kruss K11 MK3, User Manual

Page 1: ...Tensiometer K11 MK3 User Manual V3 05 KR SS GmbH Hamburg 2000 2010...

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Page 3: ...15 3 5 Assembling a thermostat jacket optional 16 3 5 1 Assembling an external temperature measuring probe optional 18 3 5 2 Inert gas connector optional 18 3 5 3 Installation of the protocol printer...

Page 4: ...Cleaning the ring and plate 33 5 3 Cleaning the measuring probe for determining the density 34 6 Preparing a measurement 35 6 1 Safety information 35 6 1 1 Working with highly flammable liquids 35 6 1...

Page 5: ...rsion depth 53 8 2 4 Immersion speed mm min 53 8 3 Measuring surface tension by the ring method 54 8 4 Measuring interfacial tension by the ring method 56 8 4 1 Interfacial tension pull 56 8 4 2 Inter...

Page 6: ...1 Tare 0 76 11 2 Key beep on off 2 76 11 3 LabDesk output Standard output 3 77 11 4 Print setup 4 77 11 5 Protection 5 77 12 Data transfer to external media optional 78 12 1 Printing out on a protoco...

Page 7: ...according to Wilhelmy 101 15 1 3 Ring and plate methods in comparison 102 15 2 Density measurement 103 Appendix 104 I Ranges of validity for the ring correction methods 104 II Settings for compatibili...

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Page 9: ...ion proof areas The controls of the K11 and a connected computer must not be operated when wearing protective gloves which have already been used for handling hazardous materials Do not use the K11 if...

Page 10: ...ed for thermostatting Applicable liquids are water above 0 C and below 100 C ethylene glycol vegetable oils or silicon oils KR SS does not provide for damages due to working outside the temperature ra...

Page 11: ...es Clean the unit or accessories before dispatch This applies particularly if there is contamination due to hazardous substances Use the original packaging to pack the instrument or accessories If you...

Page 12: ...port If problems should occur when working with the K11 or with LabDesk please consult the technical customer support at KR S GmbH You can contact them at KR S GmbH Technical support Tel 49 040 514401...

Page 13: ...thout consulting this manual This manual is subject to a permanent quality control The current version of the manual can always be acquired from the download section of our homepage www kruss de Possi...

Page 14: ...n and ambient conditions For operational safety and accuracy of results the K11 must be installed at an adequate location When working with liquids which are volatile toxic irritant hazardous to healt...

Page 15: ...waves near the instrument e g cell phones W LAN devices These can affect the force sensor electronics and lead to measurement errors 3 3 Levelling the instrument Level the K11 with the help of the two...

Page 16: ...cable to the LINE connector on the back of the K11 Connect the mains plug supplied to a mains outlet 100 240 V AC 3 4 2 Connecting the K11 Control Panel Control Panel Control keypad for control of th...

Page 17: ...SERIAL PC interface connector on the back of the K11 to a corresponding interface on the computer 3 4 4 Connecting an external thermostat optional Connect the thermostat outlet to the Quick Lock THERM...

Page 18: ...stat jacket before fitting the vessel p 18 2 Remove the screw fitted to the shaft of the thermostat jacket 2 5 mm hexagon socket wrench 3 Plug the multi pin plug on the bottom of the thermostat jacket...

Page 19: ...up page 17 4 Slide the rubber sleeve over the shaft as far as the lower edge of the vessel 5 Connect the two Quick Lock closures of the hoses coming from the thermostat jacket to the two sockets in t...

Page 20: ...e temperature sensor connector in the measuring chamber Connect the sensor plug to the sensor connector To read out the temperature of the external sensor when taking measurements Select the option ex...

Page 21: ...page 19 3 5 3 Installation of the protocol printer optional Connect the SERIAL PC interface connector on the back of the K11 to the protocol printer Connect the printer to the mains supply using the...

Page 22: ...ocedure and controlling the motor are carried out using the control panel alone 4 1 Switching the instrument on and off 4 1 1 Mains switch To connect and disconnect the K11 from the mains Use the POWE...

Page 23: ...temperature before measurements can be started This requires a warming up time of at least 2 hours In the standby mode the balance retains its operating temperature this means that no warming up time...

Page 24: ...ways shown at the top right hand side The letter I or E below the character indicates whether the temperature shown has been measured by the sensor inside the thermostat vessel I or by the external se...

Page 25: ...is a vessel filled with a hazardous substance this in turn can lead to a risk due to the hazardous substance X Keep your hands away from the area of movement while the platform is in motion Make sure...

Page 26: ...Move to the required upper position of the sample platform using the rotary knob 2 Press the key for about 2 seconds 3 Move to the required lower position of the sample platform using the rotary knob...

Page 27: ...Functions Instrument switch on only if in standby mode Instrument switch off if pressed for a longer time Ends the current entry jumps back to the particular main menu point if pressed down briefly M...

Page 28: ...in function changing the parameters in the current menu Secondary functions no 0 when entering parameters special characters when entering text Decimal point when entering parameters In the main menu...

Page 29: ...nus plate method ring method or density you can start a measurement with the ENT key enter After the start instructions for the particular steps to be taken during the measurement appear on the displa...

Page 30: ...values applicable to the particular parameter is shown Numbers are entered by pressing the keys 0 9 For the decimal point the key is used Parameter changes are confirmed with the Enter key The displa...

Page 31: ...tical arrow keys Parameters are entered in exactly the same way as for measuring methods see previous section Entering the letters given on the keys below the numbers is carried out in the same way as...

Page 32: ...f with the key The stirrer bar continually changes its direction of rotation at regular intervals Stirrer speed and interval duration of rotation in one direction are entered in the setup menu The sti...

Page 33: ...nd Only grip the shaft of the measuring probe Check from time to time if the measuring probes are in proper shape Read the instructions on pages 90 f Grip the shaft of the measuring probe and slide it...

Page 34: ...n surfactants soap rinsing agents or any alkaline cleaning agents Use only pure solvent and clean lint free cloths 5 1 1 Step 1 Cleaning with water Rinse out the sample vessel under hot flowing water...

Page 35: ...measures Clean the glass with a concentrated oxidising acid This work must only be carried out by persons who are familiar with the dangers involved when handling acids and who are familiar with the...

Page 36: ...e of a flame that is too small or too cool may damage the measuring probe as can excessive heating X Only use a gas burner Spirit burners or lighters are not suitable X When heating make sure that the...

Page 37: ...ent X Let the heated measuring body cool down before attaching it to the probe holder 6 1 2 Measurements at high temperatures Risk of burns and scalding by hot components and liquids At higher tempera...

Page 38: ...w its upper rim A larger volume is more easily able to compensate any interference If you have to use your sample liquid sparingly the filling level must be at least double the given immersion depth s...

Page 39: ...nnot be started In the run of the measurement user interactions are required for example exchanging the phases for an interfacial tension measurement The necessary interactions are indicated on the di...

Page 40: ...ll Make sure that the parameters in the main menu and setup are suitable for the measurement The probe plate ring or density probe must been cleaned and attached to the probe holder The probe and the...

Page 41: ...nt settings for measurements with the plate method in the four lines in the centre If you want to retain the settings then you can start the measurement with the ENT key for the measurement itself ch...

Page 42: ...ating the standard deviation is set When a measurement is finished because the deviation conditions were matched the average value is calculated not from all values but from the values that were most...

Page 43: ...ich affect the course of the measurement with the plate method Assumingly they rarely need to be altered Only those parameters which are relevant for the plate method are described here the complete S...

Page 44: ...ase it by much as otherwise the detected surface height becomes less accurate 7 2 3 Immersion depth mm This is the distance by which the sample stage is moved upwards after detection of the surface in...

Page 45: ...Maximum 22 characters Only if defined in Setup In succession Field 1 Field 2 Field 3 Enter the required contents in the text fields The text fields whose number is defined in Setup are called up in s...

Page 46: ...found are used to display the mean value of the surface tension the standard deviation and the temperature 7 4 Measuring interfacial tension by the plate method Check whether all the requirements con...

Page 47: ...to the corresponding data of the current measurement User please enter a name Use the keypad to enter an operator name Maximum 22 characters Insert the light phase and immerse the probe completely Ins...

Page 48: ...verlay the heavy phase with the light phase best done by running it down the vessel side from a pipette Measuring Displays the individual measured values automatic Returns to the found surface height...

Page 49: ...surface tension and 8 4 interfacial tension To make alterations to the settings press the key ESC exits the Modify mode The alterations are stored and retained 8 1 1 Measuring mode Here you can choose...

Page 50: ...rection are available for the K11 None 0 If measurement values are to be compared with data from other tensiometers for which no correction was used the option None can be selected For any other case...

Page 51: ...easured values are multiplied by a factor obtained from the quotients of the actual surface tension of pure water 72 8 mN m and the uncorrected measured value for water The linear correction was suffi...

Page 52: ...d the average value is calculated not from all values but from the values that were most recently used for calculating the standard deviation 8 1 4 Heavy density For surface tension measurements the d...

Page 53: ...measurement to be increased unnecessarily Ring tear off mode With the ring tear off method not the maximum force is measured but the height of the ring above the surface at which the lamella breaks T...

Page 54: ...s where the speed at which the sample stage moves up or down to determine the maximum force is defined The default value of 3mm min mainly needs to be reduced for interfacial tension measurements and...

Page 55: ...t value of 3 mm has proven itself in practice In the IFT push measuring mode the immersion depth is irrelevant In this mode the ring is not immersed as it is already surrounded by the lighter phase 8...

Page 56: ...22 characters Only if defined in Setup In succession Field 1 Field 2 Field 3 Enter the required contents in the text fields The text fields whose number is defined in Setup are called up in succession...

Page 57: ...oved back upwards the value of the maximum force is now determined exactly Relaxing automatic The liquid is moved upwards again until the maximum force is reduced by the percentage value given under R...

Page 58: ...table shows the course of the measurement Ring method Interfacial tension pull Display Action Explanation Sample enter a name for the liquid system Insert the sample and use the keypad to enter a syst...

Page 59: ...sert the heavy phase and position the probe above the surface Carry out activities according to display At the end move the surface up until it is just below the probe Searching automatic Searches for...

Page 60: ...aximum force is now determined exactly Relaxing automatic The liquid is moved upwards again until the maximum force is reduced by the percentage value given under Relaxation The steps Measuring and Re...

Page 61: ...a name for the liquid system Insert the sample and use the keypad to enter a sample name Maximum 22 characters Only if defined in Setup In succession Field 1 Field 2 Field 3 Enter the required content...

Page 62: ...completely immersed in the light phase The heavy phase must not come into contact with the ring Taring automatic Taring the ring in the light phase Searching automatic Searches for the surface the li...

Page 63: ...e value given under Relaxation The steps Measuring and Relaxing are repeated until all the measurement has been completed Finished Displays the final results Average mN m Standard deviation mN m Tempe...

Page 64: ...ey The relevant parameters for the ring method are the parameters Immersion speed and Detection speed on the first page of the setup menu 9 1 1 Detection speed mm min The contact between the plate and...

Page 65: ...the holder 9 2 Measuring the density Check whether all the requirements contained in the check list ch 6 5 have been met Before starting the measurement the empty holder for the density probe must be...

Page 66: ...n the text fields The text fields whose number is defined in Setup are called up in succession max 3 and are used to describe the measurement The text fields can be named in LabDesk and these fields a...

Page 67: ...device and the liquid surface is registered Immersing automatic The sample vessel is moved further upwards at the entered search speed until the holding device is completely immersed The entered imme...

Page 68: ...ntering the density of a different probe The density value for the probe used for determining the density only needs to be altered on rare occasions If you use a different probe from the one supplied...

Page 69: ...are occasions however you should still make sure that the currently set parameters are suitable for the intended measurement The setup menu consists of five pages these are described in the following...

Page 70: ...determine the maximum force used in calculating the surface tension is defined here You should not increase the default measuring speed of 3mm min by very much because as the speed increases the deter...

Page 71: ...t any problems as only the approximate height of the surface needs to be known in order for the probe to be immersed deeply enough Values between 0 2 and 100 mm min can be set for the search speed 10...

Page 72: ...rom the start and is therefore not immersed This is why the immersion speed is irrelevant in this measuring mode The immersion depth is also irrelevant for density determinations as the probe always r...

Page 73: ...d There will always be at least so many values recorded as are entered under the main menu item Settings Number of values for SD There will always be at the most so many values recorded as are entered...

Page 74: ...of the rotary controller 10 3 2 Oscillating period The stirrer does not move continuously in one direction but continually changes its direction Under oscillating period you can enter the time for wh...

Page 75: ...he character an I stands for the internal and E for the external sensor If no thermostat jacket but the platform is installed then only the external temperature sensor is available If the selected tem...

Page 76: ...r an individual measurement to these fields The name of your company the time and the date can be entered in succession The time is entered as six numbers without separators the first two positions ar...

Page 77: ...e access to Setup should be informed of it Once you have defined a password it is impossible to open Setup without this password and it is not possible to switch off the password function or alter the...

Page 78: ...rsion number of the operating system and Firmware are shown 11 1 Tare 0 Before each measurement the weight of the inserted probe is tared automatically With the special function Tare 0 you can tare th...

Page 79: ...protocol printer The protocol printer cannot process the CSV format The raw data weight values from the force sensor are only transferred when LabDesk output is switched on 11 4 Print setup 4 When the...

Page 80: ...e printer connection Connect the printer to the mains supply using the power unit supplied Information about inserting and replaced the roll of paper and the ink ribbon can be found in the manufacture...

Page 81: ...n program does not start automatically Start the Setup exe program in the root directory of the CD 3 Choose the language for the installation dialogue Click on Next 4 A Welcome window will appear Clic...

Page 82: ...abDesk version Click on Next 8 Enter a company name optional Click on Next 9 You can include or exclude software components by checking or unchecking the boxes KR SS recommends Install all available c...

Page 83: ...to be carried out via USB port a driver installation step is necessary Two driver components must be installed so that the installation routine of the hardware wizard must be carried out twice 1 Inse...

Page 84: ...If the Driver was not located by the wizard it can be selected with Browse in a further Step The referring folder on the CD is Drivers USBRS232 6 The hardware assistant reports that the installation...

Page 85: ...he Special Functions menu key of the K11 Press the key 3 to switch to LabDesk output Only for serial interface Selecting the COM port 1 Start LabDesk using the LabDesk icon on the Windows desktop or b...

Page 86: ...the measuring data shown in the Data Logger window Copy Copies a section marked in the Data Logger window into the clipboard Insert Inserts data from the clipboard into editable fields see Section 11...

Page 87: ...ow transferred measured values are listed below 3 Data transfer is terminated with the button when the measurement or series of measurements are complete The recorded measuring data cannot be saved wh...

Page 88: ...c Preferences Under Enable Editing you can define whether subsequent editing of the transferred data table is to be allowed If this option is switched on then the table fields can be opened for editin...

Page 89: ...ert the data table automatically when it is opened The target language for the conversion is not given by the language of the program interface but from the language of your Windows version With the F...

Page 90: ...n if necessary 2 Select Tools Specific Preferences from the menu Select the Field names tab 3 Assign the desired names to the fields When defining a measurement on the K11 you can then assign the corr...

Page 91: ...n the View section elements of the LabDesk user interface can be shown or hidden In the Toolbars section the various possible symbol bar positions can be assigned to a display style In the lower Appli...

Page 92: ...f the ring can be assessed as follows Hold the ring by the shaft and rotate it by turning the shaft between your thumb and forefinger The ring should rotate without any recognizable variation in heigh...

Page 93: ...water place it on the sample stage and move it upwards until the plate just does not touch the liquid surface The light gap between the plate and the liquid surface must also be exactly parallel Use...

Page 94: ...the adjustment please check that the instrument is level If necessary adjust the feet until the bubble in the spirit level on the top of the instrument is located in the inner circle 2 Suspend the emp...

Page 95: ...in 2 Enter your Username and Password Click on Login You should have received the user name and password by e mail shortly after delivery of the K11 If you do not have this information please register...

Page 96: ...ng documentation 2 Connect your computer to the K11 ch 3 4 3 and switch on the instrument 3 Open the Windows Explorer and go to the directory in which you have extracted the files from the ZIP archive...

Page 97: ...lease press the reset button at the measuring device Ctrl Break to abort 7 Carry out this procedure The instrument now starts to initialise itself The firmware is then transferred from the PC to the K...

Page 98: ...o the higher construction an extension for PT100 holder must be built in 2 Normally the thermostatted sample vessel holder and gas thermostatting ring are switched in series i e the thermostat liquid...

Page 99: ...of the liquid This effect can be compensated by thermostatting the gas phase separately with a second thermostat In this case no alterations need to be made to the thermostat jacket connections Most t...

Page 100: ...located just above the liquid surface 6 Place the two parts of the glass ring cover on the glass ring The placed cover must not touch the probe or the adapter 7 The cover has a second opening for the...

Page 101: ...rface or interfacial tension with a measuring probe suspended from a force sensor This probe is a ring or a plate consisting of a material with optimum wetting properties material platinum respectivel...

Page 102: ...he distance of the ring from the surface increases In practice the distance is first increased until the area of maximum force has been passed through The sample vessel containing the liquid is then m...

Page 103: ...the correction is performed automatically with the correction method selected in the ring method menu The method according to Harkins Jordan can be used in most cases 15 1 2 The plate method accordin...

Page 104: ...plate method In contrast to the ring method no correction is required for measurement values obtained by the plate method The densities of the liquids don t have to be known as they have to be with th...

Page 105: ...he surface line between a ring and the liquid is more even than that of a plate 15 2 Density measurement The K11 provides an option for determining the density of liquids If you need the density of th...

Page 106: ...heck whether the expected surface or interfacial tension lies within the range of validity for the correction method If the expected value means that several correction methods are possible then you s...

Page 107: ...l acceleration 9 80665 m s2 Immersion depth 2 mm Sensitivity 0 008 g Min standard deviation not relevant because Reading limit 1 Number of values for SD not relevant because Reading limit 1 Measuring...

Page 108: ...me and after the battery has been exchanged Set the current time and date ch 10 4 18 Battery was empty and has been exchanged standard values set Only occurs immediately after the battery has been cha...

Page 109: ...r at upper limit On switch on only information for the operator During measurement no film tearing is recorded or no surface is found The sample carrier moves upwards to the limit Briefly press the ES...

Page 110: ...6 MB minimum 1Ghz single core Windows Vista Dependent on the Vista version The following requirement for LabDesk should be allowed in addition to the working memory recommended by Microsoft minimum 12...

Page 111: ...ed 2 0 10 0 s maximum load of the force sensor 120 g VI Warranty and caveat emptor The warranty terms and deadlines are described in the general terms and conditions of KR SS GmbH There is no warranty...

Page 112: ...e and does not represent any obligation by KR SS GmbH Neither this manual nor any part of it may be reproduced or transmitted for any purpose whatsoever in any form and by any means electronic or mech...

Page 113: ...peed 62 detection speed 42 52 62 69 display 22 E error messages 21 106 F flammable liquids 35 force sensor taring 76 G gravitational acc 69 H Harkins Jordan 48 Huh Mason 48 I illumination 30 immersing...

Page 114: ...nterfacial tension 56 light density 50 main menu 47 measuring mode 47 measuring speed 52 parameters in the setup 52 pull 48 56 push 48 59 reading limit 50 relaxation 50 surface tension 54 ring tear of...

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