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Ring method measurements

page 61

Display

Action

Explanation

Relaxing

automatic

The liquid is moved downwards
again until the maximum force is
reduced by the percentage 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)
Temperature (°C)

automatic

The measurement is complete.
The data found are used to
display the mean value of the
interfacial tension, the standard
deviation and the temperature.

Содержание K11 MK3

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

Страница 2: ......

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 8: ......

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 115: ......

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