Operation Manual AUTO MELTING POINT APPARATUS · PDF fileMPA-12 User Manual V1.0 - 1 - I....

MPA-12

PLEASE READ THIS MANUAL CAREFULLY BEFORE OPERATION

3, Hagavish st. Israel 58817 Tel: 972 3 5595252, Fax: 972 3 5594529 [email protected]

MRC.12.16

Operation Manual AUTO MELTING POINT APPARATUS

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Contents

I. SUMMARY .....................................................................................................- 1 -

II. TECHNICAL PARAMETERS ......................................................................- 2 -

III. STRUCTURE ...............................................................................................- 3 -

IV. OPERATION ..............................................................................................- 20 -

V. NOTICES......................................................................................................- 21 -

VI. MAINTENANCE ........................................................................................- 23 -

VII. SUPPLEMENT .........................................................................................- 25 -

MPA-12 User Manual / v1.1

Warning: The instrument can not provide the designed protection for

operators who do not follow the right procedures and requirements given by the manufacturer.

Warning: All solutions must be handled with care according to the

lab’s safety regulation. Please make a reference to the related material safety data sheet. Wear the lab-gown, goggle and rubber gloves all the time. Be care of hot reagents.

Warning: Be aware of the risk of electric shock. Only the trained

professionals are permitted to open the face panel or back cover.

MPA-12 User Manual V1.0

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I. Summary

According to the definition in physical chemistry, the melting point of a substance means the temperature at which it changes from solid state into liquid state. In the field of organic chemistry, melting point test is the basic method to identify nature character of a substance, and is one of the important means to measure purity as well. MPA-12 Auto Melting Point Apparatus adopts photoelectric inspection, digital temperature display and other advanced technologies and has the functions of automatically displaying initial temperature, final temperature and others. Linear correction platinum resistor is employed by temperature system of the apparatus as its detection component and the instrument is featured by accuracy, high efficiency and convenience, etc.

MPA-12 Auto Melting Point Apparatus is widely used in chemical industry and medical research, and is one of the necessary instruments for the production of drugs, flavors, dyes and other organic crystalline substances.


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II. Technical Parameters

1. Melting Point Measuring Range: Room temperature +5 ~℃ 400℃;2. Setting rate for starting temperature:Room temperature +5 ~℃ 400℃ within 7min; 400℃~room temperature within 7.5min; 3. Minimum reading for temperature display: 0.1℃;4. Temperature accuracy: ±0.4℃(<200℃),±0.7℃(<300℃); 5. Linear heating rate: 0.1 /min℃ , 0.2 /min℃ , 0.5 /min℃ , 1 /min℃ ,2 /min℃ , 3 /min℃ , 4 /min℃ , 5 /min℃ , eight options in total. 6.Repeatability: 0.2 at ℃ heating rate of 0.2 /min℃ 7. Size of standard capillary: inner diameter: 1.0mm,outer diameter: 1.4mm 8. Power supply: 220VAC±10%, 50HZ9. Power: 150W10. Dimensions: 455mm*312mm*200mm11. Weight: 12kg


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III. Structure

1. ComponentsMPA-12 is a melting point apparatus used for melting point test. The apparatus consists of heating and testing systems. For structure of the instrument, please see the following figures. Figure 1 Side View of the Instrument.

Figure a 1. Heating furnace 2. Multicolor LCD touching screen 3. Power switch


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Figure b 4. Power interface 5. Reserved data interface 6. Heating fuse 220V, 3A 7.Power supply fuse 220V, 3A 8. Fan outlet 9. Fan outlet 2. Functions2.1 Welcome Interface When the instrument starts, a welcome screen is displayed hereunder in Figure 2.

Figure 2


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2.2 Function Interface Four functions in the function interface: Test, Calibration, Help and Attention, as shown in Figure 3.

Figure 3 2.3 Setting Interface In function interface, slightly touch “Test” to enter parameter setting interface, which is to set two parameters here: “Preheating Temperature” and “Heating Rate”. Default preheating temperature is the previous preheating temperature while heating rate is the previous heating rate. Meanwhile,setting interface is displayed in Figure 4 reminds the user to input the preheating temperature and the heating rate. After inputting the desired preheating temperature and the heating rate, click “OK” to enter test interface, or click “Cancel” to return to Figure 3.


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Figure 4 2.4 Preheating Temperature Setting Interface Slightly touch “Preheating Temperature”, a small numeric keypad pops up and corresponding numbers can be put into set preheating temperature as the interface shown in Figure 5. With the prompt “Please input preheating temperature, temperature range: 0-400℃”, input the preheating temperature using the numeric keypad. Click “Cancel” to delete or “Enter” to confirm the input, as shown in Figure 5.


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Figure 5 The preheating temperature will be displayed after the input. For example, if you input “100” and then click “Enter” to confirm, it will display “Preheating Temperature: 100.0 ”, as ℃ shown in Figure 6. Click “OK” to finish the setting and return to parameter setting interface (Figure 4); or click “Cancel” to return directly to Figure 4.

Figure 6


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2.5 Heating Rate Setting Interface As shown in Figure 4, in Parameter Setting Interface, select “Heating Rate” to enter setting interface. With the prompt “Please select Heating rate”, click arrow marks to set the rate. The rate can be increased or reduced, as shown in Figure 7. Click “OK” to finish the setting and return to the parameter setting interface (Figure 4); or click “Cancel” to return directly to Figure 4.

Figure 7 2.6 Melting Point Test Interface After completion of temperature and heating rate settings, in parameter setting interface (Figure 4), click “OK” to enter melting point test interface, as shown in Figure 8. “Actual temperature, Preheating temperature and Heating rate” are displayed at the same time. Prompt: “1. Please press Preheating to begin heating”. Measured values and average values in three successive tests are displayed.


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Figure 8 Click “Preheating” to enter heating state and heating furnace temperature is displayed at all times. Meanwhile, it prompts “2. Heating… Till it reaches preheating temperature. Put the sample in and press Heating key, as shown in Figure 9.

Figure 9


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When it reaches the preheating temperature, put the sample in and press “Heating” and start melting point test subject to the actual temperature. On the screen, it reads “3. Sample melting point testing…Please wait.” As shown in Figure 10.

Figure 10 When it reaches the preheating temperature, if there is no sample put in but Heating key is clicked, it will prompt “Please make sure you have put sample in. Please press Heating key to restart the test”, as shown in Figure 11.


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Figure 11 When the sample reaches its initial melting point, the initial melting temperature will be displayed. To continue heating test, the interface is displayed as shown in Figure 12.

Figure 12 When the final melting point of the sample reaches, it completes the melting point test and in the meantime, initial and final melting temperatures of the sample are displayed, as shown in Figure 13.


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Figure 13 After the display of initial and final melting temperatures of the sample for a few seconds, the device automatically records the measured data and average values. After the measurement, the apparatus will return automatically to the original preheating temperature for a next test. Click “Return” to exit test interface and return to the function interface, as shown in Figure 14.

Figure 14


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Note: If “Preheating” is clicked again after the test, the apparatus will clear the measured data and preheat the sample to the setting temperature and start test again. If “Heating” is selected, then the measured data are saved and the apparatus returns to the original preheating temperature, allowing the test of the same sample to be repeated. With Preheating unchanged, press Heating and return to the original preheating temperature for re-tests of the same sample. On the screen, measured data and average values of three times can be displayed simultaneously, as shown in Figure 15.

Figure 15 2.7 Calibration Interface On the function interface (Figure 3), click “Calibration” to enter calibration interface. Apparatus can be calibrated with this interface. After respectively measure the melting points of three reference materials, which are, naphthalene, adipate and anthraquinone, the apparatus will calibrate automatically. On the screen, as it prompts “Please input successively the melting point temperatures of the reference materials”, input the melting point temperatures and preheating temperatures of the reference materials in the


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interface, as shown in Figure 16.

Figure 16 If reference material Naphthalene is selected, default preheating temperature 76℃ and default heating rate 1.0 / min℃ are shown. Meanwhile, the system prompts “… Please press Preheating key to reach preheating temperature.” The preheating temperature is usually 5-10 lower than ℃ the reference melting point temperature. Interface is shown in Figure 17.

Figure 17


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Press “Preheating” key for preheating. Actual temperature is displayed at real time, and the system prompts “2 Heating… Please wait. Till it reaches preheating temperature, put sample in and press Heating key.” at the same time, as shown in Figure 18.

Figure 18 When it reaches the preheating temperature, put test reference material in and press “Heating” to start test. It reads on the screen “Use reference sample to calibrate instrument. 3 Melting point of reference material is being measured. Please wait” as shown in Figure 19.


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Figure 19 When the initial melting temperature and the final melting temperature are displayed, test of the reference material is accomplished. As the system prompts “2. Heating… Please wait. When it reaches preheating temperature, put sample in and press Heating.”, press “Heating” to re-measure the reference material. Press “OK” to select a next reference material for calibration. Repeat the above calibration procedures. Three successive measured values and average values can be displayed on the same melting point test interface, as shown in Figure 20.


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Figure 20 When “Cancel” is clicked during calibration process, the system will prompt “Instrument Calibration is canceled” and exit the calibration process, returning to the function interface. When three reference materials are measured completely, the system prompts “Instrument Calibration Completed!” as shown in Figure 21. Turn off the apparatus and restart it so as to complete the calibration process.

Figure 21


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2.8 Attention Interface In the function interface (Figure 3), click “Attentions” to enter the following interface. In this interface, details and attentions during apparatus operation are introduced, as shown in Figure 22.

Figure 22 Click “Page Down”, it goes to the next page, as shown in Figure 23. Press “Return” to return to the function interface (Figure 3).


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Figure 23 2.9 Help Interface In the function interface (Figure 3), click “Help” to enter HELP interface, as shown in Figure 24. Press “Return” to return to the function interface.

Figure 24


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IV. Operation

1. Capillary Sample PreparationPut test sample into agate mortar, then pestle and dry. Take an 800mm long, dry and clean glass tube and stand it vertically on a magnetic plate or glass plate. Put the capillary with test sample into the tube and make it fall free. Repeat the free fall eight times till sample powder gathers tightly at the bottom (About 3mm in height).

2. Melting Point Apparatus Test2.1 Turn on the power switch and warm up the apparatus for 20minutes. 2.2 Enter the function interface and select Test. Set proper preheating temperature and heating rate. 2.3 Heat after confirmation. When it reaches the preheating temperature, put the sample in and test. 2.4 When the test is completed, initial melting temperature and final melting temperature are displayed. Record test data and take out tested sample. Press Heat key to re-test the same sample. 2.5 Click “Return” to return to the function interface after test. Reset relevant parameters and test a next sample.

3. Apparatus Calibration Test3.1 Start the instrument and warm up for 20 minutes. Click the icon at the lower right corner to enter the function interface. 3.2 Select “Calibration” to enter calibration interface. 3.3 Select one reference material, e.g. naphthalene, the system will display default preheating temperature and default heating rate. 3.4 Select Preheating to begin preheating and heating. When it reaches the preheating temperature, put the sample in and click “Put in sample” for


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melting point measurement. 3.5 After the test, the instrument will automatically record the initial and final melting temperatures. Take out the sample and measure the second reference material with the same test procedures. 3.6 When three reference materials are tested, turn off the apparatus. Restart the instrument to complete calibration. Note: Melting Point Apparatus is calibrated before it leaves the factory. It does not need calibration after use in a short time.

V. Notices

1. Test sample shall be baked as required, pestled in dry and clean mortar.Tap the capillary with free falling method till sample is filled tightly. Height of the sample in the capillary shall be no less than 3mm. Height of the sample in the same batch number shall be consistent so as to ensure accordant test results.

2. Turn on the instrument and then set preheating temperature. When it isclose to the preheating temperature, put the sample in and press OK key.

3. The starting temperature set shall not exceed operation range of theapparatus, or the instrument may be damaged.

4. The starting temperature of some samples has great effect on melting pointtest results, please operate according to regulations. We suggest the capillary be inserted 3-5 minutes ahead. If linear heating rate is 1 /min℃ , the starting temperature shall be 3-5℃ lower than melting point; if heating rate is 3 /min℃ , the starting temperature shall be 9-15℃ lower than melting point. Usually, optimum test conditions are determined according to specific test content.

5. Different linear heating rates lead to different test results. Properregulations and standards shall be formulated. Usually the higher the


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heating rate, the larger the readings. Melting point reading of each heating rate can be unified by test correction value. For the sample with unknown melting point, quick heating or higher heating rate is employed first.; when it reaches initial melting point range, fine measurement is used.

6. When there is a reference sample, test the reference sample first. Selectcertain starting temperature and heating rate for comparative measurement as required. Initial and final melting point readings of reference sample can be used as examination evidence.

7. It is better to fill test sample into five capillaries once a time. Test themrespectively and delete the maximum and minimum values. Take the average value of the remaining three readings as test results. This can eliminate accidental error caused by capillary and sample filling.

8. Capillary inserted in the sample chamber must be clean and standard, fordirt will deposit and it is easy to damage the capillary, making the test impossible.

9. Handle with care the instrument in use. Keep it away from acid and alkalinesolution. Prevent it from use in strong light. Please do not touch sample chamber during heating process in case of scald.

10. If the capillary is broken in the sample chamber, please turn off powersupply, cool the instrument, and then take it out.

11. If the instrument may not be used for a long time, please disconnectpower cable. The apparatus shall be warmed up for 10 minutes before put into use again.


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VI. Maintenance

1. The instrument shall be used in dry and ventilated rooms. Prevent it fromwater and humidity. The instrument uses three-core power plug. The grounding terminal shall be grounded to the earth and can not be replaced by a neutral line.

2. The capillary used in the instrument must be supplied by our company. Nomanually-drawn capillary can be used instead in case it is too tight to break. Fine capillaries shall be selected.

3. If capillary of the instrument is broken in the tube seat, please first turn offpower supply, and cool the furnace, then pull out the tube seat. The tube seat shall be pulled out like this: one hand holds the electrothermal furnace, and the other hand lifts the tube seat. Please do not just lift the tube seat. Improper force on the seat may damage the support board of the electrothermal furnace. Then use capillary breaker to smash the broken capillary in the tube seat. Empty the shatter from the seat and then insert the tube seat again into the furnace. The notch on the tube seat shall be aligned with the flange on the electrothermal furnace. Check the entire instrument after these operations and contact the service department of the company for repair if necessary.

4. If there is no display on the screen when the apparatus is turned on, theheat dissipation fan does not work, or the heating furnace does not heat, please shut off power supply and check if the fuse on the rear panel of the instrument is burnt. Replace it in time.

5. Accuracy test：Accuracy test is performed with reference materials ofGBW13238 national standard on melting point, which are approved by (1989) No. 335 Document of State Bureau of Technical Supervision. The apparatus currently uses three of the reference materials for test: naphthalene (final melting point 81.0 ), adipate (final melting point ℃


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152.9 ) and anthraquinone (final melting point 286.0℃ ℃) (final melting point of samples subject to test report). The heating rate 10 /min ℃ is selected, and the starting temperature is set 5 ℃ lower than the final melting point value. Repeat the test for five times as required. Delete the maximum and minimum values and the remaining three values are used as test results. Average the three values and the deviation value shall be within stipulated range.

6. Display Value Calibration:Enter calibration interface and use reference materials naphthalene, adipate and anthraquinone to calibrate the apparatus one by one. After test of the three substances, turn off the instrument and complete calibration.

Symptoms Causes Troubleshooting

Panel does not work when instrument is started.

Power is not supplied. Re-plug power plug or turn on the main switch.

Function of each operation unit fails.

Program-controlled heating system is damaged.

Return to the factory for repair.

Melting point tested is not accurate.

Position of platinum resistor changes; there is dirt in the core of the electrothermal furnace.

Reset and fix the platinum resistor. Clean the furnace core frequently.

Poor repeatability. Inconsistent sample filling. Capillary size different. Lower sample purity.

Make strict sample filling regulations. Select proper capillaries. Use high-purity sample and make sure the instrument is normal.


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VII. Supplement

The whole warranty lasts for one year from the date of product sale (starting from the date on invoice), but the following cases are not in warranty: 1. The date over warranty period;2. The damage caused by misuse;3. The damage caused by dismantlement without manufacture’s permission;4. The damage caused by improper transportation and storage.

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