-I PRIME Viscometers with temperature probe option. Brookfield Engineering Laboratories, Inc. Page 5

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The equivalent units of measurement in the SI system are calculated using the following conversions:

 

SI

CGS

Viscosity:

1 mPa•s

=

1 cP

Torque:

1 Newton-m

=

10 7 dyne-cm

References to viscosity throughout this manual are done in CGS units. The DV-I PRIME Viscometer provides equivalent information in SI units.

I.1

Components

Component

Part Number

Quantity

DV-I PRIME

For cone/plate versions

varies

1

Model G Laboratory Stand

Model G

1

Spindle Set with Case*

varies

1

LVDV-I PRIME set of four spindles (#61 through #64)

(SSL)

RVDV-I PRIME set of six spindles (#02 through #07)

(SSR)

HA/HBDV-I PRIME set of six spindles (#02 through #07)

(SSH)

Shipping Cap*

B-30-3Y

1

Power Cord (115V/230V)

DVP-65/66

1

Guardleg* (not supplied with HA/HB versions)

varies

1

LVDV-I PRIME

B-20Y

RVDV-I PRIME

B-21Y

Carrying Case

DVE-106

1

Operating Manual

M07-022

1

Torque Decals

T05-1012

1

Spindle wrench

CP-23

1

Cone spindle

CPE-XX

1

Sample cup

varies

1

Standard

CPE-44Y

With embedded temperature probe and cable

CPE-44PY

The following applies to DV-I PRIME Viscometers with the temperature probe option. Look for the symbol Tp throughout this manual for instructions pertaining specifically to DV-I PRIME Viscometers with temperature probe option.

to DV-I PRIME Viscometers with temperature probe option. OPTIONAL ITEMS RTD Temperature Probe Probe Clip RTD

OPTIONAL ITEMS RTD Temperature Probe Probe Clip RTD Cable when supplied with Cone/Plate version

OPTIONAL ITEMS RTD Temperature Probe Probe Clip RTD Cable when supplied with Cone/Plate version
OPTIONAL ITEMS RTD Temperature Probe Probe Clip RTD Cable when supplied with Cone/Plate version

DVP-94Y

1

DVE-50A

1

SC4-61Y

1

Please check to be sure that you have received all components and that there is no damage. If you are missing any parts, please notify Brookfield Engineering or your local Brookfield agent immediately. Any shipping damage must be reported to the carrier.

* Not supplied with Cone/Plate version.

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I.2

Utilities

Input Voltage:

Input Frequency:

Power Consumption:

Power Cord Color Code:

115 VAC or 230 VAC 50/60 Hz 22 WATTS

United States

Outside United States

Hot (live)

Black

Brown

Neutral

White

Blue

Ground (earth)

Green

Green/Yellow

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I.3 Components and Dimensions DV-I Prime Viscometer Model G Laboratory Stand Spindle Set Shipping Cap
I.3
Components and Dimensions
DV-I Prime Viscometer
Model G Laboratory Stand
Spindle Set
Shipping
Cap
LV Guard
Leg
Cone/Plate Option Wrench Cone Spindle Sample Cup
Cone/Plate Option
Wrench
Cone Spindle
Sample Cup
Temperature Probe Option • For use with SSA or C/P : Te mperature Cable SC4-61Y
Temperature Probe Option
• For use with SSA or C/P :
Te mperature Cable
SC4-61Y
• For use in beaker :
Te mperature Probe Clip
Te mperature Probe

Figure I-1

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Figure I -2 Brookfield Engineering Laboratories, Inc. Page 9 Manual No. M/07-022-D0613

Figure I-2

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I.4

Specifications

 

Speeds:

0.0, 0.3, 0.6, 1.5, 3, 6, 12, 30, 60,

(rpm)

0.5, 1, 2, 2.5, 4, 5, 10, 20, 50, 100

Weight:

Gross Weight

20 lb

9 kg

 

Net Weight

17 lb

7.7 kg

Carton Volume

1.65 cu ft

0.05 m 3

Operating Environment:

Analog Torque Output:

Viscosity Accuracy:

Viscosity Repeatability:

Torque Output: Viscosity Accuracy: Viscosity Repeatability: Tp Temperature Sensing Range: T p Temperature Accuracy:

Tp Temperature Sensing Range:

T p Temperature Accuracy: Tp Temperature Accuracy:

Tp Temperature Sensing Range: T p Temperature Accuracy: Tp Analog Temperature Output: 0°C to 40°C Temperature

Tp Analog Temperature Output:

0°C to 40°C Temperature Range (32°F to 104°F) 20% - 80% R.H.: non-condensing atmosphere

0 - 1 Volt DC (0 - 100% Torque)

±1% Full Scale Range in Use (See Appendix D for range calculation)

0.2% of Full Scale Range in Use

-100°C to +300°C (-148°F to +572°F)

±1°C: -100°C to +149°C ±2°C: +150°C to +300°C

0-4 Volt DC (10 mV/°C)

Electrical Certifications:

Conforms to CE Standards:

BSEN 61326: Electrical equipment for measurement, control and laboratory use - EMC requirements

BSEN 61010-1:

Safety requirements for electrical equipment, for measurement, control and laboratory use

Notice to customers:

measurement, control and laboratory use Notice to customers: This symbol indicates that this product is to

This symbol indicates that this product is to be recycled at an appropriate collection center.

Users within the European Union:

Please contact your dealer or the local authorities in charge of waste management on how to dispose of this product properly. All Brookfield offices and our network of representatives and dealers can be found on our website: www.brookfieldengineering.com

Users outside of the European Union:

Please dispose of this product according to your local laws.

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I.5

Setup

1. To assemble the Model S Laboratory Stand, place the upright rod into the base (refer to assembly instructions in Appendix H). The rack gear and clamp assembly should face the front of the base. The upright rod is held in place with a screw, which is attached from the bottom of the base. Tighten this screw with a screwdriver.

2. Be sure that the clamp screw, VS-41Y, is loose. Insert the mounting rod on the back of the DV-I PRIME Viscometer into the hole on the clamp assembly.

3. Tighten the VS-41Y clamp screw. Adjust the Viscometer to be as close to level as possible while tightening the clamp screw.

Tp
Tp
Tp 4. Connect the optional RTD temperature probe to the temperature port on the rear panel

4. Connect the optional RTD temperature probe to the temperature port on the rear panel of the DV-I PRIME, if provided.

5. The Viscometer must be level. The level is adjusted using the two Leveling Screws (VS-3) on the base. Adjust so that the bubble level on top of the DV-I PRIME is centered within the circle. Check level periodically during use.

6. Remove Shipping Cap

 

7. Make sure that the AC power switch at the rear of the DV-I PRIME is in the OFF position. Connect the power cord to the socket on the back panel of the instrument and plug it into the appropriate AC line.

 
  The AC input voltage and frequency must be within the appropriate range as

The AC input voltage and frequency must be within the appropriate range as

shown on the nameplate of the viscometer.

The DV-I PRIME must be earth

 

grounded to ensure against electronic failure!

 

8. For Cone/Plate models, refer to Appendix A.

 

I.6

Safety Symbols and Precautions

Safety Symbols The following explains safety symbols, which may be found in this operating manual.

Indicates hazardous voltages may be present.safety symbols, which may be found in this operating manual. Refer to the manual for specific

Refer to the manual for specific warning or caution information to avoid personal injury or damage to the instrument.manual. Indicates hazardous voltages may be present. Precautions If this instrument is used in a manner

Precautions If this instrument is used in a manner not specified by the manufacturer, the protection If this instrument is used in a manner not specified by the manufacturer, the protection provided by the instrument may be impaired.

This instrument is not intended for use in a potentially hazardous environment.the protection provided by the instrument may be impaired. In case of emergency, turn off the

In case of emergency, turn off the instrument and then disconnect the electrical cord from the wall outlet.not intended for use in a potentially hazardous environment. The user should ensure that the substances

The user should ensure that the substances placed under test do not release poisonous, toxic or flammable gases at the temperatures to which they are subjected to during the testing. testing.

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I.7

Key Functions

Figure I-3 shows the control keys on the face of the DV-I PRIME Viscometer. The following describes each key’s function.

UP ARROW This key is used to scroll UP (in an increasing value direction) through the available This key is used to scroll UP (in an increasing value direction) through the available speed or spindle tables.

DOWN ARROW This key is used to scroll DOWN (in a decreasing value direction) through the available This key is used to scroll DOWN (in a decreasing value direction) through the available speed or spindle tables.

Tp Note : Pressing and holding the DOWN ARROW key during the POWER ON will

Tp Note: Pressing and holding the DOWN ARROW key during the POWER ON will change the temperature display between °C and °F.

MOTOR ON/OFF Turns the motor ON or OFF . Turns the motor ON or OFF.

°C and °F. MOTOR ON/OFF Turns the motor ON or OFF . Figure I -3 SET

Figure I-3

SET SPEED Causes the DV-I PRIME to begin running at the currently selected speed. Used for Time Causes the DV-I PRIME to begin running at the currently selected speed. Used for Time to Torque and Timed Stop tests. (see Section II.9 - Timed Modes for Viscosity Measurement.)

AUTO RANGE/ENTER Auto range presents the maximum (100% torque) viscosity attainable (known as Full Scale Range) for Auto range presents the maximum (100% torque) viscosity attainable (known as Full Scale Range) for the spindle/speed selected. This feature is functional when the motor is running. Viscometer accuracy is 1% of the maximum (100% torque) viscosity value; minimum recommended viscosity range is 10% of the maximum viscosity value.

Note:

Pressing and holding the AUTO RANGE key during power on will enable the viscosity display to be changed between CGS and SI units (see Section II.5).

ENTER Use to enter parameters in the Timed Stop Mode(see Section II.9.2).

TIMED OPTION Used to select timed modes for viscosity measurement (see Section II .9), and to select Used to select timed modes for viscosity measurement (see Section II.9), and to select temperature offset mode (see Section II.9.4).

SELECT SPINDLE This initiates spindle selection on the first press and then selects the currently scrolled-to spindle This initiates spindle selection on the first press and then selects the currently scrolled-to spindle when pressed a second time. Used for Time to Torque and Timed Stop tests (see Section II.9 - Timed Modes for Viscosity Measurement).

PRINT Initiates print modes (see Section II .10. ) Initiates print modes (see Section II.10.)

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I.8

Preventative Maintenance and Cleaning

Make sure the instrument is in a decent working environment (dust-free, moderate temperature, low humidity, etc.)I.8 Preventative Maintenance and Cleaning Make sure the instrument is on a level surface. Hands/fingers must

Make sure the instrument is on a level surface.(dust-free, moderate temperature, low humidity, etc.) Hands/fingers must be clean and free of residual sample. Not

Hands/fingers must be clean and free of residual sample. Not doing so may result in deposit build up on the upper part of the shaft and cause interference between the shaft and the pivot cup.etc.) Make sure the instrument is on a level surface. Be sure to remove spindle from

Be sure to remove spindle from the instrument prior to cleaning. Note left-hand thread. Severe instrument damage may result if spindle is cleaned in place.and cause interference between the shaft and the pivot cup. Instrument and Keypad: Immersed Components: Clean

Instrument and Keypad:

Immersed Components:

Clean with dry, non-abrasive cloth. Do not use solvents or cleaners.

Spindles and guard leg are made of stainless steel. Clean with non-abrasive cloth and solvent appropriate for sample material that is not aggressive to immersed components.

When cleaning, do not apply excessive force, which may result in bending spindles.material that is not aggressive to immersed components. Brookfield Engineering Laboratories, Inc. Page 13

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II.

GETTING STARTED

II.1

Auto Zero

Before readings may be taken, the Viscometer must be Autozeroed. This action is performed each time the power switch is turned on. The display window on the Viscometer will guide you through the procedure as follows:

NOTE:

Check instrument level before proceeding - see Section I.5.

Turn the power switch (located on the rear panel) to the ON position. This will result in the following screen display:

BROOKFIELD

PRIME

DV-I

VISCOMETER

Figure II-1

After a few seconds, the following screen appears:

 

BROOKFIELD

DV-I

Instrument Torque

RV

V6.0

Firmware Version

 

Figure II-2

No key press is required at this point. After a short time, the display will clear and the following will be displayed:

REMOVE SPINDLE PRESS ANY KEY

Figure II-3

After removing the spindle and pressing a key, the DV-I PRIME begins its Autozero. The screen will flash “Autozeroing Viscometer”.

AUTOZEROINGVISCOMETER

AUTOZEROING

VISCOMETER AUTOZEROING

VISCOMETER

Figure II-4

NOTE:

Be sure that the viscometer is level before initiating Autozero.

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After approximately 15 seconds, the flashing stops and the following screen appears:

REPLACE SPINDLE PRESS ANY KEY

Figure II-5

Pressing a key at this point results in the display of the DV-I PRIME default screen:

Calculated Viscosity Speed

Tp
Tp
 

cP 0.0

S01

Spindle Selected

 

OFFRPM

% 0.0

% Torque

(without Temperature Probe) Figure II-6a

 

cP 0.0

70.1°F

Temperature

OFFRPM

% 0.0

(with Temperature Probe) Figure II-6b

The display will vary slightly depending upon the status of the last spindle entry.

II.2

Spindle Selection

LVDV-I PRIME Viscometers are provided with a set of four spindles and a narrow guardleg; RVDV-I PRIME Viscometers come with a set of six spindles and a wider guardleg; HADV-I PRIME and HBDV-I PRIME Viscometers come with a set of six spindles and no guardleg (see Appendix F for more information on the guardleg.)

The spindles are attached to the viscometer by screwing them on to the lower shaft. Note that the spindles have a left-hand thread. The lower shaft should be held in one hand and lifted up. The spindles should be screwed to the left. The face of the spindle nut and the matching surface on the lower shaft should be smooth and clean to prevent eccentric rotation of the spindle. Spindles can be identified by the number on the side of the spindle nut.

The DV-I PRIME requires a Spindle Entry Code number to calculate viscosity values. The two-digit entry code for each spindle can be found in Appendix D.

NOTE:

The DV-I PRIME will remember the Spindle Entry Code that was in use when the power was turned off.

II.2.1

Spindle Selection for Models WITHOUT Temperature Display

Pressing the SELECT SPINDLE key will cause the characters on the top line of the display to begin to blink. It will blink for about three seconds. If the UP or DOWN ARROW keys are pressed (while

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S is blinking) the two character spindle value to the right of the S character will begin to change (in either an increasing or decreasing direction depending upon which ARROW key is pressed) for each press of the key. If the ARROW key is pressed and held, the display will scroll through the spindle codes for as long as the ARROW key is depressed. When it reaches the last item in the list (either at the top or bottom of the list) the spindle code displayed will “roll-over” to either the first or last spindle code and the scroll action will continue.

When the desired spindle code is displayed, release the ARROW key to halt further scrolling. Press the SELECT SPINDLE key once again. This will cause the S character to cease blinking and the new spindle code will be accepted for use in viscometer calculations.

NOTE: You have approximately three seconds in which to press the SELECT SPINDLE key before the blinking stops. If you fail to press the SELECT SPINDLE key before the blinking stops you will have to repeat the above steps and re-select the desired spindle.

The DV-I PRIME will begin to calculate using the new spindle parameters as soon as the SELECT SPINDLE key is pressed the second time.

NOTE: The number 99 spindle is for use with special spindles when using Brookfield’s WINGATHER32 computer program. Refer to WINGATHER32 operator manual for further information on using “99” spindles.

DV-I PRIME remembers last spindle selected when power is shut down.

remembers last spindle selected when power is shut down. T p II.2.2 Spindle Section for Models

Tp II.2.2

Spindle Section for Models WITH Temperature Display

The steps for selecting and accepting a spindle entry are the same as Section II.2.1 except that when SELECT SPINDLE is depressed, the temperature display is temporarily replaced by the spindle entry code until the entry code is accepted (Figure II-7):

entry code until the entry code is accepted (Figure II -7): cP 123.4 S31 10 RPM
cP 123.4 S31 10 RPM % 89.7 Figure II-7
cP 123.4
S31
10 RPM
% 89.7
Figure II-7

Once the spindle entry code is accepted, the screen will return to the default display:

cP 123.4

70.1°F

10

RPM

% 89.7

Figure II-8

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II.3

Speed Selection & Setting

Table II-1 shows the available speed selections.

DV-I PRIME SPEEDS SETS

Beginning

0.0

 

0.3

When scrolling

0.6

“UP”

1.5

3.0

   

6.0

12

30

60

0.0

0.5

1.0

2.0

2.5

4.0

5.0

10

20

50

100

100

Table II-1

NOTE: DV-I PRIME speeds are organized to conform to the historical speed sets available on the Brookfield Dial Reading viscometer. Speeds from 0.3-60 RPM are traditionally found on the LVT viscometer. Speeds from 0.5-100 RPM are traditionally found on RVT, HAT, and HBT viscometers.

To select a viscometer speed first press either the UP or DOWN ARROW keys which will cause the area to the right of RPM (on the bottom line) to display the currently selected speed. Figure II-9 shows the DV-I PRIME had been operating at 10 RPM, and the current selected speed is 10 RPM.

cP 872.0 S01 10RPM10 % 87.2 Operating Speed “Selectable” Speed
cP 872.0
S01
10RPM10 %
87.2
Operating Speed
“Selectable” Speed

Figure II-9

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If the ARROW key is pressed just once and then released, the characters RPM will blink for three seconds, then will cease blinking resulting in no change to the speed entry.

NOTE:

The speed selection process remembers the last value of scrolled-to speed so that the next time you initiate a speed change (by pressing an ARROW key), the DV-I PRIME will begin its scroll display from the last entered value.

The last scrolled-to-speed does not necessarily have to be the same as the speed at which the DV-I PRIME is currently running. The user may operate at a given speed and pre-set the DV-I PRIME to the next desired speed before that speed will be used. For example, if the DV-I PRIME is currently running at 10 RPM and was previously scrolled to 20 RPM, a single press of either ARROW key would result in the Figure II-10 screen display:

cP 872.0 S01 10 RPM20 % 87.2
cP 872.0
S01
10 RPM20
%
87.2

Operating Speed

Scrolled to Selected Speed

Figure II-10

Pressing the SET SPEED key would cause the DV-I PRIME to begin running at 20 RPM.

If motor is off, pressing the MOTOR ON/OFF key immediately starts the DV-I PRIME running at the last scrolled-to-speed. If you had been running at 10 RPM, pressed MOTOR ON/OFF and then re-started the DV-I PRIME by pressing MOTOR ON/OFF once again, you would again be running at 10 RPM. However, if while the motor was off you had scrolled to a new speed of 20 RPM, pressing the MOTOR ON/OFF key would start the DV-I PRIME running at 20 RPM.

DV-I PRIME remembers last speed selected when power is shut down.

NOTE:

During both spindle or speed selection and scrolling operations, the DV-I PRIME will continue to calculate and display viscosity (cP) and torque (%).

II.4

Autorange

The AUTO RANGE key allows you to determine the maximum calculated viscosity (full scale reading) possible with the current spindle/speed setting. Pressing the key at any time will cause the current viscosity display to change and show that maximum viscosity. The screen torque display will now display a flashing “%100.0” to indicate this special condition. This maximum viscosity and flashing %100.0 value will be displayed for as long as the AUTO RANGE key is depressed. Figure II-11 shows the AUTO RANGE function for the situation where the No. 3 RV spindle is rotating at 20 RPM. The Full Scale Range is 5000 cP (or 5000 mPa . s).

cP 5000

S03

 
 
 

20 RPM

%100.0

%100.0

Figure II-11

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NOTE:

If the motor is off or the RPM is 0.0, the maximum viscosity displayed will be 0.0 cP (or 0.0 mPa . s).

II.5

CGS or SI Units Selection

 

Pressing and holding the AUTO RANGE key during power on will enable the viscosity display to be read in either CGS or SI units. To change the unit format:

1. Turn the power off.

 

2. Press and hold the AUTO RANGE key and turn the power ON.

The DV-I PRIME will retain the unit selection when the viscometer is turned OFF.

 

CGS

SI

 

Viscosity

cP

mPas

 

II.6

Temperature Display in °F or °C

Pressing and holding the DOWN ARROW key during power on will enable the temperature display to be read in either degrees Fahrenheit or degrees Centigrade. To change the units format:

1. Turn the power OFF.

 

2. Press and hold the DOWN ARROW key and turn power ON.

The DV-I PRIME will retain the unit selection when the viscometer is turned OFF.

Figure II-12 depicts the changes to the default screen when displaying temperature in the Fahrenheit scale and viscosity display in SI units:

   

mPas123.4

70.1°F

 

10 RPM

% 89.7

II.7

Out of Range

Figure II-12

Brookfield recommends taking viscosity readings between 10% and 100% of scale. The DV-I PRIME gives indications for out of specification or out-of-range operation. When % (Torque) readings exceed 100.0 % (over-range), the display changes to that shown in Figure II-13:

cP EEEE

S01

10 RPM

% EEEE

Figure II-13

You must change either speed or spindle to correct this condition. If you operate at spindle speeds that produce % (Torque) below 10.0 % (under-range), the DV-I PRIME flashes both % (Torque) and cP (Viscosity) on and off:

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cP 78.010 RPM20 S01 % 7.8

10 RPM20

S01

cP 78.0 10 RPM20 S01 % 7.8

% 7.8

Figure II-14

Negative % (Torque) will be displayed as shown in Figure II-15:

cP ----10 RPM20 S01 % -0.2

10 RPM20

S01

cP ---- 10 RPM20 S01 % -0.2

% -0.2

Figure II-15

Viscosity values will be displayed as “- - - -” when the % (Torque) is below zero.

II.8

Operation

The following procedure is outlined for making a viscosity measurement in a 600 mL low form Griffin beaker.

1. Mount the guardleg on the DV-I PRIME Viscometer (LV and RV series). Attach the spindle to the lower shaft. Lift the shaft slightly, holding it firmly with one hand while screwing the spindle on with the other (note left-hand thread). Avoid putting side thrust on the shaft.

2. Insert and center spindle in the test material until the fluid’s level is at the immersion groove in the spindle’s shaft. With a disc-type spindle, it is sometimes necessary to tilt the spindle slightly while immersing to avoid trapping air bubbles on its surface. You may find it more convenient to immerse the spindle in this fashion before attaching it to the Viscometer.

3. To make a viscosity measurement, select the desired speed setting. Allow time for the indicated reading to stabilize. The time required for stabilization will depend on the speed at which the Viscometer is running and the characteristics of the sample fluid. For maximum accuracy, readings below 10% should be avoided. Additional information on making viscosity measurements is available in Appendix C or the Brookfield publication “More Solutions to Sticky Problems”.

4. Record the reading and relevant test parameters. Brookfield recommends you record both % torque and viscosity in centipoise. Relevant test parameters might include: viscometer model, spindle, speed, temperature, container and time of test.

5. Press the MOTOR ON/OFF key to turn the motor “OFF” when changing a spindle or changing samples. Remove spindle and guardleg before cleaning. Clean spindles and guardleg after use, see Section I.8 for general cleaning recommendations.

6. Interpretation of results and the instrument’s use with non-Newtonian and thixotropic materials is discussed in the booklet, “More Solutions to Sticky Problems”, and in Appendix C: Variables in Viscosity Measurements.

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II.9

Timed Modes for Viscosity Measurement

The Timed Modes allow the viscometer user to implement Timed Stop and Time to Torque capabilities with the DV-I PRIME Viscometer. This feature will allow the user to set up the viscometer (i.e. select spindle and speed) and then record readings for a fixed period of time (Timed Stop) or until a set torque value is attained (Time to Torque). A series of menus will ask the user to input minutes and seconds (Timed Stop) or % torque (Time to Torque) and will then begin timing when the user presses the MOTOR ON/OFF key to ON. A message will be displayed showing time remaining (or time elapsed) and the appropriate display item (viscosity or torque) will be updated continuously during the event. Upon completion, the viscometer will display a screen stating that the test is complete and will also display the final recorded value for the viscosity in the first case, and the time in minutes and seconds to reach the torque limit in the second case.

II.9.1

Set Up

1. The user must pre-select the display unit option: CGS or SI (see Section II.5).

2. The user then selects (via the UP and DOWN arrows) the spindle speed (see Section II.3).

NOTE: If 0.0 RPM is the selected speed setting (the default after executing AUTOZERO) the timed modes can be executed; however, the results will be meaningless showing no viscosity values.

3. Next, the user selects the spindle number corresponding to the spindle attached.

4. Now, the user presses the MOTOR ON/OFF key to ensure that the motor is OFF. Setting the motor to the OFF condition sets up the viscometer for executing the Timed Modes.

5. The user presses the TIMED OPTION key to enter either of the timed test modes. Immediately, the following screen appears:

TIMED STOP

TIME TO TORQUE

Figure II-16

The user presses either the UP or DOWN ARROW key to select the test method of choice, which will be flashing.

II.9.2

Timed Stop

1. After pressing the ENTER key when in the display of Figure II-16, the user is presented with the following screen:

TIMED STOP

SET MIN’S:00

Figure II-17

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Using the UP and DOWN ARROW keys, the user enters a value for the minutes portion of the time to stop. This value can be as high as 99 minutes.

2. When satisfied, the user presses the ENTER key again to enter the seconds setting display:

TIMED STOP

SET SEC’S:00

Figure II-18

Using the UP and DOWN ARROW keys, the user enters a value for the seconds portion of the time to stop. This value will be between 0 and 59 seconds.

The user presses the ENTER key one more time at which point the viscometer will display the following screen:

TIMED STOP:PRESS MOTOR ON/OFF

Figure II-19

3. At this point, the user need only press the MOTOR ON/OFF key to begin the timed stop operation.

4. We will assume that the user pressed the MOTOR ON/OFF key to ON and is now presented with the following screen for the duration of the timed run:

CP 123456789

MIN: 15

SEC: 13

Figure II-20

NOTE: When this mode has begun, a press of the MOTOR ON/OFF key will interrupt the Timed Stop sequence and return the user to normal operation.

The seconds display will decrement from 59 to zero (0) in one (1) second intervals. When seconds reaches zero (0), the minutes value will decrement by one (1) minute. This will continue until all of the time has elapsed at which point the viscometer will display the following screen:

cP 123456789 TIMED STOP DONE

Figure II-21

At this point, the viscometer will stop the motor and continue to display this screen until the user presses the UP or DOWN ARROW keys to view the Torque and Speed that were current at the Timed Stop completion. This display would appear as follows:

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%=76.4 RPM=100 TIMED STOP DONE

Figure II-22

The display will switch between that of Figures II-21 and II-22 for each press of either the

UP or DOWN ARROW key.

The test can be repeated by pressing the motor ON/OFF key.

Pressing any key except the UP or DOWN ARROW keys or motor ON/OFF will cause the viscometer to exit the Timed Stop mode and resume normal operation.

NOTE: For the Timed Stop method, the DV-I PRIME Viscometer will retain the last value for the time interval in MEMORY so that it will become the default the next time the user elects to use this method.

II.9.3

Time to Torque

1. After pressing the UP OR DOWN key when in the display of Figure II-16, the user selects time to torque when flashing and presses enter.

The following screen will be presented:

TIMED TORQUE SET TORQUE:00%

Figure II-23

Using the UP and DOWN ARROW keys, the user enters a value for the torque level, which the viscometer must achieve. This value can be as high as 99%.

2. The user presses the ENTER key one more time to end the torque input at which point the viscometer will display the following screen:

TIMED TORQ:PRESS MOTOR ON/OFF

Figure II-24

3. At this point, the user need only press the MOTOR ON/OFF key to begin the timed torque operation.

4. We will assume that the user pressed the MOTOR ON/OFF key to ON and is now presented with the following display for the duration of the timed torque run:

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TORQUE = 24.2%

MIN: 15

SEC:13

Figure II-25

NOTE:

key will

interrupt the time to torque operation and return the user to normal operation.

When this mode has begun, a press of the MOTOR ON/OFF

The seconds display will increment from zero (0) to 59 in one (1) second intervals and the current value of the viscometer torque will be updated continuously. When seconds reach 59, the minutes value will increment by one (1) minute. This will continue until the user selected torque value is attained at which point the viscometer will display the following screen:

TORQUE = 85.0% TIMED TORQ DONE

Figure II-26

At this point, the viscometer will stop the motor and continue to display this screen until the user presses the UP or DOWN ARROW keys to view the viscosity that was current at the Timed Torque completion. The display would appear as follows:

22M 54S TO 85% TIMED TORQ DONE

Figure II-27

CP 123456789 TIMED TORQ DONE

Figure II-28

The display will switch between that of Figures II-27 and II-28 for each press of either the

UP or DOWN ARROW key.

The test can be repeated by pressing the motor ON/OFF key.

Pressing any key except the UP or DOWN ARROW key or motor ON/OFF will cause the viscometer to exit the Timed Torque mode and resume normal operation.

The time to torque value can be as high as 99 minutes and 59 seconds.

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NOTE: For the Time to Torque method, the DV-I PRIME Viscometer will retain the last entered torque in MEMORY for use when the user elects to perform a time to torque test again.

when the user elects to perform a time to torque test again. T p II.9.4 Temperature

Tp II.9.4

Temperature Offset

When the optional temperature probe is available with the DV-I PRIME, it is sometimes useful to be able to adjust the temperature readout to agree with an external temperature device. This can be accomplished utilizing the Temp Offset mode.

1. Enter the Timed Options menu by pressing the TIMED OPTION key. Use the up or down arrow key to select Temp Offset. The following screen will be presented.

TEMP OFFSET  TIMED STOP TEMP OFFSET
 TEMP OFFSET  TIMED STOP TIMED STOP

 TEMP OFFSET  TIMED STOP
 TEMP OFFSET  TIMED STOP

Figure II-29

2. Press ENTER. Figure II-30 will appear.

SET TEMP OFFSET? NO $# THEN ENTER $# THEN ENTER

Figure II-30

3. Press the UP/DOWN keys for YES or NO.

4. If NO is entered, temperature offset is disabled and display will return to default screen.

5. If YES is entered, the screen in Figure II-31 appears.

ENTER TEMP $# +0.0 OFFSET

Figure II-31

6. Use UP/DOWN arrows to scroll from +5.0 to -5.0 degrees C offset in 0.1º increments. (When temperature units are set to Fahrenheit, offset range is -9.0 to +9.0 degrees F)

7. Press ENTER to choose Temp Offset. The offset will be confirmed by the following screen, which will be displayed for 5 seconds, then returns to default screen.

TEMP OFFSET ENABLED

Figure II-32

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When Temp Offset is enabled the temperature units display will be underlined.

Cp 0.0

70.1°F

0.0 RPM

% 0.0

Figure II-33

NOTE: Temp. offset remains active when unit is powered down and powered up again.

II.10

Print Modes

NOTE:

The print key is inactive when the motor is off. The printer must be attached to the appropriate rear panel output connector. See Appendix G.

1. Press the print key once (less than 3 seconds) and DV-I PRIME will print one standard line to a printer through the serial port output.

Figure II-34 shows examples of the print strings for CGS and SI units.

For the case of CGS units with non-exponential results:

1

10

20

30

 

40

50

60

70

 

80

RPM=XXX M=XXXXX S=XX %=XXX.X

cP=XXXXX

D/CM2=XXXXX

1/SEC=XXXXX

T=XX.XC

ZXX:XX

and CGS units with exponential results.

 

1

10

20

30

 

40

50

60

70

 

80

RPM=XXX M=XXXXX S=XX %=XXX.X

cP=XXXeX

D/CM2=XXXeX

 

1/SEC=XXXXX

T=XX.XC

ZXX:XX

Similarly, for SI units with non-exponential results.

 

1

10

20

30

 

40

50

60

70

 

80

RPM=XXX M=XXXXX S=XX %=XXX.X

mPas=XXXXX N/M2=XXXXX

1/SEC=XXXXX

T=XX.XC

ZXX:XX

and SI units with exponential results.

 

1

10

20

30

 

40

50

60

70

 

80

RPM=XXX M=XXXXX S=XX %=XXX.X

mPas=XXXeX

N/M2=XXXeX

1/SEC=XXXXX

T=XX.XC

ZXX:XX

M = To rque

T = Te mperature

Z = Time

Figure II-34

2. To initiate a continuous print mode, press and hold the print key for more than 3 seconds and the following screen appears.

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PRINT INTERVAL SET MIN’S: 00

Figure II-35

3. Use up and down arrows to enter desired minutes for print interval (00 to 99).

4. Press enter to accept minute value and advance to set sec (00 to 59).

PRINT INTERVAL SET SEC’S: 00

Figure II-36

5. Press enter and the instrument will start to print at the interval, which has been set. The instrument display will show a flashing P in front of the % sign when operating in continuous print mode.

front of the % sign when operating in continuous print mode. CP123.4 S01 10RPM P% 19.7
CP123.4 S01 10RPM P% 19.7 Figure II-37
CP123.4
S01
10RPM
P%
19.7
Figure II-37

6. To pause printing, turn motor off.

7. To stop continuous print mode, press print key.

II.11

Communication with Wingather Software

The DV-I PRIME can be used in conjunction with the Brookfield software program Wingather. Wingather will collect the data output from the DV-I PRIME and allow for; data storage, data printing, graphing, and mathematical analysis.

NOTE: Wingather must be version 3.0 or higher for use with DV-I PRIME.

The DV-I Prime must be set to continuous print mode for proper communication to Wingather (Refer to Section II.10 for instruction). Set the print interval to 00MIN and 01SEC. Data collection modes are detailed in the Wingather Help files. All test controls will remain at the DV-I PRIME (spindle selection, speed selection, speed change). The communication cable (part number DVP- 80) for connecting the DV-I PRIME to the computer is supplied with the Wingather software.

Important features and benefits in Wingather, which enhance operator versatility in performing viscosity tests, include the following:

• 32-bit operation for rapid performance.

• Wingather version 3.0 is compatible with Windows™ 2000, NT, XP, Vista, and Windows™ 7 operating systems for flexible operation.

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• Brookfield’s DVLoader software (for setting up test programs) is integrated intoWINGATHER. DV Loader is an easy-to-use, structured command language, which makes detailed viscosity tests simple to program (see Section V).

• Easy-to-use data gather modes including automatic follow up events (save data, analyze data, print data).

• Manual scaling of plot axes.

• Auto range feature which shows in screen display the complete viscosity range which can be measured at any shear rate for a specific spindle geometry.

• Concurrent plotting of six data sets on one graph.

The following figures show the principal screens associated with Wingather:

show the principal screens associated with Wingather: Figure II -38: Dashboard Screen Brookfield Engineering

Figure II-38: Dashboard Screen

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Figure II -39: Gather Screen Figure II -40: DV Loader Screen Brookfield Engineering Laboratories, Inc.

Figure II-39: Gather Screen

Figure II -39: Gather Screen Figure II -40: DV Loader Screen Brookfield Engineering Laboratories, Inc. Page

Figure II-40: DV Loader Screen

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Figure II -41: Run/Data Screen Figure II -42: Analysis Screen Brookfield Engineering Laboratories, Inc. Page

Figure II-41: Run/Data Screen

Figure II -41: Run/Data Screen Figure II -42: Analysis Screen Brookfield Engineering Laboratories, Inc. Page 30

Figure II-42: Analysis Screen

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II.12

Math Models

Math models provide parameters that indicate how materials will behave in various circumstances where shear stress and shear rate vary. The data and calculated model parameters can be used to help QC and R&D characterize how a product will behave for the customer and how it will behave during processing.

When selecting a math model, it is important to take into consideration the parameters that need to be measured, as well as, the confidence of fit (CoF). A CoF above 98 is recommended. This appendix discusses the parameters of the following four models, what kinds of materials they should be used with, and provides an example of each. All models discussed are available with Brookfield’s Rheocalc™, Wingather™, and RHEO 3000™ software.

• Power Law (Ostwald)

• Herschel-Bulkley

• Bingham

• Casson

In addition to the above models, this section also briefly covers the NCA/CMA Casson model and the IPC Paste Model. These can be found at the end of this section.

II.12.1

The Power Law (Ostwald) Model

end of this section. II.12.1 The Power Law (Ostwald) Model ( t = shear stress, k

( t

= shear stress, k = consistency index,

What does it tell you?

stress, k = consistency index, What does it tell you? = shear rate, and n =

= shear rate, and n = flow index)

The Power Law model provides a consistency index, k, which is a product’s viscosity at one reciprocal second. (Reciprocal seconds are the units of measurement for shear rate.) It also provides a flow index, n, which indicates the degree with which a material exhibits non-Newtonian flow behavior. Since Newtonian materials have linear shear stress vs. shear rate behavior and n describes the degree of non-Newtonian flow, the flow index essentially indicates how “non-linear” a material is.

essentially indicates how “non-linear” a material is. Figure II -43 Brookfield Engineering Laboratories, Inc.

Figure II-43

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When n < 1 the product is shear-thinning or Pseudoplastic. This means the apparent viscosity decreases as shear rate increases. The closer n is to 0, the more shear thinning the material is.

When n > 1 the product is shear-thickening or Dilatant. Their apparent viscosity increases as shear rate increases.

When should you use it?

This model should be used with non-Newtonian, time-independent fluids that do not have a yield stress. These fluids will begin to flow under any amount of shear stress. Graphs of such material generally intersect the y-axis at 0.

An Example of the Power Law Model at Work

Formulators at a personal care company would like to use a substitute ingredient to decrease cost. They use the Power Law model to evaluate the effect the new ingredient will have on the behavior of their shampoo. They need to know how it will behave during processing and how it will behave when it is being used be the consumer

With the new ingredient the shampoo has a flow index (n) of 0.08. This indicates that the shampoo is shear-thinning enough to flow properly during processing and that it will flow properly for the end-user. The consistency index, k, indicates how the shampoo behaves when it experiences low shear rates. The power law values show that the shampoo becomes quite thin at process shear rates and therefore it can be easily pumped into filling equipment, hold tanks, etc. The consistency index of 91,071 cP shows that the shampoo is very viscous at low shear rates, and as a result, it will appear to customers to be“rich and creamy” while still being easy to apply.

Shampoo

Flow Index (n) = 0.08 Consistency Index (k) = 91071cP

II.12.2

The Herschel-Bulkley Model

Index ( k ) = 91071cP II.12.2 The Herschel-Bulkley Model ( t = shear stress, t

( t = shear stress, t o = yield stress, k = consistency index,

What does it tell you?

stress, k = consistency index, What does it tell you? = shear rate, and n =

= shear rate, and n = flow index)

The Herschel-Bulkley model is simply the Power Law model with the addition of t o for yield stress. Yield stress, t o , denotes how much shear stress is required to initiate flow. This model also provides a consistency index, k, which is a product’s viscosity at 1 reciprocal second, and a flow index, n, which indicates the degree with which a material exhibits non-Newtonian flow behavior. Since Newtonian materials have linear shear stress vs. shear rate behavior and n describes the degree of non-Newtonian flow, the flow index essentially indicates how “non-linear” a material is. For Herschel-Bulkley fluids, n will always be greater than or less than 1.

When n < 1 the product is shear-thinning or Pseudoplastic. This means the apparent viscosity decreases as shear rate increases. The closer n is to 0, the more shear thinning the material is.

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When n > 1 the product is shear-thickening or Dilatant. It’s apparent viscosity increases as shear rate increases.

apparent viscosity increases as shear rate increases. When should you use it? Figure II -44 The

When should you use it?

Figure II-44

The Herschel-Bulkley model should be used with non-Newtonian, time-dependent materials that have a yield stress. Products with a yield stress only begin to flow after a certain amount of shear stress is applied. As a result, the flow curve intersects the y-axis at a point greater than 0. After yielding, the product creates a flow curve and behaves as a Power Law fluid so that n indicates where there is a shear-thinning or shear-thickening tendency. (In this case, if n =1, the material is behaving as a Bingham fluid, which is discussed next.)

An Example of the Herschel-Bulkley Model at Work

A company uses a gel-like substance as part

of their production process. Upon arrival

theytestthematerialandapplytheHerschel-

Bulkley model to ensure it will perform correctly during process. The results in Figure II-44 show that the consistency index is 8,550

cP, the flow index is 0.66, and the yield stress

is 51.0 dynes/cm 2 . These results indicate that

this batch of gel does not quite meet specification. While the consistency index is within

spec, the yield value is higher than normal so the fluid will not begin to flow as easily. With

a flow index of 0.66, this batch is also less shear thinning than normal. Pump and mixer speeds must be adjusted before using this material.

Gel-Like Substance

n = 0.66

t o = 51.0 dynes/cm 2

k = 8550 cP

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II.12.3

The Bingham Model

t = t o + h D ( t = shear stress, t o = yield stress, h = plastic viscosity, and D = shear rate)

What does it tell you?

t o , which is the amount of shear stress

The Bingham model indicates a product’s yield stress,

required to initiate flow. It also provides the plastic viscosity, h, which is the viscosity after a product yields.

h , which is the viscosity after a product yields. Figure II -45 When should you

Figure II-45

When should you use it?

This model should be used with non-Newtonian materials that have a yield stress and then behave in a Newtonian fashion once they begin to flow. As a result, the shear stress-shear rate plot forms a straight line after yielding. (Products that have a yield stress only begin to flow after a certain amount of shear stress is applied. They are also called “viscoplastic”. Their shear stress vs. shear rate graphs intersect the y-axis at a point greater than 0.)

An Example of the Bingham Model at Work

A manufacturer of drilling fluid applies the

Bingham Model to ensure the quality of their product. Results from a recent batch, shown in Figure II-45, showed that the yield stress and plastic viscosity were both below the

pass/fail criteria, which would cause the fluid to insufficiently hold-up the cuttings. The shipment was cancelled and the root-cause

of the problem was identified.

Drilling Fluid

Plastic Viscosity (h)

Yield Stress (

= 6621 cP

t

o ) = 166.4 dynes/cm 2

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II.12.4

The Casson Model

t = t o + h D
t =
t o + h D

( t = shear stress, t o = yield stress, h = plastic viscosity, and D = shear rate)

What does it tell you?

The Casson model provides parameters similar to that of the Bingham model. However, unlike the Bingham model, it was developed for materials that exhibit non-Newtonian flow after yielding. The Casson model indicates the product’s yield stress ( t o ), which is the amount of shear stress required to initiate flow, and the product’s plastic viscosity, h, which is the viscosity of the product after it yields.

h , which is the viscosity of the product after it yields. Figure II -46 When

Figure II-46

When should you use it?

The Casson model should be used with non-Newtonian materials that have a yield stress and that do not exhibit a “Newtonian-like” behavior once they begin to flow. This model is most suitable for fluids that exhibit Pseudoplastic or shear thinning, flow behavior after yielding.

These fluids have a non-linear flow curve. The point at which it crosses the y-axis is the product’s yield stress ( t o ). To protect the point at which the curve will intersect with the y-axis, the Casson model linearizes or straightens the plot by taking the square root of the data. To ensure accurate extrapolation to yield stress it is best to take some data at low shear rates.

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An Example of the Casson Model at Work

Before releasing a new over the counter gel, a pharmaceutical company needs to learn how it will behave which it is being used by the end consumer. They perform a full viscosity profile and apply the Casson model. From the results, shown in Figure II-46, they learn that

their ointment has a higher yield stress, t o , and lower plastic viscosity, h, than they originally intended. As a result it is difficult or dispense from its container (due to the high yield stress) and it does not hold it shape very well (due to the low plastic viscosity), making it difficult to apply a small amount to the affected area of the skin. Based on this data, formulators are able to modify the ingredients accordingly. Once a formulation is established, multi-point tests and the Casson model are performed as a QC tool to check batches before and after processing.

Pharmaceutical Gel

Plastic Viscosity (h)

Yield Stress (

= 329.8 cP

t

o ) = 325.8 dynes/cm 2

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II.12.5

Other Common Rheological Models

The NCA/CMA Casson Model

(1 + a)

t
t

= 2

Rheological Models The NCA/CMA Casson Model (1 + a) t = 2 t o + (1

t o + (1 + a)

NCA/CMA Casson Model (1 + a) t = 2 t o + (1 + a) h

hg ( t

= shear stress, t o = yield stress, h = plastic viscosity, and

, t o = yield stress, h = plastic viscosity, and = shear rate) The NCA/CMA

= shear rate)

The NCA/CMA Casson model is designed by the National Confectioners Association and the Chocolate Manufacturers Association as the standard rheological model for the industry. This model determines yield and flow properties under specified conditions and closely approximates the plastic behavior of chocolate before final processing.

the plastic behavior of chocolate before final processing. Figure II -47 When chocolate is used for

Figure II-47

When chocolate is used for enrobing, it must have a yield stress high enough to stay in place once it enrobes the filling. In the case of decorating chocolate, the yield stress must be high enough so it can keep its shape once it has been squeezed into place through a nozzle. For molding chocolate, the plastic viscosity must be low enough to completely fill the mold.

(The NCA/CMA lists Brookfield’s HA-spring range viscometer with a Small Sample Adapter, SC4-27 spindle and SC4-13R sample chamber as the approved apparatus.)

The IPC Paste Model

h=kR n

(h = viscosity, k = consistency index, R = rotational speed, n = shear sensitivity factor)

The IPC Paste Model was developed for solder pastes. It calculates the viscosity of solder pastes at 10rpm. The IPC Paste Model requires that the product be tested with a Brookfield Spiral Adapter at multiple speeds. More details can be found in the IPC-TM-650 Test Methods Manual (methods 2.4.34.2 and 2.4.3).

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This model is a variation of the Power Law Model. Unlike the Power Law Model, which relates apparent viscosity to shear rate, the IPC Paste Model relates apparent viscosity to the testing speed (rpm).

Model relates apparent viscosity to the testing speed (rpm). Figure II -48 Figure II -49 Brookfield

Figure II-48

viscosity to the testing speed (rpm). Figure II -48 Figure II -49 Brookfield Engineering Laboratories, Inc.

Figure II-49

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III.

MAKING VISCOSITY MEASUREMENTS

III.1 Quick Start

Viscosity Measurement

The DV-I PRIME Viscometer uses the same methodology for viscosity measurement as the Brookfield Dial Reading Viscometer and DV series of Digital Viscometers. If you have experience with other Brookfield equipment, this section will give you the quick steps for taking a viscosity reading. If you have not used a Brookfield Viscometer before, skip this section and go to Section III.2 for a detailed description.

A) Assemble and level the viscometer (Section I.5).

B) Autozero the viscometer (Section II.1).

C) Enter the spindle number using the SELECT SPINDLE key (Section II.2).

D) Introduce the spindle into the sample and attach the spindle to the coupling nut. NOTE: Left-hand threads.

E) Enter the speed of rotation using the ARROW KEYS and SET SPEED key (Section II.3).

F) Record % torque and viscosity.

III.2

Preparations for Making Measurements

A) VISCOMETER: The DV-I PRIME should be turned on, leveled and autozeroed. The level is adjusted using the two feet on the bottom of the base and confirmed using the bubble on the top of the head. Adjust the feet until bubble is inside the center target. Set the level prior to autozero and check the level prior to each measurement.

Proper level is essential for correct operation of the DV-I PRIME.

B) SAMPLE: The fluid to be measured (sample) must be in a container. The standard spindles, supplied with the DV-I PRIME (LV (1-4), RV (2-7), or HA/HB (2-7)), are designed to be used with a 600 mL low form Griffin beaker (or equivalent container with a diameter of 8.25cm). The same applies to the optional RV1, HA/HB1. Many other spindle systems are supplied from Brookfield with specific sample chambers such as the Small Sample Adapter, UL Adapter and Thermosel.

Brookfield recommends that you use the appropriate container for the selected spindle. You may choose to use an alternate container for convenience; however, this may have an effect on the measured viscosity. The DV-I PRIME is calibrated considering the specified container. Alternate containers will provide results that are repeatable but not “true.”

The LV (1-4) and RV (1-7) spindles are designed to be used with the guardleg attached. Measurements made without the guardleg will provide repeatable results but may not provide “true” results.

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When comparing data with others, be sure to specify the sample container and presence/absence of the guardleg.

Many samples must be controlled to a specific temperature for viscosity measurement. When conditioning a sample for temperature, be sure to temperature control the container and spindle as well as the sample.

Please see our publication, “More Solutions to Sticky Problems”, for more details relating to sample preparation.

III.3

Selecting a Spindle/Speed

The DV-I PRIME has the capability of measuring viscosity over a wide range (for example, the RVDV-I PRIME can measure fluids within the range of 100-13,000,000 cP) (see Appendix B). This range is achieved through the use of several spindles over many speeds.

The process of selecting a spindle and speed for an unknown fluid is normally trial and error. An appropriate selection will result in measurements made between 10-100 on the instrument % torque scale. Two general rules will help in the trial and error process.

1. Viscosity range is inversely proportional to the size of the spindle.

2. Viscosity range is inversely proportional to the rotational speed.

In other words: to measure high viscosity, choose a small spindle and/or a slow speed. If the chosen spindle/speed results in a reading above 100%, then reduce the speed or choose a smaller spindle.

Experimentation may reveal that several spindle/speed combinations will produce satisfactory results between 10-100%. When this circumstance occurs, any of the spindles may be selected.

Non-Newtonian fluid behavior can result in the measured viscosity changing if the spindle and/ or speed is changed. See our publication, “More Solutions to Sticky Problems,” for more detail.

When viscosity data must be compared, be sure to use the same test methodology: the same instrument, spindle, speed, container, temperature and test time.

III.4

Multiple Data Points

The majority of viscosity measurements are made at the quality control level and often consist of a single data point. The test is conducted with one spindle at one speed. The data point is a useful benchmark for the go/no-go decision in a production setting. The DV-I PRIME can be used for single point measurement.

Many fluids exhibit a characteristic change in viscosity and yield stress with a change in applied force. This non-Newtonian flow behavior is commonly seen in paints, coatings and food products as a decrease in viscosity as shear rate increases or an increase in yield stress as rotational speed

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increases. This behavior cannot be detected or evaluated with the single point measurement. Non-Newtonian flow is analyzed through the collection of viscosity data over a range of shear rates and the generation of a graph of viscosity versus shear rate (a rheogram). This information will allow for a more complete characterization of a fluid and may help in formulating and production of the product. The DV-I PRIME is capable of collecting multiple data points for comprehensive analysis of flow behavior. Wingather Software can be used for this type of analysis.

More information on flow behavior, shear rate and rheograms is available in our publication, “More Solutions to Sticky Problems.”

Brookfield Engineering Laboratories, Inc.

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Manual No. M/07-022-D0613

Appendix A - Cone/Plate Viscometer Set-Up

This Cone/Plate version of the DV-I PRIME uses the same operating instruction procedures as described in this manual. However, the “gap” between the cone and the plate must be verified/ adjusted before measurements are made. This is done by moving the plate (built into the sample cup) up towards the cone until the pin in the center of the cone touches the surface of the plate, and then by separating (lowering) the plate 0.0005 inch (0.013mm).

DV-I PRIME Cone/Plate Viscometers have an Electronic Gap Setting feature. This feature enables the user to easily find the 0.0005 inch gap setting that was established at Brookfield prior to shipment.

The following information explains how to set the Electronic Gap and verify calibration of the DV-I PRIME Viscometer.

A.1 Electronic Gap Setting Features

TOGGLE SWITCH allows you to enable/disable the Electronic Gap Setting Feature: left position is OFF (disabled), right position is ON (enabled).

PILOT LIGHT is the red (LED) light; when illuminated, it means the Electronic Setting Function is sensing (enabled).

CONTACT LIGHT is the yellow (LED) light; when it first turns on, the “hit point” has been found.

SLIDING REFERENCE MARKER is used after finding the “hit point;” it is the reference for establishing the 0.0005 inch gap.

MICROMETER ADJUSTMENT RING is used to move the cup up or down in relation to the cone spindle. Turning the ring left (clockwise) lowers the cup; turning it right (counterclockwise) raises the cup. Each line on the ring represents one scale division and is equivalent to 0.0005 inch movement of the plate relative to the cone.

Pilot Light

(red)

Toggle Swtich

Contact Light

(yellow)

Sliding Reference

Marker

Micrometer

Adjustment Ring

Pilot Light (red) Toggle Swtich Contact Light (yellow) Sliding Reference Marker Micrometer Adjustment Ring

Figure A-1

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A.2 Setup

1. Be sure that theViscometer is securely mounted to the Laboratory Stand, leveled and zeroed with no cone or cup attached and 0% torque is displayed.

2. Figure A-2 shows a typical water bath setup. Connect the sample cup inlet/outlet ports to the water bath inlet and outlet and set the bath to the desired test temperature. Allow sufficient time for the bath to reach the test temperature. The temperature range of the Sample Cup (CPE-44Y or CPE-44PY) is 0-100°C. Brookfield recommends a maximum temperature of 80°C to allow for direct hand contact for adjustment of the micrometer ring. When using the sample cup at temperatures near 0°C, be careful to avoid frost buildup on the top surface of the cup; this could prevent a proper fit with the micrometer ring. Please refer to the bath manual for the proper selection of bath fluid and tubing to ensure safe and proper operation.

3. TheViscometer has been supplied with aspecial cone spindle(s), which contains the Electronic Gap Setting feature. The “CPE” part number designation on the cone verifies the Electronic Gap Setting feature.

4. With the motor off, thread the cone spindle by using the spindle wrench to secure the viscometer coupling nut (see Figure A-3); gently push up on the coupling nut and hold this securely with the wrench. Thread the cone spindle by hand. Note: Left Hand Threads.

5. Attach the cup, taking care not to hit the cone with the cup (Figure A-4). There must be no fluid in the cup.

6. Option: The sample cup is available with an optional purge fitting. The user can connect a dry gas line to this and put a blanket of dry gas over the sample during measurement, if desired.

Micrometer Ring Cup Outlet Bath Bath Outlet Inlet Cup Sample Inlet Cup Bath/Circulator (CPE-44Y or
Micrometer
Ring
Cup
Outlet
Bath
Bath
Outlet
Inlet
Cup
Sample
Inlet
Cup
Bath/Circulator
(CPE-44Y
or
CPE-44PY)
Figure A-2
Micrometer Adjustment Ring Coupling Nut Spindle These surfaces must be clean! Wrench (CPE) Cone Figure
Micrometer
Adjustment
Ring
Coupling Nut
Spindle
These surfaces
must be clean!
Wrench
(CPE) Cone
Figure A-3
Do Not hit the CONE with the CUP! Figure A-4
Do Not hit the
CONE with the CUP!
Figure A-4

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A.3 Setting the Gap

1. Move the toggle switch to the right; this will turn on (enable) the Gap Setting Feature. The Pilot (red) light will be illuminated.

2. If the contact light (yellow) is illuminated, turn the micrometer adjustment ring clockwise (as you look down on the instrument) until the light is just breaking contact, i.e., flickering (see Figure A-5).

3. If the yellow contact light is not illuminated, slowly turn the micrometer adjustment ring in small increments (one or two scale divisions) counter-clockwise.

Continue moving the micrometer adjustment counter-clockwise until the contact light (yellow) turns on. Back off (rotate clockwise) until the light is just breaking contact, i.e., flickering.

4. Adjust the sliding reference marker, right or left, to the closest full scale division mark (see Figure A-6).

5. Turn the micrometer adjustment ring one scale division to the left to meet the line on the sliding reference marker. THE YELLOW CONTACT LIGHT SHOULD GO OFF.

6. You have established the gap space needed for measurement. NOW TURN THE TOGGLE SWITCH OFF (LEFT); THE RED PILOT LIGHT SHOULD GO OFF.

This viscoity of “electrically conductive” fluids may be affected if readings are taken with the Electronic Gap Setting feature “on”. Be sure to shut the feature “off” before taken readings!

7. Carefully remove the sample cup.

Moves Away from Hit Point Moves Towards Hit Point (clockwise) (counter-clockwise) LEFTx RIGHT ring slowly
Moves Away
from Hit Point
Moves Towards
Hit Point
(clockwise)
(counter-clockwise)
LEFTx
RIGHT
ring
slowly
Figure A-5
Figure A-6

Figure A-6

Notes: 1.

The cup may be removed and replaced without resetting the gap, if the micrometer adjustment ring has not been moved.

2. Remove the spindle from the viscometer when cleaning.

3. Re-establish the hit point every time the spindle is attached/detached.

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A.4 Making Measurements with Cone/Plate Geometry

Viscosity measurements are made on the DV-I PRIME C/P viscometer in the same way as the DV-I PRIME viscometer with several exceptions.

1. Prepare the viscometer as is described in Section III.2.

2. Brookfield recommends that you always make cone/plate measurements with temperature control. Be sure that the sample cup is connected to a circulating waterbath and that it is at the target temperature. If the set temperature is far from ambient, you may wish to preheat the spindle as well as the cup. The spindle can be preheated by removing it from the viscometer and resting it in the cup (be careful not to scratch the measurement surfaces on the spindle or cup). Attach the spindle to the viscometer prior to the next step.

3. Set the Gap (see Appendix A; Section A.3) Brookfield recommends that the gap be set at the same temperature at which the measurement will be made.

4. Remove the sample cup.

5. Measure the precise volume of sample required for the spindle. See Table A-1. Sample volume can have a great affect on the measurement. In general it is better to over fill the gap slightly than it is to under fill. It is also beneficial to establish a method of sampling that is repeatable to contribute to the repeatability of your viscosity measurement.

6. Insert the sample into the center of the sample cup. Avoid air bubbles when possible.

7. Attach the sample cup to the viscometer (be careful not to tilt the sample cup as this would reposition the sample from the center).

8. Wait for thermal equilibrium. Brookfield recommends a minimum of 1 minute for thermal equilibrium. You may want to increase this time if; there is a large difference in temperature between the sample and the control point, or if you have not preheated the spindle.

9. Operate the viscometer (see Section II.8, Steps 3 – 6). Refer to Section III.3 for assistance in selecting a spindle or speed.

10. Remove the sample cup at the conclusion of the test. Be careful to lower the cup so that no contact is made between the cup and spindle.

11. Remove the spindles (Refer to Appendix A; Section A.2, Step 4).

Cleaning: Refer to Section I.8 for general cleaning recommendations. Clean the cup and spindle at the conclusion of each test. Be careful not to let the sample dry or harden onto the spindle or cup since mechanical scraping may damage the measurement surfaces. Brookfield recommends that you remove the spindle prior to cleaning.

Take care not to scratch the measurement surface of the cup or spindle during the cleaning process. Take care not to drop the spindle; any dent on the outer edge of the spindle will affect the measurement.

The sample cup may be provided with an embedded temperature probe. The temperature probe connection should not be exposed to the cleaning solution or the test sample. Do not immerse the sample cup in a cleaning solution.

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A.5 Verifying Calibration

1. Determine the appropriate sample volume. Refer to Table A-1 to determine the correct sample volume required for the spindle to be utilized.

2. Select a Brookfield Viscosity Standard fluid that will give viscosity readings between 10% and 100% of Full Scale Range. Refer to Appendix B for viscosity ranges of cone spindles; ranges listed apply to CPE cones.

Do not use a silicone viscosity standard fluid with a viscosity value greater than 5000 cP with a Cone/Plate. Brookfield offers a complete range of mineral oil viscosity standards suitable for use with Cone/Plates for viscosities above 5,000 cP or shear rates above 500 sec -1 ; see Table E-1 and E-2 in Appendix E for a list of available fluids.

It is best to use a viscosity standard fluid that will be close to the maximum viscosity for a given cone spindle/speed combination.

Example:

LVDV-I PRIME Viscometer, Cone Spindle CPE-42, Brookfield Silicone Viscosity Standard having a viscosity of 9.7 cP at 25°C.

At 60 RPM, the Full Scale Viscosity Range is 10.0 cP. Thus, the viscometer reading should be 97% torque and 9.7 cP viscosity ± 0.197 (closer to ±0.2) cP. The accuracy is a combination of viscometer and fluid tolerance (refer to Interpretation of Calibration Test Results at the end of Appendix E).

3. With the motor off, remove the sample cup and place the viscosity standard fluid into the cup.

Cone Part No.

Sample Volume

CPE-40

0.5

mL

CPE-41

2.0

mL

CPE-42

1.0

mL

CPE-51

0.5

mL

CPE-52

0.5

mL

Table A-1

4. Attach the sample cup to the viscometer and allow sufficient time for the sample, cup and cone to reach temperature equilibrium.

5. Turn the motor on. Set the desired speed(s). Measure the viscosity and record the reading in both % torque and centipoise (cP).

NOTE:

The cone spindle must rotate at least five (5) times before a viscosity reading is taken.

6. Verify that the viscosity reading is within the allowable 1% deviation, as explained earlier, for the specific viscosity standard fluid(s) that you are using.

* The CPE designation on the cone spindle indicates use with Electronic Gap Setting Cone/Plate Viscometers/Rheometers only.

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Appendix B - Viscosity Ranges

LV (#1-4) and RV,HA,HB (#1-7) Viscometers

Viscosity Range (cP)

 

Viscometer

Minimum

Maximum

LVDV-1 PRIME

15

2,000,000

RVDV-I PRIME

100*

13,300,000

HADV-I PRIME

200*

26,600,000

HBDV-I PRIME

800*

106,400,000

*Minimum viscosity is achieved with optional RV/HA/HB-1 spindle. (Spindle Code 01)

Vane Spindles

Spindle

Torque

 

Shear Stress Range dyne/cm 2

Viscosity Range cP (mPa•s) @ 10 rpm

Range

Pa

V-71

LV

NOT RECOMMENDED FOR USE ON LV TORQUE

 

V-72

LV

.188-1.88

1.88-18.8

199

-

1990

V-73

LV

.938-9.38

9.38-93.8

996

-

9960

V-74

LV

9.38-93.8

93.8-938

4990

-

49900

V-75

LV

3.75-37.5

37.5-375

1996

-

19960

V-71

RV

 

.5-5

5-50

262

-

2620

V-72

RV

2-20

20-200

1110

-

11100

V-73

RV

10-100

100-1000

5350

-

53500

V-74

RV

100-1000

1000-10000

54300

-

543000

V-75

RV

 

40-400

400-4000

21300

-

213000

V-71

HA

 

1-10

10-100

524

-

5240

V-72

HA

4-40

40-400

2220

-

22200

V-73

HA

20-200

200-2000

10700

-

107000

V-74

HA

200-2000

2000-20000

108600

-

1086000

V-75

HA

 

80-800

800-8000

42600

-

426000

V-71

HB

HB

 

4-40

16-160

40-400

160-1600

2096

8880

 

20960

88800

-

V-72

-

V-73

V-74

V-75

HB

HB

80-800

800-8000

800-8000

8000-80000

42800

-

434400 -

428000

4344000

HB

320-3200

3200-32000

170400

-

1704000

Notes:

1) 1 Pa = 10 dyne/cm 2 2) 1 cP = 1 mPa•s 3) Possibility of turbulence at speeds above 10 rpm may give artificially higher viscosity readings.

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Small Sample Adapter and Thermosel

SSA and

   

Thermosel

Viscosity Range (cP)

Shear Rate sec-1

Spindle

LVDV-1 PRIME

SC4-16

120

-

400,000

.29N

SV4-18

3

-

10,000

1.32N

SC4-25

480

-

1,600,000

.22N

SC4-31

30

-

100,000

.34N

SC4-34

60

-

200,000

.28N

SC4-81

3

-

10,000

1.29N

SC4-82

3

-

10,000

1.29N

SC4-83

11

-

38,000

1.29N

SSA and

 

Viscosity (cP)

 

Shear Rate

Thermosel

     

sec-1

Spindle

RVDV-1 PRIME

HADV-I PRIME

HBDV-I PRIME

SC4-14

1,250

-

4,165,000

2,500

-

8,330,000

10,000

-

33,360,000

.40N

SC4-15

500

-

1,660,000

1,000

-

3,320,000

4,000

-

13,280,000

.48N

SC4-25

0

-

167,000

100

-

334,000

400

-

1,336,000

.93N

SC4-27

250

-

830,000

500

-

1,660,000

2,000

-

6,640,000

.34N

SC4-28

500

-

1,660,000

1,000

-

3,320,000

4,000

-

3,280,000

.28N

SC4-29

1,000

-

3,330,000

2,000

-

6,660,000

8,000

-

26,640,000

.25N

Thermosel

37

 

10,000

73.0

 

10,000

292

 

10,000

1.29N

-

-

-

SC4-81

SSA

37

 

10,000

73.0

 

10,000

292

 

10,000

1.29N

-

-

-

SC4-82

SSA

121

 

50,000

243

 

50,000

970

 

50,000

1.29N