BROOKFIELD RS-CPS+ RHEOMETER Operating Instructions Manual No. M08-218-B0212 (for serial numbers beginning with “304”) SPECIALISTS IN THE MEASUREMENT AND CONTROL OF VISCOSITY with offices in: Boston • Chicago • London • Stuttgart • Guangzhou BROOKFIELD ENGINEERING LABORA TORIES, 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. II. General Description................................................................................................ 5 I.1 Use of the Rheometer..................................................................................... 5 I.2 Measuring Principle......................................................................................... 5 System Configuration............................................................................................. 6 II.1 R/S-CPS+ Rheometer.
VI.6.1 Utilities → Zero Calibration.................................................................. 32 VI.6.2 Utilities → Edit Program....................................................................... 33 VI.6.3 Utilities → Print Programs.................................................................... 36 VI.6.4 Utilities → Measuring Systems............................................................ 37 VI.6.5 Utilities → Print Memory.................................................................
I. General Description This section has general information about the instrument and operating principles. I.1 Use of the Rheometer The R/S-CPS+ Rheometer is used in quality control, product development and research. The instrument measures Newtonian and non-Newtonian fluids, records flow curves and determines the viscosity functions in steady shear flows. I.2 Measuring Principle The R/S CPS+ Rheometer is a rotational, controlled-stress rheometer.
II. System Configuration The R/S CPS+ Rheometer system consists of: • Rheometer head containing electronic unit and measuring drive integrated in one housing • Basic instrument with temperature sensor PT100 • AC Adapter Available Accessories: • Measuring cones and measuring plates (see Appendix A)* • Bath/Circulator* • Computer system • Rheo 3000 software *The accessories in bold print are necessary for a minimal configuration. See Figure II-1 for illustration of the R/S CPS+ Rheometer System Components.
R/S-CPS+ Rheometer 1 12 3 11 2 8 4 7 5 10 6 9 1 2 3 4 5 6 7 8 9 10 11 12 Measuring Head of R/S-CPS+ Rheometer Measuring Element Coupling Cooling Flange Dial Gauge Bottom Measuring Plate Bank Indicator Height Adjusting Lever Micrometer Ring (Nonius) for fine adjustment AC Adapter DC Connecting Socket Main Connection Cable Data Transmission Cable Figure II-1: Configuration of the R/S-CPS+ Rheometer Brookfield Engineering Labs., Inc. Page 7 Manual No.
II.2 Measuring Devices The basic instrument is equipped with a temperature controlled bottom measuring plate. At least one measuring cone or one measuring plate is required as a rotating element for an operational measuring system. These rotating elements are not part of the basic equipment of the R/S CPS+ Rheometer; they must be ordered explicitly depending on your requirements. II.
III. Instrument Installation In this section you will learn how to set up and use the R/S CPS+ Rheometer for the first measurement, which include: -- Assembly of the R/S CPS+ Rheometer, -- Electric connections -- Installation of accessories such as thermostatting device, cooling device, and measuring systems -- Hose connections III.1 Mounting the Instrument The R/S CPS+ Rheometer should be positioned on an even surface, such as a laboratory bench.
III.2.1 Temperature Sensor The connecting cable of the temperature sensor Pt 100 (100 ohm DIN alpha RTD) is inserted into the socket labelled “Pt100” at the back side of the rheometer head. III.2.2 AC Adapter Do not use a power supply other than the AC adapter delivered by Brookfield for the R/S CPS+ Rheometer.
III.2.4 Computer Connection If the R/S-CPS+ Rheometer has to be used in “REMOTE” mode with a PC (Rheo 3000 program package) or with serial data-terminal for data-logging, the RS232 cable needs to be connected to the 25 pin connector labelled “RS232” on the back of the instrument. -- Turn the R/S-CPS+ Rheometer off with the “POWER” switch at the back of the instrument. -- Turn the computer system off.
The following working fluids are usually used in the temperature bath: -10°C to +90°C -20°C to +250°C Water (de-ionized) - Glycol Mixture Silicone Bath Oil Suitable bath fluids can be ordered from BROOKFIELD. We recommend strongly that the upper temperature limit be set at the liquid circulating thermostat to +95°C if water is used and to +250°C if oil is used. III.3.2 The Peltier Temperature Control Device If the R/S CPS+ has been equipped with a Peltier temperature control system (i.e.
Drawer G Fuse 5x20 1A (delay) Main Switch AC Power Supply Peliter Control Cable IN Peltier Power Supply IN Fig. 4-B: Back View of Peltier Supporting Unit P-TS The P-TS is powered via a grounded main socket. The AC voltage must be the same as the rated voltage shown on the plate. The cables for Peltier control are connected to the related sockets (see Figure 4-B).
IV. Environment, Handling, Cleaning and Maintenance IV.1 Operating Environment Find a comfortable, convenient work place for the installation of the R/S CPS+ Rheometer. There should be enough room to place the Rheometer, the measuring systems, the measuring substances and the peripheral devices (e.g. printer, computer and bath/circulator). You need a grounded AC plug to operate the R/S CPS+ Rheometer and additional plugs for the connection of each peripheral device (i.e. Bath, Peltier).
IV.4 Maintenance The R/S Rheometer system is designed for long-term operation. Should the instrument require repair, contact Brookfield or your authorized Brookfield dealer. Only authorized service personnel may work on the control electronics, all accessories, the meauring device, as well as the AC Adapter and all electric circuits and connections! Measurement accuracy can be checked by the user at any time.
V. Measuring Systems This section covers the various measurement geometries. The following types of measuring systems are suited for use with the R/S CPS+ Rheometer: a) cone/plate measuring systems b) plate/plate measuring systems Please select a suitable measuring system in the measuring range required for your measurements (see Appendix A.1). When measuring cones are used, the shear rate is the same across the whole measuring gap. The most common cone angles are α=1° and α=2°.
Micrometer Ring or Nonius Fig. 6: Setting the gap on the R/S-CPS+ Rheometer Set the micrometer ring (Nonius) to ZERO (scale division 0.01 corresponds to 10 μm). The micrometer ring (Nonius) bottom line has to be aligned with the ZERO level marking. Looking down onto the micrometer ring (Nonius) from the top, turn it counter-clockwise to lower the head and reduce the gap. Turning the micrometer ring (Nonius) clockwise will raise the head and increase the gap.
V.2 Filling the Measuring Systems Place the sample material on the bottom plate with the instrument head in the upper position. Air bubbles in the sample will affect test results and should be avoided. Remove excess sample from around the cone or plate with the provided spatula, taking care not to scratch the surface of the bottom plate. Remove excess sample from cone or plate edge. Set the bath/circulator to the required temperature if measurements are to be taken under controlled temperature.
VI. Operation and Menu System The following section summarizes the operation and the menu system of the R/S CPS+ Rheometer for both manual and PC-controlled measurement. Menu prompts for the R/S CPS+ Rheometer are available in the following languages: • English • German The language is selected via the menu level Configuration→Language (if English is active) or Konfiguration→Sprache (if German is active). For more details on language selection, see Section VI.7.6: Configuration → Language.
VI.1 Keyboard MAIN MENU - Single measurement - Program measurement - Remote > R/S + RHEOMETER - Select previous menu entry - Input: increment numerical value/letter ON - Select next menu entry - Input: decrement numerical value/letter ST OK - One digit to the right START/STOP - Back to parent menu - Abort - Start of measurement - Abort measurement OK - Accept - Select - One digit to the left All user inputs are made using the six keys located below the LCD. Some of the keys have multiple uses, i.
Key Operation 1) Menu Function of Key Example 1) Return to parent menu (turn 1) Utilities → Main page downward) 2) Input of numerical 2) Stop input (only if possible) values ST 3) Selection from list 3) Stop selection (only if possible) 3) Select meas.
VI.
Menu Handling Since the LCD of the R/S CPS+ Rheometer cannot show all menu items simultaneously, only three entries are displayed on the menu at a time. Arrows (>) on the right side of the display indicate that there are more menu entries. The arrow on the 2nd line indicates there are more menu entries above and the arrow on the 4th line indicates more menu entries below. The currently active (but not yet selected) entry is marked by a blinking field (cursor) on the left side of the LCD.
Example: Select Meas.system: 1) C25-2/30 2) C50-1/30 3) C50-2/30 VI.4 Input of Numerical Values and Alphanumeric Texts Most user defined entries are numbers. User defined values such as the Start and End values of a ramp, number of measuring points, factors, time, date, etc. are entered as numbers with or without decimal digits. If the display shows the decimal point in a number to be entered, input of a floating-point number is requested.
Input of Values: Val.[1/s]: 0290.00 Nr. of MP: 010 Time[s]: 0100 Note: If you press and hold one of the or keys while entering numbers, the digit will first increment or decrement by +/- 1. However, after a short period of time, the process will continue automatically. This corresponds to the Repeat Function of computer keyboards. key was pressed and held until the “9” was displayed. The repeat In this example, the function is only active during numerical and alphanumeric input.
Adjustable Temperature Set Value Error Indication (00 = no error) THERMOSTAT TS: 20.0 T: 20.0 Status: 00 p/q Info on Temperature Value That Can Be Varied Permanent Indication of Actual Temperature Value The last adjusted set point TS is always saved when the rheometer is turned off. When the rheometer is re-started, the Peltier will return to the last set point. Modify the set point temperature with the and keys.
Values and Alphanumeric Texts) • Input of the measurement duration in seconds. The minimum allowed interval between two measuring points is different for controlled rate and controlled stress, as follows: - shear rate measurement tMP >= 4 s - shear stress measurement tMP >= 1 s Note: The longer the time between two measured values, the higher the accuracy of the physical values determined! • Input of ID (15 character maximum) for the Test Measurement (see Section VI.
This message will be displayed until the first measuring point is reached and displayed. Torque Duration 100.5 ‰ 000.90 1/s Eta: 1.728Pas Tau: 1.572Pa 04s 20.7°C User defined value Measurement results #01 Step (in single meas. always 01) Temperature If the torque is below 10‰ (scale is 0‰ to 1,000‰), the measurement results may not be as accurate as desired. In this case the user defined parameters should be changed so the torque is higher than 10%.
The Run Program function starts one of the available programs defined in the memory. If there is no program available, the following error message is displayed: No valid program Enter program first! In this case, the user has to define a program first (see Section VI.6.2: Utilities → Edit Program). Use the OK key to return to the main menu. If programs are available, a list appears to select from. Select the program to be started (see Section VI.3: Selecting from Lists).
Measurements can be taken with the memory full but the results will only be shown at the LCD and will be lost after completion of the measurement. If you try to send results to a printer and it is not connected or has no paper in it, an error message will be displayed until the printer is connected and operational or until you stop the activity. When you start the measurement, the instrument shows: Program running... Wait for 1.
VI.5.4 MAIN Menu → Remote The “Remote” function initiates measurements to be made under PC control. In this mode, all functions of the R/S-CPS+ Rheometer are controlled by a PC. For PC-controlled measurements, you need the Rheo 3000 Software. This software operates under Microsoft Windows 7™, Windows 2000™, Windows XP™ and Vista™. More detailed information on Rheo 3000 software can be obtained from Brookfield or an authorized dealer.
VI.6 Menu Entries in the Utilities Menu The Utilities menu contains several useful functions. Zero Calibration Initiates the zero calibration procedure of the rheometer Print Programs Prints all parameters of all the programs in memory to the printer Edit Programs Measuring Systems Print Memory Delete Memory Temperature Meas.
VI.6.2 Utilities → Edit Program This function allows the input of new programs and the modification of existing programs. The programs may be run after a successful creation via the menu level “Program Measurement” in the main menu.
The first user defined value ( = the first measuring point) is always the start value of the ramp. The last measuring point is determined as the end value of the user defined value range. As in our example, to reach the values D = 10, 20, 30, ... , 100 [s-1] a starting value of 10 [s-1] is used with increments of 10, therefore, 10 measuring points is required. To check: 100-10/(10-1) = 10.
Available Measurement Types User Defined Range Shear Rate D{s-1] Depends on the measuring system Shear Stress Tau [Pa] Depends on the measuring system Speed n[rpm] Torque M[‰] 0.1 - 1,000 rpm 0 - 999 promille (= 0 to 50 mNm) Select the type of measurement and press the OK key (in our example “D[1/s]”). Now enter the user defined values for each step one after the other. The following inputs have to be made for each step: End Value Input Step #1 Start[1/s]:0010.00 End[1/s]: 0100.
Maximum step duration: 3600 s The instrument will automatically check the input. If there is a range error, “Range error” would be displayed together with the allowable range. The more time between two measuring points, the higher the accuracy of the determined physical parameters! The input procedure for start and end value, number of measurement points and step duration is repeated for the next step. The procedure is repeated until all steps have been entered.
ERROR #1 Printer not ready! cont. stop If this error message appears, ensure the printer is ready and contains paper. Press the OK key to try printing again or press the ST key to return to the menu. VI.6.4 Utilities → Measuring Systems This function provides a method to create new measuring systems or change existing measuring systems.
=storing Name: C50-1/30 tau_prom: 01.1418 k_gamma: 01.2910 Use the OK key to store the new information, otherwise press the ST key to return to the menu without storing. VI.6.5 Utilities → Print Memory This function allows the output of the data stored in the instrument memory to either a printer or to the RS232 serial interface of the rheometer. The instrument will prompt you to select the output device, as follows: Sel.
Before deleting, ensure that the data has been archived to a printer or PC. Before the memory is cleared, the following prompt is displayed: Clear Memory? -NO -YES If “YES” is selected, the results will be cleared from the memory; if “NO” is selected, no deletions are made and the user is returned to the menu. VI.6.7 Utilities →Measure Temperature This function displays the temperature with the temperature sensor connected to the rheometer.
VI.7.1 Configuration → Output Mode This function defines the output device (printer, serial interface) which will receive the results. This setting is independent of the internal memory in the rheometer for data storage. When tests are run, the data is automatically stored in memory in addition to being sent to the configured output device.
Resetting only via function meascount Select meascount mode: -No resetting -Reset every day Automatic resetting at first measurement of the day After choosing one of two reset modes, the user will be returned to the Configuration Menu. VI.7.3 Configuration → MeasCount=0 This function resets the measurement series counter regardless of how the MEASCOUNT is set. VI.7.4 Configuration → Time/Date This function allows the user to set the internal clock and internal calendar.
VI.7.5 Configuration →RS232 Parameters This function allows the preselection of interface parameters. The serial interface operates without handshake. Data is transferred as ASCII text.
When all parameters have been selected, the new parameters are displayed: RS232: 19200,8,n,1 =storing Accept the set parameters by pressing the OK key. The new settings are now stored and will remain in the rheometer memory even after switching off the instrument. VI.7.6 Configuration → Language This function selects the user language of the R/S-CPS+ Rheometer. Available languages are: • German • English Select the desired language and press the OK key.
1. Switch the rheometer and the PC off. 2. Connect the rheometer (RS232 connector port at the back side of the instrument) to a free serial interface (e.g. COM2) of the PC. Use the cable supplied by Brookfield. 3. Switch the PC and the rheometer on. 4. Set the data transfer parameters at the rheometer (see Section VI.7.5). Here: Standard setting 4800 Baud, Parity n, Stopbit 1, Databit 8. 5. Select the RS232 interface as the output device at the rheometer (see Section VI.7.1). 6.
VII. Measuring VII.1 Measuring in Manual Operation You can measure in manual mode by following these brief instructions: Install the R/S-CPS+ Rheometer (see Section III: Instrument Installation). Connect the AC adapter (see Section III.2.2: AC Adapter). Connect the printer, which is optional (see Section III.2.3: Printer Connection). Fill and mount the measuring system (see Section V: Measuring Systems).
VIII.
Value Speed Torque (relative) (1000 ‰ = 50 mNm) Temperature Time Shear rate Symbol n M Physical Unit [min-1] [1} T t [°C] [s] [s-1] γ⋅ Shear stress τ [Pa] Dynamic viscosity h [Pas] Brookfield Engineering Labs., Inc. Page 47 Manual No.
Appendix A A.1 Data Sheets of Standard Measuring Systems Table A-1: Cone/Plate Measuring Systems according to DIN 53018 (consisting of measuring cone and the bottom measuring plate of the instrument) Measuring System RC3-25-1 RC3-25-2 RC3-50-1 RC3-50-2 RC3-75-1 RC3-75-2 Shear rate range [s ] 0-6,000 0-3,000 0-6,000 0-3,000 0-6,000 0-3,000 Shear stress range [Pa] 0-12,223 0-12,223 0-1,528 0-1,528 0-452 0-452 0.25-1,629 0.5-3,259 0.03-203 0.06-407 0.009-60 0.
A.2 Error Messages The R/S-CPS+ Rheometer is user-friendly regarding errors. When errors occur, they are trapped, and the user is informed on the LCD. The most frequent error messages are explained in this chapter. Range Error Cause: User’s error at input. The user has tried to input a value that is less than the allowed minimum value or is more than the allowed maximum value. Example of Faulty Input Allowed of a Preset minimum value Value: Range error End value: Min: 0.90 Max: 1032.
Zero Calibration Error Cause: An impermissibly high value was measured during the zero point calibration of the rheometer. Example Message Error #3 Zero cal. error! Please retry cal. cont.
Abort: Speed Max Cause: Example Message The maximum speed has been exceeded during a measurement. Possible reasons: a] the selected shear stress or torque value for this measurement is too high b] a torque or shear stress measurement has been started without sample in the measuring cup ABORT:speed max! Single measurement total time: 60 s total no. of MP: 10 What to Do: a] press the OK key b] select smaller shear stress or torque for this measurement A.
A.4 Requirements to the AC Power Connecting Cables The AC adapter unit of the R/S-CPS+ Rheometer permits operation of the rheometer with supply voltages ranging from 100 to 240 VAC with frequencies from 50 to 60 Hz. The main connecting cable supplied with the R/S-CPS+ Rheometer may not, in some cases, meet the requirements of every country. It is absolutely necessary that you use a main connecting cable that meets the specific requirements and regulations of the relevant country.
Other countries • The connectors of the mains connecting cable must be approved and certified by the responsible authorities in the respective countries. These authorities are: Australia — EANSW Great Britain — BSI Belgium — CEBEC Netherlands — KEMA Austria — OVE Denmark — DEMKO Finland — SETI France — UTE Germany — VDE Italy — IMQ Norway — NEMKO Sweden — SEMKO Switzerland — SEV -- The cable must be three-phase HAR-cable, type HO5VV-F3, with a minimal phase cross-section of 1.0 mm2.
Appendix B Calibration Check Procedure B.
1. Turn on the R/S-CPS+ Rheometer. 2. Turn on the temperature controller. Set the controller to 25°C. 3. Allow the R/S-CPS+ Rheometer to be on for a minimum of 10 minutes prior to taking measurerment data or running a zero calibration. • Zero Calibration does not have to be executed prior to every test, but should be run no less than once a week. • Zero Calibration takes approximately eight (8) minutes. • Best Practice: run the R/S-CPS+ Rheometer at 100 rpm for 30 minutes just prior to zero calibration. 4.
11. Manually turn the outside ring of the dial indicator so that the needle is on zero. Note: Each division on the dial indicator corresponds to 0.01 mm (or 10mm). 12. Move the rheometer head up and down to confirm that the dial indicator needle remains at zero when the rheometer head is in the down (measuring) position. 13.
B.5 Calibration Check Procedure The R/S-CPS+ calibration check can be performed with or without software. If software is not being used, proceed to B.5.1 Calibration Check in Stand-alone Mode. If software is being used, proceed to B.5.2 Calibration Check with Rheo3000 Software. B.5.1 Calibration Check in Stand-alone Mode 1. Input Measuring System’s Constants a. On the rheometer head, select “Measuring System” within the Utilities menu. b. Select the appropriate measuring system. c.
Step Nr 1 Start [‰] : End [‰] : Nr. Of Mp: time [s] : 250 250 40 60 Step Nr 2 Start [‰] : End [‰] : Nr. Of Mp: time [s] : 500 500 40 60 Step Nr 3 Start [‰] : End [‰] : Nr. Of Mp: time [s] : 750 750 40 60 6. Enter the following information in the general block data: a. Viscosity Standard Name (e.g. B11000) b. Lot Number c. Expiration Date e. Viscosity Value f. Spindle Serial Number 7. Upon test completion, click the Analysis button.
Other Faults Indication Possible Cause Solution Dial indicator reading is inconsistent. Set pin has lost hold power. Pin may need to be replaced. Call for service. Viscosity reading is low. Viscosity reading is low and spindles does not mvoe freely when hex nut is disengaged. Viscosity reading is low. Micrometer ring was not lined up with zero on shaft. Head is too high. Contamination has entered the gap between the spindle cone piece and spindle shaft.
B.5.5 Cone Spindle Data Example Brookfield Engineering Labs., Inc. Page 60 Manual No.
Appendix C: Online Help and Other Resources www.brookfieldengineering.com The Brookfield website is a good resource for additional information and self-help whenever you need it. Our website offers a selection of “how-to” videos, application notes, conversion tables, instruction manuals, material safety data sheets, calibration templates and other technical resources. http://www.youtube.com/user/BrookfieldEng Brookfield has its own YouTube channel.
Appendix D: Warranty and Repair Service Brookfield Viscometers 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 (NIST). The Viscometer must be returned to Brookfield Engineering Laboratories, Inc. or the Brookfield dealer from whom it was purchased for no charge warranty service. Transportation is at the purchaser’s expense.