Operation Manual Extraction System B�811 096675 en
Table of contents Table of contents 1 2 3 4 3 About this manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 1.1 Reference documents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 1.2 Abbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 Safety . . . . . . . . . . . . . . . . . .
Table of contents 5 6 7 8 9 10 11 4 Putting into operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29 5.1 Installation site . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29 5.2 Electrical connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29 5.3 Mounting the glass parts . . . . . . . . . . . . . .
1 1 About this manual About this manual This manual describes the Extraction System B-811 and provides all information required for its safe operation and to maintain it in good working order. It is addressed to laboratory personnel 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 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. ATTENTION With the general “Read this” symbol, ATTENTIONs indicate the possibility of equipment damage, malfunctions or incorrect process results, if instructions are not followed. NOTE Useful tips for the easy operation of the instrument. 2.
2 2.5.2 Safety Other hazards WARNING Certain solvents in or in the vicinity of the Extraction System B-811 can form peroxides and/or are highly inflammable. • A lways be aware of the explosion risk when working with hazardous substances or with substances of unknown composition. • Always provide a good ventilation within or in the vicinity of the system. 2.5.
2 2.6 Safety General safety rules Responsibility of the operator The head of laboratory is responsible for training his personnel. The operator shall inform the manufacturer without delay of any safety-related incidents which might occur during operation of the instrument. Legal regulations, such as local, state and federal laws applying to the instrument must be strictly followed.
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.
3 Technical data Table 3-4: Standard/LSV accessories (cont.
3 Technical data Table 3-5: Mixed instrument accessories Product Order number 4 Condensers 36711 2 Extraction chambers 36710 2 Extraction chambers LSV 37902 2 Condensation tubes 37482 2 Condensation tubes LSV 37903 2 Sample holders 36559 2 Sample holders LSV 37904 1 Set of solvent beakers, 4 pieces 37276 1 Set of solvent beakers LSV, 4 pieces 38597 1 Set of glass sample tubes 37281 1 Set of glass sample tubes LSV 37563 2 Thimble holders 33 x 94 mm (part of set thimble holders 37279
3 Technical data Table 3-6: Standard/LSV/mixed instrument accessories Product Order number 1 Power cable Type CH 10010 Type Schuko 10016 Type GB 17835 Type USA 10020 Type AUS 17836 1 Operation Manual B-811 3.1.
3 Technical data Table 3-7: Optional accessories (cont.
3 Technical data Table 3-7: Optional accessories (cont.) Product Order number Order number B-811 Standard B-811 LSV Paper roll for Star printer 512 38684 Set of fluororubber seals (4 pieces) 42654 Quartz sand (0.3 - 0.9 mm), 2.5 kg 37689 Paper thimbles 25 x 100 mm (25 pieces) 18105 Paper thimbles 43 x 123 mm (25 pieces) 18106 Silicone tubes 6/9 04133 Silicone tube 12/14, 2 cm 04134 Angle 01992 LSV upgrade kit (Standard to LSV) 3.
3 Technical data Table 3-8: Technical data (cont.) 3.3 Extraction System B-811 Extraction System B-811 LSV variant Cooling water consumption 60 l / h 60 l / h 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 Instrument function There are several important components integrated into the B-811 extraction system which allow you to use the instrument for many kinds of applications in the area of solid-liquid extraction. 1. T he solvent and extract only come in contact with glass and PTFE.
4 4.2 Description of function Overview of the instrument 7 6 1 5 2 4 a Operating panel b Protective shield c Main power switch d Heating element 3 e Beakers f Extraction chamber g Condenser Fig. 4.1: Overview of the instrument 1 2 3 4 7 a Condenser b Glass sample tube c Upper heating element d Solvent beaker e Glass valve f Lower heating element g Optical sensor 5 6 Fig. 4.
4 4.3 Description of function The three steps in general The complete extraction process is set with the operating panel and follows a defined program. The process consists of three individual steps - Extraction, Rinsing and Drying – which runs automatically according to the parameters set in the program. 4.3.1 Extraction The sample is placed into the glass sample tube or thimble and put into the extraction chamber.
4 4.3.3 Description of function Drying After the rinsing process is completed, the glass valve closes while the lower heating is activated again. The solvent recovery is carried out. The solvent is evaporated, condensed at the condenser, and collected in the extraction chamber. At the end of drying the entire solvent is evaporated and collected in the extraction chamber to be eventually re-used. Fig. 4.5: Drying 4.4 The three steps in detail 4.4.
4 Description of function a Lower heating element activated 1 Fig. 4.6: Procedure of Soxhlet Standard Soxhlet Warm The method “Soxhlet Warm” follows a real Soxhlet extraction known from the glass apparatus. The extraction is carried out under enhanced conditions because the Soxhlet extraction chamber is additionally heated up. • T he solvent is heated up by the lower heating element and evaporated. The vapor rises up to the condenser.
4 Description of function Hot Extraction In case of a “Hot Extraction” the sample is placed in the boiling solvent and extracted. This method is also know as Randall or Goldfisch extraction. • T he solvent is heated up by the lower heating element and evaporated. The vapor rises up to the condenser. The condensed solvent flows down along the condensation tube into the extraction chamber with the sample inside. The condensed solvent is collected in the extraction chamber while the glass valve is closed.
4 Description of function a Lower heating element activated 1 Fig. 4.9: Procedure of Continuous Flow 4.4.2 Rinsing - Step 2 Once the extraction (step 1) is completed (time and/or number of cycles are reached), the glass valve opens on all positions and the solvent is released into the beaker. The solvent evaporates, rises up to the condenser, condenses and flows down along the condensation tube through the sample into the beaker.
4 Description of function completely evaporated, a few milliliters of solvent are automatically released into the beaker. Again, this solvent evaporates, a temperature increase on the heating element’s sensor is detected and again a few milliliters of solvent are released. This occurs three times. After the third solvent drain is happened, several milliliter of solvent remain in the beaker. Then the heating element is automatically turned off and the position stands in the wait mode.
4 4.5.2 Description of function Extractions with rinsing and without drying Step 1: Enter the parameters of step 1 according to table. Step 2: Enter lower heating level and rinsing time. Step 3 - 9: Set parameters to 0. Store program.
4 4.5.4 Description of function Extractions with rinsing and with drying Step 1: Enter parameters of step 1 according to table. Step 2: Enter lower heating level and rinsing time. Step 3-9: Enter lower heating and drying time for every further step. Store program.
4 4.
5 5 Putting into operation Putting into operation This chapter describes how the instrument is installed and gives instructions on the initial start-up. 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 NOTE We recommend to operate the instrument under a fume hood if e.g.
5 5.3 Mounting the glass parts 6 7 1 8 2 9 10 3 11 7 6 4 5 Fig. 5.1: Mounting the glass parts 5.4 Putting into operation 1. P lace the PTFE seal f into the holder ring g so that it clicks into place on both sides. 2. Screw both (upper and lower) holder rings g onto the extraction chamber i (¼ turn with slight pressure) until they click into place. Make sure that the Büchi logo is aligned to the vapor duct. 3. Screw the magnetic valve k onto the extraction chamber i. 4.
5 5.5 Putting into operation Connecting to tap water a Cooling water outlet b Nitrogen connection c Cooling water inlet Fig. 5.2: Rear view of the B-811 The water pressure may have a maximum of 6 bar (operating pressure 2 - 6 bar). The screw cap nut of the water connection has an R 1/2” standard thread. The counterpressure at the cooling water outlet may be at a maximum of 0.5 bar.
5 5.7 Connecting to a recirculating chiller 5.7.1 When is it recommended to work with a recirculating chiller? Putting into operation The temperature difference between the boiling point of the solvent and the cooling water temperature should be 20 - 25 °C to achieve a good condensation of the solvent in the condenser and to keep a good solvent recovery throughput during the extraction. When using solvents like dichloromethane or petroleum ether, a recirculating chiller (e.g.
5 5.7.2 Putting into operation Connection to the cooling water sensor 5 4 3 a Silicone tube from the left condenser (see Fig. 5.6) b Outlet to chiller inlet c Not used d Angle e Closed internal tube f Impeller water meter with cooling water sensor 6 1 2 Fig. 5.4: Connection to the cooling water sensor To connect the cooling water sensor proceed as follows: • • • • • 5.7.3 Turn off the B-811 and disconnect it from the power supply. Disconnect the back board.
5 5.7.4 Putting into operation Connection to the condensers 2 left 2 2 3 1 2 right 4 a Left condenser connection to impeller water meter and then to chiller inlet b Not used c Water connection between the condensers d Right condenser connection to chiller outlet Fig. 5.6: Connection to the condensers (rear view) To connect the condensers proceed as follows: • Untie the tubes b and fix them with cable binders. • Connect a silicone tube c (approx.
6 6 Operation Operation This chapter gives examples of typical instrument applications and instructions on how to operate the instrument properly and safely. WARNING Risk of injury • Never operate the instrument when glassware is damaged or when a heating element is broken. 6.1 Description of the function keys Function key Description START Starts the program currently in the program window. STOP in Standby mode 1x: T he extraction parameters can be changed.
6 6.2 Operation Preparing for an extraction To prepare the instrument for an extraction, proceed as follows: 1. Turn the condenser to the right and release it. 2. Press the stop key, the condensers move out. 3. Insert the glass sample tubes/thimbles into the sample holders. 4. Pull the condensers down with both hands (see Fig. 6.5) until they clicks into place. 5. Close the condenser by turning it to the left. 6. Set the height of the optical sensor (solvent must cover the sample). 7.
6 Function key Display Description Display H: MIN blinks Select the rinse time (0 to 99:99 h) using the / Operation keys The only stop criterion used for STEP 2 is the rinse time Display STEP 3 blinks (STEP 3 = Drying) Display HEATING blinks Select the heating level (1 - 20) using the Select level 4 for petroleum ether 40/60 Display H: MIN blinks Select the drying time (0 to 99:99 h) using the / keys / keys The only stop criterion used for STEP 3 is the drying time In case of oxygen-sensitiv
6 Function key Display Operation Description Display STEP 2 blinks (STEP 2 = Rinsing) Only the lower heating elements are activated Display HEATING blinks Select the heating level (1 - 20) using the Select level 13 for toluene / keys In case of oxygen-sensitive analytes, the gas supply must be activated by pressing the INERT GAS key The inert gas valve is automatically opened up while the step starts Display H: MIN blinks / Select the rinse time (0 to 99:99 h) using the keys The only stop crite
Function key Display Description Display H: MIN blinks Select the extraction time (0 - 99:99 h) using the 6 Operation / keys In the Hot Extraction Mode the only stop criterion used is the extraction time.
6 Function key Display Description Display HEATING blinks Select the heating level (1 - 20) using the Select level 9 for petroleum ether 40/60 / Operation keys In case of oxygen-sensitive analytes, the gas supply must be activated by pressing the INERT GAS key The inert gas valve is automatically opened up while the step starts Display H: MIN blinks / Select the rinse time (0 to 99:99 h) using the keys Display STEP 3 blinks (STEP 3 = Drying) Display HEATING blinks Select the heating level (1 -
6 6.8 Operation Printing Online documentation To keep an online log of an extraction, the B-811 must be connected to a printer. The extraction data are then printed out accordingly for each event that occurs.
6 6.9 Operation Optical sensor 1 cm 1 The optical sensor a detects the solvent level. In order to achieve the optimum extraction efficiency, the solvent level should be about 1 cm above the sample b. The solvent should cover the sample during the extraction process. 2 Fig. 6.3: Adjustment of the optical sensor 6.10 Handling the sample/sample holder The sample holder can handle paper thimbles of various sizes. The corresponding glass holders are listed in the accessories and spare parts list.
6 6.11 Operation Choosing the heating parameters The following heating parameters are recommended: Heating setting Heating setting Solvent BP / °C lower upper Acetone 56.1 11 3 Ethanol 78.4 16 4 Methanol 64.6 14 4 Xylol 139.5 15 10 Dichloromethane 39.9 9 2 Petroleum ether 40/60 40-60 9 2 n-Hexane 68.8 10 4 Toluene 110.6 13 6 Methylethylketone (MEK) 79.6 11 4 Water 20 10 100 If further heating parameters are required, please refer to the Application Note Nr.
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 All maintenance and repair work requiring the opening or removal of instrument covers may only be carried out by trained personnel and with the tools provided for this purpose. WARNING Electrical hazard: • P rior to all maintenance work on the instrument switch off the power supply and remove all sources of flammable vapor.
7 7.4 Maintenance and repairs Magnetic glass valve 6 4 a Cover cap b Glass valve c Valve housing d Anchor e Spring f Inductor coil 5 3 1 2 Fig. 7.1: Exploded view of the glass valve • • • • 7.5 Insert the spring e into the anchor d. Screw the valve housing c and the magnetic valve together f. Push the valve onto the glass part b. Screw the cover a on and tighten slightly.
7 7.7 Maintenance and repairs Holder ring with seal 1 a Holder ring b PTFE seal 2 Fig. 7.3: Holder ring with seal ATTENTION When removing and reinstalling the seals, make sure not to damage them. Never apply grease to the seals and never touch them with sharp objects, otherwise they will get damaged and cause solvent loss. To prolong the lifetime of the seals, rinse them regularly with distilled water or alcohol. Afterwards, dry them with a soft cloth. 7.
7 7.11 Maintenance and repairs Customer service Only authorised service personnel are allowed to perform repair work on the instrument. These persons have a comprehensive technical training and knowledge of possible dangers which might arise from the instrument. Addresses of official Buchi customer service offices are given on the Buchi website under: www.buchi.com. If malfunctions occur on your instrument or you have technical questions or application problems, contact one of these offices.
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”.
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, unplug the power cord, remove the cooling water, and remove all glass parts from the instrument.
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.
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BÜCHI Labortechnik AG CH-9230 Flawil 1 / Switzerland T +41 71 394 63 63 F +41 71 394 65 65 www.buchi.
