Operation Manual Melting Point M�560 093251 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 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .19 6.1 Basic operating principles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19 6.1.1 Display during idle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19 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-560 and provides all the information required for its 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-560 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. Therefore the manual must always be available to all persons performing the tasks described herein. 2.
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 areas at risk 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-560 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.
3 3.1.
3 Technical data Table 3-2: Optional accessories (cont.) 3.
3 Technical data Table 3-4: Technical data of the Melting Point M-560 Melting Point M-560 ±0.3 °C to ±0.5 °C 250 °C to 400 °C Repeatability of melting point at 0.5 °C/min ±0.1 °C Accuracy of boiling point at 1.0 °C/min up to 400 °C ±0.5 °C Repeatability of boiling point at 1.0 °C/min ±0.3 °C Temperature gradients, °C/min 0.1, 0.2, 0.
4 4 Description of function Description of function This section explains the basic principle of the Melting Point M-560 and provides a functional description of the assemblies. 4.1 Melting Point The Melting Point M-560 is an instrument for manual (visual) 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. The boiling point can be determined for one sample.
4 4.3 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 through 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-560 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. Accessories • P lace the melting point capillaries in the hole of the housing. The second hole is a reservoir for used capillaries.
5 5.2.2 Putting into operation Power connection ATTENTION Make sure that the voltage of the socket corresponds to the voltage given on the type plate of the instrument. Ensure that the instrument is grounded. External connections and extension cables must be provided with a grounded conductor lead (3-pole couplings, cable, or plug equipment) as the mains lead has a molded plug to avoid risks due to inadvertently defective wiring.
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-560 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 of 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 advice and instructions.
6 Screen during melting point determination 6.1.3 Settings menu Operation Result indication (numeric result) 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. 6.1.4 Using the external keyboard NOTE The instrument can be operated using an external keyboard.
6 6.2 Operation Melting point determination NOTE For exact melting point determination, use original capillaries from BUCHI only. If other capillaries are used, the results may be inaccurate. Use the following items: Product Order number Melting point capillaries, 100 units 017808 Melting point capillaries, 1000 units 001759 Fig. 6.1: Melting point capillaries 6.2.1 Sample preparation NOTE Use only capillaries from BUCHI. They are precise and adequate for this kind of operation.
6 6.2.2 Operation Determination without pre-registered melting point method • Choose the menu for melting point determination. • Make sure that all samples are removed. • Press START to begin the determination process immediately with the last parameters used. They always remain saved in the instrument and are indicated in the green field in the lower part of the screen.
6 • Press START to begin the determination, and follow the on-screen instructions. • 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). Operation • I nsert samples and press START to begin the determination. • T o register additional temperature stamps, manually press the SET button for the related sample. Each button can be pressed three times.
6 • T o run through the result, turn the rotary knob up and down. • Press End or STOP to return to the idle screen. Operation • Press START to measure again with the identical measuring parameters. • The result is printed out automatically if a printer is connected. NOTE The last result is stored in the device until a new measurement is started or the instrument is switched off. • A fter turning back to idle, the last result can be checked again by pressing Result.
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. 6.2.4 Using and handling methods • T urn the rotary knob to select a method. • Press START to start the determination.
6 6.2.5 Operation 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.” (see 6.5). a • T urn the rotary knob to display the current parameter set. • Adjust the parameters by pressing Edit. Adjusting the parameters does not affect the saved method. 6.2.
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 may 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. 6.2: 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 begin the determination and follow the instructions on the screen. 29 • The instrument requests a sample ID during preheating (for details on entering text see 6.1.3).
6 • Delay: to ensure equilibrium between oven temperature and sample temperature. During this delay time some air bubbles escape from the boiling point capillary. This request can be changed in the setting “Boiling sample conditioning” (see 6.5). Bubble frequency is an indicator. When frequency of air bubbles coming out of the capillary is equal the indicator press Set. 6.3.3 Operation • T o run through the result, turn the rotary knob up and down. • Press End or STOP to return to the idle screen.
6 Operation When a measurement is completed, 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 Manual pressed results d General information e Signature of person making the determination c d e 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 Operation • 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. Press Save. • T o register temperature stamps manually press the Set button for the related sample. Each button can be pressed once.
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 performing 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. Table 6-1: Setting parameters Language English, German, French, Italian, Spanish, Japanese, Chinese Param. adj. during meas.
6 Operation Table 6-1: Setting parameters 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 Maintenance • 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. • I f glass parts of a melting point capillary are stuck in a hole of the metal heating block, use the cleaning tool as shown in the picture.
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 8-3: Error messages Error number Possible cause Remedy Error 01 Memory data loss, all data are reset. Calibrate device. In case of recurrence contact customer service. Error 02 Automatic restart, firmware problem possible. In case of recurrence contact customer service. Error 03 Board temperature sensor defective. Contact customer service. Error 04 Temperature sensor defective. Contact customer service. Error 05 Heating defective. Contact customer service.
8 8.1.1 Setting the printer baud rate • O pen compartment on the bottom of the printer. 8.2 Troubleshooting • T he following setting should be selected. 1,2,3,4,5,7,8,9,10 = ON 6 = OFF Customer service Only authorized service personnel are allowed to perform repair work on the instrument. They have comprehensive technical training and knowledge of possible dangers that might arise from the instrument. Contacts for official BUCHI customer service offices are available on the BUCHI website at: www.
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/Schweiz T +41 71 394 63 63 F +41 71 394 65 65 www.buchi.
