PLEASE READ THIS MANUAL CAREFULLY BEFORE OPERATION

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1 Hand Motion Shaker MPA-3 Operation Manual PLEASE READ THIS MANUAL CAREFULLY BEFORE OPERATION Hagavish st. Israel Tel: , Fax: mrc@mrclab.com MRC.12.16

2 Contents I. SUMMARY II.TECHNICAL SPECIFICATIONS III. STRUCTURE IV. OPERATION V. NOTICES VI. MAINTENANCE VII. SUPPLEMENT

3 Warning: The operator shall be clear that the protection function of the instrument may be weakened if the instrument is not used in the method required by the manufacturer. Warning: Please handle with care all kinds of solution used in accordance with laboratory safety instructions and consult relevant safety documents of corresponding substances. Make sure to wear lab coat, goggles and rubber gloves whenever you make a test. Please be careful not to be burnt while handling hot reagent. Warning: Risk of electric shock. Only professionals can open the instrument cover and panel.

4 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 the nature character of a substance, and is one of the important means to measure purity. Model MPA-3 Automatic Melting Point Apparatus adopts excellent ergonomic design, color LCD touching screen, photoelectric inspection and other advanced technology and can test simultaneously three different or identical samples. It has the functions of automatic initial temperature and final temperature display, automatic record of melting process curve and etc. Linear correction platinum resistor is employed for temperature system of the apparatus as its detection component and it is characterized by accuracy, high efficiency and convenience, and so on. Model MPA-3 Automatic Melting Point Apparatus is widely used in chemical industry and medical research and is one of the necessary instruments for drug, flavor, dye and other organic crystalline substance production

5 II. TECHNICAL SPECIFICATIONS Melting point range Initial temperature" setting rate 7 min( ) 7.5 min( ) Temperature resolution 0.1 Repeatability 0.2 at heating rate of 0.2 /min Temperature accuracy ±0.4 (<200 ),±0.7 (<300 ) Temperature gradients /min(default 0.1 /min, 50 classes) Standard capillary size I.D. 1.0mm, O.D. 1.4mm Capacity per batch 3pc./batch (3 different samples) Control & Display model LCD color touch screen Power supply 220VAC±10% 50Hz Power 300W Net weight 17kg Dimensions 523mmX332mmX216mm - 2 -

Figure 1 1. Indicator 2. Color LCD touching screen 3. Heating furnace 4. Heating furnace 5. Heating furnace 6. Power adapter 7.

6 III. STRUCTURE 1. Components Model MPA-3 is a melting point apparatus used for melting point measurement. The apparatus consists of setting, heating and testing systems. Structure of the instrument refers to the following figure (Figure 1). Figure 1 1. Indicator 2. Color LCD touching screen 3. Heating furnace 4. Heating furnace 5. Heating furnace 6. Power adapter 7. Power socket (with fuse in) 8. Power switch 9. Power output line 10. USB data interface 11. Cooling fan 12. Power input interface 13. Serial data interface 14. Furnace protective cover - 3 -

7 2. Functions 2.1 Welcome Interface When the instrument starts, a welcome screen as shown in Figure 2 Figure Function Interface After the instrument is started, it will automatically enter Function Interface, as shown in Figure 3. The function interface includes: Test, Data, Setting, Calibration and Help. Figure 3-4 -

8 2.3 Test Interface In Function Interface, click [Test] to enter sample-test select interface as shown in Figure 4. Users can select desired procedures to test the same samples or different samples. Figure Measurement of Same Samples Click [Same Sample] at sample test select interface and then click [OK] button to enter parameter setting interface for same sample test, as shown in Figure 5. Corresponding heating furnace can be selected and controlled by click the [Switch] under the numbers. If is displayed under the number, it indicates that the furnace is going to be put into work; and mark x indicates that the furnace will not be used. Click [Cancel] button to return to the previous interface. Figure 5 shows that No.2 Furnace will not be used this time

Figure 5 Click [Sample Name] in the test parameter setting interface to enter sample name setting interface as shown in Figure 6 for sample name setting.

9 Figure 5 Click [Sample Name] in the test parameter setting interface to enter sample name setting interface as shown in Figure 6 for sample name setting. For example, if the sample is named A1, just input A1 (at most six letters or numbers can be used for sample name) with the screen keyboard. Click [OK] to complete name setting, or [Del] to delete the sample name, or [Cancel] to return to the previous interface. Figure 6-6 -

Click [Preheating Temperature] in the [Test Parameter] interface to enter preheating temperature setting interface, as shown in Figure 7 to set preheating temperature (preheating temperature setting

10 Click [Preheating Temperature] in the [Test Parameter] interface to enter preheating temperature setting interface, as shown in Figure 7 to set preheating temperature (preheating temperature setting range 50 ~400 ) for the sample. If preheating temperature is 76.0, click the keyboard to enter 76.0 and then click [Enter] button and [OK] button to complete the setting. Figure 7 Click [Heating Rate] item in the test parameter interface to enter heating rate setting interface, as shown in Figure 8 to set heating rate (settable heating rate is 0.1 /min~ 5.0 /min). For example, if desired heating rate is 1.0 /min, click the keyboard to enter 1.0 and then click [Enter] button and [OK] button to complete the setting

11 Figure 8 Figure 9 After completion of test parameter settings, system will return to the main test interface as shown in Figure 9. Click [OK] button to enter an interface as shown in Figure 10 and heating furnace begins pre-heating process

12 Figure 10 Note: In the figure shown above, TT represents current temperature of the heating furnace; TP means set pre-heating temperature; RH indicates set heating rate, TA indicates initial melting value of sample and TC is the final melting value of sample. When the temperature in the heating furnace reaches preset heating temperature and becomes stable as shown in Figure 11, put the test sample in. Click [Heating] item to start sample test. The test program can be checked via the melting curve with temperature as its abscissa and transmittance as its ordinate, as shown in the figure. Click [Return] to terminate the test and return to setting interface. Figure

13 When the sample test process is completed, initial melting value and final melting value of each sample are displayed in the interface. If you are going to save the data, click [Save] item in the interface to save the data into data storage table. After the data are saved, it will automatically drop to the preheating temperature. When the temperature in the heating furnace is stable at preheating temperature, the apparatus will start the next test of the same samples. Click [Stop] to stop the test at any time and return to the preheating temperature automatically. When the temperature in the heating furnace is stable at preheating temperature, the apparatus will start the next test of the same samples Measurement for Different Samples Click [Different Sample] at sample test select interface and then click [OK] button to enter parameter setting interface for different sample test, as shown in Figure 12. Referring to the setting methods as parameter settings for the same sample, users can control working status, sample name, preheating temperature and heating rate of each heating furnace. Figure 12 And then click [OK] button to preheat the heating furnace and enter an interface as shown in Figure 13. Click [Cancel] button to return to the previous interface. When the real-time temperature of heating furnace reaches preheating temperature, click [Heating] and [Stop] buttons for separate control of test processes of the three samples. Sample measuring

process and data storage process refer to those for [Same Sample]. Figure 13 2.

Click [Page Up] and [Page Down] to check results of tested samples.

14 process and data storage process refer to those for [Same Sample]. Figure Data Inquiry In function interface, click [Data] button to enter data inquiry interface, as shown in Figure 14. Click [Page Up] and [Page Down] to check results of tested samples. Click [Return] button to return to the function interface. Figure Setting Interface In function interface, click [Setting] button to enter setting interface as shown in Figure

Click [Cancel] to abandon the setting data. Click [Return] to return to the setting interface.

15 Figure 15 Click [Clock] button in the setting interface to enter time-date setting interface as shown in Figure 16. Move cursor with left and right narrows and change numbers with + and buttons. Click [OK] button to save the settings. Click [Cancel] to abandon the setting data. Click [Return] to return to the setting interface. Figure 16 Click [Communication] in the setting interface to enter communication setting interface, as shown in Figure 17. Select in the interface the port to connect with PC and then click [Return] to return to the main setting interface

16 Figure 17 Click [System Parameter] button in the setting interface to enter system parameter setting interface, as shown in Figure 18. Figure 18 Click the number of heating furnace, you can set parameters of the selected one separately, as shown in Figure 19. Click [Actual Tem] as indicated in the interface, system will display real-time temperature of current heating furnace. Click [Final Melt Tem] button, you can set final melting temperature value with the help of the numeric keys in the interface. For example, for sample naphthalene, you can input 85 as its final melting temperature, and then

put naphthalene into the furnace and the heating furnace begins to heat the sample. Click [Transmittance] to display the transmittance value of the tested sample in the controlled heating furnace.

17 put naphthalene into the furnace and the heating furnace begins to heat the sample. Click [Transmittance] to display the transmittance value of the tested sample in the controlled heating furnace. When the transmittance value is stable, check if the sample is completely melted at the temperature. If the sample is melted, you can put sample in again till it reaches the maximum transmittance value. Click [Save Transmittance] to save current transmittance of the sample in the furnace chamber at final melting point. Click [Final Melt Per]. Use the numeric keys under it to set the instrument and determine transmittance percent at final melting point. Click [Initial Melt Per]. Use the numeric keys under it to set the instrument and determine transmittance percent at initial melting point. Figure 19 If the set parameters are to be saved, click [Save Setting] to complete the storage. If you want to resume factory settings, click [Restore Factory Settings] and enter an interface as shown in Figure 20. Click [OK] to resume factory parameter settings. Click [Cancel] to return to the previous interface

Apparatus can be calibrated with this interface.

18 Figure Calibration Interface In function interface, click [Calibration] button to enter calibration interface, as shown in Figure 21. Apparatus can be calibrated with this interface. Naphthalene, adipate and anthraquinone are used respectively as standard substances for melting point calibration. Set working status of heating furnace, melting point and preheating temperature of standard samples in this interface. Parameter setting method is the same as the one used for identical sample measurement. Figure

19 After setup of all the parameters in the interface as shown in Figure 22, click [OK] button to enter an interface as shown in Figure 23. The apparatus begins to preheat the furnace. When the heating furnace reaches the preheating temperature, put the standard sample in and click [Heating] button and the instrument begins melting point test on the standard sample. Figure 22 Figure 23 When the melting point of the standard sample is measured, click [Save] button to complete the first calibration. Take out the sample and click [Stop] button and wait the furnace to get to the preheating temperature and perform

7 Help Interface In function interface, click [Help] button to enter help interface as shown in Figure 24.

20 the second calibration of the sample. Calibrate three times on each sample. The standard sample is defaulted by the instrument. After calibration, the system displays OK. Take out the sample and start calibration on another type of standard sample with the same test procedures. 2.7 Help Interface In function interface, click [Help] button to enter help interface as shown in Figure 24. If you need to learn more about the use of the instrument, click [Operation Instruction] to enter instruction interface as Figure 25 and Figure 26 show. Click [Return] to return to function interface. Figure 24 Figure

21 Figure 26 IV. OPERATION 1. Capillary Sample Preparation Put test sample into agate mortar, pulverize and dry it. Take an 800mm long, dry and clean glass tube and stand it vertically on a magnetic plate or a glass plate. Put the capillary with test sample into the glass tube and make it fall freely. Repeat the free fall eight times till sample powder (about 4~5mm tall) gathers tightly at the bottom. 2. Melting Point Apparatus Test 2.1 Turn on the power switch and warm up the apparatus about 20 minutes. 2.2 Enter function interface and select Test. Set proper preheating temperature and heating rate. 2.3 Preheat the furnace after confirmation. When it reaches preheating temperature and is stable, put sample in and test. 2.4 When the test is completed, initial melting temperature and final melting temperature are displayed. Record or save test data and take out tested sample. Click [Stop] and wait till the real-time temperature gets to preheating temperature. Repeat testing sample of the same group

22 2.5 Click Return to return and enter parameter setting interface after test to re-set parameters, and then test the next group of samples. 3. Apparatus Calibration Test 3.1 Start the instrument and warm up 20 minutes. 3.2 Select [Calibration] to enter calibration interface. 3.3 Select the heating furnace to be calibrated and input melting point of standard sample, preheating temperature and heating rate. 3.4 Click [OK] and begin preheating. When it reaches preheating temperature and is stable, put sample in and click [Heating] for melting point measurement. 3.5 After the test, the instrument will display initial and final melting temperatures. Click [Save] button to complete the first melting point calibration. Take out the sample and click [Stop] button and wait the furnace to get to the preheating temperature and perform the second calibration of the sample. Calibrate three times on each sample. The standard sample is defaulted by the instrument. After calibration, the system displays OK. Take out the sample and start calibration on another type of standard sample with the same test procedures. V. NOTICES 1. Test sample shall be baked as required, pulverized in dry and clean mortar. Tap the capillary with free falling method till sample is filled in tightly. Height of sample in the capillary shall not be less than 3mm. Height of sample within the same batch number shall be consistent to ensure accordant test results. 2. Turn on the instrument and then set preheating temperature. When it gets close to the preheating temperature, put sample in and operate as instructions. 3. Starting temperature set shall not exceed operation range of the apparatus, or the instrument may be damaged

23 4. Starting temperature of some samples has great effect on melting point test results, please operate according to instructions. We suggest capillary shall be inserted 5 minutes ahead. If linear heating rate is selected as 1.0 /min, starting temperature shall be 3-5 lower than melting point; if heating rate is 3.0 /min, starting temperature shall be 9-15 lower than melting point. Usually optimum test conditions are determined according to specific test conditions 5. Different linear heating rates lead to different test results. Proper instructions and standards shall be worked out. Usually the higher the heating rate, the test result will be bigger than the actual value. Measured melting point value at each heating rate can be uniformed by test-modified values. 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. Select certain 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 several capillaries once a time to avoid accidental error caused by capillaries and filling in of test sample. Test them respectively and delete the maximum and minimum values. Take the average value of the remaining readings as test results. 8. Capillary inserted in the sample chamber must be clean and standard, or dirt will deposit and it is easy to damage the capillary, making test impossible. 9. Handle with care the instrument in use. Keep it away from acid and alkaline solution. Prevent it from use in strong light. Please do not touch sample chamber during heating process in case of being burnt. 10. Take care while putting in or taking out capillaries to prevent them from being broken. If a capillary is broken or damaged in the sample chamber, please turn off power supply, cool the instrument, and then take it out. Employ a capillary pulverizer to mix the broken capillary. 11. If the instrument may not be used for a long time, please disconnect power cable

24 V. MAINTENANCE 1. Instrument shall be used in dry and ventilated rooms. Prevent it from water 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. Capillary used by the instrument must be supplied by the Company. No manually drawn capillary can be used instead, in case it is too tight and may break. Fine capillaries shall be selected for test purpose. 3. If a capillary is broken in the sample chamber, please first turn off power supply, and cool the furnace, then pull out the tube seat. The tube seat shall be pulled out like this: one hand holds the heating 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 components of the instrument. Then use a capillary pulverizer 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 furnace. Check the entire instrument after that 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, or cooling fan does not work, or heating furnace does not heat, please shut off power supply and check if the fuse on the power socket of power adapter is burnt, and replace it in time. 5. Accuracy test: Accuracy test is performed according to rules stipulated by GBW13238 Melting Point Certified Reference Materials (1989, No.335) approved by State Bureau of Technical Supervision. The apparatus uses three of the reference materials: naphthalene (final melting point ), adipate (final melting point ) and anthraquinone (final melting point ), as examination standard (final melting point of sample subject to test report). 1.0 /min heating rate is selected, and starting temperature is set 5 higher than final melting point value. Repeat the test for five times as required. Delete the maximum and minimum values and the remaining three

25 values are used as test results. Average the three values and the deviation value shall be within stipulated range. 6. Instrument Calibration: Enter calibration interface and use reference material naphthalene, adipate and anthraquinone to calibrate the apparatus one by one. After test of the three substances, turn off the instrument and complete calibration. VII. SUPPLEMENT Symptoms Causes Troubleshooting Panel does not work when instrument is started. Function of each operation unit fails. Melting point tested is not accurate. Poor repeatability. Power is not supplied. Program-controlled heating system is damaged. Position of platinum resistor changes. There is dirt in the sample chamber. Inconsistent sample filling. Sizes of capillaries are different. Low sample purity. Re-plug power plug or turn on the main switch. Return to the factory for repair. Reset and fix the platinum resistor. Clean the sample chamber frequently. Make sample filling strictly as per instructions. Use high-purity sample and make sure the instrument is normal

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