BROOKFIELD DV3T Rheometer Operating Instructions Manual No. M13-2100 SPECIALISTS IN THE MEASUREMENT AND CONTROL OF VISCOSITY with offices in: Boston • Chicago • London • Stuttgart • Guangzhou BROOKFIELD ENGINEERING LABORATORIES, INC. 11 Commerce Boulevard, Middleboro, MA 02346 USA TEL 508-946-6200 or 800-628-8139 (USA excluding MA) FAX 508-946-6262 INTERNET http://www.brookfieldengineering.
Table of Contents I. INTRODUCTION................................................................................................... 5 I.1 Components................................................................................................................................6 I.2 Utilities.......................................................................................................................................8 I.3 Specifications................................................................
IV.5 Test Parameters......................................................................................................................51 IV.6 Running a Yield Test..............................................................................................................54 IV.7 Results....................................................................................................................................56 V. SETTINGS.......................................................................
I. INTRODUCTION The Brookfield DV-III Rheometer series has been the leading industrial rheometer since it was first introduced in 1989. Brookfield has continued to develop and improve the DV-III to provide the best value in the market for both quality control and research customers. The Brookfield DV3T Rheometer continues in this tradition of innovation, quality and value.
All units of measurement are displayed according to either the CGS system or the SI system. 1. Viscosity appears in units of centipoise (cP), Poise (P), milliPascal-seconds (mPa•s) or Pascalseconds (Pa•s) on the DV3T Rheometer display or centistokes (cSt) or millimeter squared per second (mm2/sec). 2. Shear Stress appears in units of dynes/square centimeter (D/cm2) or Newtons/square meter (N/m2)/or Pascals (Pa). 3. Shear Rate appears in units of reciprocal seconds (1/sec). 4.
COMPONENT DIAGRAM DV3T Rheometer Model G Laboratory Stand Bubble Level Spindle Set Shipping Cap Guard Leg LV Spindle Set shown above Leveling Screw Cone/Plate Option Temperature Probe Wrench Temperature Probe Clip Toggle Switch for Electronic Gap Tension Bar Cone Spindle Sample Cup Temperature Probe Figure I-1 Brookfield Engineering Labs., Inc. Page 7 Manual No.
I.2 Utilities Input Voltage: Input Frequency: Power Consumption: Power Cord Color Code: Hot (live) Neutral Ground (earth) 115 VAC or 230 VAC 50/60 Hz 150 VA United States Black White Green Outside United States Brown Blue Green/Yellow Main supply voltage fluctuations are not to exceed ±10% of the nominal supply voltage. I.3 Specifications Speeds: 0.01 - 250 RPM Gross Weight 23 lbs. 10.5 kg. Net Weight 20 lbs. 9 kg. Carton Volume 1.65 cu. ft. 0.05 m3 Carton Dimensions 22 in. (56 cm) W x 11 in.
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: This symbol indicates that this product is to be recycled at an appropriate collection center.
Note: The DV3T must be earth grounded to ensure against electronic failure!! 7) Turn the power switch to the ON position and allow the rheometer to warm up for 10 minutes before performing autozero. 8) For Cone/Plate models, refer to Appendix A. 9) If appropriate, connect USB cable (DVP-202) to USB port for connection of DV3T to PC or printer. 10) Review Read Me file. The Read Me file contains notes on the DV2T Firmware. This file can be found on the CD that contains the PG Flash Software.
I.5 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. Refer to the manual for specific warning or caution information to avoid personal injury or damage to the instrument. Precautions If this instrument is used in a manner not specified by the manufacturer, the protection provided by the instrument may be impaired.
Status Bar: The Status Bar provides information relating to the date and time (as configured by the user) and various connections to the DV3T Rheometer. Test Name: The Test Name identifies the name of the currently loaded test. Title Bar: The Title Bar identifies the activity to be conducted in the current view and includes any navigation icons that are relevant. Data Fields: The Data Fields include measurement results and test parameters.
II. GETTING STARTED II.1 Power Up The DV3T will go through a Power Up sequence when the power is turned on. The Rheometer will issue a beep, present a blue screen, and finally show the DV3T About screen for 5 seconds. The About screen is shown below and includes several critical parameters about the rheometer including; rheometer torque (LV, RV, HA, HB, or other), firmware version number, model number (DV3TLV for example) and the serial number.
Figure II-2 The operator must ensure that the rheometer is level (see Section I.4) and remove any attached spindle or coupling. When the Next button is pressed, the rheometer will operate for approximately 13 seconds. After the AutoZero is complete and the operator presses the Next button, the rheometer will transition to the Configure Viscosity Test screen. If the AutoZero was performed from the Settings Menu, then the rheometer will return to the Settings Menu.
II.4 Navigation The DV3T Rheometer uses a touch screen display. Navigation of the instrument features is done using a variety of Data Fields, Arrows, Command Keys and Navigation Icons. The operating system has been designed for intuitive operation and employs color to assist the user in identifying options. Data Fields require that the user touch the screen to initiate the data entry / selection process. These fields are normally outlined in black. They may also include a blue arrow.
II.5 Home Screen . The Home screen shows The DV3T Home screen can be accessed by using the Home Icon the Main Menu functions and provides access to User Log In and Settings (see Section V.4). Figure II-3 Configure Viscosity Test: Create and Run viscosity tests. Configure Yield Test: Create and Run yield tests. Load Test: Load a test that has previously been saved or created with PG Flash software. Tests may be loaded from internal memory or a USB Flash Drive.
The basic Configure Viscosity Test view is shown in Figure II-4. This view includes the Status Bar (Section II.3), Title Bar (which includes the Home and Settings icons), test name, test parameters, the More/Less bar, and Command Keys (see Section II.4). Status Bar Title Bar Test Name Test Parameters More/Less Bar Command Keys Figure II-4 The user can see the name of any test that has been loaded through the Load Test function.
The Command Keys include Clear, Save and Run. Clear: Clear all data that has been entered into the test parameters and restore the values to the factory default. Save: Save the current test. Run: Run the current test. The Test Parameter area includes many elements of the viscosity test as well as live measurements of Torque % and Temperature. Temperature data will only be displayed if a Brookfield temperature probe is connected to the DV3T Rheometer. Torque: A live signal from the rheometer.
All elements related to the measurement of yield are selected within Configure Yield Test . Tests that are created can be saved to the internal memory of the DV3T Rheometer or onto a connected USB . Flash Drive. Tests can be loaded from memory by selecting Load Test from the Home Screen TIP: Many aspects of configure Yield Test can be limited when User ID and Log In functions are implemented (see Section V.4.2). The basic Configure Yield Test view is shown in Figure II-6.
The command Keys include Clear, Save and Run. Clear: Clear all data that has been entered into the test parameters and restore the values to the factory default. Save: Save the current test. Run: Run the current test. The test parameter area includes many elements of the yield test as well as live measurement of temperature. Temperature data will only be displayed if a Brookfield temperature probe is connected to the DV3T Rheometer. Spindle: Immersion Mark: The currently selected spindle.
II.5.3 Load Test Test programs that are created (Configure Viscosity Test/Configure Yield Test) can be saved to the internal memory of the DV3T or to a USB Flash Drive. These files can be reloaded into the DV3T for immediate use through the Load Test function. A file that is placed onto a USB Flash Drive can be loaded onto any DV3T Rheometer. Within the Load Test function, the user can access the internal memory of the rheometer or any .
II.5.6 External Mode The DV3T Rheometer can be controlled from a computer through the use of optional Brookfield Software RheocalcT. The rheometer must be placed into external control mode from the Main . The rheometer must be connected to the computer with a USB A cable (DVP-202). Menu TIP: The Status Bar will indicate a proper connection to the computer by displaying the Computer . Icon The DV3T will display External Mode when configured for operation with the computer.
II.7 Out of Range The DV3T Rheometer will give on screen indications when the measurement is out of range of the instrument. When the %Torque reading exceeds 100% (over range), the display of %Torque, Viscosity, and Shear Stress will be EEEE (see Figure II-7). If the %Torque value is between 0 9.9%, the data field label will flash. When the %Torque is below zero (negative values), the display of Viscosity and Shear Stress will be ----.
II.8 Printing The DV3T Rheometer can communicate to a Dymo Label Writer 450 Turbo label printer. This printer can be purchased from Brookfield (Part No. GV-1046). The communication to the printer is by USB (cable provided with the printer). When the printer is connected to the DV3T, the printer icon will be visible in the status bar. The DV3T Rheometer can configure the print out for several formats of paper/labels. These various paper/label stocks are available from Brookfield. 1. 2. 3.
Data Label (Large) TIP: When printing to a label, if the data set includes more than one point, only the last point will be printed. Data Continuous Brookfield Engineering Labs., Inc. Page 25 Manual No.
III. MAKING VISCOSITY MEASUREMENTS III.1 Quick Start The DV3T Rheometer uses the same methodology for viscosity measurements as the Brookfield Dial Reading Viscometers and DV series of Digital Viscometers. If you have experience with other Brookfield equipment, this section will give you quick steps for taking a viscosity reading. If you have not used a Brookfield Rheometer before, skip this section and go to Section III.2 for a detailed description.
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 detail relating to sample preparation. III.3 Programming The DV3T Rheometer provides a powerful programming capability for data collection.
Two multi step Tests are shown below. The first test shows a three step test where each step has a different speed with a single data point collection. The results will include three viscosity points, one for each speed. The second test shows a two step test where the first step is a pre shear step. The pre shear is conducted at 200 rpm for one minute and no data is collected. The second step generates a single data point.
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. There are 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.
III.5 Temperature Control The DV3T Rheometer provides the ability to control the temperature of a connected Brookfield temperature control device such as the Thermosel (HT-106 controller) and water baths with SD or AP controllers (for example: TC-550SD). The Thermosel or water bath can then be used to control the temperature of the sample under test. The DV3T connects to the temperature control device through a dedicated communication cable. The Thermosel requires cable DVP-141.
Figure III-7 Initiate temperature control by pressing the Test Connection. The connection status will be confirmed with a message box and the appearance of the bath icon in the status bar (see Section II.3). The Default Temperature is the temperature value that the control device will return to at the conclusion of a Test. This value is set only if the check box is checked. When the check box is unchecked, the temperature controller will hold at the last set point used in the Test.
III.7 Selecting Data Collection The DV3T Rheometer offers several options for data collection. The Data Collection setting is shown in Configure Viscosity Test directly under the Temperature display. The factory setting is Single Point (see Figure III-8). Pressing the blue arrow, in this field, will present the Data Collection screen (see Figure III-9). Figure III-8 Figure III-9 Single Point: Collect only a single data point when the End Condition is met. Brookfield Engineering Labs., Inc.
Single Point Averaging: Specify an amount of time over which to average measured data. Collect a single data point when the End Condition is met. This data point is an averaged value. If the time for averaging is shorter than the total time for the step, then the average will be performed for the specified time at the end of the test.
at Step End. During the test, the total time required to reach 200 cP is 65 seconds. Total points collected will be 7 with the last data point taken at 65 seconds, an average of the 5 seconds after point #6. Example 8: End Condition is set to Viscosity = 200 cP, Multi Point Data Interval is 1 minute. Averaging Duration is 20 seconds. Check the check box to Also Collect Single Point at Step End. During the test, the total time required to reach 200 cP is 10 minutes 40 seconds.
TIP: An End Condition of zero Time can be useful when measuring a new material. During the test, the speed can be changed without ending and then rerunning the test (see Section III.10). This method can allow you to quickly evaluate the spindle selection to determine the best speeds for testing. # of Points: The test will complete when the specified number of data points has been collected. Data is collected according to the Data Collection setting (see Section III.6).
A violation of the QC Limits during the test will be indicated by a flashing yellow box around the display for the specified parameter. Note that Time does not have a dedicated display. A violation will also result in an audible beep and a one time warning message (see Figure III-11). Data will continue to be collected while the warning message is displayed.
Instructions: Record specific instructions to the operator. This information will be presented immediately when the program is Run (see Figure III-13). The operator is required to acknowledge the message before the program will continue. Figure III-13 TIP: If the operator selects “Do not show this message again” within the Instructions message box, then Instructions will no longer be displayed for any test. This condition can be reset to allow Instructions to be displayed .
III.10 Running a Test A viscosity test is started by pressing the Run button on the Configure Viscosity Test screen. When Run is pressed, the display will change to the Running Viscosity Test screen (see Figure III-14). Status Bar Title Bar Test Name Measurement Data Real Time Graph Command Keys Figure III-14 The Running Viscosity Test screen provides information on the current measurement including: Torque, Viscosity, Shear Stress, Shear Rate, Temperature and Speed.
Temperature is the input value from a connected Brookfield temperature probe. The DV3T is provided with a DVP-94Y probe that can be inserted into the test sample or a water bath. The Cone/Plate version of the DV3T can be utilized with a sample cup that includes an embedded temperature probe. Some Brookfield accessories include temperature probes (Thermosel) or optional chambers with embedded temperature probes (Small Sample Adapter). The units of .
Figure III-15 The More/Less Bar can be used to reduce the number of parameters shown in the display. The Speed parameter is active in this view. The operator can change the speed of test without returning to the Configure Viscosity Test screen. TIP: If the speed is changed during the execution of a saved test, then the test status will be changed to “Unsaved Test”. This will also be reflected if the collected data is saved. View Test includes the Stop Test command key and a Back Arrow navigation key.
The Results screen includes several Navigation Icons and Command Keys. Home: Return to the Home Menu. Down Arrow: Select Results Options. Blue Arrow: Select Page of Results Table. Print: Print Data to USB printer. Save: Save data. Configure Test: Return to Configure Viscosity Test screen. Scroll Bar: Move up/down through a page of data. The Results screen offers several options for viewing test data.
Table: Display all data points. Data will be shown in a scroll list where each page can hold a maximum of 50 points. If the data set has more than 50 points, then additional pages will be indicated at the bottom of the screen. Additional pages of data can be accessed through the use of the Blue Arrows Each data point includes: Viscosity, Torque, Speed, Temperature, Time, Shear Stress (SS), Shear Rate (SR), Density, and Accuracy.
Graph: Display a graph of the collected data. The axis will default to the values selected in the Report section of the Test. The value displayed on each axis can be changed by selecting from the blue drop down arrow in each field. Individual data points can be selected and the X / Y coordinate values will be displayed. The selected point is represented by a blue dot (other points are shown as grey dots). TIP: Some spindle selections do not allow for the calculation of shear stress and shear rate.
Figure III-19 shows the Power Law equation for a typical set of data. A brief definition of the equation will be shown if the i (information) button is pressed. Figure III-19 Detailed information about Math Models is presented in Section VII. III.12 Data Averaging The DV3T Rheometer offers two techniques to average data, Live Averaging and Post Test Averaging. Data averaging can be useful when measuring samples with entrained air or suspended particles that case some variation in measurement results.
Multi Point Averaging requires a definition of 1) Data Interval, the frequency of data collection and 2) Averaging Duration, the amount of time for which readings will be averaged. These two parameters will work in conjunction to generate multiple data points each of which represent the average of all data measured during the average duration within the specified Data Interval. Post Test Averaging of data occurs after the test is complete, through the Results screen.
Step Averaging: Calculate Average and Standard Deviation for all data collected within a single step test. Step Averages will be displayed as shown below in Figure III-21. Figure III-21 Test Averaging: Calculate Average and Standard Deviation for all data collected within step specified. Test Averages will be displayed as shown below in Figure III-22. Figure III-22 Brookfield Engineering Labs., Inc. Page 46 Manual No.
IV. MAKING YIELD MEASUREMENTS IV.1 Quick Start The DV3T Rheometer uses the same methodology for yield measurements as the Brookfield YR-1 and DV-III Ultra Rheometers. If you have experience with other Brookfield equipment, this section will give you quick steps for making a yield measurement. If you have not used a Brookfield Rheometer before, skip this section and go to Section IV.2 for a detailed description. A) B) C) D) E) F) G) H) I) Assemble and level the DV3T Rheometer (Section I.4).
IV.3 Selecting a Spindle/Speed The DV3T has the capability of measuring yield stress over an extremely wide range. For example, the DV3TRV can measure fluids within the range of 0.5-400 Pa. This range is achieved through the use of several vane spindles over many speeds. See Appendix B for details. 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.
If your instrument has the EZ-Lock system, the spindles are attached as follows: With one hand hold the spindle, while gently raising the springloaded outer sleeve to its highest position with the other hand, as shown in Figure IV-2. Insert the EZ-Lock Spindle Coupling so that the bottom of the coupling is flush with the bottom of the shaft, and lower the sleeve. The sleeve should easily slide back down to hold the spindle/coupling assembly in place for use.
Figure IV-3 Select Temperature Controller and you will be presented with the Default Temperature menu (see Figure IV-4). This menu allows the user to 1) initiate communication with the temperature controller and 2) set a default temperature. Figure IV-4 Initiate temperature control by pressing the Test Connection. The connection status will be confirmed with a message box. Brookfield Engineering Labs., Inc. Page 50 Manual No.
The Default Temperature is the temperature value that the control device will return to at the conclusion of the Test. This value is set only if the check box is checked. When the check box is unchecked the temperature controller will hold at the last set point used in the Test. TIP: When a test involves several temperature set points, set the Default Temperature to the first set point used in the Test. This will reduce the transition time from one Test run to the next Test run. IV.
Pre-Shear Speed and Time An optional Pre-Shear step can be included in the test parameters. The user must supply the pre-shear speed (0.01 - 250 rpm) and pre-shear time (1 second - 5 minutes 59 seconds). Pre-shearing is the shearing of sample before measuring its yield properties. This process breaks down the sample’s structure. It is particularly useful if the investigator wants to eliminate previous shear history (e.g.
Torque Reduction Torque Reduction is percentage change in torque value between successive data points. That is, the material yields or begins to break down and, as a result, the measured incremental torque begins to decrease. A value of 100% for this parameter causes the test to stop as soon as there are no torque increases during a base time increment. Some users may wish to see a drop in torque after the yield point.
Save Path Define the memory location (internal or USB Flash Drive) where the Test Results will be saved. TIP: Selecting a data path can help to organize data storage in the internal memory of the DV3T. By preselecting the data path, operators are directed to put the data from specific tests into specific areas. TIP: If you select a data path that includes a USB Flash Drive location and the Flash Drive has been removed, an error message will be displayed. IV.
TIP: Torque on the DV3T is equivalent to the % reading from the DV-III Ultra and the YR-1 Rheometer. Stress is the calculated stress based on the Speed, Torque, and Spindle. Strain is the Apparent Strain placed on the sample. The Apparent Strain is the angular distance that the spindle rotates in the sample. Temperature is the input value from a connected Brookfield temperature probe. The DV3T is provided with a DVP-94Y probe that can be inserted into the test sample or a water bath.
IV.7 Results Measurement data is viewed in the Results screen. This screen is presented at the conclusion of a . test or when data is loaded through the View Results selection from the Home Menu The DV3T utilizes a comprehensive data format. Data files include the complete set of measurement results and calculated values along with the test protocol. All elements of the test can be viewed in the Results screen. The DV3T Rheometer allows for 5000 total data points per file.
The Results screen offers several options for viewing test data. These options are accessed via the Down Arrow in the Navigation Bar at the top of the screen (see Figure IV-8). Figure IV-8 Table: Display all data points. Data will be shown in a scroll list where each page can hold a maximum of 50 points. If the data set has more than 50 points, then additional pages will be indicated at the bottom of the screen.
Compare Results: Load two data sets and view side by side. Figure IV-9 Device Info: Display basic information about the data file and the specific DV3T Rheometer used to collect the data including: date and time the test started, completed and was saved; if user accounts are active, which user saved the data; rheometer serial number, firmware version, rheometer Torque range (LV, RV, HA, HB, other). Graph: Display the final data point and graph.
V. SETTINGS The Settings menu provides access to the many controls and features of the DV3T Rheometer. This which is often present in the Title Bar. menu can be accessed through the Settings Navigation Icon Figure V-1 shows the Settings Menu which is divided into: Device Setup, User Settings, Global Settings, and Admin Functions. Global Settings include items that affect the complete range of features within the DV3T. Admin Functions include items related to administrator level controls. Figure V-1 V.
The temperature menu provides access to three functions: Temperature Offset, Temperature Controller Access, and Temperature Display/Settings. Figure V-2 Temperature: The Temperature Offset setting allows the user to create up to 10 temperature offset values for connected temperature probes.
Figure V-3 The creation of a Temperature Offset requires input of the offset value and a name. The offset value must be in the range of -9.9 to 9.9˚C. The Name can be up to 14 characters long. To delete an existing Temperature Offset, first select the offset from the list, then press the Delete command key at the bottom of the screen. The use of a Temperature Offset will be indicated in the Temperature field displayed in the Configure Viscosity Test screen with a (o) beside the Live indication.
Communication is established when the Test Connection command button is pressed. You must press this button every time the DV3T Rheometer is powered on. Be sure that the temperature controller is turned on prior to pressing the Test Connection button. The Default Temperature screen also allows the user to set a Default Temperature. The Default Temperature is the set point value that will be used by the DV3T when a test (Viscosity Test or Yield Test) is not in use.
• • • Turn the coupling until the % Torque reading is 10 – 15 %. Gently let go of the coupling. Watch the reading. The % Torque reading should decrease smoothly and oscillate about 0.0%. Selecting Oscillation Check in the Device Setup menu will present the user first with a screen instructing to level the rheometer and remove the spindle. Confirmation of level and spindle removal will present the user with the Oscillation Check screen as shown below.
Figure V-6 TIP: The information on the About screen will be needed when contacting Brookfield for support. To return from the About screen, press the Left Arrow navigation button in the Title Bar. V.2 User Settings The User Settings menu includes settings related to specific users. The DV3T may be set up for a single user setting (used by one or more operators) or for multiple users who access through a Log In and Password.
The Language Setting is selected by pressing the Language field and choosing the appropriate language from the list. The selected language will be implemented immediately. Pop-Up Messages can be toggled on/off through the check box (see Figure V-7). This check box applies to all Pop-Up Messages. Pop-Up Messages can be toggled off individually through the check box that appears within the message box. Once the Pop-Up is turned off, it will not be shown again.
Measurement Units: The Measurement Units menu displays the current selections for measurement units. Each unit can be changed by pressing the blue down arrow and selecting the desired value. Measurement Units are part of the data file for saved results.
Regional Settings: The Regional Settings menu displays the current selections for the default language, number format, date format and day separator. Each setting can be changed by pressing the blue down arrow and selecting the desired value. Regional Settings are part of the data file for saved results. The Language setting established the default language for the DV3T. Individual users can choose a different language for use with their specific log in (see Section V.2).
Figure V-8 The Running Viscosity Test display will show a colored box around the data parameter associated with the Global Alarm. When the alarm condition is first met, the colored box will be yellow. If the measurement parameter returns to the acceptable range, then the colored box will be removed. When the alarm condition is met a second time, the colored box will be red (see Figure V-9). The audible alarm will only sound once.
Spindle List: The selection of Spindle in Configure Viscosity Test can be done by using either a number pad or a scroll list. (This choice is selected through the navigation button in the Set Spindle screen.) The contents of the scroll list are defined in the Spindle List menu. Each spindle can be individually selected or deselected through the use of a check box. Spindles, shown with both their name and their number, are listed numerically according to their spindle entry number.
Code The code is the numerical value used to select the spindle. This value must be unique and can not be the same as a standard Brookfield spindle. The acceptable range for Code is 100-199. Name The Name is a unique value to describe the spindle. The Name will be displayed in the Spindle field. The Name can be comprised of alpha and numeric characters. SMC The SMC (Spindle Multiplier Constant) is used to convert the measured torque to viscosity. The acceptable range of SMC is 0.001 – 500.
V.4 Admin Functions The Admin Functions menu includes settings related to access and basic instrument management of the DV3T. The Admin Functions menu is only available to the Administrator when Log In is required. Users and Power Users do not have access rights to the Admin Functions.
User ID from the drop down list and then enter their password. The Log In requirement is removed when the check box is unchecked. The Allow Lock Out check box controls the Running Viscosity Test Lock Out function. This function is only available when User Login is required. When Allow Lock Out is checked, the found in user may lock the DV3T during a test. The Lock Out is set by pressing the Lock Icon the Navigation Bar of Running Viscosity Test.
Table V-1: Factory Default User Settings (continued on following page) General Settings Administrator Power User User Set Default Temperature Set Point N/A N/A N/A Temperature Probe Offset • • Allow Test Done Alarm • • • QC Alarm • • • Global Alarm • • • Pop-Up Warnings • • • Dismiss Pop-Up Warnings • • Customize Data Access Functions Load A Test Save a Test Load Data Save Data Other Options Viscosity Test Setup Set Brookfield Engineering Labs., Inc.
Yield Test Setup Set Administrator Power User Spindle • • Immersion Mark • • Pre-Shear Speed • • Pre-Shear Time • • Wait Time • • Run Speed • • Zero Speed • • Torque Reduction • • Yield Limits • • Temperature Setpoint • • Graph Axes • • Instructions • • Save Path • • User Table V-1: Factory Default User Settings (continued from previous page) Brookfield Engineering Labs., Inc. Page 74 Manual No.
V.4.3 Set Time and Date The Time and Date is displayed on the Status Bar at the top of every screen. These parameters are set within the Set Time and Date menu. The format for setting Time and Date will be based on the Regional Settings (see Section V.3). Change from Set Time to Set Date by pressing the command key at the bottom of the screen. When both Date and Time are set correctly for your location, press OK to accept the change. V.4.
V.4.5 Default Path The Path is the location where data or tests are stored. The DV3T will allow for storage to the Internal Memory or to an attached USB Flash drive. The path will also include any file structure that has been created. The Default Path identifies what location will be used as the initial location when Results are saved. The Default Path defined in Reports - Configure Viscosity Test (saved test or unsaved test) will take priority over the Default Path.
V.4.8 Calibration Reminder The DV3T can be programmed to provide the user with a reminder that calibration is due. Two parameters must be set: Frequency in Months and Start Date. When both parameters are entered, the Calibration Reminder screen (see Figure V-13) will calculate and display the day when the reminder will be presented. Check the Calibration Reminder On check box to activate this feature.
V.4.9 Save Audit Trail The Audit Trail is a collection of instrument check values that can assist Brookfield with troubleshooting activities. You may be asked to provide the Audit Trail files. Use Save Audit Trail to create an Audit Trail file on a USB stick. Two files will be created: Users.bin and Service.bin. Brookfield Engineering Labs., Inc. Page 78 Manual No.
VI. PG FLASH SOFTWARE Viscosity Test programs for the DV3T can be created on a computer through the use of PG Flash software. PG Flash is provided with all DV3T Rheometers on a CD that contains several different Brookfield utility software programs. PG Flash is designed to operate on the Windows platform XP or higher. PG Flash software provides all Viscosity Test controls that are available on the DV3T. Additionally, multiple step Viscosity Test programs can be created for use on DV3T.
The General Parameters section includes all Viscosity Test program controls that will apply to every step of the program. Spindle: The spindle to be used with this Viscosity Test. All calculations will be based on this spindle number. Report Screen: Select the view to be presented upon the conclusion of the Viscosity Test. Save Results Path: Select if a path for saving data is to be defined. Define the save path. Post Test Averaging: Select the type of averaging to perform at the end of the test.
Units Setup Figure VI-2 Sample Viscosity Test programs can be seen in the following figures. Figure VI-3 demonstrates a typical single step test. Figure VI-4 demonstrates a multiple step test. Figure VI-3 Figure VI-4 Brookfield Engineering Labs., Inc. Page 81 Manual No.
Yield Test parameters are shown in a single area within PG Flash without a Program Grid (only a single step for Yield Tests). All yield parameters are available including Spindle Settings, Test Settings and Test Instructions & Path Settings. Spindle: The currently selected spindle. All Yield and Stress calculations will be made based on the Spindle selection and the Immersion Mark. Spindle choice is limited to vane spindles or user defined custom spindles.
VII. MATH MODELS VII.1 The Power Law (Ostwald) Model (τ = shear stress, k = consistency index, = shear rate, and n = flow index) What does it tell you? 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.
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 Shampoo Flow Index (n) = 0.08 Consistency Index (k) = 91071 cP With the new ingredient the shampoo has a flow index (n) of 0.08.
VII.2 The Herschel-Bulkley Model (τ = shear stress, τo = yield stress, k = consistency index, = shear rate, and n = flow index) What does it tell you? The Herschel-Bulkley model is simply the Power Law model with the addition of τo for yield stress. Yield stress, τo, denotes how much shear stress is required to initiate flow.
When should you use it? 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.
VII.3 The Bingham Model τ = τo + hD (τ = shear stress, τo = yield stress, h = plastic viscosity, and D = shear rate) What does it tell you? The Bingham model indicates a product’s yield stress, τo, which is the amount of shear stress required to initiate flow. It also provides the plastic viscosity, h, which is the viscosity after a product yields.
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 VII-3, 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. Brookfield Engineering Labs., Inc.
VII.4 The Casson Model √τ = √τo + √hD (τ = shear stress, τo = 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.
An Example of the Casson Model at Work Before releasing a new over the counter gel, a Pharmaceutical Gel pharmaceutical company needs to learn how it will behave which it is being used by the Plastic Viscosity (h) = 329.8 cP end consumer. They perform a full viscosity Yield Stress (τo) = 325.8 dynes/cm2 profile and apply the Casson model. From the results, shown in Figure VII-4, they learn that their ointment has a higher yield stress, τo, and lower plastic viscosity, h, than they originally intended.
VII.5 Other Rheological Models The NCA/CMA Casson Model (1 + a) √τ = 2√ τo + (1 + a) √ηD (τ = shear stress, τo = yield stress, h = plastic viscosity, and = 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.
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). Figure VII-6 Figure VII-7 Brookfield Engineering Labs., Inc. Page 92 Manual No.
Appendix A - Cone/Plate Rheometer Set-Up This Cone/Plate version of the DV3T 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 (0.013 mm).
A.2 Setup 1. Be sure that the Rheometer 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. 3.
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. Note: The motor should be OFF. 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 no longer illuminated (see Figure A-5). 3.
A.4 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. Brookfield uses mineral oil viscosity standard fluids to calibrate Wells Brookfield Cone/Plate Rheometers at the factory.
Appendix B - Viscosity Ranges Viscosity Range Tables Viscosity ranges shown are for operational speeds 0.1 through 200 rpm. LV Rheometer with LV spindles #1-4 and RV/HA/HB Rheometers with spindles #1-7 Viscosity Range (cP) Rheometer Minimum Maximum DV3TLV 15 6,000,000 DV3TRV 100 40,000,000 DV3THA 200 80,000,000 DV3THB 800 320,000,000 Small Sample Adapter and Thermosel SSA and Thermosel Spindle Viscosity (cP) DV3TLV DV3TRV DV3THA DV3THB Shear Rate sec-1 Å S SC4-14 58.6 - 1,171.
UL Adapter Viscosity (cP) UL Spindle YULA-15 or 15Z Shear Rate sec-1 DV3TLV DV3TRV DV3THA DV3THB 1 - 2,000 3.2 - 2,000 6.4 - 2,000 25.6 - 2,000 1.22N DV3THB Shear Rate sec-1 DIN Adapter Accessory DAA Spindle Viscosity (cP) DV3TLV DV3TRV DV3THA 85 0.6 - 5,000 6.1 - 5,000 12.2 - 5,000 48.8 - 5,000 1.29N 86 1.8 - 10,000 18.2 - 10,000 36.5 - 10,000 146 - 10,000 1.29N 87 5.7 - 50,000 61 - 50,000 121 - 50,000 485 - 50,000 1.
Vane Spindles Spindle Torque Range V-71 Shear Stress Range (Pa) Viscosity Range cP (mPa·s) NOT RECOMMENDED FOR USE ON LV TORQUE V-72 LV .188-1.88 104.04-1.04K V-73 LV .938-9.38 502-5.02K V-74 LV 9.38-93.8 5.09K-50.9K V-75 LV 3.75-37.5 1.996K-19.96K V-71 RV .5-5 262-2.62K V-72 RV 2-20 1.11K-11.1K V-73 RV 10-100 5.35K-53.5K V-74 RV 100-1K 54.3K-543K V-75 RV 40-400 21.3K-213K V-71 HA 1-10 524-5.24K V-72 HA 4-40 2.22K-22.2K V-73 HA 20-200 10.
Special Considerations In taking viscosity measurements with the DV3T Rheometer, there are two considerations which pertain to the low viscosity limit of effective measurement. 1) Viscosity measurements should be accepted within the equivalent % Torque Range from 10% to 100% for any combination of spindle/speed rotation. 2) Viscosity measurements should be taken under laminar flow conditions, not under turbulent flow conditions. The first consideration has to do with the precision of the instrument.
Appendix C - Variables in Viscosity Measurements As with any instrument measurement, there are variables that can affect a Rheometer measurement. These variables may be related to the instrument (Rheometer), or the test fluid. Variables related to the test fluid deal with the rheological properties of the fluid, while instrument variables would include the Rheometer design and the spindle geometry system utilized.
Rheometer Related Variables Most fluid viscosities are found to be non-Newtonian. They are dependent on Shear Rate, time of test and the spindle geometry conditions. The specifications of the Rheometer spindle and chamber geometry will affect the viscosity readings. If one reading is taken at 2.5 RPM, and a second at 50 RPM, the two cP values produced will be different because the readings were made at different shear rates. The faster the spindle speed, the higher the shear rate.
Appendix D - Spindle and Model Codes Each spindle has a two digit entry code which is entered via the keypad on the DV3T. The entry code allows the DV3T to calculate Viscosity, Shear Rate and Shear Stress values. Each spindle has two constants which are used in these calculations. The Spindle Multiplier Constant (SMC) used for viscosity and shear stress calculations, and the Shear Rate Constant (SRC), used for shear rate and shear stress calculations.
SPINDLE ENTRY CODE SMC SRC T-A 91 20 0 T-B 92 40 0 T-C 93 100 0 T-D 94 200 0 T-E 95 500 0 T-F 96 1000 0 ULA 00 0.64 1.223 DIN-81 81 3.7 1.29 DIN-82 82 3.75 1.29 DIN-83 83 12.09 1.29 DIN-85 85 1.22 1.29 DIN-86 86 3.65 1.29 DIN-87 87 12.13 1.29 SC4-14 14 125 0.4 SC4-15 15 50 0.48 SC4-16 16 128 0.29 SC4-18 18 3.2 1.32 SC4-21 21 5 0.93 SC4-25 25 512 0.22 SC4-27 27 25 0.34 SC4-28 28 50 0.28 SC4-29 29 100 0.
Table D-2 lists the model codes and spring torque constants for each Rheometer model. Table D-2 MODEL TK MODEL CODE ON DV3T SCREEN DV3TLV 0.09373 LV 2.5DV3TLV 0.2343 L3 5DV3TLV 0.4686 L5 1/4 DV3TRV 0.25 RQ 1/2 DV3TRV 0.5 RH DV3TRV 1 RV DV3THA 2 HA 2DV3THA 4 A2 2.5DV3THA 5 A3 DV3THB 8 HB 2DV3THB 16 B3 2.
Appendix E - Calibration Procedures The accuracy of the DV3T is verified using viscosity standard fluids which are available from Brookfield Engineering Laboratories or your local Brookfield agent. Viscosity standards are Newtonian, and therefore, have the same viscosity regardless of spindle speed (or shear rate). Viscosity standards, calibrated at 25°C, are shown in Table E-1 (Silicone Oils) and Table E-2 (Mineral Oils). For more help you can go to the website, www.brookfieldengineering.
Brookfield Viscosity Standard Fluid General Information We recommend that Brookfield Viscosity Standard Fluids be replaced on an annual basis, one year from date of initial use. These fluids are pure silicone and are not subject to change over time. However, exposure to outside contaminants through normal use requires replacement on an annual basis. Contamination may occur by the introduction of solvent, standard of different viscosity or other foreign material.
Calibration Procedure for a Small Sample Adapter Brookfield recommends a two step check. First, verify the calibration of the rheometer using the standard rheometer spindles (LV #1-3, RV #2-6, HA #2-6 and HB #2-6 or cone/plate spindles) as detailed in this appendix. Second, verify the calibration of the rheometer using the Small Sample Adapter. The use of an accessory device may increase the accuracy of measurement associated with the DV3T.
When a UL or DIN UL Adapter is used, the water bath is stabilized at the proper temperature: 1) Put the proper amount of viscosity standard fluid into the UL Tube (refer to the UL Adapter instruction manual). 2) Attach the spindle (with extension link and coupling nut) onto the DV3T. 3) Attach the tube to the mounting channel. 4) Lower the tube into the water bath reservoir, or if using the ULA-40Y water jacket, connect the inlet/outlets to the bath external circulating pump.
Calibration Procedure for Cone/Plate Rheometers 1) Follow the above procedures for mechanically adjusting the setting of the cone spindle to the plate. 2) Refer to Appendix A; Table A-1, and determine the correct sample volume required for the selected spindle. 3) Select a 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.
Brookfield Viscosity Standards Fluids are accurate to (+/-) 1% of their stated value. Example: Calculate the acceptable range of viscosity using DV3TRV with RV-3 Spindle at 2 RPM; Brookfield Standard Fluid 12,500 with a viscosity of 12,257 cP at 25°C: 1) Calculate full scale viscosity range using the equation: Full Scale Viscosity Range [cP] = TK * SMC * 10,000 RPM Where: TK - 1.
3) Total accuracy is the sum of the values n (1) and (2): At 6 RPM, accuracy is: 15.6 cP + 1.0 cP = +/- 16.6 cP At 12 RPM, accuracy is: 7.8 cP + 1.0 cP = +/- 9.8 cP At 30 RPM, accuracy is: 3.1 cP = 1.0 cP = +/- 4.1 cP 4) Therefore, at each speed, the acceptable windows within which the measured viscosity value must lie is calculated relative to the viscosity value of the standard: At 6 RPM: 84.9 cP to 118.1 cP At 12 RPM: 91.7 cP to 111.3 cP At 30 RPM: 97.4 cP to 105.
Appendix F - The Brookfield Guardleg The guard leg was originally designed to protect the spindle during use. The first applications of the Brookfield Rheometer included hand held operation while measuring fluids in a 55-gallon drum. It is clear that under those conditions the potential for damage to the spindle was great. Original construction included a sleeve that protected the spindle from side impact.
should be known that this type of torque reading will not convert into a correct centipoise value when using a Brookfield factor if the boundary conditions are not those specified by Brookfield. The guard leg is a part of the calibration check of the Brookfield LV and RV series Viscometer/ Rheometer. Our customers should be aware of its existence, its purpose and the effect that it may have on data.
Appendix G - Speed Selection Brookfield Rheometers offer a variety of speeds to provide for a wide range of viscosity measurement capabilities. Brookfield has traditionally supplied a defined set of speeds with specific Torque ranges: LV RV 0.3, 0.6, 1.5, 3.0, 6.0, 12, 30, 60 0.5, 1.0, 2.0, 2.5, 4.0, 5.0, 10, 20, 50, 100 The DV3T and earlier Brookfield DV-III Series Rheometers offer additional speeds to enhance measurement capabilities. The DV3T offers speeds from 0.
Appendix H - Laboratory Stands Model G is the standard laboratory stand which comes with the DV3T Rheometer. 1 2 3 4 5 Item 1 2 3 4 5 Part No. VS-CRA-14S VS-CRA-18S GV-1201 GV-1203 502028071S33B 50S311832S01B Description Upright Rod and Clamp Assembly Upright Rod and Clamp Assembly Base, includes 2 GV-1203 leveling screws Leveling Screws available separately or in assembly above Flat Washer 5/16 X 7/8 X .
Model Q is an optional laboratory stand which can be ordered for use with the DV3T Rheometer. The advantage is the rapid speed of movement for lowering and raising the rheometer head. 1 Actuation lever for up/down movement 2 3 4 5 Item 1 2 3 4 5 Part No. VSQA-001Y GV-1201 GV-1203 502028071S33B 50S311832S01B Description Upright Rod and Clamp Assembly Base, includes 2 GV-1203 leveling screws Leveling Screws available separately or in assembly above Flat Washer 5/16 X 7/8 X .
Unpacking Check carefully to see that all the components are received with no concealed damage. 1 Base, GV-1201, with 2 Leveling Screws, GV-1203, packed in a cardboard carton 1 Upright Rod with attached Clamp Assembly in the instrument case Assembly (Refer to Figures H-1 or H-2) 1. Remove the base assembly from the carton. 2. Remove the screw and washer from the upright rod. Place the rod and clamp assembly into the hole in the top of the base.
Appendix I - DVE-50A Probe Clip Probe Clip DVE-50A is supplied with all model DV3T Rheometers, DV-III Rheometers, and Digital Temperature Indicators. It is used to attach the RTD temperature probe to the LV Guard Leg (Part No. B-20Y) or 600 mL low form Griffin beaker. Figure I-1 is a view of the Probe Clip, showing the hole into which the RTD probe is inserted, and the slot which fits onto the LV guard leg.
Appendix J - Fault Diagnosis and Troubleshooting Listed are some of the more common problems that you may encounter while using your Rheometer. ❏ Spindle Does Not Rotate ✓ Make sure the rheometer is plugged in. ✓ Check the voltage rating on your rheometer (115, 220V); it must match the wall voltage. ✓ Make sure the motor is ON and the desired rpm is selected. ❏ Spindle Wobbles When Rotating or Looks Bent ✓ Make sure the spindle is tightened securely to the rheometer coupling.
❏ Rheometer Will Not Return to Zero ✓ Rheometer is not level • Check with spindle out of the sample. • Adjust the laboratory stand. ✓ Pivot point or jewel bearing faulty • Perform an Oscillation Check* ✓ Remove the spindle and turn the motor OFF; select display to % torque mode. ✓ Gently push up on the rheometer coupling. ✓ Turn the coupling until the digital display reads 10-15 on the % display. ✓ Gently let go of the coupling.
Appendix K - Instrument Dimensions Brookfield Engineering Labs., Inc. Page 122 Manual No.
Appendix L - Online Help and Additional Resources www.brookfieldengineering.com** The Brookfield website is a good resource for additional and self-help whenever you need it. Our website offers a selection of “how-to” videos, application notes, conversion tables, instructional manuals, material safety data sheets, calibration templates and other technical resources. http://www.youtube.com/user/BrookfieldEng Brookfield has its own YouTube channel.
Appendix M - Warranty Repair and Service Warranty Brookfield Viscometers/Rheometers are guaranteed for one year from date of purchase against defects in materials and workmanship. They are certified against primary viscosity standards traceable to the National Institute of Standards and Technology (N.I.S.T.). The Rheometer must be returned to Brookfield Engineering Laboratories, Inc. or the Brookfield dealer from whom it was purchased for no charge warranty service.
MODEL SPINDLE RPM DIAL READING % TORQUE BY: DATE: FACTOR VISCOSITY SHEAR cP RATE TEMP °C FOR: TIME NOTES BROOKFIELD ENGINEERING LABORATORIES, INC. • 11 Commerce Blvd. • Middleboro, MA 02346 • TEL: 508-946-6200 or 800-628-8139 FAX: 508-946-6262 • www.brookfieldengineering.com • VTR1207 CONCLUSIONS: SAMPLE TEST INFORMATION: VISCOSITY TEST REPORT This tear-off sheet is a typical example of recorded test data.
