Operation Manual Melting Point M�565 093256 en
Table of contents Table of contents 1 2 3 4 5 About this manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 1.1 Reference documents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 1.2 Abbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 Safety . . . . . . . . . . . . . . . . . .
Table of contents 6 7 8 9 10 11 4 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .23 6.1 Basic operating principles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23 6.1.1 Display during idle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23 6.1.2 Display during a process or in menus . . . . . . . . .
1 1 About this manual About this manual This manual describes the Melting Point M-565 and provides all the information required for the safe operation and to maintain it in good working order. It is addressed in particular to laboratory personnel and operators. NOTE The symbols pertaining to safety (WARNINGS and ATTENTIONS) are explained in section 2. 1.
2 2 Safety Safety This section highlights the safety concept of the Melting Point M-565, Sample Loader M-569 and the MeltingPoint Monitor software and contains general rules of behavior and warnings about hazards concerning the use of the product. The safety of users and personnel can only be ensured if these safety instructions and the safety- related warnings in the individual sections are strictly observed and followed.
2 2.4 Safety Warning notices used in this manual WARNING Generally, the triangular warning symbol indicates the possibility of personal injury or even loss of life if the instructions are not followed. WARNING Hot surface. WARNING Electrical hazard. WARNING Biohazard. ATTENTION The “read this” symbol for ATTENTION indicates that equipment damage, malfunctions, or incorrect processes may result if the instructions are not followed. NOTE Useful tips to facilitate operation of the instrument. 2.
2 2.5.3 Safety Safety measures Always wear personal protective equipment such as protective goggles and protective clothing, when working with the instrument. 2.5.4 Safety elements Anti-seismic tie-down • T he instrument is equipped with a fixture to tie it down in the event of an earthquake (see bottom side of the instrument). 2.6 General safety rules Responsibility of the operator The head of laboratory is responsible for training the lab personnel.
3 3 Technical data Technical data This section introduces the reader to the Melting Point M-565 and its main components. It contains technical data, requirements, and performance data. 3.1 Scope of delivery Check the scope of delivery according to the order number. NOTE For detailed information on the listed products, see www.buchi.com or contact your local dealer. 3.1.
3 Technical data Table 3-1: Standard accessories (cont.) B B A Product Order number Sample holder 11055014 Cleaning tool 051978 A) Boiling point tubes, 10 units 019697 B) Boiling point capillaries, 10 units 051850 Protective cover 051935 Compaction wire 036721 CD Demo Melting Point Monitor 051983 USB cable, 2.
3 3.1.
3 Technical data Table 3-2: Optional accessories (cont.
3 Technical data Table 3-2: Optional accessories (cont.) Product Order number IQ/OQ: After installation OQ: For repeat use For further information please contact your local affiliate or distributor.
3 3.2 Technical data Technical data overview Table 3-3: Technical data of the Melting Point M-565 Melting Point M-565 Manual melting point determination √ Manual boiling point determination √ Automatic melting point determination √ Automatic boiling point determination √ Homogeneous sample loading – Positions for melting capillaries 3 Positions for boiling capillaries 1 Precision magnifying lens √ Magnification of lens 2.
3 Technical data Table 3-3: Technical data of the Melting Point M-565 (cont.) Melting Point M-565 Storable methods for melting point 50 Storable methods for boiling point 50 Compliant with Pharmacopeia methods PH. EUR. 6.1.2.2.60, USP XXI 741 and JP NOTE Temperature measuring accuracy refers to pharmacopoeia melting point. 3.
4 4 Description of function Description of function This section explains the basic principle of the Melting Point M-565 and provides a functional description of the assemblies. 4.1 Functional principle The Melting Point M-565 is an instrument for automatic and visual (manual) determination of melting point, melting range, and boiling point at ambient temperatures +10 °C up to 400 °C. The melting point of three samples can be determined at the same time.
4 4.1.1 Description of function Pharmacopoeia and thermodynamic melting points The melting process of a substance does not take place instantaneously - it requires a finite amount of time. The melting process begins at the point where the first particles of the substance turn into the liquid state (thermodynamic melting point). The end of the melt is reached when the last solid particles have gone over into the liquid phase (pharmacopoeia melting point).
4 4.1.2 Description of function Boiling points The boiling point is determined by the “Siwoloboff” method. The Melting Point M-565 can be used to determine the boiling point of a small amount of liquid. The heating block has one insert available for boiling point tubes (outside left). The moment of boiling is determined automatically or visually. Detection is done as follows: The beam of light illuminates the boiling point tube from the front, and the camera records the image. Fig. 4.
4 4.2 Description of function Controls and connections a Power switch; turns the instrument on/off b Start; starts process c Stop; stops process, starts/stops ventilation, returns to idle screen d 3 Select and Set buttons e Rotary knob for navigation in the menu and for select characters f Display f a b c d e Fig. 4.
5 5 Putting into operation Putting into operation This section describes the installation of the Melting Point M-565 and gives instructions for initial startup. NOTE Inspect the instrument for damage during unpacking. If necessary, prepare a status report immediately to inform the postal company, railway company, or transport company. Keep the original packaging for future transport. 5.1 Installation site Place the instrument on a stable, horizontal surface adequate for the maximum product dimensions.
5 Putting into operation • Glass window • Glass window with glass holder • I nstall the glass window with glass holder on the front side of the heating block. • Press the glass holder down. • Install the cover.
5 Putting into operation Accessories • P lace the melting point capillaries in the hole of the housing. The second hole is a reservoir for used capillaries. 5.2.2 Connecting to a PC with MeltingPoint Monitor software The Melting Point M-565 can be operated in connection with the MeltingPoint Monitor software. In this case, connect the instrument with the PC or laptop using the USB cable. For detailed information check installation guide on software CD.
6 6 Operation Operation This section explains the operating elements and possible operating modes. It gives instructions on how to operate the Melting Point M-565 properly and safely. ATTENTION Before use it is recommended to calibrate the apparatus. Use supplied calibration substances only. The calibration mode is described in section [6.4 Calibration]. 6.1 Basic operating principles WARNING The heating oven can reach temperatures up to 400 °C. 6.1.
6 Operation Different menus can be accessed by turning the rotary knob. Each menu has its own symbol. These idle screens are the starting points for all actions. The corresponding symbol is displayed during all processes. 6.1.2 Melting Point Boiling Point Calibration Tools Display during a process or in menus a b a Shows where you are and gives hints and instructions.
6 6.1.3 Screen during melting point determination Settings menu Result indication (numeric result) Result indication (replay) Operation Entering text Text can be entered by using the rotary knob, an external keyboard. Rotary knob: • Turn the rotary knob to select a character and press Enter. Press Save after entering all characters.
6 6.1.4 Operation Using the external keyboard NOTE The instrument can be operated using an external keyboard. For the softkeys, the following keys of the external keyboard are assigned: • • • • 6.2 ENTER = right softkey Alt = center softkey Esc = left softkey In the method menu: To navigate quickly to a method name press the initial letter. Melting point determination NOTE For exact melting point determination, use original capillaries from BUCHI only.
6 Operation Preparation of the samples: • T he samples being investigated must be fully dry, homogenous, and in powdered form. Moist samples must be dried first (the pharmacopoeias prescribe that the substance needs to be dried in a vacuum for 24 hours over silica gel R). Coarse crystalline samples and non-homogeneous samples are finely ground in a mortar. • To fill the capillary tubes with the sample, the open ends of the tubes are pressed into the substance.
6 Operation NOTE Insert samples only when the start temperature is reached (as soon as prompted). • Press START to start the determination, and follow the instructions on the screen. The instrument requests a sample ID during preheating (for details on entering text see 6.1.3). This request can be switched off by changing the setting “Sample ID request” (see 6.5). • I nsert samples and press START to start the determination.
6 • T o run through the results, turn the rotary knob up and down. • To replay the recorded melting process, press Replay. • Press End or STOP to return to the idle screen. • Press START to measure again with the identical measuring parameters. • The result is printed out automatically if a printer is connected. • Back: Turns back to the result menu. • Sample: Switches between sample left, middle, and right. • Play: Replays recorded video automatically.
6 6.2.3 Operation Creating a method Instead of entering and using the parameters directly from the idle screen, it is also possible to store parameter sets as methods. • T o enter the method menu, press Method. • T o create a new method, press Options New then OK. • E nter a method name. To finish press Save. • A djust a parameter and press Next. Then Save. 6.2.
6 • T urn the rotary knob to select a method. • Press START to start the determination. • Use Edit to adjust method parameters. 6.2.5 Operation • Press the Options key to get further functions: • New: Creates a new method. • Delete: Deletes the method. • Rename: Changes the method name. Adjusting parameters during a determination NOTE Measuring parameters can be modified during preheating or a determination. This function is possible only if enabled by the setting “Param. adj. during meas.
6 6.2.7 Operation Melting result NOTE Changing the determination mode does not affect the principle of measurement, but it does influence the interpretation and the appearance of the results. The mode can be selected in the settings menu. The default and most frequently used mode is the pharmacopoeia melting point. Melting range is convenient for substances with a wide melting range. The thermodynamic melting point should be used for special application only. For detailed information see Section 4.1.1.
6 a b c Operation Printout a Instrument type b Determination parameters c Automatically detected results d Manual results e Curve sample left f Curve sample center g Curve sample right h General information i Signature of person making the determination d e f g h i NOTE The Average is calculated on the basis of the temperature values with two positions after the decimal point.
6 Operation 6.2.7.2 Melting range • I n the settings, change the melting result to Melting range and press Save. An additional parameter is shown. The default value is set to 15%. This value can be used for most of substances. The result mode shows a range for each sample: XX.X–XX.X °C In the replay mode, the melting range is shown in gray backlit. 34 Threshold: This value is needed only for melting range determination. The default value is set to 15%. This value can be used for 80% of substances.
6 a b c Operation Printout a Instrument type b Determination parameters c Automatically detected results d Manual results e Curve sample left f Curve sample center g Curve sample right h General information i Signature of person making the determination d e f g h i 35 Melting Point M-565 Operation Manual, Version D
6 Operation 6.2.7.3 Melting point thermodynamic • I n the settings, change the melting result to Melting point thermodynamic and press Save. Experimental measurements have shown that in most cases a good approximation to the factor for thermodynamic correction of the BUCHI Melting Point M-565 is a value of ~1.5. Empirical calculation for thermodynamic correction is recommended when more accurate results are required for specific substances.
6 a b d c Operation Printout a Instrument type b Determination parameters c Correction factor for thermodynamic determination d Automatically detected results e Manual results f Curve sample left g Curve sample center h Curve sample right i General information j Signature of person making the determination d e f g h i NOTE The Average is calculated on the basis of the temperature values with two positions after the decimal point.
6 6.3 Operation Boiling point NOTE For exact boiling point determination, use boiling point tubes and capillaries from BUCHI only. If other glass parts are used, incorrect or no results can be obtained. Use the following items: B B A Product Order number A) Boiling point tubes, 10 units 019697 A) Boiling point tubes, 100 units 019007 B) Boiling point capillaries, 10 units 051850 B) Boiling point capillaries, 100 units 051890 A Fig. 6.3: Boiling point tube and capillary 6.3.
6 • U se the rotary knob to choose the start temperature and press Next. • U se the rotary knob to choose the stop temperature and press Next. Operation • U se the rotary knob to chose the temperature gradient and press Save. NOTE Insert sample only when the instrument has reached the start temperature. • P ress START to start the determination, and follow the instructions on the screen. 39 The instrument requests a sample ID during preheating (for details on entering text see 6.1.3).
6 73.2 73.4 Delay: to ensure equilibrium between oven temperature and sample temperature. During this delay time some air bubbles turns out of the boiling point capillary. This request can be changed in the setting “Boiling sample conditioning” (see 6.5). 6.3.3 Operation 76.4 76.6 • T o run through the results, turn the rotary knob up and down. Video replay is not available for boiling point determination. • Press End or STOP to return to the idle screen.
6 Operation When a measurement is done, the last method parameters are always retained in the instrument. To start the same method, just press START. NOTE Results are stored in memory until a new measurement is started or the instrument is switched off. 6.3.5 Printout a b Printout a Instrument type b Determination parameters c Automatically detected results d Manual results e General information f Signature of person making the determination c d e f Boiling temp. = Temperature sample boiled.
6 6.4 Operation Calibration NOTE BUCHI recommends calibrating each new instrument after installation. Furthermore it is recommended that the instrument be recalibrated every year. 6.4.1 Calibration principle NOTE The instrument is calibrated using melting point standards. The calibration is valid for boiling points as well. Use the calibration set (11055018). This calibration set contains the melting point standards listed below.
6 6.4.2 Operation Calibration procedure To start calibration, turn the rotary knob to Calibration. Press START and follow the instruction on display. The instrument automatically heats to the start temperature of the first substance. In the meantime, prepare at least 6 samples of the given substance. For this process, follow section 6.2.1. • C hoose the correct pharmacopoeia melting point value with the rotary knob. The pharmacopoeia melting point is written on the certificate of analysis.
6 6.4.3 Operation Printout a b c Printout a Instrument type b General information regarding calibration c Results 4-nitrotoluene d Results diphenylacetic acid e Results caffeine f Results potassium nitrate g General information h Signature of person making the calibration d e f g h NOTE The Average is calculated on the basis of the temperature values with two positions after the decimal point.
6 6.4.4 Operation Verification To verify the calibration, proceed as follows: • Measure all standards (BUCHI recommends using the verification set (11055019) but it is also possible to use your internal standards. NOTE The verification is not a guided process. • W hen all measuring results were within the required tolerances, click on Verified. The following screen appears: • Enter the following password: VER. The current date is now indicated under “Last verification”. 6.
6 • Press the Test button to enter the functional test, and follow the instructions. • Press the SysInfo button to open the system information menu. Printout is possible if a printer is connected. Operation • Press the Settings button to enter the settings menu.
6 Operation Table 6-1: Setting parameters (cont.) Thermodynamic correction 0.0–3.0; default value: 1.1 Company name The name of a company can be entered. Date (DD.MM.YYYY) XX.XX.XXXX Time (24 h) XX:XX Date format DD.MM.YYY, MM/DD/YYYY, YYYY-MM-DD Time format 24 h, AM/PM Temperature unit °C, °F, K Table 6-1: Setting parameters Buzzer volume 0, 1, 2, 3, 4 External Keyboard CH, USA Display brightness 0–100% Automatic detection Enable or disable the automatic detection.
6 6.5.
6 6.5.
7 7 Maintenance Maintenance This section provides instructions on all maintenance work to be performed to keep the instrument in good working condition. WARNING All maintenance and repair work requiring the opening or removal of the instrument housing must be carried out by trained personnel and only with the tools provided for this purpose. WARNING Electrical hazard: • Prior to any maintenance work on the instrument, switch off the power supply.
7 7.4 Maintenance Cleaning the heating block Remove broken capillaries from the heating block. ATTENTION • Wait for the heating block to cool down before touching it! • Remove the cover. • Follow the instructions mentioned below on the use of the cleaning tool 051978. • I f a melting point capillary is broken and is stuck in the heating block, use the cleaning tool (Order number: 051978). • R emove the cover and glass holder with glass window.
8 8 Troubleshooting Troubleshooting The following section describes how to resume operation of the instrument in the event of any minor problem. It lists some possible occurrences, their probable cause, and suggests how to remedy the problem. The troubleshooting table below lists possible instrument malfunctions and errors and describes courses of action that can be used by operators to correct some of those problems. The appropriate course of action is listed in the column “Remedy”.
8 Troubleshooting Table 8-1: General malfunctions and their remedy Malfunction Possible cause Remedy Sample decomposes during the melting process (formation of bubbles, sample turns brown, etc.
8 Troubleshooting Table 8–4: Error messages Error number Possible cause Remedy Error 11 Internal clock, power loss. Contact customer service. Error 13 5V input voltage missing Contact customer service. NOTE If several errors are pending, the one with the highest priority will be displayed. 8.1.1 Setting the printer baud rate • O pen compartment on the bottom of the printer. 8.2 • T he following setting should be selected.
9 9 Shutdown, storage, transport and disposal Shutdown, storage, transport, and disposal This section provides instructions on how to shut down the instrument, how to pack it for storage or transport, and specifies the storage and shipping conditions. 9.1 Storage and transport WARNING Biohazard: • Remove all dangerous substances from the instrument, and clean it thoroughly. • Store and transport the instrument in its original packaging.
10 10 Spare parts Spare parts This section lists spare parts, accessories, and optional extras, including all of the relevant order information for ordering from BUCHI. Always state the product designation and part number when ordering any spare parts. To ensure optimum system performance and reliability, use only genuine BUCHI consumables and spare parts for maintenance and repair. Prior written permission of the manufacturer should be obtained before any modifications are made to the spare parts used.
11 11 Declarations and requirements 11.1 FCC requirements (for USA and Canada) Declarations and requirements English: This equipment has been tested and found to comply with the limits for a Class A digital device, pursuant to both Part 15 of the FCC Rules and the radio interference regulations of the Canadian Department of Communications. These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment.
11 11.
BÜCHI Labortechnik AG CH-9230 Flawil 1 / Switzerland T +41 71 394 63 63 F +41 71 394 65 65 www.buchi.
