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1 THE OSMOMAT 070 VAPOR PRESSURE OSMOMETER

1. 26 User Guide OSMOMAT 070 Version 1 1 Please ensure that the windows of the vapor wicks are aligned with the cell window 3 1 2 Preparing the cell head A standard Osmomat 070 vapor pressure osmometer is delivered with built in Type 100 measuring probes see 1 2 5 Exact height adjustment of the probe is required to prepare the cell head To test this insert a syringe with spring in the syringe positions 0 0 1 2 3 4 sequentially see 1 2 4 If the syringe is pushed right down the end of the needle should be about 1 mm above the probe coil see 1 2 5 It may be necessary to correct the height of the probe slightly You can correct the height by loosening the Allen screws in the probe screws Once you have adjusted the height carefully tighten the Allen screws again using as little force as possible At the same time check whether the needle ends close to the probe tube so that the solutions can reach the top end of the coil Any corrections can be made by carefully aligning the guide tubes by hand 3 1 3 Installing the cell head in the measurement cell Insert the prepared cell head with measuring probes so that the two probes protrude through the holes of the vapor wick and the connection cables are guided to the rear panel from the probes and cell head in the grooves of the black cell ring The bottom end of the head is immersed in the beaker which presses against the inside of the glass wall with the teflon lip seal and thus seals the
2. G9 e Cell temperatures Hanae Set Measured goren Luhta 2 jee BBE ER MEJ 000 Calibration SAMPLE TIME EI Base Line Adjustment Calibration Untitled 02 09 2007 09 32 To AR 100 resp MEEEHI A 1885 Fleasavinsirid inseri Baseline Adjustment Select V KERSE 90 B 1888 N e Calibration Standard an press iai te Natt a 5 continua nr Carica to Hal 200 Select B dos D agori ina Cell p measuamani SampeNoi 230 4 gonsi Sample No 2 B50 Select f Parameters F3 __Parameters 3 Sample No 3 2000 Select f User Interrupt F2 SampleNo 4 Seean SampleNo 5 See F4 Sample No 6 Select Sample No 7 Select Sample No 8 Select MINIE THIS DIALOG WATE ca BUTTON hl Select Next Sample Finish Zoom T 13196 t A tz 98 min Calibration istae A Gy EB Bg o smomat Untitled an Egg 10 31 am 5 3 Measurement of osmolality After the cell constant has been determined and the system calibrated with it the samples can quickly be measured sequentially You should fill four syringes with the sample solutions and insert them in Positions 1 4 Readjust the baseline by rinsing it 2 5 minutes after inserting the syringes then measure the samples again The measured values are displayed
3. Calibration Standard Q k Natl 300 Select T 8 2 D Sample No 1 Eel it 9288 IE ample No 290 Sample No 2 850 Sample No 3 2000 Sample No 4 Parameters F3 User Interrupt F2 er ol I QU Sample No 8 S i Select Next Sample Cancel ol Br Zoom Res 10 10 eel lll 100 gt A tz 13min 16 Base Line Adjustment if stat If aag ll EjjUsmomat Untitled an Gy Exploring My Documents Sir osmo2 Paint Ba 4 16 PM User Guide OSMOMAT 070 Version 1 0 43 44 User Guide OSMOMAT 070 Version 1 1 You can start calibration after the baseline is stable Different calibration standards are available See Appendix Just as with molecular weight determination two drops of the calibration standard can be added to the right probe and a drop of water to the left probe followed by another two drops of the calibration standard to the right probe At the end of the sampling time a reading is generated that is immediately converted into a cell constant The cell constant indicates the number of digits corresponding to 1 mOsmol Because the measurement effects behave proportionally to the osmolal concentration a one point calibration is adequate You should check the calibration several times and correct it if necessary until a reproducible measurement value has appeared Figure 5 4 Calibration with a calibration standard File View Options wo EL amp
4. The grounding connection is absolutely necessary to prevent injury due to electric shock and interference with the functionality of the measurement system 2 1 Starting the OSMOMAT 070 explanation of the software The OSMOMAT program starts automatically after the control unit switches on and displays the following screen visja 2 ve ie Cell temperatures Measured Solvent MHEG soo SAMPLE TIME ME RESP NN A Please ont OSMOMAT alej B c D Figure 2 2 Welcome screen 14 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 15 The different program modes can be selected and started The choice between membrane osmometer 090 and vapor pressure osmometer 070 directs you to the system specific program portions For the vapor pressure osmometer 070 the selection of measurement modes for molecular weight determination and determination of osmolality includes the option of postprocessing data that has already been measured and a Cleaning mode The Start Only button top right launches a system independent mode for viewing old measurements This can be selected via the mouse or the selection highlighted in white can be confirmed by pressing ENTER on the keyboard If you ended the program the Windows user interface is displayed You can restart the OSMOMAT program at any time by clicking on Start Programs Gonotec Osmomat Pap
5. Z 49 Plunger stop 49 50 Glass syringe body eae 51 Metal Luer needle lock 50 52 Springs for raising the syringes into the upper position 9l 52 2 Starting up the measurement system with the control unit SA The equipment has to be set up in a dry shock free and draft free area It has to be kept from direct sunlight as well as external heat sources such as lighting and heating equipment The measurement cell unit is connected to the relevant control unit via the supplied network cable and data cable When using the control unit SA the data cable from the measurement cell is connected to the socket labeled Cell Unit The network cable is used to connect the measurement cell and the control unit A monitor keyboard mouse and possibly a printer are also connected The power cord of the control unit is then connected to a power outlet The line voltage of your power supply system has to comply with the voltage stated on the type plate of the equipment 110 115 or 220 230V Make sure that the equipment grounding is connected to the protective grounding of the power supply The supplied power cord automatically provides grounding contact If the connector of the standard User Guide OSMOMAT 070 Version 1 0 13 14 User Guide OSMOMAT 070 Version 1 1 power cord is replaced by another connector you have to ensure that the grounding cable green yellow is connected to the protective grounding Figure 2 1
6. 070 Version 1 0 47 48 6 APPENDIX User Guide OSMOMAT 070 Version 1 1 6 1 Suitable Solvents for Vapor Pressure Osmometry Solvent 1 3 5 Trimethylbenzene Mesitylene Acetone Acetonitrile Ethanol Ethylacetate Ethylene chloride Ethyl bromide Ethylene bromide Benzene Bromobenzene Bromoform Butanone 2 Methyl ethyl ketone Butyl acetate Chlorobenzene Chloroform Cyclohexane Diethyl ether Dimethyl sulfoxide Dioxane Furane Methanol Methylene bromide Methyl isobutyl ketone Methylene chloride N N dimethyl formamide n heptane n hexane n propanol o dichlorobenzene o xylene Pyridine Carbon disulfide Tert butanol Carbon tetrachloride Toluene Trichloroethylene Water Boiling Point C 164 6 56 2 81 6 78 32 77 1 83 6 38 3 131 6 80 2 156 2 149 5 79 6 126 1 131 7 61 2 80 8 34 6 100 101 32 64 7 96 5 116 9 40 6 155 98 34 68 8 97 2 179 5 143 115 5 46 25 82 55 76 7 110 8 87 100 Recommended Approximate Values for Working Temperature Measurement Effects C Digits 90 130 37 45 37 60 24 30 45 60 24 30 37 60 32 40 25 60 25 60 90 25 60 48 60 60 130 37 90 37 60 45 90 60 90 25 45 56 70 37 60Chl 60 75 25 30 40 50 60 90 8 10 60 25 48 60 45 20 25 37 60 45 60 25 56 70 90 120 36 45 37 60 37 60 45 60 28 35 90 130 56 70 90 60 90 36 45 25 37 60 75 45 60 25 45 48 60 37 90 40 50 37 60 48 60 37 60 8 10 Measu
7. OOSTMO VANITY eR dc C E CC 21 2 3 1 MMS eree nesgo e tees rede ete esee tet re tet eo etis toes sene A e een ce mes dd hardware Rea neo ts 21 2 3 2 Parameter Dialog f i eE n e ore aet eet vmm eed 22 2 3 3 Measurement and calibration iiss enairar areenan i AEE ASOR e SEEEN E O ETETEN 22 2 3 4 Evaluation Dialog nhe gei aane pe nep pv iode ee 23 pr MENT nm 24 2 5 Evaluating external data 4 eeeeee eee eee eese eese eese ense tn setate stas tas etas tens tens etas tae ta setas tasto senes ease tassa senate 24 PEE OLI 25 MEEMUrn 25 3 PERFORMING THE MEASUREMENT nneeeeeeeeeeeneennn nnne 25 3 1 Preparing the measurement system for measurement ceres ee ee eese eese en seen sense tense tn seas ts sense tas ena 25 3 1 1 Installing the Vapor WICKS ni onte idence Hte rit e et Rp eee eei SEATA VEEE VANESS TEA R EEEE 25 3 1 2 Preparing the cell head aea tee dte a ie d Ee CER ee cese CR d eee peius 26 3 1 3 Installing the cell head in the measurement cell eese 26 3 1 4 Solvents and substances oed ier IR Dd estesa ee e n ga a EE e dte s E E Ad ead eet 27 3 1 5 Making calibration solutions ener nennen rennen trennen eterne tnrennn ines 27 3 1 6 Making solutions for the sample measurement eese eene een eene 28 4 MOLECU
8. Version 1 0 35 Figure 4 6 Calibration measuring solutions Example 2 solution 11 53 E 3 Mole kg NEXT SOLUTION The first reading is taken after the sampling time has run its course After another dropwise addition and when the sampling time has run its course a second reading is saved Repeat the rinsing process until a reproducible measurement has appeared This normally takes three or four rinsings Up to eight but at least three solutions are thus measured in a graduated concentration Only rinse the baseline again after rinsing the final solution Figure 4 7 Example Finished calibration fe a bed Med pe User Guide OSMOMAT 070 Version 1 0 35 36 User Guide OSMOMAT 070 Version 1 1 4 1 6 Determining the cell constants After you have rinsed the baseline again the calibration is terminated Click Finish to access the Evaluation Dialog The result of a calibration measurement is a cell constant that indicates how large the measurement effect is if a solution was measured with a 1x10 Mol kg concentration At least three solutions with an increasing osmolal concentration must be measured to determine the molecul
9. and finish of the measurement the program calculates the drift from the baseline values and corrects it You can also switch off this drift compensation if you don t want it It is important to perform the measurement under the same conditions temperature probes sampling time solvent as the calibration 36 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 37 Figure 4 8 Example Linear regression a TTENTEE 0 00 cl 0 00 2 00 4 00 6 8 00 10 00 12 00 14 00 16 00 io 00 2 0 41994 37 09 E03 0 98621 37 09 E03 4 2 Solution measurement 4 2 1 Entering parameters You can start a measurement after calibrating the measurement system Click on File then New Measurement and then on 070 Molecular Weight Measurement to access the Parameter Dialog Figure 4 9 Example Entering parameters for measurement Se 2 lem bhd bhd eS L e 4 I p ES heed i User Guide OSMOMAT 070 Version 1 0 37 38 User Guide OSMOMAT 070 Version 1 1 Enter the parameters for measurement in the Parameters screen The values of the last calibration are preallocated If you change a parameter you will see a warning message that the device is not calibrated with these parameters and that it is not advisable to perform a measurement under these conditions If all parameters on the screen correspond to the test set
10. cell space When making the insertion apply some pressure to make the seal fit the inner diameter of the beaker Fix the cell head in place by manually screwing both nuts to the threaded bolt Connect the probe cables to the sockets in the rear panel making sure that the Position A probe is plugged into the A socket and the position B probe is plugged into the B socket The connection cable of the heating head is also plugged into the rear panel in Position HEAD Figure 1 2 Osmomat 070 Rear and the plug secured with the collar To prevent damage do not twist the plug or pull on the cables 26 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 27 3 1 4 Solvents and substances Please note the following points for choosing a suitable solvent The substance must fully dissolve in the chosen solvent The substances must not chemically interact with the solvent and should be chemically and thermally stable The solvent itself must be chemically and thermally stable and should contain no impurities of any kind that have a high intrinsic vapor pressure Try to use solvents that neither have a tendency to form peroxides nor are hygroscopic Use toluene if possible because this solvent is especially suitable 3 1 5 Making calibration solutions The first step in determining molecular weights with the OSMOMAT 070 vapor pressure osmometer is to carry out a calibration measurement with a suitable calibration
11. including the average and additional control elements and buttons The lower left portion of the screen shows the control elements for the graphical resolution You can set the optimal resolution for your work here The graphic can be optimized for subsequent printing so that only the important part is printed only the part visible in the screen is printed User Guide OSMOMAT 070 Version 1 0 21 22 User Guide OSMOMAT 070 Version 1 1 2 3 2 Parameter Dialog You are now in Parameter dialog which contains all parameters needed for the measurement Run the Cleaning mode to clean the solvent residue of previous measurements from the measurement cell and prepare it again See 2 4 If the measurement cell is prepared you can now enter the parameters with which the subsequent measurement is to be performed Osmomat 070 Osmolality Untitled lel xl File View Options 2 melal a m e aly Cell temperatures Tonos Set Measurea S0Nent Ejerne vets EBEN soio SAMPLE TIME ANNE A Solvent distiled Water x Cell Set Temperature Boiling Point 1000 oy Sampling Time 2 00 min Last Cell Const 53 38 RESP Sa Hid Untitled 03 17 1998 15 15 Te a oom 300 70 Thermistor Probe Serial Numbers 123 B 1235 603 60 40 320 F DoCalibration Cancel 205 m Zoom T D m Res 10 10 Zoom 37 t 35 min Res 1 Beginning n
12. is an empirically determined value The empirical value for toluene is 4 minutes for a measurement temperature of 45 C If there are no experiences with other solvents the sampling time should be set to about 10 minutes and the adjustment characteristics observed on the screen After the measurement has started the sampling time proceeds in the form of a countdown If a stable baseline has appeared you can terminate the countdown by pressing the F2 key or clicking the User Interrupt button The adjustment time can be read on the X axis and entered as a new sampling time 4 1 2 Creating the solvent If you are not using a solvent from the list you can create a new solvent by clicking on the top right button with your right mouse button and entering the required parameters in the screen form User Guide OSMOMAT 070 Version 1 0 31 32 User Guide OSMOMAT 070 Version 1 1 Figure 4 2 Example Creating the solvent iw Cay bed Wed 2271 fs 3 4 1 3 Preparing the syringes Fill two syringes with solvent and up to four syringes with the prepared solutions The syringes must be clean and dry and should be filled without air bubbles Insert the two syringes with the solvent in Positions 0 and 0 Figure 1 5 Place the four syringes with solutions in Positions 1 4 starting with the solution that has the lowest concentration 4 1 4 Rinsing the probes Dropwise addition and rinsing of solvents and solutions must b
13. should therefore be calibrated with solutions whose molality or osmolality is known Because the osmotic pressure of polymer solutions does not behave linearly according to the concentration at least three solutions of the substance to be gauged are measured in a graduated concentration A subsequent statistical calculation of the measurement results by means of a linear regression calculation eliminates nonlinear behavior 1 2 Description of the system 1 2 1 The measurement system The measurement system is comprised of the OSMOMAT 070 cell unit and a control unit The cell unit contains the measuring probes suspended in the measurement cell including bridge amplifiers and all electronic components for thermostatic regulation while the control unit is responsible for power supply control and measured value display and evaluation The control unit SA has a monitor and a keyboard uses software to guide the user through the measurement displays the data graphically calculates the molecular weight and can print the measurement result with linear regression and the graphic via a connected printer not included in the delivery There is a Help file for the control unit SA 4 User Manual OSMOMAT 070 Version 1 2 User Manual OSMOMAT 070 Version 1 2 5 1 2 2 The cell unit On the front of the OSMOMAT 070 Figure 1 1 there are two LEDs on the left hand side Power 1 for displaying the supply voltage und Ready 2 for displaying the c
14. solution that has a known molecular weight You will need 4 solutions of the calibrating substance in a concentration range of 1 mMol kg to 30 mMol kg for this A standard concentration series for these solutions is 2 mMol kg 4 mMol kg 8 mMol kg und 12 mMol kg Pour the solutions into small glass containers that are easy to close and have a volume of about 25 ml Use an analytical scale to record the precise net weight The sole aim of this is to accurately record the respective net weights of the substance and solvent and not to check exact compliance with the molal concentration specified above The result of a calibration measurement is the cell constant The cell constant indicates the measuring sensitivity of the entire measurement system under the selected measuring conditions This cell constant has the dimension Digit 10E3 per mol of the substance dissolved in 1 kg of solvent Benzyl with a molecular weight of 210 23 g mol has proved a suitable substance for calibration measurement of all standard solvents The benzyl made by Merck Darmstadt is recommended for synthesis with a concentration greater than 99 Calculation of each net weight The molecular weight of benzyl is 210 23 g mol For a solvent net weight of 1 mMol kg the molecular weight will thus be 210 23 mg of benzyl solvent kg User Guide OSMOMAT 070 Version 1 0 27 28 User Guide OSMOMAT 070 Version 1 1 Take 20 25 g of solvent when using glass c
15. suitable solvent and must not dissociate or influence chemical interactions with the solvent Measurements can be performed in a temperature range of 30 130 C A molecular weight of 50 50 000 Daltons can be recorded in organic solvents and up to about 5000 g mol in water At least three solutions of each substance to be gauged must be measured in a graduated concentration Calibration is carried out with solutions of a known molality or osmolality The OSMOMAT 070 is also suitable for determining the total osmolality of aqueous solutions 1 1 The measurement method Two thermistors connected as measuring probes in a differential measuring circuit are suspended in a thermostatically controlled measurement cell The measuring probes which are initially coated with solvent drops conform to the cell temperature so that there is no difference in their temperatures After one of the two solvent drops has been replaced by a drop of solution the solvent vapor condensates as a result of the lower solvent vapor pressure over the solution drop The resulting heat of condensation leads to a measurable temperature increase on the drop of solution The temperature difference produced between both temperature sensors which are part of a Wheatstone bridge with a resolution of 5 x 10E 5 C is converted into a DC voltage signal The measured value is proportional to the solution s osmolal concentration but may be affected by heat losses The measurement system
16. 0 Zoom 31 Res 10 10 100 sp t 13 min phe 1 Beginning new measurement iste A 3j Eg Elf osmomat Untitied an Egg s164M After you have switched on the control unit and selected Molecular weight measurement on the Start screen Chapter 2 2 Page3 you will be taken to the part of the program that goes through molecular weight determination with the OSMOMAT 070 Select a solvent from the solvent menu right drop down arrow or create a new solvent 2 2 2 Page 16 by clicking your right mouse button on the right hand button and selecting New solvent You will also need to enter the desired measurement temperature cell set temperature and measuring time sampling time The serial numbers of the probes should also be noted because they are saved in conjunction with the cell constant If you accept the parameter page without making any changes the saved cell constant is used for measurement and you should check the Do Calibration box to perform a calibration If a parameter is changed the Do Calibration box is automatically checked and you can start calibration by clicking the Calibration button 4 1 1 1 Cell temperature Please bear the following points in mind when adjusting the cell temperature The temperature can be adjusted from 15 130 C in one degree stages The lower limit of the cell temperature should be at least 5 C above room temperature The maximum working temperature is 130 C 30 User Guide OSM
17. 0010 70 9 0020 70 9 0030 70 9 0040 30 9 0020 30 9 0290 30 9 0850 30 9 2000 Glass syringes with glass plungers exchangeable complete with Luer cone 6 needles for glass syringes with springs 25 vapor wicks Special cylindrical beaker for cell unit 50 ampoules calibration standard 300 mOsmol kg 10 ampoules reference solution OSMOREF 290 mOsmol kg 10 ampoules calibration standard 850 mOsmol kg 10 ampoules calibration standard 2000 mOsmol kg User Guide OSMOMAT 070 Version 1 0 49 50 6 3 Specifications Molecular weight range Minimum detectable concentration Concentration range of solutions to be measured Specific vapor pressure of the substance to be measured Sample volume Temperature range Solvent quantity Analog output Calibration substance for molecular weight determination Measuring range for osmolality determination User Guide OSMOMAT 070 Version 1 1 50 50 000 Daltons in organic solvents 50 5 000 Daltons in water 3 3 x 10 mol kg in toluene 1 7 x 10 mol kg in water 0 1 1 5 Osmol kg in water 1x10 3x 10 Osmol kg in organic solvents 0 196 of the used solvent Approx 1 ml per solution at least three solutions in graduated concentration 5 C above room temperature up to 130 C in 1 C stages At least 20 40 ml 1 mV digit 10V max Benzyl benzoic acid naphthalene Up to 3000 mOsmol with control unit SA Up to 1500 mOsmol with control unit B Calibration solution fo
18. 16 Measuring probe in position B for sample regulation solution 25 Measuring channel for checking the cell 17 Measuring channel for checking the head temperature externally temperature externally 26 Beaker 18 Vapor wicks 27 Cell space with saturated solvent vapor 19 Heat absorbing filter 28 Cell block with filament winding and 20 Solvent temperature sensor for thermostatic control 21 Window for observing the drop size on the measuring probes User Manual OSMOMAT 070 Version 1 2 7 8 User Guide OSMOMAT 070 Version 1 1 There are two measuring channels in the cell and cell head for external temperature checking 1 2 4 The cell head The cell head has its own thermostat that automatically adjusts itself to the cell temperature It closes the measurement cell upward and ensures that the syringes are preheated Fine adjustment of the temperature to optimize the temperature difference between the cell and cell head can be carried out with a potentiometer on the rear Figure 1 2 6 The temperature of the cell head should be about 0 5 C lower than the cell temperature Temperatures can be checked with an external thermometer in the corresponding measuring channels Figure 1 6 Measurement of the head cell temperature To prevent temperature effects the cell head has a cover that is fastened with a knurled screw Figure 1 4 Osmomat 070 cell head 13 14 15 16 y 4 YY 29 I RD 29 Teflon lip seal for sealing the cell space
19. 30 Guide tube for aligning the syringe needles to the dropwise addition point of the measuring probes 8 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 9 Figure 1 5 Cell head cover top view 38 31 Threaded bolt for screwing on the cell head manual screwing 32 Position A of the reference measuring probe 33 Position B of the measuring probe 34 Syringe position 0 Solvent for reference measuring probe 35 Syringe position 0 Solvent for baseline 36 Syringe position 1 Lowest concentration of the sample 37 Syringe position 2 Next highest concentration of the sample 38 Syringe position 3 Next highest concentration of the sample 39 Syringe position 4 Highest concentration of the sample 40 Knurled screw for fastening the cell cover Figure 1 6 Measurement of the head cell temperature SS i l 42 41 Hole for placing a thermometer to check the head temperature The knurled screw 40 needs to be removed for this 42 Hole for placing a thermometer to check the cell temperature User Guide OSMOMAT 070 Version 1 0 9 1 2 5 Measuring probes User Guide OSMOMAT 070 Version 1 1 Thermistors acting as temperature sensors are located in the measuring probes The probe coils keep drops to a minimum size and ensure that the probe tip is evenly washed when drops are being added The thermistors resistance values are temperature sensitive and should ideally be between 5 k ohms and 70 k ohms for measu
20. 4 eee eee sees sees eres eee eene enean setas tease tasto seas ete sense tastes seas etas eta 47 5 APPENDIX iri naiec nere diede ger perio France Teva E rare eT Er eee FR CEU UTK VE YESEE 48 6 1 Suitable Solvents for Vapor Pressure Osmometry eere sees e eese eee enses etta etna etas etas etas etas esses etas toao 48 6 2 List of Spare Parts and Expendables creer esee seen sete e eene een etna tensa stats sense ta setas esses seas eas etas enae 49 EMEN TOTIS 50 2 User Manual OSMOMAT 070 Version 1 2 User Manual OSMOMAT 070 Version 1 2 3 It should be mentioned again that the control unit is a personal computer that is equipped with additional hardware by Gonotec not limited to the installation of a special interface card The OSMOMAT program designed specifically for this purpose ensures smooth and reliable functioning of the measurement system provided that no other programs are started As a result Gonotec cannot ensure smooth functioning of the measurement system if additional hardware or software is installed User Manual OSMOMAT 070 Version 1 2 3 4 User Manual OSMOMAT 070 Version 1 2 1 The OSMOMAT 070 Vapor Pressure Osmometer The OSMOMAT 070 is suitable for determining the average molecular weight Mn of polymers in aqueous or organic solvents The materials used should be within a concentration range of 1x10 E 3 to 50x10 E 3 mol kg The substances to be measured must be fully soluble in a
21. 85 mMol kg For the solutions to be accurate both the substances and solvents have to be weighed out Never make solutions with dilution series or volumetric measurement of the solvent 3 1 6 Making solutions for the sample measurement Solutions for determining molecular weight are made in the same way as calibration solutions As much as possible you should use the same molal concentrations as you did for calibration A standard concentration series for these solutions is 2 mMol kg 4 mMol kg 8 mMol kg und 12 mMol kg 28 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 29 If an approximate magnitude of the molecular weight is already known you can make solutions according to the concentrations shown in the table Table for calculating net weights for corresponding molecular weight ranges Molecular weight 2mMol kg 4mMol kg 8mMol kg 12 mMol kg g mol g kg g kg g kg g kg 210 23 0 42 0 8405 1 6815 2 5225 1 000 2 4 8 12 10 000 20 40 80 120 20 000 40 80 160 240 50 000 100 200 400 600 If no information is available for the substance to be measured you should firstly perform a measurement with a solution of any concentration in order to determine the magnitude of the molecular weight 4 Molecular weight determination with the control unit SA After the measurement system has been installed as described in Chapter 2 Page 13 and the cell prepared fo
22. Cell Set Temperature EH Boiling Point 100 0 C z 8 803 ay iT Sampling Time 3 00 min Last Cell Const 0 00 273 0 7 70 Parameters F3 Thermistor Probe Serial Numbers A 3507001 B 38 070102 a fi 40 30 IV Do Calibration Cancel Measurern Analysis al al vl OSMOLALITY PARAMETER 20 10 10 t 209 min Beginning new measurement istae A A E Eff smomat Untitled an Gy Exploring My Documents EBA 4 08 PM In the Start screen you will be prompted to enter the measurement temperature sampling time and probe serial numbers A measurement temperature of 37 C is recommended for measuring the osmolality of aqueous solutions The sampling time is determined in the same manner as described in Chapter 4 1 1 2 You can enter comments If a calibration has already been carried out previously the cell constant is entered and it is not absolutely essential to perform another calibration You can start the measurement immediately However it is advisable to check the calibration occasionally The cell constant is the result of the calibration and indicate the number of digits that correspond to a mOsmol After you have entered the parameters quit the screen dialog by clicking Next 42 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 43 Figure 5 2 Entering the used calibration standard Ceci Lii
23. File View Option fo Ca bed Wel wi gt Cell temperatures Toho Set Measured Solvent La relie Be BEEJ sciution SAMPLETIME ME RESP MEME aet OE Mm E A L Calibration Standard Osmolality ar u Naci 300 mOsmol kg vx c ls Solutions E Sample No 1 290 9 2730 7 Sample No 2 850 70 Parameters F3 Sample No 3 200 Sample No 4 nl Sample No 5 LO A Sample No B I Sample No 7 Sample No 8 p Aa e C el Measurem Analysis MINIMIZE THIS DIALOG WITH THE E BUTTON gt t 209 min rime cu e s M Beginning new measurement istae A A ES Bi smomat Untitled an By Exploring My Documents S osmo Paint EG g osPM Enter the concentration of the calibration standard in the next screen The osmolality indication in mOsmol kg is required to calculate the cell constants and it is absolutely essential that you enter this After you have clicked Start to confirm you will be prompted to rinse the baseline Figure 5 3 Rinsing the baseline Ele View Option a oo tel S wi a r Cell temperatures Set Measured Solvent Distilled Water 37 C BE Solution Base Line Adjustment SAMPLE TIME IO J Base Line Adjustment ant DEE res MERIH 9288 s sgaid insert Baseline Adjustment Select 1 8
24. LAR WEIGHT DETERMINATION WITH THE CONTROL UNIT SA 29 4 4 Calibrating the Osmomat 070 eeeeeeeeee eee eese esses eee eene enean sensns enses estne tasa sens tn sens enata essen senten senatu sen 30 4 1 1 R cording tbe parameters enit requete ed e SH O e ee THUS 30 4 1 2 Creaung the solvent sec eoe HU e aU EREE EPEe IRT dees 31 4 1 3 Preparing the syringes unori e pU UR en etit p epe eio 32 4 1 4 Rinsing the probes eter e eee uere er ue erred 32 4 1 5 Starting calibration ss 2 rei t en eG unda ure t ER 33 User Manual OSMOMAT 070 Version 1 2 1 2 User Manual OSMOMAT 070 Version 1 2 4 1 6 Determining the cell constants dro RR Recte tee me Nod Recte B e ee I HIERO 36 PAMEMUU 37 4 2 1 Entering parameters eite tree RT tr aere ertet e etit d ets 37 4 2 2 Bertorming the measurement au eter ar e reed ce e eges 38 4 2 3 Calculating the molecular weight ee tem ede dete 39 5 DETERMINING THE TOTAL OSMOLALITY OF AQUEOUS SOLUTIONS 41 5 1 Preparing the measurement system ee eeeee eene eene eene enne en setas ttn stata setas etas etos eae sense ense tastes sess ense tas eoa 41 5 2 Calibrating the measurement system for determining osmolality eee eee eere eene eee een ennee 42 5 3 Measurement BO RITE 44 5 4 Evaluating the measurement results
25. OMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 31 The upper limit must be at least 5 C below the boiling temperature of the solvent If the correct boiling temperature for the solvent is entered the software will only allow temperatures up to 5 C below the boiling point The optimal temperature range for vapor pressure osmometry is 37 45 C if the selected solvent allows this Temperature selection depends on the type of solvent and the substance to be measured A higher temperature normally results in higher measurement effects and faster adjustment times But a higher temperature may also result in decomposition of the solvent or substance which leads to longer adjustment times and inaccurate measurement results Temperature control begins immediately after a calibration or measurement has been started The unit begins to heat up and the Heating LED on the front panel of the measurement cell changes color from green to red Figure 1 1 Depending on the temperature chosen it takes about 5 30 minutes for the measurement temperature to be reached and another 10 30 minutes before a stable reading appears 4 1 1 2 Determining the measuring time sampling time The sampling time is the time required to reach the baseline again after a temperature error caused by rinsing The existing reading is saved after the sampling time has expired A bridge balance may also be carried out automatically when the baseline is rinsed The sampling time
26. Start If the temperature of the measurement cell does not match the required temperature parameter a message informs you that the system is waiting for the correct temperature A selection dialog will guide you through the following measurement procedures The measurement starts with a baseline adjustment with an additional zero hardware adjustment during the initial adjustment After rinsing the measuring probes with solvent click Start The selection screen disappears until a measurement value has been applied The measurement value is applied automatically if the Sample Time has expired or if you interrupt the measurement by selecting User Interrupt The selection dialog re appears Click the arrow icon in the lower left corner of the dialog to minimize it for a better view of the measurement graph Click the Continue button to re display the selection dialog Repeat the baseline measurement cycle until the baseline appears to be constant You can now measure your sample solutions one by one While you can perform any number of measurements with a sample solution only the last four measurements per sample solution are recorded and identified in the graphic on the main screen as A B C and D These last four values per sample solution are also used for the subsequent evaluation The sample solutions are selected by clicking the relevant Select button or choosing Select Next Solution The procedure is identical to the baseline adjustment If yo
27. TIME BI Calibration 51 290 S2 860 ant Untitled 02 09 2007 09 32 1005 resp MESSI P H Baseline Adjustment Select 4 al B 848 Calibration Standard c ls l Nati 300 ssa 4 as B e 5 wa Sample No 1 290 Select f a Sample No 2 850 Select B 7 L SampleNo 3 290 Select art Sample No 4 Select Sample No 5 Select H Parameters F3 User Interrupt F2 5 50x SampleNo 6 Seea 4 Sample No 7 Select 40 Sample No 8 Select t 3 1 30 i Select Next Sample Finish 2t il 4 20 Res em Moo j d d H HH T K A 8 A 8 A t 20min 4 Rinse and insert next solution Sal AB EJ Bposmomat untitied an Slosmosi Paint BA 1045 am User Guide OSMOMAT 070 Version 1 0 45 45 46 User Guide OSMOMAT 070 Version 1 1 Figure 5 7 Example Sample measurement 2000 mOsmol 46 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 47 5 4 Evaluating the measurement results A total of 8 samples can be measured and their measurement results saved Clicking Finish takes you to an overview of the 8 last measured samples The measurement values and mean are displayed Save the measurement as a file by clicking Stop and Save Bm BEES ICICI User Guide OSMOMAT
28. User Manual OSMOMAT 070 Version 1 2 1 1 THE OSMOMAT 070 VAPOR PRESSURE OSMOMETER eee 4 11 The measurement method eese eee esee eee eterne senta tn statuant inen s tosta tasto sensns tosta enata sensns ens en ens en sensn sn 4 1 2 Description of RICE EIS t RR eose sosote 4 1 2 1 The measurem ernt System euenire reete en ee ee ee e eade eo EVER e re EH Pee R eia cate e ia eee end 4 1 2 2 The celLl nts e eerte rere HE tror eiii e AES tre e etd 3 1 2 3 Design of the measurement cell essent a r nette enne nennen renes 6 1 2 4 The cell Wedd 5e ee Ret ete reo eher deci eb te eint dea staves a ais nertebhies 8 1 2 5 Measuring probes e e Ere RED Pee Lae y He i eret eie test 10 1 2 6 Vapor WICKS stet darn eet e tee teh a e E ce e ced e ng 12 1 2 7 SVEIDBeS S555 duse e e eletto nee ere tired Tee Desire nee e ts 13 2 STARTING UP THE MEASUREMENT SYSTEM WITH THE CONTROL UNIT SA13 2 1 Starting the OSMOMAT 070 explanation of the software 4 eene eee eese eese eese eene enne en setas tna snae 14 2 2 OSMOMAT 070 molecular weight determination eere eee e esee e eene ente nenn tenen sensns tns en sensu 16 2 2 1 Main SCre eine E EE 16 2 2 2 P rameter dialog ud eee Re ha tee fe e ee Neda peter e eee e i ta eed 16 2 2 3 erint EE 18 2 2 4 Me as rement EU 19 2 2 Evaluation Dialog dtes eR ge HH de eed e bles re Pe TL eee eds 20 2 3
29. ar weights of polymer substances Because substances with an increasing concentration more frequently exhibit less than ideal behavior the measurement effect is not proportional to the concentration For this reason the osmolal concentrations of calibration solutions should be in a narrow range and should match the feasible osmolal concentration of the substance to be measured as closely as possible The measurement results are calculated with a special evaluation method to eliminate the nonlinear effect This evaluation method opposes the concentration measuring effect quotient to the particular concentration If the measurement effect behaves in proportion to the concentration a horizontal curve is generated With polymers a curve with a negative or positive increase is displayed The curve is extrapolated up to a concentration of zero and thus eliminates the effect of the concentration The software performs a linear regression The intercept determined from the regression calculation is the cell constant A graph of the calibration and readings is displayed at the end of the calibration measurement The measured values can be seen here and you can click to suppress individual values if you wish These values are not used for calculation Use the Lin Regression button to toggle between the graph and measurement values The cell constant is accepted after the calibration has been saved and is now available for the subsequent measurements At the start
30. ding the average and additional control elements and buttons The lower left portion of the screen shows the control elements for the graphical resolution You can set the optimal resolution for your work here The graphic can be optimized for subsequent printing so that only the important part is printed only the part visible in the screen is printed 2 2 2 Parameter dialog You are now in Parameter dialog which contains all parameters needed for the measurement Run the Cleaning mode to clean the solvent residue of previous measurements from the measurement cell and prepare it again Figure2 4 Parameter Dialog Osmomat 070 Molecular Weight Measurement Untitled 1 181 x File View Options 2 List 1 i e fcr Cell temperatures Set Measured Solvent tapete BE BEES soiton SAMPLETIME AMEN RESP MEN NN i Untitled 03 17 1998 15 05 D A d Solvent 005 ii calibration 03 17 1998 11 49 B New Solvent Dell Set Temperature 35 C Bol Edit Solvent 80 Sampling Time 1 00 min C Delete Solvent T0 Thermistor Probe Serial Numbers 11 50 LII BEGIN MEASUREMENT 30 20 Zoom Res 10 10 gt Zoom 37 t 36 min Res 1 Beginning new measurement x 16 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 17 If the measurement cell is prepared you can now select t
31. e istae A A E If smomat Untitied an BA 920m Begin calibration by clicking Start Rinse the baseline first followed by the individual solutions Don t start rinsing the solutions until the baseline is sufficiently stable Figure 4 5 Example Calibration rinsing the baseline Untitled and Unsaved i LI F pti su E m Cell temperatures Set A Solvent toluol creation 08 14 2006 14 30 Le Le rude EHE LX NETES Solution Base Line Adjustment SAMPLE TIME ITO Base Line Adjustment In Untitled Calibration 08 15 2006 10 16 AR rese MEI III A 156 00 00 L 2 insani insert Baseline Adjustment Select f feme 9 903 B 158 00 00 Solution No 1 4 02E 3Mole kg Select c 162 00 00 kK 8 Solution No 2 747E 3Mole kg Select 80 D 180 00 00 Solution No 3 11 53E 3Mole kg Select 1593 7 zz T Solution No 4 1496E 3Mole kg Select f Parameters F3 d Solution No 5 5 aa 6 605 User Interrupt F2 Solution No 6 s Solution No 7 Tax Solution No 8 i Tao Baseline Correction Select AO Ir _Select Next Solution Cancel Zoom Res 103 10 10096 4 ol t 13 min Base Line Adjustment MStart A A B Bjosmomat Untitled an EBA 10524M 34 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070
32. e performed very conscientiously and within the same timeframe Before every rinsing process press the Light key on the front panel of the device to switch on the interior lighting for about 20 seconds and observe the dropwise addition through the mirror Because measurement effects are measured with a temperature resolution of about 1x10E 5 C any temperature errors should be reduced to a minimum For a reproducible measurement the size of the drop around the end of the probe is extremely important To generate an optimal reproducible drop size and efficiently rinse the measuring probe you should proceed as follows During rinsing press the syringe down securely so that the end of the needle is above the probe coil Carefully press down the plunger and turn it slightly at the same time to apply the liquid to the probe coil Rinse the temperature sensor and moisten it with liquid After two or three drops have dripped off stop the inflow for a moment while a drop is falling The afterflow of the liquid causes a medium sized 32 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 33 drop to remain suspended This drop surrounds the temperature sensor Carefully let go of the syringe and return it to its original position The homogeneity of the drop size is critical for the measurement s reproducibility Figure 4 3 Rinsing the probes Always follow the same procedure when carrying out a complete rinsing process Fir
33. ent solvents the Parameter Dialog will give you a list of solvents and their associated parameters You can make selections from the list according to your requirements Please note however that only calibrated solvents under associated parameters have a valid cell constant and are acceptable to use for a molecular weight determination You can use solvents without calibration by unchecking the Do Calibration option To carry out a measurement you must now manually enter a cell constant that you are aware of Please bear in mind that this cell constant will not have been determined in the usual way and as such the subsequent results of your work should be treated with reservation A corresponding comment appears in both the Comments field and the printout If you only want to change a solvent s parameters you can make your entries directly in the Parameter Dialog Another calibration will be necessary and after you have been asked whether you are sure you wish to proceed a copy of the old solvent with new parameters and a new constant will be generated If you do not want a copy the subsequent measurement will be performed with your altered parameters However the parameters will not be saved with the solvent in this instance you are only temporarily changing the measuring parameters To permanently change a solvent s parameters select Edit Solvent see Figure 2 5 Creating a solvent and change the corresponding parameters in t
34. ew measurement Figure 2 6 Parameter Dialog In any case it is advisable to do a calibration However a calibration is not needed if there is a cell constant Just uncheck the Do Calibration box After clicking Yes at the prompt continue the measurement process by clicking Next 2 3 3 Measurement and calibration Start a new measurement by selecting New Measurement from the File menu followed by 070 Osmolality Measurement After any changes to the parameters the device should be calibrated with these parameters The device will prompt you to do a calibration In the dialog box that now appears you can specify the Calibration Standard but you must enter the Osmolality of your calibration sample The data will be used as additional identification of your measurement on the printout and the Osmolality value will be included in the calculation of the cell constants 22 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 23 You can measure up to eight samples and enter them in this dialog box with clear designations However these entries are optional and are only used for identification on subsequent printouts Once you have entered all data quit the input dialog box by clicking Start If the temperature of the measurement cell does not match the required temperature parameter a message informs you that the system is waiting for the correct temperature A selection dialog will guide you throu
35. gh the following measurement procedures The measurement starts with a baseline adjustment with an additional zero hardware adjustment during the initial adjustment After rinsing the measuring probes with solvent click Start The selection screen disappears until a measurement value has been applied The measurement value is applied automatically if the Sample Time has expired or if you interrupt the measurement by selecting User Interrupt The selection dialog re appears Click the arrow icon in the lower left corner of the dialog to minimize it for a better view of the measurement graph Click the Continue button to re display the selection dialog Repeat the baseline measurement cycle until the baseline appears to be constant Calibration can now be performed in an identical manner to the baseline adjustment Each measured value is displayed in the A B C and D fields while the calculated cell constant is shown in the Cell Const field below If you are satisfied with the consistency of the readings choose your first sample in the selection screen and start the sample measurements You can now measure your sample solutions one by one While you can perform any number of measurements with a sample solution only the last four measurements per sample solution are recorded and identified in the graphic on the main screen as A B C and D These last four values per sample solution are also used for the subsequent evaluation The sample sol
36. he corresponding solvent from the available list or add a new solvent to the list To add a new solvent to the list click the top right button in the Parameter Dialog and select New Solvent from the drop down menu Figure 2 5 Creating a solvent Osmomat 070 Molecular Weight Measurement Untitled 8 x File View Options 2 Bisley e 2 all Cell temperatures ONERE m Set Measured Bet ura BE EEA ee SAMPLE TIME ANNE RESP MENN NEN ATE ra AR 100 U ntitied 03 17 1998 15 05 xj Y Calvani i Hint After your changes the Calibration Check will be set to prevent you from measure without calibration If you still want to measure e manipulated values clear the Calibration Check after your change Solvent Name Creation Time 03171898 1508 Cell Set Temperature 0 C Boling Point 0c Sampling Time 000m Cell Const 0 003 Enter D if unknown Calibrated with Thermistor Probe Serial Number NOT CALIBRATED cme Cancel Calibration 20 20 a oom 300 70 eow sot 40 30 Iv Do Calibration 10 10 Zoom Res gt sed s Zoom 37 Res 1 a gt t 35 min Beginning new measurement ast ul A new dialog box appears in which you need to enter all relevant parameters for the solvent You can use the mouse or TAB key to toggle between the input fields Terminate the entry by clicking OK or
37. he subsequent dialog box Click OK to quit the dialog box The new parameters will then be permanently saved with the solvent Please note that any calibration previously performed may be lost because the parameters no longer correspond to the ones with which the calibration was performed To delete a solvent from the list do the same as you would for creating a solvent but select Delete Solvent instead of New Solvent from the menu A prompt will appear asking whether you are sure that you want to delete this solvent 2 2 0 Calibration After a solvent has been edited the device should be calibrated with these parameters and the solvent 18 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 19 The device will prompt you to perform a calibration As described in 2 2 2 you can also manually enter a cell constant However because this constant was not determined by carrying out a corresponding measurement with this program the following results of your work should be treated with reservation the corresponding text will appear in both the Comments field and the printout The following dialog prompts you to enter the concentration of the sample solutions You can also enter the Calibration Standard and Molecular Weight of your calibration sample for easier identification on measurement printouts After entering a minimum of one or a maximum of eight concentrations you can exit the dialog by selecting
38. hitting the ENTER key The newly added solvent with its associated parameters now appears in the list of solvents in the Parameter Dialog You can enter other parameters related to the measurement cell and add comments about the next measurement or calibration Because the device has not yet been calibrated with this solvent under these parameters you will now be prompted to perform a calibration by clicking the Calibrate button You can see the parameters by clicking the Parameter button in either the Calibration mode or Measurement mode but you cannot edit them in these modes If the calibration has been performed and a cell constant Cell Const determined a message will appear in the Parameter Dialog behind the solvent stating that the device has been calibrated with this solvent You can now switch to the Measurement mode Because calibration is sometimes a lengthy process in the case of a complete measurement the cell constant is permanently saved with the solvent You can use this solvent with its associated parameters with a valid cell constant at any time for molecular weight determinations User Guide OSMOMAT 070 Version 1 0 17 18 User Guide OSMOMAT 070 Version 1 1 It is naturally a good idea to repeat or check the calibration after a longer period of time Click in the Do Calibration checkbox then click on the Calibrate button You can now perform the calibration again If you frequently use and thus generate differ
39. ierkorb CX Dokumente Ed Einstellungen gt Paint Shop Pro E Zubsh BG MS DOS Eingabeaufforderung Figure2 3 Restarting Osmomat It should be mentioned again that the control unit is basically a personal computer that is equipped with additional hardware by Gonotec not limited to the installation of a special interface card The OSMOMAT program designed specifically for this purpose ensures smooth and reliable functioning of the measurement system provided that no other programs are started As a result Gonotec cannot ensure smooth functioning of the measurement system if additional hardware or software is installed User Guide OSMOMAT 070 Version 1 0 15 16 User Guide OSMOMAT 070 Version 1 1 2 2 OSMOMAT 070 molecular weight determination After you have selected Molecular weight measurement on the Start screen you will be taken to the part of the program that goes through molecular weight determination with the OSMOMAT 070 2 2 1 Main screen All dialogs necessary for the measurement are displayed on the main screen Appropriately modified versions guide you through the entire measurement The main screen displays the graphic measurement sequence and additional current information The left side shows the defined and measured cell temperature the running sample time the current measured value provided by the measurement cell the history of the last four measured values for the particular sample solution inclu
40. ker shaped measurement cell is located in a thermostat with a very constant temperature that can be adjusted in one degree stages between 30 C and 130 C The cell thermostat surrounds a cylindrical beaker that contains a small amount of solvent filling level is about 1 cm To achieve 10096 vapor saturation the beaker contains vapor wicks in the form of filter paper strips Two measuring probes with temperature sensors are suspended in the cell space saturated with solvent vapor The bottom ends of the measuring probes are coated with drops of solvent or solution An even drop size is achieved through wire coils attached to the bottom end of the measuring probes They make it easier to rinse the probes because the liquid can drain off spirally and the probes can be thoroughly wetted The solvents or solutions are fed through glass syringes that are placed in the cell head along with the measuring probes 6 User Manual OSMOMAT 070 Version 1 2 User Manual OSMOMAT 070 Version 1 2 Figure 1 3 Osmomat 070 measurement cell E 13 14 a ere A 15 23 16 INN ss 17 Wi I GR N D Zr 7 N 24 NG Dw mE ZA SS AU A AL 7 26 AY BY 18 19 26 20 27 S p a 22 7 l 7 Y a l UY jj A 13 Syringe for dropwise addition of solvent 22 Swivel mirror 14 Syringe for dropwise addition of a solution 23 Cell cover 15 Measuring probe in position A for solvent 24 Cell head with separate thermostatic
41. lect it and then select File Set as Default Printer Select File Close to close the list of printers To install a printer access the list of printers as described above and double click the New Printer icon You are guided through a set of dialogs to select a printer from a list of manufacturers and to set it as Default select Yes when prompted Typically the default settings can be accepted with Next because the printer interface requires no further configuration Print a test page for verification 3 Performing the measurement 3 1 Preparing the measurement system for measurement 3 1 1 Installing the vapor wicks The first step in preparing the measurement system is to remove the cell head To do this remove the cell cover after loosening the knurled screw and unscrewing both nuts from the threaded bolt After you have disconnected the connection cable for the cell head from the socket 5 Figure 1 2 you can remove the head from the cell Please make sure that neither the probes nor the guide tubes for the syringes are bent You can remove the beaker and insert vapor wicks in it as described in Chapter Vapor wicks 1 2 6 Next pour about 20 40 ml of solvent over the vapor wicks and place the beaker in the measurement cell It is critical that the solvent used in the measurement cell and solvent syringes comes from the same stock bottle as the solvent that was used for adding each of the solutions User Guide OSMOMAT 070 Version 1 0 25
42. n Dialog The evaluation dialog shows the measurement values including the respective concentrations of the sample solutions You can click the individual measurement values to activate and include them in the evaluation Activated values are displayed in bold letters while deactivated values excluded from the evaluation are displayed in plain letters First the values are used to establish the R C quotient for each sample solution A linear regression is applied to these values The generated value is displayed and is factored into the molecular weight calculation or calculation of the cell constants when a calibration is being performed Any drift can moreover be removed from the measurement values with the Drift Correction option The drift is regarded here as constant over time and accordingly removed from the measurement values The linear regression can be graphed by clicking the Lin Regression button If you are not satisfied with the results of a sample solution you can return to the measurement by clicking the Back to Measurement button You can now repeat the measurement of the respective sample solution You must note however that all sample solutions following this sample solution and the baseline drifts have to be re measured For example if you repeat the measurement of sample 20 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 21 solution 4 you have to re measure the following sample solutions if a
43. ng a cell constant Individual measurement values can be activated or deactivated similarly to evaluating a real measurement see 2 2 5 However the entry field is divided by a horizontal line Click the area above the line to enter a new value and use the area below the line to activate or deactivate the value The results can be printed and saved to a file 24 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 25 2 6 Printing To print from the main screen select Print from the File menu or click the printer icon in the toolbar When printing from the main screen only the contents of the graphic window and some additional information is printed The evaluation can be printed using the Print Analysis button in the evaluation dialog This prints all the parameters concentrations evaluation results as well as the linear regression A print menu lets you select a printer The printer set up under Windows 95 is selected by default 2 7 Printer installation This software can print to all Windows XP printers If your connected printer is not listed in the list of available printers you have to install it Set it as the default printer to avoid having to select the printer from the print menu each time you print Exit the OSMOMAT program before installing or setting a printer as default To set a printer as default select Start Settings Printers to display the list of installed printers Click the printer to se
44. on the screen Examples are shown in the following illustrations Figure 5 5 to Figure 5 7 44 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 Figure 5 5 Example Sample measurement 290 mOsmol Untitled and Unsaved Option n temperatures TORG Solvent Distilled Water E jeie Bae BEE BEEJ solution 290 SAMPLE TIME Base Line Adjustment Calibration 1 290 ant CEE 1003 res MEZEA A zm L d ineen Baseline Adjustment Select f B 9 90 B 283 Calibration Standard e ls Natl 300 Soret v a m i D ES Sample No 1 290 Select B I LH e Sample No 2 t Parameters F3 ___Parameters F3 s Sample No 3 a Select wu User Interrupt F2 Sample No 4 Select n zl Sample No 5 Select 50 Sample No 6 Select 4 Sample No 7 Select ELI Sample No 8 Select 3 i 908 i Select Nest Sample Finish 20 Zoom Res 10 Sree lll 62 A t 20 min 16 Rinse and insert next solution 1 PAstart A Bj E Ei smomat Untitled an Sf osmos Paint Egg 10384M Figure 5 6 Example Sample measurement 850 mOsmol Untitled and Unsaved Optior mas temperatures Measured Solvent Distilled Water Betws Be BEZ ETS souio 850 SAMPLE
45. ontainers with a volume of about 25 ml Example for making calibration solutions Using 20 g of solvent results in a net weight of 4 2046 mg or 0 00420 g for a concentration of 1 mMol kg The following net weights should be produced as a result 2 mMol kg 0 00840 g 20 g of solvent 4 mMol kg 0 01681 g 20 g of solvent 8 mMol kg 0 03363 g 20 g of solvent 12mMol kg 0 05045 g 20 g of solvent When making these solutions try not to use less than 25 ml of solution because the net weights will otherwise be too low and the measurement may not be accurate The glass containers and especially the covers must be suitable for this application The covers must close tightly and the sealing material PTFE must not dissolve in the solvent being used Record the net weight as follows Place the glass jar with cover screw cap lid with PTFE foil seal on the weighing pan and tare the scale to zero Next weigh out the required quantity of benzyl Make a note of the exact net weight After resetting the scale to zero pipette the required quantity of solvent into the glass jar Then put the lid on the jar Weigh the solvent amount and note its weight The following calculation is generated for this solution Net weight of benzyl 0 0084 g Net weight of Toluol 21 6750 g 25 ml specific weight 0 867 g ml Weight concentration 0 0084 g 21 6750 g x 1000 0 388 g kg Molal concentration 0 388 210 23 0 001846 mol kg or 1
46. pplicable and the baseline drift as well If you are satisfied with your measurement results complete the measurement by clicking the Stop amp Save As button The save dialog prompts you to enter a name for your measurement This name is used to save the complete measurement sequence including graphic and evaluation which can be accessed at any time The evaluation dialog disappears after saving but can be re displayed by clicking the Measurem Analysis button If you make further changes such as activation of measurement values you are prompted to save your changes The Close button changes to a Save button which takes you back to the save dialog where the existing measurement name is displayed You can overwrite the previous measurement or enter a new name to create a new file 2 3 Osmolality After you have made a selection on the Start screen you will be taken to the part of the program that goes through osmolality determination with the OSMOMAT 070 2 3 1 Main screen All dialogs necessary for the measurement are displayed on the main screen Appropriately modified versions guide you through the entire measurement The main screen displays the graphic measurement sequence and additional current information The left side shows the defined and measured cell temperature the running sample time the current measured value provided by the measurement cell the history of the last four measured values for the particular sample solution
47. r measurement Chapter 2 Page 13 you can start measuring the solutions The OSMOMAT 070 is delivered with a cell constant This means that a cell constant for benzyl in a toluene solvent has been determined for the built in probes at a measuring temperature of 45 C and a sampling time of 4 minutes However this cell constant is only the result of a test calibration for final inspection You can use this cell constant to perform a test measurement for practice But in any case the device should be recalibrated with newly added solutions for molecular weight determination Chapter 4 1 Page 30 Recalibration is also required when just one of the entered parameters temperature measuring time solvent probe are changed User Guide OSMOMAT 070 Version 1 0 29 30 User Guide OSMOMAT 070 Version 1 1 4 1 Calibrating the Osmomat 070 4 1 1 Recording the parameters Figure 4 1 Example Entering parameters File View fot EL Wel 9 Cell temperatures Set Measured mu Wei sonent once Solution SAMPLE TIME ANNE res MEN Sabent Al D toluol calibration 08 03 2006 09 38 Ez sr D l Cell Set Temperature 45 C Boiling Point 1106C pe 8 30 bid Sampling Time 4 00 min Cell Const unknown 7 IES 70 Thermistor Probe Serial Numbers 8 2 amp 90 060103 B 91 060115 80 5 j Comment 50 3 z 3 I we ea Cancel E 2
48. r osmolality determination Sodium chloride 50 User Guide OSMOMAT 070 Version 1 1
49. rement effect for a solution with a concentration of 1x10 3 mol kg The size of the measurement effects depends a great deal on the measurement temperature Higher measurement temperatures cause higher measurement effects 48 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 49 6 2 List of Spare Parts and Expendables 00 9 0100 00 9 0101 00 9 0107 00 9 0109 00 9 0111 20 9 0100 20 9 0120 20 9 0130 20 9 0190 70 2 6027 70 6 0040 70 9 0060 70 9 0100 70 9 0110 70 9 0130 70 3 0010 70 3 0020 70 3 0030 Package with 10 fine wire fuses 0 1A slow Package with 10 fine wire fuses 0 2A slow Package with 10 fine wire fuses 2 5A slow Package with 10 fine wire fuses 4 0A slow Package with 10 fine wire fuses for cell PC board 6 3A fast Power cord 2 meters Connector cable for recorder Mains connection cable for cell and control unit SA or B Data cable for connecting the cell and control unit SA from 06 91 Lip seal for cell head Resistor plug for balancing the cell Handle for lifting the cell Allen wrench for securing measuring probes 1 5 mm Probe retaining screw complete Cover screw Measuring probe Type 100 for 37 105 C Measuring probe Type 270 for 60 105 C Measuring probe Type 30 for 0 70 C Measuring probes are used in pairs in the cell unit When making further orders for individual measuring probes please indicate the number on the nameplate of the remaining measuring probe 70 9
50. rements Two types of probes are therefore available for a temperature measuring range of 30 130 C Probe Type Temperature Range Resistance Value 100 35 105 C 63 k Ohm 5 k Ohm 270 60 130 C 63 k Ohm 5 k Ohm Figure 1 7 Probes 43 44 n W A Order No 70 3 0010 70 3 0020 43 Shielded probe cable 44 Probe shaft 45 Probe plug 46 Probe tube 47 Probe coil 48 Probe retaining screw with Allen head screw User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 11 A pair of Type 100 probes come installed with the unit The measuring probes are matched in other words the difference between their resistances should not be more than 15 The measuring probe s resistance value is the first part of the serial number e g 101060415 101 Resistance value in ohms Because the cell constant depends greatly on the built in probes each serial number for Positions A and B must be noted The probe with the lower resistance value is inserted into Position A If only one probe is replaced because of a defect the serial number of the used probe must be indicated when the order is made To change the probes the probe plug must firstly be removed from the cell and the Allen head screw on the probe retaining screw loosened after which the probe retaining screw with probe should be unscrewed The measurement system must be recalibrated after the probe change The probes should be cleaned after a change of sol
51. rforming a calibration If the baseline is stable siehe Figure 4 5 Figure 4 6 start measuring the individual solutions Then rinse the baseline again The reading is taken automatically each time after the sampling time has run its course You can accept the reading prematurely by clicking User Interrupt F2 This interrupt key is helpful if you discover after the dropwise addition that the wrong syringe has been used The reading thus accepted can later be suppressed when the measurement is being evaluated and you can repeat a rinse with the right syringe Figure 4 11 Example Measuring the baseline and rinsing it again ES SHE my epis esp ps em Base Line Correction 100 To end the measurement click Finish 4 2 3 Calculating the molecular weight Use the same procedure to evaluate the sample measurement that you did with the calibration The quotients from the measurement effects to the corresponding concentrations of the measured solutions are compared with the relevant concentrations Extrapolate up to a concentration of zero to get the measurement result while eliminating the concentration effect User Guide OSMOMAT 070 Version 1 0 39 40 User Guide OSMOMAT 070 Version 1 1 Figure 4 12 Example Result Molecular weight f ee BE Linear regression is performed au
52. rinsing the measuring probes with solvent click Start The selection screen disappears until a measurement value has been applied The measurement value is applied automatically if the Sample Time has expired or if you interrupt the measurement by selecting User Interrupt The selection dialog re appears Click the arrow icon in the lower left corner of the dialog to minimize it for a better view of the measurement graph Click the Continue button to re display the selection dialog Repeat the baseline measurement cycle until the baseline appears to be constant You can now measure your sample solutions one by one While you can perform any number of measurements with a sample solution only the last four measurements per sample solution are recorded and identified in the graphic on the main screen as A B C and D These last four values per sample solution are also used for the subsequent evaluation The sample solutions are selected by clicking the respective Select button or choosing Select Next Solution The procedure is identical to the baseline adjustment If you have taken the measurements of your sample solutions up to four measurement values per concentration are saved you also have to measure the baseline drift baseline correction The procedure here is also identical to the baseline adjustment Instead of the Cancel button you will now see a Finish button and can thus move on to the Evaluation Dialog see 2 2 5 2 2 5 Evaluatio
53. s recorded These can be electrolytes or even water soluble polymers If the electrolytes are partially dissociated the measurement result is determined by the sum of all the measured particles ions and molecules The vapor pressure osmometer is prepared as described in Chapter 3 1 Insert new dry vapor wicks into the beaker and fill it with 20 40 ml of water The vapor wicks must be completely saturated with water Insert the cell head as described We recommend that you carefully clean the ends of the measuring probes beforehand to make the surface hydrophilic This enables better wetting of the probes with the drops of water and allows a homogeneous drop to form Insert the syringes with User Guide OSMOMAT 070 Version 1 0 41 42 User Guide OSMOMAT 070 Version 1 1 distilled water into Positions 0 0 to rinse the baseline You can place the calibration standard and samples to be measured in Positions 1 4 first 5 2 Calibrating the measurement system for determining osmolality Start osmolality measurement by clicking File and then selecting New Measurement 070 followed by Osmolality Measurement Figure 5 1 Osmolality measurement Start screen File View Option he ap Ed el mu Cell temperatures S wae cn Perec E Solution SAMPLE TE ME rnea 0200 2007 1609 E RESP mm T Solvent A Please aniar ina eS a meigurament distilled Water 90 dararrieters CIEL H
54. stly rinse the right measuring probe with two or three drops then the left reference probe with one drop and the right measuring probe again with two or three drops After applying the drops click the Start button to start the sampling time 4 1 5 Starting calibration After you have entered all parameters for the solvent and clicked OK to confirm your entries start the calibration measurement by clicking the Calibrate button In the next dialog window you will be prompted to enter the concentration of the solutions for your calibration standard Enter the known molal concentration in mMol kg User Guide OSMOMAT 070 Version 1 0 33 34 User Guide OSMOMAT 070 Version 1 1 Figure 4 4 Example Calibration and entering concentrations Untitled and Unsaved EE LII m Cell temperatures Set Measures Solvent i pone ae Solution SAMPLETIME MEM cc AN c DEE Bie UT A a Calibration Standard Molecular Weight aha a py 0 mezowoe Xt e E s I ca eee i B Solution No t 402E3Moe kg 9 3570 7 SoluionNo 2 747E3MoleAkg Parameters F3 Solution No 3 11 53 E 3 Mole kg Measurem Analysis IE Solution No amp 1498 3 Molerkg Solution No 5 4 Solution No amp 0003 Mola H Solution No 7 g 1 Solution No 8 30 20 Zoom Res 10 D aucun 10095 4 gt t 13 min Beginning new measurement eer
55. there should be no solvents in the cell To prepare the cell you need to enter your desired temperature 15 C min and 125 C max The next screen displays two buttons The first of these BLA is used for baseline adjustment while the second Finish is for quitting the Cleaning mode At this point the software only shows you the graphic sequence and the measurement value This display helps you to prepare the measurement cell because you can track temperature errors affecting the measuring probes and the probes long term stability after assembly directly on your screen 2 5 Evaluating external data To evaluate existing measurement values which e g were acquired using the control unit B or are available in handwritten form only you can use the external Data mode This mode can be accessed via the start dialog or the File New external Data and 070 Molecular Weight Measurement or 070 Calibration Measurement menu items This opens the evaluation dialog where you can enter your data To calculate the molecular weight or a cell constant the measurement data have to be complemented by the respective concentrations of the solutions and the parameter dialog has to be completed To open the parameter dialog click the Parameters button However only the Cell Const parameter is necessary to calculate the molecular weight All other parameters are optional and can be entered for completeness All parameters are optional when you are calculati
56. tomatically The intercept is the result that indicates how great the measurement effect is for a substance concentration of 1g kg of solvent Figure 4 13 Example Linear regression MIERE iessung 02 02 2007 13 23 60 50 Ic Er 305 20 10 tz 41 min To calculate the molecular weight the results of the calibration measurement measurement effect mol kg are compared with the result of the sample measurement measurement effect g kg The final result is the number average of the molecular weight Mn determined by the program 40 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 41 Measurement effect mol kg_ g Mn 0 Measurement effect g kg kg After finishing the measurement save it by clicking the Save As button in the My Documents folder You can open it again at any time by selecting Open from the File menu ESSA tel fl 5 Determining the total osmolality of aqueous solutions 5 1 Preparing the measurement system The OSMOMAT 070 is suitable for directly determining the total osmolality of aqueous solutions The osmolal concentration of all particles in the solution i
57. u have taken the measurements of your sample solutions up to four measurement values per concentration are saved you also have to measure the baseline drift baseline correction The procedure here is also identical to the baseline adjustment Instead of the Cancel button you will now see a Finish button and can thus move on to the Evaluation Dialog see 2 2 5 2 2 4 Measurement To start a new measurement select the File New Measurement menu item and then 070 Molecular Weight Measurement or click the New button on the left side of the toolbar If the unit has been calibrated for the solvent used for the measurement you can click the Start button to enter the measurement mode User Guide OSMOMAT 070 Version 1 0 19 20 User Guide OSMOMAT 070 Version 1 1 The following dialog prompts you to enter the concentration of the sample solutions You can also enter a Sample ID and a Sample No for easier identification on measurement printouts After entering a minimum of one or a maximum of eight concentrations you can exit the dialog by selecting Start If the temperature of the measurement cell does not match the required temperature parameter a message informs you that the system is waiting for the correct temperature A selection dialog will guide you through the following measurement procedures The measurement starts with a baseline adjustment with an additional zero hardware adjustment during the initial adjustment After
58. up you can start the measurement by clicking Measure The screen for entering a sample net weight appears Enter the sample name a sample number and the net weights of the different sample concentrations Net weights should entered in the form of grams of the sample per kilograms of the solvent Chapter 3 1 6 explains how to make a sample for molecular weight determination Figure 4 10 Example Entering sample net weights fea Mes e 2 fe MINIMIZE THIS DIALOG WITH THE a BUTTON Em kad E p ES em 7 4 2 2 Performing the measurement A requirement for determining molecular weights is that the measurement system should be prepared for a measurement and a cell constant determined by calibration It is important to perform the measurement under the same conditions temperature probe numbering and A B positioning sampling time solvent as the calibration The substances to be measured must be fully soluble and should not chemically interact with the solvent When making solutions you should set the osmolal concentrations as high as possible At least three different concentrations that are 2 and 3 times greater than the lowest concentration must be measured Perform the measurement in the same way as the calibration 38 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 39 After clicking the Start button begin by rinsing the baseline just as you would when pe
59. urrent temperature This LED glows red during the heating phase if the measurement cell has not yet reached the specified target value and changes to green if the target value has adjusted to the temperature Pressing the Light key 3 on the front right hand side will activate an LED that lights up the interior for about 25 seconds The dropwise addition of a solution or solvent with syringes can be visually observed via a mirror 4 that is also attached to the front of the unit Figure 1 1 Osmomat 070 Front gononlec OSMOMAT 070 Vapor Pressure Osmometer Cell Unit User Manual OSMOMAT 070 Version 1 2 5 6 User Manual OSMOMAT 070 Version 1 2 The following items are located on the rear of the unit Figure 1 2 Osmomat 070 Rear CONTROL UNIT MONITOR Vv uester sen PAD MA We n ses aw H B 12 8 9 5 Socket for connecting the cell head 6 Potentiometer for fine adjustment of the head temperature 7 Connector sockets A and B for the measuring probes 9 Mains fuse for two phase protection of the cell unit 230V 2 5A 115V 4A 8 Power connector for plugging the cell unit into the mains voltage via the control unit 10 Nameplate with information on the unit type serial number supply voltage power consumption and line frequency 11 Connector socket for connection to the control unit 12 Connector socket for connection of a recorder 1 2 3 Design of the measurement cell The bea
60. utions are selected by clicking the respective Select button or choosing Select Next Solution The procedure is identical to the baseline adjustment Click Finish to go to the Evaluation Dialog 2 3 4 Evaluation Dialog The evaluation dialog shows the measurement values for the sample solutions and the average measurement value If you are not satisfied with the results of a sample solution you can return to the measurement by clicking the Back to Measurement button You can now measure the relevant sample solution again but the values already measured for this solution will be lost If you are satisfied with your measurement results complete the measurement by clicking the Stop amp Save As button The save dialog prompts you to enter a name for your measurement This name is used to save the complete measurement sequence including graphic and evaluation which can be accessed at any time The evaluation dialog disappears after saving but can be re displayed by clicking the Measurem Analysis button User Guide OSMOMAT 070 Version 1 0 23 24 User Guide OSMOMAT 070 Version 1 1 2 4 Cleaning The Cleaning mode is used to clean solvent residue from previous measurements out of the measurement cell To access this mode start the device with Cleaning or quit the Parameter Dialog by clicking Cancel and selecting 070 Cleaning under Options in the main menu After entering this mode you should have prepared the measurement cell accordingly and
61. vent especially for subsequent measurement with water The easiest way to do this is to clean the probe tip with dishwashing detergent If the probes are very dirty carefully remove the probe coil from the shaft and gently clean the tip of the shaft with steel wool After cleaning replace the coil whilst ensuring that the coil ends protrude about 1 mm above the end of the shaft We recommend that you then clean the tip with acetone in order to make the surface hydrophilic This ensures that a homogeneous drop can develop and coat the probe end via the coil User Guide OSMOMAT 070 Version 1 0 11 12 User Guide OSMOMAT 070 Version 1 1 1 2 6 Vapor wicks The vapor wicks for expanding the evaporation surface are inserted in the beaker They are composed of absorbent filter paper and are pre punched for insertion A set of vapor wicks consists of two paper strips and a round filter with two holes They are crimped and inserted in accordance with Figure 1 8 Vapor wicks are included as standard accessories Figure 1 8 Vapor wicks 362 r H 3 h 2 3 1 Xd LZ 1 1 Ck i A 12 User Guide OSMOMAT 070 Version 1 1 User Guide OSMOMAT 070 Version 1 0 13 1 2 7 Syringes The standard syringes included with the standard accessories are suitable for organic solvents with low vapor pressure and for aqueous solutions that do not have a very corrosive action Figure 1 9 Syringes 48 He iS 48 Glass syringe plunger

1 THE OSMOMAT 070 VAPOR PRESSURE OSMOMETER

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