Operation Manual Extraction Unit E�812/816 SOX 093169 en
Table of contents Table of contents 1 2 3 4 5 3 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 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .27 6.1 Main screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27 6.2 General information on buttons . . . . . . . . . . . . . . . . . . . . . . . . . . . . .28 6.3 Description of the menu functions . . . . . . . . . . . .
1 1 About this manual About this manual This manual describes the Extraction Unit E-812/816 SOX and provides all information required for its safe operation and to maintain it in good working order. It is addressed to laboratory personnel and operators in particular. Read this manual carefully before installing and running your system and note the safety precautions in section 2 in particular. Store the manual in the immediate vicinity of the instrument, so that it can be consulted at any time.
2 2 Safety Safety This chapter points out the safety concept of the instrument and contains general rules of behavior and warnings from hazards concerning the use of the product. The safety of users and personnel can only be ensured if these safety instructions and the safetyrelated warnings in the individual chapters 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 Safety warnings and safety signs used in this manual DANGER, WARNING, CAUTION and NOTICE are standardized signal words for identifying levels of hazard seriousness of risks related to personal injury and property damage. All signal words, which are related to personal injury are accompanied by the general safety sign.
2 Symbol Safety Meaning Harmful to life-forms Pinch point, mechanical hazards Fire hazard Hot item, hot surface Device damage Inhalation of substances Chemical burns by corrosives Wear laboratory coat Wear protective goggles Wear protective gloves Heavy weight, lifting requires more than one person Additional user information Paragraphs starting with Note transport helpful information for working with the device / software or its supplementaries.
2 Safety NOTE Useful tips for the easy operation of the instrument / software. 2.5 Product safety The Extraction Unit is designed and built in accordance with state-of-the-art technology. Nevertheless, risks to users, property, and the environment can arise when the instrument is used carelessly or improperly. The manufacturer has determined residual dangers emanating from the instrument • if the instrument is operated by insufficiently trained personnel.
2 Safety NOTICE Risk of instrument damage by wrong mains supply. • • 2.5.2 External mains supply must meet the voltage given on the type plate Check for sufficient grounding Warning labels on housing and assemblies The following warning sticker(s) can be found on the housing or assemblies of the instrument: Symbol 2.5.
2 2.5.4 Safety Safety elements Electronics • The heating element is equipped with an electronic over-temperature protection. • If no cooling water is detected at the cooling water output (for example, due to a leak in the condenser), the electronic over-protection will stop all processes. • To start a program at least one extraction position must be activated in the software.
3 3 Technical data Technical data This chapter introduces the reader to the instrument specifications. It contains the scope of delivery, 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 3.1.2 Technical data Standard accessories Table 3-2: Standard accessories 1 2 3 13 E-812 E-816 1 1 Beaker pliers, 50 mm a 02004 1 1 Pliers for glass sample tubes with frit b 47609 1 1 Turix wrench c 44349 5 5 Hose clamp, Ø 10.
3 Technical data Table 3-2: Standard accessories (cont.
3 Technical data Table 3-2: Standard accessories (cont.) 3 1 4 5 2 E-812 E-816 2 2 Knurled screw (for solvent hose) a 43237 2 2 Clamping ring (for solvent hose) a 43238 5 5 Hose clamp, Ø 9.6 mm b 27738 2 2 Hose, silicone, Ø 6/9 L = 1.5 m c 43940 2 2 Condenser connection hose, silicone, L = 0.35 m, mounted 49161 1 5 Condenser hose, silicone, L = 0.
3 3.1.
3 3.2 Technical data Technical data overview Table 3-4: Technical data 3.3 Extraction Unit E-812 Soxhlet Extraction Unit E-816 Soxhlet Dimensions (L x H x D) 275 x 776 x 456 mm 635 x 776 x 456 mm Connection voltage 100 - 120 VAC / 200 - 240 VAC ± 10%, 50/60 Hz 100 - 120 VAC / 200 - 240 VAC ± 10%, 50/60 Hz Power consumption max. 700/1200 W max.
4 4 Description of function Description of function This chapter explains the basic principle of the instrument, shows how it is structured and gives a functional description of the assemblies. 4.1 Overview over the instrument 1 2 3 4 5 6 a Condensers b Protective shield c Soxhlet extraction chambers with sample tube d Beaker e Heating plate f Operating panel Fig. 4.
4 4.2 Description of function Functional principle of a Soxhlet extraction The Extraction Unit E-812/816 Soxhlet is designed to extract fat quickly and product-friendly from food and feed. Thereby the sample is extracted in running cycles. The extraction process consists of 3 steps decribed in the following. 1 1 2 3 4 5 6 7 a Cooling water b Receiving funnel c Solvent tank connection d Optical sensor e Soxhlet extraction chamber with glass sample tube f Magnetic glass valve g Beaker Fig. 4.
4 4.2.2 Description of function Step 2 - rinsing The glass valve is open. The condensed solvent flows into the receiving funnel, drops down into the extraction chamber and flows back into the beaker. When the programmed rinsing time is over, the system goes to the next step. 4.2.3 Step 3 - drying The tank valve is open and removes the solvent. In the end the extract is dried as much as possible. The glass valve is still open. 4.2.
5 5 Putting into operation Putting into operation This chapter describes how the instrument is installed and gives instructions on initial startup. NOTE Inspect the instrument for damages during unpacking. If necessary, prepare a status report immediately to inform the postal company, railway company or transportation company. Keep the original packaging for future transportation. 5.1 Installation site Put the instrument on a stable, horizontal surface.
5 5.2 Putting into operation Electrical connections NOTE External connections and extension lines must be provided with a grounded conductor lead (3-pole couplings, cord or plug equipment). All used power cords must meet the input power requirements. NOTICE Risk of instrument damage by wrong mains supply. • • 5.
5 5.4 Putting into operation Soxhlet extractor a b c d e Fig. 5.2: Adjusting the Soxhlet chambers To adjust the Soxhlet chambers, proceed as follows: 1. 2. 3. 4. 5. 6. 7. Move the rack up. Pull the tray out. Remove the safety shield by loosing the screws on the side of the instrument. Remove the sealing holder from the extraction chambers. Fix the magnet valve at the glass valve of the extraction chamber (b). Connect the magnetic valve cable to the instrument (a).
5 5.6 Putting into operation Cooling water connection Connect the cooling water to the cooling water input a. The cooling water hose has to be secured on both the instrument and the water connection side by means of hose clamps. The water pressure should have a maximum of 4 bar. The built in valve reduces the water flow to 1.2 liters per minute. The flanged screw coupling for the water connection has a standard screw thread of G 3/4“. a Cooling water input b Cooling water output 1 2 Fig. 5.
5 5.7 Cooling medium connection 5.7.1 Recirculating Chiller B-740/41 or equivalent model Putting into operation When you operate with a BUCHI Recirculating Chiller B-740/41 or an equivalent model of another manufacturer, use the adapter (see figure below) to connect the water input to the chiller output. Make sure, that the axial seal is inserted. A temperature of 10 °C is recommended. • Adapter 5.7.
5 5.8 Putting into operation Solvent hose connection Fix the solvent hose to the solvent connection on the left of the instrument by pushing it on the connector and tightening the knurled screw. Fig. 5.6: Solvent hose connection The solvent hose consists of two parts, a transparent Tygon hose (with FEP veneer) and a white PTFE hose. The PTFE hose is solvent resistant, thus it has to be inserted into the Tygon hose. NOTE Only the PTFE hose must come into contact with solvent, see picture below.
6 6 Operation Operation This chapter gives examples of typical instrument applications and instructions on how to operate the instrument properly and safely. 6.
6 6.
6 6.3 Description of the menu functions 6.3.1 Starting up the instrument Operation Make sure, that the instrument is correctly connected to the mains supply and the cooling water. Then switch on the instrument at the main switch. The main screen appears: Fig. 6.1: Main screen 6.3.2 Instrument settings To define the instrument settings, press the Menu button. The following screen opens: Fig. 6.2: Menu Select instrument settings and press the forward button. Fig. 6.
6 Operation You can now change the settings by turning the selection knob and pressing OK to confirm. Press the move up or move down button to switch between the settings. When the Beep key function is on, a beep sound is audible whenever a key is pressed. When the Beep end function is on a beep sound is audible when the extraction process is finished. Max. cycle time: If a cycle is not reached after this time, an error message apears. Standard setting: 30 min.
6 6.3.4 Operation Defining a method In the main menu select Program. The following screen opens: Fig. 6.6: Extraction solvent You can now select the desired solvent by turning the selection knob. NOTE The Extraction Unit is only tested with the solvents petroleum ether, diethyl ether, chloroform and hexane. The use of other solvents can be done by choosing “Custom” but is on the risk of the user. Please check chemical resistance of all parts in contact with the solvent prior to use.
6 Operation Fig. 6.8: Rinse step Set the rinse time by means of the selection knob and press OK to confirm it. NOTE We recommend to use the default heater setting of 100% for general extraction purposes. Press Next to continue with the drying step. Fig. 6.9: Drying step Set the drying time by means of the selection knob and press OK to confirm it. NOTE We recommend to use the default heater setting of 100% for general extraction purposes. Your method is now created. Press End to get back to the menu.
6 6.3.5 Operation Saving a method Define a method according to the chapter “Defining a method” and save it as follows: In the main menu select File. Fig. 6.10: Main screen Press the forward button to get to the submenu File. Fig. 6.11: File Press the forward button to enter a name for your new method. Fig. 6.12: Enter name Use the selection knob to select the letters for the name and press Enter each time. To delete a letter, select BACKSPACE and then Enter.
6 Operation NOTE To overwrite an existing method, select Used and press OK. To carry out minor changes in the method name, select Used, select the name you want to change, carry out the changes and press OK. 6.3.6 Opening a method In the File submenu go to Open. Fig. 6.13: File Select the method you want to open with the selection knob and press OK. The method now appears on the main screen ready for carrying out a corresponding extraction process. Fig. 6.
6 6.3.7 Operation Deleting a method In the File submenu go to Delete. Fig. 6.15: File Select the method you want to open with the selection knob and press OK. A message appears asking you whether you really want to delete this program. Press Yes to confirm and the backward button to get back to the main menu. 6.3.8 Abort function It is possible to abort a specific position during an extraction process. For all other positions the extraction is continued. For this purpose, press Abort.
6 6.3.9 Operation Skip function During the extraction process it is possible to skip one step and go directly to the next step, e.g. from the extraction step to the rinse step. For this purpose, press Skip and confirm the appearing message by pressing Yes. Fig. 6.17: Skip 6.3.10 Service functions In the main menu the submenu Service functions is available.
6 Operation Fig. 6.19: Service functions Heater testing Select Heater temperatures. Fig. 6.20: Heater temperatures Here you get an overview over the current temperatures at the individual heating positions. NOTE The indicated temperature is the temperature within the heating element, not on top of the heating plate. To get back to the Service functions press the backward button.
6 Operation Valve testing Select Valve testing. The following screen opens: Fig. 6.21: Valve testing You can now test the functioning of the three valves by changing their status. For this purpose, select a valve and press Open or Close. You will hear a corresponding sound and see a corresponding reaction, depending on your setup. NOTE Close all valves before you leave this submenu, otherwise it is not possible to start an extraction.
6 Operation • Pos. up: [ ] Pos. down [ ]: Rack is down • Pos. up: [ ] Pos. down [X]: Rack is in between To get back to the Service functions press the backward button. Operating hours Select operating hours. The following screen opens: Fig. 6.24: Operating hours - 1 Here you see the operating hours of each heating position. To see the second page press Next. The following screen appears: Fig. 6.
6 Operation Unit information Select unit information. The following screen opens: Fig. 6.26: Unit information Here you get a short overview over technical instrument data. 6.4 Example of an extraction process 6.4.1 Material and equipment Before starting an extraction process all necessary materials and chemicals must be present: • • • • • • • • • • • Fume hood (only when working with diethyl ether or chloroform) Cooling water connection Analytical balance (± 0.
6 Operation 6. Place the beakers on the corresponding positions directly on the heating plate. 7. Lower the rack. 8. Activate the occupied positions. 9. Select a previous program or enter a new one. 10.Open the cooling water flow or switch on the connected chiller. 11.Start the extraction process. 6.4.3 After the extraction process The end of an extraction process is indicated on the display and audible by a beep sound (if selected in the instrument settings).
7 7 Maintenance and repairs Maintenance This chapter gives instructions on all maintenance work to be performed in order to keep the instrument in good working condition. ! WARNING Death or serious burns by electric current at cleaning. • • • Switch off the instrument Disconnect the power cord and prevent unintentional restart Wait until the instrument is completely dry before reconneting to mains NOTICE Risk of housing and instrument damage by liquids and detergents. • • • 7.
7 7.1.4 Maintenance and repairs Solvent tank Empty the solvent tank after each extraction process. The solvent in the tank can be reused when the extraction process was normal. In case of an incident during the extraction, the solvent can be cleaned e.g. in a rotary evaporator.
7 7.2 Weekly maintenance 7.2.1 Heating elements Maintenance and repairs The ceramic heating plates should be cleaned regularly after they have cooled down. Remove dirt adhering to the plate with e.g. ethanol. Then clean the plate with a moist cloth and dry it. 7.3 Monthly maintenance 7.3.1 Cleaning the seals NOTE When replacing the seals, take care not to damage them. To avoid damaging the seals, never apply grease and never touch them with sharp objects.
7 Maintenance and repairs Fig. 7.3: Replacing the seals on the beakers 7.3.3 Condenser Unscrew the condenser connections, remove the condenser and place it in a laboratory dish washer for cleaning with a conventional agent. Use an appropriate cleaner to remove possible contaminations adhering to the condenser spiral, e.g. algae. Let the spiral soak for a while. NOTE To remove the condensers moisten the seal with water. 7.3.
8 8 Troubleshooting Troubleshooting This chapter helps to resume operation after a minor problem has occurred with the instrument. It lists possible occurrences, their probable cause and suggests how to remedy the problem. The troubleshooting table below lists possible malfunctions and errors of the instrument. The operator is enabled to correct some of those problems or errors by him/herself. For this, appropriate corrective measures are listed in the column “Corrective measure”.
8 Troubleshooting Table 8-1: General malfunctions and their remedy (cont.) 8.2 Malfunction Possible cause Corrective measure Empty solvent tank not possible Software breakdown Retry to empty the solvent tank. If this does not work, manually empty the tank by opening the emergency opening Error messages NOTE In the following table X refers to the position in the instrument starting from left to right.
8 8.3 Troubleshooting Too high/too low results There are many reasons for too high or too low results even though the extraction process ran without problems. The most important reasons are listed in the following: Results too high • • • • Work with clean and dry hands and material (weighing and sample preparation). Dry the beakers completely after extraction until a constant weight is reached. Use clean and pure solvent.
9 9 Shutdown, storage, transport and disposal Shutdown, storage, transport and disposal This chapter instructs how to shut down the instrument, how to pack it for storage or transport, and specifies the storage and shipping conditions. 9.1 Preparing the instrument for storage and transport To prepare the instrument for storage and transport, lower the rack, unplug the power cord, remove the cooling water, and remove all glass parts from the instrument.
9 ! Shutdown, storage, transport and disposal CAUTION Risk of minor or moderate injury by heavy weight of the instrument. • • • • 9.3 Consult three further persons to transport the instrument Do not drop the instrument or its transport box Place the instrument on a stable, even and vibration-free surface Keep limbs out of crushing zone Disposal To dispose of the instrument in an environmentally friendly manner, a list of materials is given in chapter 3.
10 10 Spare parts Spare parts This chapter lists spare parts, accessories, and options including their ordering information. Order the spare parts from BUCHI. Always state the product designation and the part number when ordering spare parts. Use only genuine BUCHI consumables and genuine spare parts for maintenance and repair to assure good system performance and reliability. Any modifications to the spare parts used are only allowed with the prior written permission of the manufacturer.
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.
