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Melting point

 B-540

5.7.3 Modifications of parameters during a

melting point determination

Quite frequently, the user will find out during an actual
determination that his selected parameters have to be
adapted, e.g. because the SETPOINT or the MAXPOINT are
too low or because the GRADIENT runs too slowly. In order
to adapt these parameters, it is not necessary to start the
determination again from the beginning.

The following modifications are possible:

Modifications before reaching the SETPOINT

The SETPOINT can be adapted.
The determination can be aborted.
Cooling down to ambient temperature.

Modifications in the ready mode

The MAXPOINT can be adapted.
The GRADIENT can be adapted.
The determination can be aborted.
Cooling down to ambient temperature.

Modifications between SETPOINT and MAXPOINT

The MAXPOINT can be adapted.
The GRADIENT can be adapted.
The determination can be aborted.
Cooling down to ambient temperature.

Modifications before reaching the SETPOINT

Problem: The SETPOINT has been selected too low.

The field for SETPOINT temperature begins to flash and may
be rised by actuating UP/DOWN.

The new SETPOINT temperature is confirmed with  ENTER
and the unit returns to the determination mode.

Problem: The determination is to be aborted.

The determination is to be aborted and the unit is to be cooled
down to ambient temperature.

5 Operation

TEMPERATURE

25.0 °C

SP 136 °C

Summary of Contents for B-540

Page 1: ......

Page 2: ......

Page 3: ...rograms 19 5 6 5 Printing of results 20 5 7 Running a melting point determination 21 5 7 1 Melting point determination with known melting point 21 5 7 2 Determination of the melting point with unknown melting point 22 5 7 3 Modifications of parameters during the determination of a melting point 25 5 8 Boiling point determination 27 5 9 Adjustment of subparameters 28 6 Maintenance 33 6 3 Calibratio...

Page 4: ... c 1 Metal cover for heating range 36569 d 2 Sample holders of glass 36110 e 1 Set of 100 melting point capillaries each 17808 f 1 Set of 10 boiling point tubes each 19007 g 1 Set of 10 boiling point capillaries each 01762 h 2 Spare fuses 20083 1 Mains cable PNE 2 5 m Type CH 10010 Type earthed shock proof 10016 Type GB 17835 Type USA 10020 Type AUS 17836 i 1 Brief operating instructions German 96...

Page 5: ... 60 Hz 38706 115 V 60 Hz 38707 1 Printer cable 29547 1 Melting point capillary 1000 off 01759 1 Boiling point tube 100 off 19697 1 Boiling point capillary 100 off 19698 1 Büchi Certificate for Calibration at Works G E F 97722 Remote control Meltingpoint Manual incl 3 1 2 diskette German 33758 English 33758 1 Protective cover 36625 1 Sample block for prepared melting point capillaries 36629 Table 3...

Page 6: ... be operated by persons who have the training or professional experience to comprehend the hazards that can arise when using the unit Personnel without such training or persons currently undergoing a course of training require thorough instruction This Instruction Manual should form the basis of these instructions 2 3 Proper use Theunitisdesignedandbuiltforuseinlaboratories Itisintended to be used...

Page 7: ...ust be worn such as goggles and a laboratory coat This Instruction Manual is a component of the melting point unit and as such it must remain available at any time to the operating staff where the unit is operated This also applies to manuals in other languages which are available on request 2 7 Modifications Modifications on the unit or on the spare parts or accessories as well as the use of any ...

Page 8: ...ies and the boiling point according to Silowopov For every determination the procedure is as follows 1 Selection of the SETPOINT temperature which is 10 C below the melting point to be expected 2 Selection of the temperature GRADIENT temperature GRADIENT within the range of the melting point 3 Selection of the MAXPOINT temperature at which the determination can be interrupted automatically 4 Stora...

Page 9: ...objects No containers chemicals or other appliances should be placed behind a unit 4 2 Power connections Check that the voltage of the socket is identical to the voltage specified on the unit plate Only connect the Melting Point Unit to a plug which is earthed External couplings and exten sion cables must be earthed 3 contact couplings cables and connectors Any interruption of the earth wire is pr...

Page 10: ...ating block taking care to touch the panel only laterally Figure 6 Inserting the upper ceramic part Figure 5 Mounting the glass panel Figure 7 Fitting the metal cover 5 Operation The upper ceramic part of the oven is placed onto the metal block The metal cover is placed over the heating area ...

Page 11: ...ange the cursor position horizontally when adjusting parameters on the display i UP DOWN keys to change adjustments of the relative cursor position j Keys to store measured values during a determination 5 Operation k Sample holder for melting point capillaries and boiling point tubes during determination l Receptacle for unused melting point capillaries and boiling point tubes m Receptacle for use...

Page 12: ...20 C min at which the unit will be heated up as from SETPOINT to MAXPOINT MAXPOINT Maximum temperature to be reached for the current determination This is set automatically at 15 C above the SETPOINT but may also be adapted Storage menus main menu 2 Temperature Current temperature inside of the oven Name Name of the method under which the parametersare to be stored for a melting point determinatio...

Page 13: ...per sample capillary which are arranged in vertical order 5 3 3 Graphics The unit heats up to the preselected SETPOINT The unit has reached the preselected SETPOINT and waits for the temperature program to be started With the preselected GRADIENT the unit heats up to the maximum point of the temperature program MAXPOINT The unit has reached the highest point of the temperature program MAXPOINT and...

Page 14: ... on a hard base or letting the capillary drop onto the table through a glass tube of approx 1 m length 5 5 Determination of a melting point The following items must be known before a melting point can be determined a Is the approximate melting point known if not R see 5 7 2 b Is a sample name to be entered if yes R see 5 6 1 c Where is the SETPOINT of the determination located SETPOINT input R 5 5...

Page 15: ...INT of 180 C is to be adjusted Actuate ENTER until the cursor is on the SETPOINT field Increase or reduce the value until the number 1 is in the first digit NEXT until the cursor is on the second digit Increase or reduce the value until the number 8 is in the se cond digit NEXT until the cursor is on the third digit Increase or reduce the value until the number 0 is in the third digit ENTER to tra...

Page 16: ... of the gradient is made in 0 1 0 2 0 5 1 2 5 10 20 C min in the main menu By way of example a gradient of 1 C is to be selected Actuate the ENTER key until the cursor is on the gradient field Increase or reduce the temperature rise until the value of 1 C min is displayed Actuate ENTER to transmit the selected temperature rise 5 Operation TEMPERATURE 25 0 C SETPOINT 100 C GRADIENT 2 0 C MAXPOINT 1...

Page 17: ...AXPOINT temperature of 195 C is to be increased to 230 C Actuate ENTER until the cursor is on the MAXPOINT field Increase or reduce the value until the number 2 is in the first digit NEXT until the cursor is on the second digit Increase or reduce the value until the number 3 is in the second digit NEXT until the cursor is on the third digit Increase or reduce the value until the number 0 is in the...

Page 18: ... figures or a combination of figures with letters For easy entering of sample names and sample identifications we recommend to use a keyboard Büchi Art No 29599 Actuate ENTER until the cursor is on the NAME field for entering the method name Actuate NEXT until the cursor is on the correct position of the horizontal which is to be modified An individual cursor position can be changed by actuating U...

Page 19: ...the program is stored with the selected parameters under the entered name and the display will change to main menu 1 The sample identification is not stored Possible error messages TEMPERATURE 25 0 C RECALL CLEAR STORE PRINT TEMPERATURE 25 0 C MEMORY FULL PRESS ENTER TEMPERATURE 25 0 C NO NAME NOT STORED PRESS ENTER TEMPERATURE 25 0 C NAME EXISTS ALREADY PRESS ENTER ...

Page 20: ...sor is on the RECALL field By pressing the ENTER key the stored programs are listed Choose the selected program with UP DOWN keys e g benzoic acid Recall the selected program by pressing the ENTER key The unit is now ready for the next determination with the recalled method Possible error message 5 Operation TEMPERATURE 25 0 C SETPOINT 100 C GRADIENT 2 0 C MAXPOINT 120 C TEMPERATURE 25 0 C RECALL ...

Page 21: ...he cursor is on the CLEAR field By pressing ENTER the stored programs are listed SelecttheprogramtobecancelledwithUP DOWN e g benzoic acid Press ENTER to cancel the selected program If necessary further programs may be cancelled now By pressing MENU return to the main menu Possible error message TEMPERATURE 25 0 C SETPOINT 100 C GRADIENT 2 0 C MAXPOINT 120 C TEMPERATURE 25 0 C RCL XXXXXX q XXXXXX ...

Page 22: ...d in the PRINTER box In the AUTOPRINT bix it is stipulated that for YES there will be an automatic printout after every determination NO there will not be a printout after every determination 2 Manual printout after every determination The user can stipulate for which determination he wishes to have a printout No must then be selected for AUTOPRINT in configuration menu 3 If a printout is required...

Page 23: ... confirmed with an indication on the screen A maximum of three modifications of condition per sample may be transmitted to the memory If keys are pressed more than 3x the last three temperature values will be retained When the preselected MAXPOINT has been reached the unit will cool down automatically to the previously used SET POINT The temperature program may be stopped before reaching the MAXPO...

Page 24: ...MAXPOINT must be defined By way of example a melting point is to be determined which is between the ambient temperature and 300 C For this it is sufficient to determine the approximate melting point with one capillary only Establishing the SETPOINT with unknown melting point Press ENTER until the cursor is on the SETPOINT field Increase or reduce the value until the number 0 is in the first digit ...

Page 25: ...ected temperature program The cursor jumps to the next line Adjusting the MAXPOINT with unknown melting point Increase or reduce the value until the number 3 is in the first digit Press NEXT until the cursor is on the second digit Increase or reduce the value until the number 0 is in the second digit Press NEXT until the cursor is on the third digit Increase or reduce the value until the number 0 ...

Page 26: ...reen A maximum of three modifications of condition per sample may be transmitted to the memory If keys are pressed more than 3x the last three temperature values will be retained When the preselected MAXPOINT has been reached the unit will cool down automatically to the previously used SET POINT The temperature program may be stopped before reaching the MAXPOINT temperature by pressing STOP Even i...

Page 27: ...erature Modifications in the ready mode The MAXPOINT can be adapted The GRADIENT can be adapted The determination can be aborted Cooling down to ambient temperature Modifications between SETPOINT and MAXPOINT The MAXPOINT can be adapted The GRADIENT can be adapted The determination can be aborted Cooling down to ambient temperature Modifications before reaching the SETPOINT Problem The SETPOINT ha...

Page 28: ...OWN The new temperature GRADIENT is acknowledged with ENTER and the MAXPOINT temperature flashes The MAXPOINT temperature can be increased via UP DOWN The newly selected MAXPOINT is confirmed with ENTER and the unit returns to the determination mode Problem The determination is to be aborted The determination is aborted and the user returns to the main menu 5 Operation PRESS START TEMPERATURE 135 ...

Page 29: ...oiling point is not known the SETPOINT should be selected as low as possible and the temperature GRADIENTandtheMAXPOINTashighaspossible analogously to the melting point determination section 5 6 a quick deter mination for orientation is carried out If the approximate boiling point is known enter the SETPOINT GRADIENT and MAX POINT analogously to melting point determination with known melting point...

Page 30: ...on of the printer to be used Menu window for adjusting the serial interface to the PC connection Menu window for adjustments of the unit Contrast Adjustments of the LCD display Buzzer Beep yes no Menu window for basic adjustments Time Time subdivided into 12 or 24 steps Date American or European date Unit Temperature in C or K Language Language as displayed SW version Indication of the software in...

Page 31: ...s MENU for three seconds to return to the range of submenus By pressing UP DOWN the individual digits are changed by pressing NEXT the horizontal cursor position is changed By pressing ENTER the date field will be displayed and this is then adapted in the same way as described above By pressing ENTER the field for the company name is displayedandthisisthenadaptedinthesamewayasdescribed above By pr...

Page 32: ...hree seconds to return to the range of sub menus Press MENU twice to go to the menu window By pressing UP DOWN the automatic printout will be activated after every determination and made inoperative with NO Press ENTER to change to the printer field Press UP DOWN to select the printer to be used CITIZEN EPSON also Canon and Seiko HP STAR NONE By pressing ENTER the newly entered printer will apply ...

Page 33: ...ength Parity Number of stopbits Press MENU for three seconds to return to the range of sub menus Press MENU twice to change to the menu window Press UP DOWN to select the correct RS 232 C interface When pressing ENTER the newly selected RS interface will be displayed for all determinations Press MENU again for three seconds to return to mainmenu 1 RS232 C XXXX XXX ...

Page 34: ...NU key three times to change to the menu window Menu window to unit adjustments CONTRAST LCD display adjustments BUZZER Beep on off By pressing the UP DOWN key the background illumination will be increased or reduced By the pressing the ENTER key the user return to the buzzer field By pressing the UP DOWN key the beep will remain with YES and be made inoperative with NO Press the MENU key again fo...

Page 35: ...d This also includes a periodic cleaning and checking for any damages It is also recommended to calibrate the unit periodically with adequate calibration substances 6 1 Cleaning The housing of the Melting Point Unit B 540 is coated with paint It must only be cleaned with a rag to be either dry or moistened with alcohol Do not use any chlorinated solvents acetone or similar chemical to clean the ma...

Page 36: ...king the filled capillaries on a hard surface the substances are ground in a mortar Gradient 0 5 C min Setting point 5 C below the expected melting point Determine the clear melting point sample melted completely clear 6 3 2 Evaluation of the melting point determination All measurements should be evaluated in accordance with strict criteria and checked for their usability For this we recommend tha...

Page 37: ...the expected theoretical values and the corresponding corrections made if necessary We recommend correction only in the case of errors 0 3 C 6 3 3 Correction inputs If it is ascertained during a routine check of the temperature display that the actual and rated values of the calibration sub stancesdiffer theunitmayberecalibratedbytheuserasfollows Press the MENU key for three seconds Press the MENU...

Page 38: ...ntered for the three types of calibration substances The left column indicates the last correction the right column is used to enter the new corrective value By pressing the UP DOWN NEXT keys the necessary corrective value at 83 C is entered By pressing the ENTER key change to the 2nd temperature value and adapt this analogously Then press the ENTER key to change to the 3rd temperature value and a...

Page 39: ... reference substance must be checked in at least three measurements The standard deviations should be less than 0 3 C The maximum permitted deviations of the mean value from the theoretical melting point are as follows All measurement results of the calibration the correction factors entered and control measurement values should be recorded This allows the calibration to be checked and repeated at...

Page 40: ...fic service manuals which are only available to authorised personnel Addresses of official Buchi customer service offices are given on the Buchi website under www buchi com Please contact one of these depots if the unit develops any faults or you have any technical enquiries or application problems The Büchi customer service will be pleased to provide you with the following services Spare parts se...

Page 41: ...ting Point Unit is as ecofriendly as possible you will find a list of the materials used some of which are marked with material codes in Chapter 9 Appen dix This ensures that components can be separated and where appropriate recycled Care must be taken that regulations are complied with when disposing of electrical components Furthermore allmethodsofdisposalshouldcomply with regional and local leg...

Page 42: ...l is equally prohibited Description Order no Protective cover 36625 Brief instruction manual in German 96635 Brief instruction manual in English 96636 Brief instruction manual in French 96661 Compaction wire 36721 Capillary holder of plastic 36629 Spare bulbs 29573 Spare fuse 110 120 V 19660 Spare fuse 220 240 V 20083 Upper ceramic part of oven 34564 Glass panel 34236 Metal cover for heating area ...

Page 43: ...l printers are connected through the parallel V24 interface which is connected via the communication cable centronic to the printer see section 5 1 Appropriate printer settings are selected in the configuration menu of the melting point apparatus The interface is auto matically correctly configured by the melting point apparatus 9 3 Interface configuration Parallel interface RS232 Baud rate 9600 D...

Page 44: ...rations menus Configuration menu 1 Main menu 2 Main menu 1 Main menu 3 Press MENU key for 3 seconds 9 4 Menu chart The menu chart of the Melting Point B 540 can be subdivided in 2 main parts the 3 main menus Chapter 9 4 1 the 7 configuration submenus Chapter 9 4 4 ...

Page 45: ...nue with the START key GR GRADIENT MP MAXPOINT Slow heating with selected Gradient to MAXPOINT or early stopping with the STOP key manual auto detection GR GRADIENT MP MAXPOINT Quick cooling down to SETPOINT Quick cooling to ambient temperature 9 4 3 Program memory RCL Recall Recalling the programs stored CLR Clear Clearing the programs stored Ä TEMPERATURE 25 0 C SETPOINT 100 C GRADIENT 2 0 C MAX...

Page 46: ...on with the recommended parameters see chapter 6 3 German French English ZEIT XX XX DATUM XX XX XX NAME XXXXX HEURE XX XX DATE XX XX XX NOM XXXXX TIME XX XX DATE XX XX XX NAME XXXXX AUTO PRINT XXX DRUCKER XXXXX TASTATUR XX IMPR AUTO XXX IMPRIMANTE XXXXX CLAVIER XX AUTOPRINT XXX PRINTER XXXXX KEYBOARD XX RS232 C XXXX XXX RS232 C XXXX XXX RS232 C XXXX XXX KONTRAST XXX PIEPSER XXX CONTRASTE XXX BUZZE...

Page 47: ...ame has been inserted Memory full Clear programs to obtain free memory space No printer selected Configuration menu Check the battery Lithium cell in the unit and set new time and date Calibration interval exceeded Keep pressing MENU key to go on working Last calibration Switch off the unit main switch Keep pressing the START key and switch on the unit Call customer service see chapter 6 4 Figure ...

Page 48: ...ent temperature 5 40 C Table 6 Technical data Fault Cause Remedy STORED DATA LOST The battery is exhausted Press the Menu key for 5 seconds PLEASE CHECK BATTERIE Order new battery and have it installed by techn AND SET TIME AND DATE service Date and time to be reprogrammed CALIBRATION INTERVAL The selected calibration Press the Menu key for 5 seconds EXCEEDED time has expired Calibrate the unit LA...

Page 49: ...ces du Canadian Department of communications Ces limites sont destinées à fournir une protection odéquate contre les interférences nétastes lorsque l appareil est utilisé dans un environnement commercial Cet appareil génère utilise et peut radier une énergie à fréquence radioélectrique il est en outre susceprible d engendrer des interferences avec les communications radio s il n est pas installé e...

Page 50: ... compatibility Generic immunity standard Residential commercial light industry EN 60555 2 1987 IEC 555 2 Disturbances in supply systems caused by hosehold Rotavapors and similar electrical equipment Harmonics EN 60555 3 1987 IEC 555 3 Disturbances in supply systems caused by hosehold Rotavapors and similar electrical equipment Voltage fluctuations EN 61000 3 2 1995 1996 Limits for harmonic current...

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