Operation Manual SpeedExtractor E-916/E-914 093218 en
Table of contents Table of contents 1 2 3 4 5 3 About this manual...................................................................................................................7 1.1 Reference documents......................................................................................................7 1.2 Trademarks......................................................................................................................7 1.3 Abbreviations........................................
Table of contents 6 7 8 Operation...............................................................................................................................37 6.1 Method development.....................................................................................................37 6.2 Preparing the instrument................................................................................................38 6.2.1 Solvent reservoir..................................................................
Table of contents 9 8.2 Description of the service menu.....................................................................................85 8.2.1 Checking the valves.............................................................................................86 8.2.2 Checking the sensors..........................................................................................87 8.2.3 Running the pump...............................................................................................87 8.2.
Table of contents 6 SpeedExtractor E-916/E-914 Operation Manual, Version D
1 1 About this manual About this manual This manual describes the SpeedExtractor E-916/E-914 and provides all 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 are explained in chapter 2. 1.
1 1.
2 2 Safety Safety This chapter highlights the safety concept of the SpeedExtractor 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 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 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 supplementary. Notes are not related to any kind of hazard or damage.
2 2.5 Safety Product safety The SpeedExtractor has been designed and built in accordance with current state-of-the-art technology. Safety warnings in this manual (as described in section 2.4) serve to make the user alert to and avoid hazardous situations emanating from residual dangers by giving appropriate counter measures. However, risks to users, property and the environment can arise when the instrument is damaged, used carelessly or improperly. 2.5.
2 Safety NOTICE Risk of instrument damage by liquids or mechanical shocks. • • • • • • Do not spill liquids over the instrument or its components Do not move the instrument when it is loaded with sample liquid Do not drop the instrument or its components Keep external vibrations away from the instrument Safely attach the instrument to the bench in earthquake prone regions Do not operate the instrument without the safety shield installed NOTICE Risk of instrument damage by wrong mains supply. • • 2.5.
2 2.5.4 Safety Built-in safety elements and measures • The heating element is equipped with overtemperature protection which is activated at 260 °C ±10 °C. • The pressure parts are protected by a mechanical pressure control valve which is activated at 200 bar ±20 bar. • To start a program at least one extraction position must be activated. • Safety shield sensor: To start an extraction the protection shield must be closed. • Vial rack sensor: To start an extraction the vial rack must be installed.
2 2.6 Safety General safety rules Responsibility of the operator The head of the laboratory is responsible for training his/her personnel. The operator shall inform the manufacturer without delay of any safety-related incidents which might occur during operation of the instrument or its accessories. Legal regulations, such as local, state and federal laws applying to the instrument or its accessories must be strictly followed.
2 16 Safety SpeedExtractor E-916/E-914 Operation Manual, Version D
3 3 Technical data Technical data This chapter introduces the reader to the SpeedExtractor 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 and your shipping note. NOTE For detailed information on the listed products, see www.buchi.com or contact your local dealer. 3.
3 1 1 5 Technical data 1 Number of positions 4 E-914: 4 positions 5 E-914: 4 positions mounted on pedestal 6 E-916: 6 positions Size 01 02 04 08 12 of extraction cells 10 mL (E-916 only) 20 mL (E-916 only) 40 mL 80 mL (E-914 only) 120 mL (E-914 only) Number of solvent ports 2 Ports 4 Ports d c e f b a m g h i j n o p q k l t rs List of loose parts Position Item PU Universal a b c d e f g h i FEP tube D3.2/1.6, 5 m 2 11055604 FEP waste tube 1/16", 0.
3 Technical data d c e f b a m g h i n o k j p q l t rs List of loose parts Position Item PU Universal j k l m n o p p q q r s s t t Spanner wrench 1/4" 1 053204 Spanner wrench 8/10 mm 1 053608 Torx screwdriver TX20 1 053668 USB cable 2.0 A-B, 4.
3 3.3 Technical data Materials used Materials used 3.
3 Technical data Technical data of the SpeedExtractor Description Technical data Pressure range 50 – 150 bar Pressure accuracy ±5 bar Primary pressure nitrogen connection 6 – 10 bar Flow rate pump 1 – 50 mL/min Precision flow rate ±2 % Precision mixer ±2 % (±5 % for isopropanol) Extraction cell size E-916: 10, 20, 40 mL; E-914: 40, 80, 120 mL Environmental conditions For indoor use only Temperature 5 – 40 °C Altitude up to 2000 m Humidity maximum relative humidity 80 % for temperatu
3 22 Technical data SpeedExtractor E-916/E-914 Operation Manual, Version D
4 4 Description of function Description of function This chapter explains the basic principle of the SpeedExtractor E-916/E-914 and provides a functional description of the assemblies. 4.1 Functional principle The SpeedExtractor E-916/E-914 is an automated instrument for parallel extraction of primarily organic compounds from a variety of solid or semi-solid samples. Conventional methodologies are accelerated by using a solvent at elevated temperatures.
4 Description of function a Main power switch The instrument is protected by a 14 A (240 V) circuit breaker. The main fuse button at the rear of the instrument must be pushed in. b Solvent reservoir The maximum possible number of solvent bottles depends on the type of mixer. With the 2-port mixer up to 2 different solvents, with the 4-port mixer up to 4 different solvents can be connected allowing any user-defined solvent ratios.
4 4.3 Description of function Overview of the extraction process A complete extraction process involves the following phases: Phase 1: Preparation • Creating an extraction method (see section 6.2.3). • Preparing the instrument for operation. This involves filling the solvent reservoirs and preheating the instrument to the temperature of operation (equilibration), see section 6.2.3. • Packing the extraction cell with the sample (see section 6.2.3).
4 Description of function cells is absolutely mandatory. Placing the cells in the cold instrument followed by heating up the closed system might damage the cup seals. It is therefore crucial to note that the temperature of the instrument must not be changed once the system is closed. The instrument is ready once the set temperature is reached (which is shown in the main display) and the extraction process is started by pressing START.
4 N2 b a c f e d h j g i j k l Description of function a Solvent reservoirs (3 and 4 optional) b Nitrogen tank c Solvent valves d Mixer e Pump f Media valve g Divider h Overpressure valve i Position valves j Pressure sensors k Upper cup seals l Extraction cells m Lower cup seals n Cooling units o Outlet valve p Collection vials q Exhaust r Waste m n o r q p 4.5 Controls and connections 4.5.1 Instrument controls a b c e d 27 a Display to view the instrument software.
4 Description of function NOTE The START and STOP buttons are used only for the extraction method but have no effect on functions such as preheat, leak test, or flush. All functions apart from extractions are initiated by function buttons b. 4.5.
4 a b c d e f g h j i h g f b i j k l e c d o a n m a b c d a b c d e f 29 e Description of function a Current extraction cycle/total extraction cycles b Name of the current extraction method. When the name is crossed out (DEFAULT), the current method has been changed and not yet saved (see section 6.4.3). c Total remaining time of the extraction process. d Status: PREHEAT, READY, all methods steps, PAUSE, and ABORT.
4 a b c d e Description of function a Performing a LEAK TEST (see section 6.2.5). b Flushing the lines with solvent in collection vials or a waste bottle. Parameters like time, flow rate and solvent mixtures are defined in submenus (see section 6.2.6). c Defining instrument settings like language, contrast of the display, acoustic signals, preheat demand when the instrument is turned on. d SOLVENT LIST shows the default solvent list which includes the 10 most frequently used solvents.
4 4.5.3 Description of function General information on buttons The following control buttons are available in the software for navigation and input configuration: Open the extraction menu Open the menu functions like leak test, instrument settings etc.
4 4.5.4 Description of function Rear connections a Mains supply b Main fuse c RS232 port d USB 2.0 port e Exhaust outlet for purging with nitrogen, discharge and tightness test f Waste outlet for flushing with solvent or collecting extracts c d b a e f 4.5.
5 5 Putting into operation Putting into operation This chapter describes the installation of the SpeedExtractor and gives instructions on 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 transport company. Keep the original packaging for future transport. 5.1 Installation site Put the instrument on a stable, horizontal surface. Consider the maximum product dimensions and weight.
5 Putting into operation NOTE The instrument does not have to be operated under a fume hood but the exhaust must lead into some kind of ventilation device. Never hold the instrument on the collection rack or pump heads to move the instrument. Always use the handles on the side. 5.2 Electrical connections NOTICE Risk of instrument damage by wrong mains supply.
5 5.3 Putting into operation Gas and solvent connections • C onnect nitrogen gas by means of the provided hose. The corresponding joint contains a quicklock mechanism. The nitrogen gas connection is located on the right hand side panel. The required pressure range is 6 – 10 bar. This pressure has to be set at the external pressure reduction valve. • Connect the other end of the nitrogen line to a nitrogen tank by means of the provided 1/8” Swagelok brass nut and ferrule (P/N 11055342).
5 5.4 Putting into operation Dehydration NOTE At initial start-up or after a long period of no use (>1 month), the instrument should be dehydrated for proper operation. To do so, heat up the instrument to 100°C for 1 hour (heater open, no cells). Proceed as described in section 6.3.2. 5.5 Functional test To make sure that the installation procedure has been carried out properly and the system is tight, carry out a leak test (see section 6.2.
6 6 Operation Operation This chapter explains the operating elements and possible operating modes. It gives instructions on how to operate the SpeedExtractor properly and safely. The following table provides a quick overview of main step typically being involved in an extraction: Overview of main step typically being involved 6.1 Step Action Section 1 Create a new method with default operating parameters 6.4.3 2 Preheat the instrument 6.2.3 3 Activate the positions 6.2.
6 6.2 Operation Preparing the instrument This section involves all steps required to make the instrument ready for operation. ! 3 Death or serious poisoning by contact or incorporation of harmful substances at use. • • • • 6.2.
6 Operation Never use technical grade solvent. It is strongly recommended to use particle free solvents such as p.a. quality or HPLC grade solvent to guarantee proper operation of the valves, filters and frits. Filling the solvent reservoir: To prevent air from being drawn though the lines, insert the inlet line (approx. 1 m) equipped with an intake filter (P/N 044340) into the reservoir until the filter touches the bottom. N2 FILTER 6.2.
6 Operation Adding a new solvent: • To add new solvents to the list go to an empty position (e.g. no. 11) and press EDIT. The editing display is now empty. You can create your own names now using the selection knob. For example: An extraction is performed with chlorobenzene which does not belong to the standard list. Type CHLOROBENZENE as described above and press ACCEPT to add the name to the solvent list. Chlorobenzene now appears on position 011 on the solvent list.
6 Operation Setting the preheat temperature: • Go to EXTRACTION PREHEAT to open the preheat submenu. CURRENT METHOD indicates the temperature setting of the current method. Use COPY to copy this value in the preheat entry to heat up the instrument to the temperature for the next run. Alternatively, set a new temperature using the selection knob. Activating the ECO MODE: The ECO MODE automatically turns off the heater after the next extraction run.
6 Operation Activate all positions together: • Open EXTRACTION OCCUPIED POSITIONS. Confirm “Occupy all positions?” with YES. The main display shows all activated positions as numbered cylinders. Deactivate positions: • To activate only the four middle positions, activate all positions first and then deactivate the positions 1 and 6. Go to EXTRACTION OCCUPIED POSITIONS and this time negate with NO. All positions are deactivated now.
6 Operation Method-based leak test Open the method: • Go to EXTRACTION OPEN METHOD and select the requested method (e.g. PAH-01) and confirm with OK. The name of the selected method now appears in the main display. Copy the parameters into the leak test: • Open MENU LEAK TEST. The LEAK TEST menu consists of two columns. CURRENT METHOD includes all settings of the currently active extraction method (for instance PAH-01). SELECT shows the parameters of the last used leak test.
6 Operation Reference setting for a standardized leak test Description Value Temperature 100 °C Pressure 100 bar Solvent ethanol Hold time 4 min Extraction cell all volumes Expansion element, sand Expansion element 2–120 mL (refer to chapter 10) or sand • S et the reference settings: Open MENU LEAK TEST. Instead of copying the entries of the CURRENT METHOD, set the reference settings according to the table above. For the TEMPERATURE, set 100 °C using the selection knob. Press OK.
6 Operation If the leak test shows that the SpeedExtractor is not tight, check the following options. One or more positions have a lower pressure than the others: • The drain valve is open close the valve (see section 8.1.3) • The cup seals (bottom or top) are not tight anymore. The seals can be used for at least 100 extractions, if not damaged mechanically by sand, sample, etc. check visually, replace the faulty one (see section 7.2.2).
6 Operation mode when positions are deactivated. This allows a fast and efficient flushing when using a reduced number of positions. Flush into waste: • Open MENU FLUSH. Set the time to flush with solvent. FLUSH INTO makes it possible to choose between waste or vial. Choose WASTE using the selection knob. Set the flow rate and flush with gas according to the recommended parameter in the table above. The CURRENT row in the SOLVENT section shows the settings of the currently active method.
6 6.3 Operation Preparing the sample The following sections describe all operations being involved to prepare the sample for the actual extraction process. 6.3.1 Sample preparation To maximize extraction efficiency, samples that are coarse, lumpy or rocky must first be ground and/or sieved to achieve a uniform particle size. Conversely, fine mesh samples may form tightly compressed beds which restrict solvent penetration and impede solvent discharge.
6 6.3.2 Operation Extraction cell selection NOTE The process parameters are optimized to each type of extraction cell. Therefore, never mix extraction cells of different sizes in the same run. Different cell sizes in the same run result in inhomogeneous heat transfer. There are various extraction cell sizes available, depending on the number of positions (see adjacent table).
6 Operation Alternatively, use a paper or glass fiber thimble to fill in your sample. The thimbles are recommended for polymers and plastics (samples with tendency to melt during the extraction process) and sticky samples, when not mixed with sand or diatomaceous earth. They are specially recommended for the method development of the mentioned sample types. Glass fiber thimbles are beneficial for gravimetric and residue determinations (lower blank value than paper thimbles).
6 Operation C Keep the sealing surfaces clean Insert the upper cellulose g (P/N 049572 for E-916, P/N 051249 for E-914) or glass fiber filter (P/N 11057189 for E-916, P/N 11057190 for E-914) carefully uniformly into the cell using the plunger h. The top glass fiber filters are recommended for trace and ultra-trace analysis. Again, visually inspect the cell for remaining grains above the filter and make sure that the filter is in full lateral contact with the cell.
6 6.4 Operation Extraction process Each extraction procedure occurs according to a set of predefined operating parameters such as pressure, temperature, flow rates etc. which are all part of the extraction method. The SpeedExtractor can store up to 100 methods. The optional PC software SpeedExtractor Record allows to create and manage an unlimited number of methods.
6 Operation he heating block is fixed on movable guide rails. T This allows the operator to push the heating block to the back to get easy access to the cup seals (for inspection or exchange) and to pull it out to load the extraction cells. Proceed as follows: Push the protective shield to the top and pull out the heating block as far as possible. Use the extraction cell gripper (P/N 053030 for E-916, P/N 053026 for E-914) to place the cells into the heating block.
6 Operation to 1/3 and 2/3 of the final pressure. The HEAT UP time is defined as the time during which the pressure remains at 1/3 of the total pressure. A further prerequisite is that the temperature of the heating block reached its equilibrium. It is a method-dependent intrinsic parameter which depends mostly on the size of the extraction cell and is therefore not adjustable by the operator.
6 Operation Specify the vial volume: • Specification of the volume of the collection bottle is an important safety feature, since it alerts the operator if there is a conflict with the total volume used for the subsequently defined extraction volume. The volumes of the most frequently used bottles (60 mL, 150 mL, 220 mL and 240 mL) are predefined. If using other volumes than the mentioned ones, select “unspecified”. It is also possible to extract into the waste.
6 Operation Define the cycles: • Specify the number of cycles and go to the CYCLES submenu. The CYCLES submenu contains all cycles including their operating parameters such as HEATUP, HOLD and DISCHARGE time. There are only as many cycles shown as defined in NUMBER OF CYCLES. All other entries are not applicable (n/a). • To change parameters of a given cycle, move the cursor to the corresponding cycle and press EDIT.
6 Operation Save the method: • In order to save the modified new method, go to SAVE METHOD back in the EXTRACTION menu, select an empty position, and press OK. Alternatively, choose an already occupied position to overwrite it. Modify the name in the ENTER METHOD NAME window or write a new one by pressing DELETE. To type a name, choose the corresponding characters and press SELECT. Confirm the changes with ACCEPT.
6 Operation Operation parameters Parameter Function Value range TYPE Type of solvent in solvent reservoir 1 – 2 or 1 – 4 depending on the list of 20 solvents instrument configuration. (default: 10 solvents) RATIO Percentage of solvent 1 – 2 or 1 – 4 used to create the extraction method. The sum is always 100 %. 1 – 100 % sum: 100 % NUMBER OF CYCLES How many times the HEAT-UP, HOLD, and DISCHARGE steps are performed.
6 6.4.5 Operation Example of an extraction method Example: Extraction of 6×5 g sample in 10 mL extraction cells with acetone 50 % and DCM 50 %, 3×5 min at 80 °C and 100 bar. Procedure: • Connect the solvent reservoirs to the corresponding ports: a: acetone, b: DCM • Activate the extraction positions: EXTRACTION OCCUPIED POSITIONS YES. • Flush with solvent (optional): Insert empty extraction cells in all positions.
6 6.4.7 Operation Optimize a process The following guidelines may help to optimize an extraction process in terms of yield and time. Guidelines to optimize an extraction process Action Raising of the temperature In general, raising the temperature increases the yield of the extraction process. However, particularly for temperature sensitive compounds, it is advisable to keep this parameter rather low to prevent degradation.
6 6.4.8 Operation Start, pause, stop and abort extraction Use the green START and the red STOP buttons to start, pause, abort, or interrupt an extraction process. These buttons are only applicable to the extraction process. All other procedures such as flush or preheat are controlled by the function buttons (see also section 4.5.1). • Start: Go to the main display and press START once. The START button is only active in the main display. • Pause: Press STOP once.
6 Operation Cleaning the seals • If necessary, rinse the seals with organic solvent (e.g. ethanol) with the help of beaker. Always visually inspect the seals for dust, sand or scratches. NOTE Never clean the cup seals with a wet towel or wipe. Any kind of residue might cause a leak and/or reduce the lifetime of the cup seals. Cleaning the upper cup seal frit • In case of unexpected contamination, remove the top cover plate (position 4 on page 97) and clean it in an ultrasound bath.
6 62 Operation SpeedExtractor E-916/E-914 Operation Manual, Version D
7 7 Maintenance Maintenance This chapter provides instructions on all required maintenance 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 reconnecting the power supply NOTICE Risk of housing and instrument damage by liquids and detergents. • • • 7.
7 7.2 Periodic maintenance 7.2.1 Sealing system Maintenance The condition of the cup seals is crucial for the tightness of the system. Any kind of contamination on either the sealing surface of the extraction cell or the seal itself significantly reduces the lifetime of the seals. Therefore, always proceed as described in section 6.3.3 to fill the cell. Rinse the seals thoroughly with organic solvent (e.g. ethanol) with a wash bottle and a beaker to collect the solvent.
7 Maintenance Replacing the lower cup seals • To replace the lower cup seals, push in the heating block until it is locked in the back position. Unscrew the metal piece a manually and pull out the seal b. a NOTE In contrast to the upper cup seal, no tool is required for removal of the metal piece a. • Replace the old seal with a new one (P/N 053670) and proceed in reverse order to install the new seal. Screw the metal piece a hand tight.
7 Maintenance Exhaust connections A good indication for clogged needles or EXHAUST lines is a reproducible residual pressure of approx. 1 – 2 bar after each run. In this case the lift does not open and an error message appears (see section 8.1.2). Other evidence for possibly clogged needles or lines is a difference in receiving volumes after flushing the system (see section 6.2.6).
7 a Maintenance Needles The needles need to be replaced regularly (i.e. at least after every 6 months) to reduce the risk of clogging by particles of the septa or when they are bent. To do so, remove the covers a and b. Unscrew the needles with the wrench P/N 053204 and pull them out from the bottom. Needles are available as sets of 12, P/N 053675. Clogged needles can be cleaned with thin wire. b NOTE Make sure that the sloped sides of the two needles of one position always point away from each other.
7 7.3 Maintenance Pump maintenance d e f c Pump designations a Mixer outlet line b Pump inlet lines (left, right identical) c Pump heads d Pump outlet capillary left e Pump outlet capillary right f By-pass valve c b b a 7.3.1 Connections FEP tubings Use FEP tubing OD 1/8”, ID 1/16” for the mixer outlet and pump inlet lines. Make sure that the ferrule (P/N 053664) is flush with the end of the tubing.
7 7.3.2 Maintenance Back washing Back washing is an important maintenance procedure when not only pure and filtered solvents are used such as for example buffer solutions. The pump consists of two heads for alternate pumping and purging. They are both equipped with a Luer cone in the upper part, into which a plastic syringe (P/N 034882) can be inserted as shown in the picture. Both heads are equipped with piston seals (P/N 053612).
7 70 Maintenance SpeedExtractor E-916/E-914 Operation Manual, Version D
8 8 Troubleshooting Troubleshooting The following chapter 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 malfunctions and errors of the instrument and describes operator-enabled courses of action to correct some of those problems. The appropriate course of action is listed in the column “Remedy”.
8 Troubleshooting General malfunctions and their remedy Malfunction Display information Possible cause Remedy Error 6 Heater timeout. Temperature not achieved. Please refer to user manual. Temperature is not within ±3 °C of the set temperature after 60 min preheating time. Acknowledge the message and wait until the temperature is reached. If this occurs frequently, contact BUCHI customer service. The heater may have a problem. Error 7 Method not complete.
8 Troubleshooting General malfunctions and their remedy Malfunction Display information Possible cause Remedy Error 21 No power consumption of vial lift motor. Please refer to user manual. The motor is either disconnected Contact BUCHI customer service. or damaged. Errors related to pressure sensors or pressure in general. Error 22 Calibration of pressure sensor not successful. Please refer to user manual. A pressure sensor is defective. The defective pressure sensor needs to be replaced.
8 Troubleshooting General malfunctions and their remedy Malfunction Display information Possible cause Remedy Error 51 Pump pressure too high. Please refer to user manual. During Extraction Check the state of the media, position and outlet valve. Open the corresponding valve(s) in the SERVICE FUNCTIONS > VALVE menu. Calibrate the rotating valves (media and outlet valve) if necessary. The pump is purging against a closed system, i.e. a closed valve.
8 Troubleshooting General malfunctions and their remedy Malfunction Display information Possible cause Remedy Error 61 to error 64 Solvent valve X: Does not close. Please refer to user manual. The solvent valve X or connection to the valve is faulty and needs to be exchanged or repaired. Connect the solvent bottle to a different port (if possible) and manually select the new position in the menu EXTRACTION EDIT METHOD SOLVENT. Contact BUCHI customer service to exchange the defective parts.
8 8.1.3 Troubleshooting Handling and resolving blockages When a position gets clogged, the pressure is not relieved when the outlet valve opens and discharges the extract. As a result, the pressure remains high in this clogged position. This entails two problems: Firstly, there is a possible chance of cross contamination between the pressurized clogged position and the adjacent low pressure positions during the heat-up step of the subsequent cycle.
8 ! Troubleshooting CAUTION Risk of minor or moderate injuries by hot steam of solvent when opening the drain valve. • Use a towel or insulated gloves for protection There are three cases to distinguish depending of the pressure in the clogged position and the number of clogged positions. In the following paragraphs, the work flows of the different scenarios are explained with flow charts. Pressure <80 bar in clogged position (Errors 29 – 34, see section 8.1.
8 Troubleshooting Error 29 – 34 Position X clogged: press START to disable position or repeat to discharge no Repeat START Pressure released? Wobble position: position is disabled yes Extraction with other positions Extraction with all positions End: heater opens Error 42 A clogging occurred during extraction. Do you want to open the cell lift? Alternatively, relive the pressure manually.
8 Troubleshooting Error 35 – 40 Position X clogged: press repeat to discharge or relieve the pressure manually. no Repeat Control of pressure in STATUS Relieve pressure manually Error 35 – 40 Pressure released? yes repeat START No wobble position; position is deactivated.
8 Troubleshooting Error 41 Position X clogged: press repeat to discharge or relieve the pressure manually. Control of pressure in no STATUS Repeat Relieve pressure manually of all clogged positions Error 41 Pressure released? yes Extraction with all positions End: heater opens repeat START One position is deactivated, extraction of other positions continues Error 41 Error 29 – 34 No error Error 42 A clogging occured during extrantion.
8 8.1.4 Troubleshooting The pump is not aspirating properly NOTE When the pump is running but the solvent is not aspirated check first if the right solvent port is selected (see section 6.2.6). A new pump or a pump that has been out of operation for a long time may sometimes be difficult to start. The cause is a dried out solvent on the check valves and air bubbles stuck on the pumping mechanism. Both causes result in pressure fluctuations, or solvent intake fails completely.
8 8.1.5 Troubleshooting Replacement of check valves The principle of a check valve is a precise ball and seat located in a casing of PEEK material with stainless steel reinforcement. By a stream of liquid the ball is pressed down to the seat, thus creating a seal. With respect to high pressures in the pump, any minute impurity stuck on the surface of the ball or the seat causes pressure fluctuation, or the pump fails to start at all.
8 Troubleshooting Replacement of seals A damaged seal manifests itself in the form of pressure fluctuations, and drops of solvent begin to appear below the opening of the backwash head. Replacement of the seal is the same in both pumping blocks. • Carefully remove the purging head. • Remove the defective seal with a blunt object or by hand. • Insert the new seal and carefully put the purging head on the piston. • Put the pumping head on the piston. Tighten the four nuts on the pumping head.
8 8.1.7 Troubleshooting Malfunctions of the rotating valves The outlet and media valves are rotating valves with a defined start position. This reference point can get lost. In consequence, the extracts are transferred in wrong position (e.g. into waste instead of vials) for the outlet valve, or the solvent mixture at the media valve is misdirected to the nitrogen inlet instead of the divider. The rotating valves can be calibrated in the SERVICE menu. For this purpose, proceed as follows: Go to MENU.
8 8.2 Troubleshooting Description of the service menu The service menu provides direct access to all technical process components such as valves, sensors, pump, lift and fan independent of any extraction method. It is therefore possible to switch valves, run the pump or move the lift for troubleshooting purposes. In addition instrument information is available, like operating hours and version of certain components.
8 Troubleshooting Description of the service menu 8.2.1 Service function Description Typically used for: Lift (see 8.2.5) The lift for the heating block (cell lift) and the collection rack (vial lift) can be moved up and down. Light barriers show the corresponding position and the used current indicates possible blockage of the lift. To open the cell lift after manual draining of the extract in case of clogged cells. To check the proper interaction of the lift and light barriers. Fan (see 8.2.
8 8.2.2 Troubleshooting Checking the sensors Go to SERVICE FUNCTIONS SENSORS. The position of the lift for the heating block (CELL), the lift for the collection rack (VIAL), the heating block (HEATER), the protection shield (SHIELD), and the presence of the collection rack (RACK) is shown. Crossed brackets [X] indicate the present position. Press NEXT to enter the PRESSURE SENSORS submenu. The overall pressure between the media valve and the divider (indicated by PUMP; see section 4.
8 8.2.4 Troubleshooting Inspecting the lines (flow test) Go to SERVICE FUNCTIONS FLOW. Define the parameters using the selection knob. Press START to start with the flow test. • Place empty extraction cells (no sand, no expansion element, no plug screw) into the heating block and empty vials in the collection rack (see section 6.4.1). Close the cell and vial lift manually (see section 8.2.5). Use the same solvent as used during the extraction when the blockage occurred.
8 Troubleshooting Test 4: Heater in the back position, beaker underneath. If no pressure is built up, the blockage is located between lower seal holder and outlet valve. The following parts can be blocked: lower seal holder, cooling unit, capillary, outlet valve. These parts must be exchanged or cleaned by a service technician. A leak test must be carried out to ensure the tightness of the SpeedExtractor. If pressure builds up, the top cover plate or the parts up to the solvent valve are blocked.
8 8.2.5 Troubleshooting Moving the cell and vial lift Go to SERVICE FUNCTIONS LIFT. The position of the lift for the heating block (CELL) and the collection rack (VIAL) is shown by crossed brackets [X]. Select the CELL or VIAL lift using the selection knob and press UP or DOWN to move the lift. Press stop to STOP movement. The changes in the position are shown by light barriers (open [ ] or crossed [X] brackets). The current entry is an indication of possible blockage of the lift.
8 8.3 Troubleshooting Customer service Only authorized service personnel are allowed to perform repair work on the instrument. These persons have comprehensive technical training and knowledge of the possible dangers that can arise from the instrument. Contacts for official BUCHI customer service offices are provided on the BUCHI website at: www.buchi.com. If your instrument malfunctions or you have technical questions or application problems, please contact one of these offices.
8 92 Troubleshooting SpeedExtractor E-916/E-914 Operation Manual, Version D
9 9 Shutdown, storage, transport and disposal Shutdown, storage, transport and disposal This chapter instructs how to shut down and to pack the instrument for storage or transport. Specifications for storage and shipping conditions can also be found listed here. 9.1 Storage and transport Switch off the instrument and remove the power cord. To disassemble the SpeedExtractor follow the installation instructions in section 5 in reverse order.
9 9.2 Shutdown, storage, transport and disposal Disposal For instrument disposal in an environmentally friendly manner, a list of materials is given in chapter 3.3. This helps to ensure that the components can be separated and recycled correctly by a specialist for disposal. For disposal of liquids and consumables such as catalyst or acid, see data sheets of these chemicals. Follow valid regional and local laws concerning disposal. For help, please contact the local authorities.
9 9.3 Shutdown, storage, transport and disposal Health and safety clearance Health and Safety Clearance Declaration concerning safety, potential hazards and safe disposal of waste. For the safety and health of our staff, laws and regulations regarding the handling of dangerous goods, occupational health and safety regulations, safety at work laws and regulations regarding safe disposal of waste, e.g.
9 96 Shutdown, storage, transport and disposal SpeedExtractor E-916/E-914 Operation Manual, Version D
10 10 Spare parts Spare parts This chapter lists spare parts and optional extras, including all of the relevant order information for ordering from BUCHI. Always indicate the product designation and part number when ordering any spare parts. Use only genuine BUCHI consumables and spare parts for maintenance and repair, in order to ensure optimum system performance and reliability. Prior written permission of the manufacturer should be obtained before any modifications are made to the spare parts used.
10 Spare parts Accessories related to the standard collection unit Item 98 PU Order no. a Caps and septa for wide-necked vial, GL 45 thread 12 11056528 b Septa for wide-necked vials 12 053677 c Analyst vessel, 1.0 mL appendix, GL 45 thread 12 11056498 c Analyst vessel, 1.0 mL appendix, GL 45 thread, amber glass 12 11056910 d Analyst vessel, 0.3 mL appendix, GL 45 thread 12 11056499 d Analyst vessel, 0.
10 Accessories related to the flask collection unit (only for E-914) b Item a c Spare parts PU Order no. a Conversion kit for the flask collection unit 1 11056130 b Flask collection unit 1 11056043 c 500 mL round bottom flask with 29.2/32 flange 1 000434 d 250 mL round bottom flask with 29.2/32 flange 1 000433 d Accessories related to the SpeedExtractor E-914, mounted on the pedestal Item 99 PU Order no. a Flask collection unit for longer flasks, e.g.
10 Spare parts Accessories related to the Syncore® Analyst R-6 collection unit (only for E-914) Item b a PU Order no. a Conversion kit for R-6 collection unit 1 11058211 b Analyst R-6 collection unit 1 11058344 c R-6 vessel, 1.0 ml appendix 6 038569 d R-6 vessel, 0.3 ml appendix 6 038485 e Cover for R-6 vessels, PTFE 4 11058655 f Septa for cover for R-6 vessels, PTFE 100 11058656 Accessories related to waste/solvent bottles Item PU Order no.
10 Spare parts Accessories related to the extraction cell Item PU Order no.
10 Spare parts Disposables a b Item PU Order no. Weighing boat 250 053202 a Quartz sand, dried at 750°C 2.5 kg 037689 b Diatomaceous earth 1.0 kg 053201 Accessories related to tubing, fittings Item i j a h b g c d e f PU Order no. a Solvent inlet, exhaust tube, FEP, OD 1/8" 5m 11055604 a Waste outlet tube, FEP, OD 1/16", 0.
10 Spare parts PU Order no. 1 053610 Piston seal, black, PTFE 1 053612 Piston seal, white 1 11056588 Accessories related to the pump Item f Check valves f Further accessories Item a PU a 4 port solvent mixer* 053381 b Small cooling unit for viscous samples* 053682 *Technician required for installation. Pressure reference sensor b Order no.
10 Spare parts Accessories related with the process workflow evaporation to dryness Item PU Order no. 6 port parallel evaporator, Multivapor™ P-6 with inert membrane pump, 220–240 V 1 MP21199S22 6 port parallel evaporator, Multivapor™ P-6 with inert membrane pump, 100–120 V 1 MP22199S22 Sealing adapters for 60 mL vials 6 049692 Sealing adapters for 220 mL vials 6 049761 Sealing adapters for 240 mL vials 6 049716 Blank adapters 6 049729 Vacuum membrane pump (1.
10 Spare parts Tools Item a b c d e f g h i j PU Order no. a Bit wrench 1 052783 b Torx screwdriver TX20 1 053668 c Brush large 1 053257 d Brush small 1 053256 e Filter hook 1 053316 f Spanner wrench 8/10 mm 1 053608 g Spanner wrench ¼” 1 053204 h Allen wrench 3 mm 1 000610 i Turix wrench 1 044349 j Extruder rod 1 11055284 Documents Product Qty Order no. Product Qty Order no.
10 106 Spare parts SpeedExtractor E-916/E-914 Operation Manual, Version D
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.
