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Buchi SpeedExtractor E-914, Operation Manual

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Buchi SpeedExtractor E-914 Operation Manual Download Page 7

1  About this manual

6

SpeedExtractor E-916 / E-916XL / E-914 Operation Manual

1.3 

Abbreviations

Process-related
ASE 

Accelerated Solvent Extraction

PSE 

Pressurized Solvent Extraction

Materials and chemicals
FEP 

Combination of tetrafluoroethylene and hexafluoropropylene

FFPM 

Perfluoro caoutchouc

PTFE Polytetrafluoroethylene
POM 

Polyoxymethylene (commercialized as Delrin® by DuPont)

PEEK 

Polyether ether ketone

THF Tetrahydrofurane

Miscellaneous
FW 

firm ware

qty quantity

D

T 

Temperature difference

D

p 

Pressure difference

Summary of Contents for SpeedExtractor E-914

Page 1: ...SpeedExtractor E 916 E 916XL E 914 Operation Manual 093218G en...

Page 2: ...reserves the right to make changes to the manual as deemed necessary in the light of experience espe cially in respect to structure illustrations and technical detail This manual is copyright Informat...

Page 3: ...6 General safety rules 13 3 Technical data 15 3 1 Scope of delivery 15 3 2 Instrument configurations 15 3 3 Materials used 18 3 4 Technical data overview 18 4 Description of function 21 4 1 Functional...

Page 4: ...ameters 54 6 4 5 Example of an extraction method 56 6 4 6 Open an existing method 56 6 4 7 Optimize a process 57 6 4 8 Start pause stop and abort extraction 58 6 4 9 Post extraction procedures 58 6 5...

Page 5: ...onent with the aid of this manual without prior written agreement is also prohibited The English manual is the original language version and serves as basis for all translations into other languages I...

Page 6: ...refer to the corresponding manuals Complementary devices MultivaporP 6 P 12 OperationManual VacuumController OperationManual Vacuum Pump Operation Manual Syncore Platform Operation Manual SyncoreAcces...

Page 7: ...d Solvent Extraction Materials and chemicals FEP Combination of tetrafluoroethylene and hexafluoropropylene FFPM Perfluoro caoutchouc PTFE Polytetrafluoroethylene POM Polyoxymethylene commercialized a...

Page 8: ...a basis for instruction 2 2 Proper use The instrument has been designed and built for laboratory use only It serves for activities associated with the parallel extraction of multiple samples by means...

Page 9: ...ussituationwhich ifnotavoided couldresult in death or serious injury CAUTION Indicatesahazardoussituationwhich ifnotavoided mayresult in minor or moderate injury no NOTICE Indicates possible property...

Page 10: ...r 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 informat...

Page 11: ...ditional warning messages can be found whenever actions and situations described in this manual are related to situational hazards WARNING Death or serious injuries by formation of explosive atmospher...

Page 12: ...late Check for sufficient grounding 2 5 2 Warning labels on housing and assemblies The following warning sticker s can be found on the housing or assemblies of the SpeedExtractor Symbol Meaning Locati...

Page 13: ...ar 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...

Page 14: ...nsible for the proper condition of instrument This includes maintenance service and repair jobs that are performed on schedule by authorized personnel only Spare parts to be used Use only genuine cons...

Page 15: ...2 Safety 14 SpeedExtractor E 916 E 916XL E 914 Operation Manual...

Page 16: ...rmation on the listed products see www buchi com or contact your local dealer 3 2 Instrument configurations The SpeedExtractor is available in 21 different configurations differing in the number of po...

Page 17: ...e Extraction Record demo license 1 053074 f Extraction cell carrier 1 053691 053690 11069547 g Solvent filter 4 044340 h Turix wrench 1 044349 Number of positions 1 1 5 1 Size of extraction cells Numb...

Page 18: ...63 p Cup seals bottom 12 053670 q Cellulose filter top 100 051249 049572 11069533 q Glass fiber filter bottom 100 11055932 r Swagelok nut and ferrules 1 8 1 11055342 s UNF 28 Fitting 1 8 green 10 0536...

Page 19: ...ve PEEK FFPM Mixer PEEK FFPM Media valve PEEK PTFE Lines to and from heating block Stainless steel Pressure gauges Stainless steel Position valves Stainless steel PTFE Outlet valves PEEK PTFE Heating...

Page 20: ...y II Degree of protection IP21 Pollution degree 2 Temperature control range 30 200 C Temperature accuracy 3 C Pressure range 50 150 bar Pressure accuracy 5 bar Primary pressure nitrogen connection 6 1...

Page 21: ...3 Technical data 20 SpeedExtractor E 916 E 916XL E 914 Operation Manual...

Page 22: ...rated in parallel using the Multivapor P 6 or Syncore Analyst R 12 Hence the whole process workflow can be performed in parallel with up to 6 samples The SpeedExtractor E 916 can be used for 6 samples...

Page 23: ...are loaded into the collection unit After extraction the extracts containing the analytes are collected in these bottles Different collection units and adapters are available to accom modate small via...

Page 24: ...the outlet valve opens and the liquid extract is DISCHARGEd and collected in collection vials or a waste bottle by means of pressure compensa tion All three steps are repeated several times according...

Page 25: ...vides a schematic representation of the pathways of the different media for the E 916 Up to four different solvents a and nitrogen b are connected to the E 916 A media valve f switches between solvent...

Page 26: ...aste 4 5 Controls and connections 4 5 1 Instrument controls a b c d e a Display to view the instrument software b Function buttons to operate the instrument soft ware c START button to start an extrac...

Page 27: ...function buttons the three main displays STATUS EXTRACTION and MENU are accessible B STATUS shows a diagram of the lines valves solvent reservoirs extraction cells and collection vials of the instrume...

Page 28: ...er e Pump f Media valve g Overall pressure sensor h Divider i Position valves j Pressure sensors for each extraction position k Extraction cells E 916 6 pos E 914 4 pos l Outlet valve Discharging into...

Page 29: ...ain instrument components for first quick trouble shooting purposes All valves can individually be opened or closed All safety sensors which check the position of the heating block safety shield or co...

Page 30: ...creen message Negate a screen message Switch on the position or function Switch off the position of function Switch on all extraction positions Copy the entry of currently active parameter of the extr...

Page 31: ...in 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 4 5 5 Side connections bc d...

Page 32: ...hemicals or other items behind the instrument WARNING Death or serious injuries by use in explosive environments Do not operate the instrument in explosive environments Do not operate the instrument w...

Page 33: ...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 External mains supply must meet the volt...

Page 34: ...ke sure that the ferrule is pointed towards the fitting to avoid leaking and flush with the end of the tubing NOTE Close vacant ports with a blind fitting P N 035665 to avoid any unwanted contaminatio...

Page 35: ...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 inst...

Page 36: ...s optional 6 4 7 12 Flush the system with the solvent used for the next run optional 6 2 6 6 1 Method development A method must be developed before beginning an extraction to define the operating para...

Page 37: ...SpeedExtractor If there is any question about solvent suitability contact BUCHI Solvents NOT being compatible with the process Component Formula Reason Carbon disulfide CS2 Autoignition temperature 1...

Page 38: ...programmed in the SOLVENT LIST by default However this list can be expanded or changed to include your own solvents or solvent mixtures Open the list Go to MENU SOLVENT LIST to open the default solve...

Page 39: ...lt solvent list Move the cursor to position 001 The move up function button is now replaced by DEFAULT Press DEFAULT and confirm the message Load default solvent list First 10 entries replaced The fir...

Page 40: ...nstrument It is therefore possible to configure the instrument so that PREHEAT submenu appears as soon as the instrument is turned on To activate this function open MENU INSTRU MENT SETTINGS Go to PRE...

Page 41: ...therefore recommended and is mandatory after a longer period of non use and or after replacement of the cup seals There are two distinct approaches to perform a leak test Firstly very commonly the tig...

Page 42: ...the green START button closes the extraction cells and starts elevating the pressure by pumping solvent into the cells A first TIGHTNESS test checks the presence of the extraction cells using nitroge...

Page 43: ...the presence of the cells is first checked using nitrogen 7 bar before the set pressure 100 bar is reached Evaluation of leak tests The absolute values depend on different parameters These are Set te...

Page 44: ...e solvent and the cell are not heated up to the set temperature In order to get good reproducible results it is therefore advisable to perform a leak test twice It is always possible to switch to the...

Page 45: ...IAL for the FLUSH INTO entry using the selection knob Set all other parameters as described above and shown in the reference settings table NOTE When changing the solvent reservoirs e g from hexane to...

Page 46: ...the extraction cell This is the case particularly with solvent mixtures with acetone In these cases blending the samples with DE before loading into the extraction cell is highly recommended Never us...

Page 47: ...or dispersing agents For very small samples an expansion element may be used to fill up the void volume of partially filled extraction cells P N 053708 NOTE This expansion element fits only 10 mL ext...

Page 48: ...P N 11069547 E 914 P N 053691 to provide more stability In order to carefully load the sample into the cell using the optional weighing boat f P N 053202 Rinse the weighing boat with some additional...

Page 49: ...metal frits Bottom filter cellulose qty 100 049569 Bottom filter glass fibre qty 100 11055932 Top filter E 916 cellulose qty 100 049572 Top filter E 916XL cellulose qty 100 11069533 Top filter E 914 c...

Page 50: ...owing sections describe the individual stages of an extraction process how to create store and open methods and how to optimize existing procedures 6 4 1 Placing the cells and bottles vials into the i...

Page 51: ...Generally every extraction method consists of a number of cycles which can be divided into 3 phases the heat up hold and discharge time Prior the first cycle the tightness test is carried out Tightnes...

Page 52: ...meters the sample s property and packing in the cell and the size of the extraction cell The accurate values are therefore only available in hindsight The remaining time used to finish process which i...

Page 53: ...ter using the selection knob NOTE If the total extract volume gets too large and or the extract of different cycles are to collect separately insert a vial change in the method to exchange the collect...

Page 54: ...the collection vials between the cycles to separately collect extracts of different cycles or when the total volume of the extract exceed the vial volume In this case the warning Vial overflow possibl...

Page 55: ...ions can be found in the corresponding Application booklet Operation parameters Parameter Function Value range TEMPERATURE DefinedsettemperatureusedfortheHOLDtime Thisvaluealso influences the time use...

Page 56: ...HOLD Time used for the extraction at constant temperature 0 60 min default 2 min DISCHARGE Time used to empty the extraction cells This step is not supportedbynitrogengas Purgingwithnitrogenisachieved...

Page 57: ...oromethane 50 Remove the extraction cells Preheat EXTRACTION PREHEAT 80 C OK ON The oven starts heating Create method EXTRACTION EDIT METHOD Temperature 80 C pressure 100 bar vial 60 mL cell 10 mL sol...

Page 58: ...igherpressuresoftenprovidebetterresultsin termsofyieldandextractionefficiency Thisismostlyduetobetter matrixpenetrationofthesolventandhencefasterdiffusionofthe analyte from the matrix into the solvent...

Page 59: ...main at their operating positions All actions such as releasing the lift or opening the position valves can be controlled manually using the service menu Recommended action in case of an unexpected oc...

Page 60: ...optional Optional PC software is available P N 053073 which allows communication between the SpeedEx tractor and a PC via a USB port The SpeedExtractor Record software allows you to fully create edit...

Page 61: ...6 Operation 60 SpeedExtractor E 916 E 916XL E 914 Operation Manual...

Page 62: ...completely dipped into the solvent Empty the waste bottle if needed Inspect the cup seals for visual damage or contamination by sand or dust If necessary replace the seals according to section 7 2 1...

Page 63: ...e to seal the extraction cells properly 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 2 2 Replacin...

Page 64: ...k the orientation of the cup seals Make sure that the spring always points to the extraction cell NOTE Never remove the cup seals using your fingernails or any kind of tools because that might damage...

Page 65: ...rules and fittings 1 4 UNF 28 D 1 16 To reduce any dead volume and potential sources of contamination make sure that the ferrule is always flush with the end of the tube The pointed end of the ferrule...

Page 66: ...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 NOTE Make sure that the sloped sides of the two needles of one position...

Page 67: ...way screw it into the input block while continuously pressing the tubing to the inside until the end of the tubing is firmly seated on the bottom of the opening Outlet capillary Unscrew the capillary...

Page 68: ...in the upper part into which a plastic syringe P N 034882 can be inserted as shown in the pic ture Both heads are equipped with piston seals P N 053612 When operating with buffer solutions there is a...

Page 69: ...7 Maintenance 68 SpeedExtractor E 916 E 916XL E 914 Operation Manual...

Page 70: ...lock starting from left to right General malfunctions and their remedy Malfunction Display information Possible cause Remedy Error 1 Not defined Error 2 Heatertemperatureoutofrange DT 30 C Start not a...

Page 71: ...r to user manual Theliftismechanicallyblocked Inspect the lift for physical blockage Contact BUCHI customerserviceiftheproblem persists Error 12 Targetpositionofheatingblock not achieved Please check...

Page 72: ...struc tions outlined in section 8 1 3 Error 35 to error 40 PositionXclogged pressrepeat todischargeorrelievethepres sure manually Please refer to user manual ThepressureatpositionXistoo high 80 bar Pr...

Page 73: ...o error 57 Position X Pressure too high Please refer to user manual During Extraction The pressure at position X is toohigh mostprobablydueto clogging of the sample in the extractioncellduringoperatio...

Page 74: ...not get anywhere contactBUCHIcustomerservice Error 67 Nocommunicationwithpump Please refer to user manual Thepumpisnotsuppliedwith current ContactBUCHIcustomerservice Error 68 to error 73 Positionval...

Page 75: ...amples For more detailed information about sample preparation and method development consider BUCHI s Application Notes Technical Notes and the SpeedExtractor Application Book let Please contact your...

Page 76: ...ber 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 2 for er...

Page 77: ...es that it does not make sense to follow this way due to moving in circles Error 29 34 Position X clogged press START to disable position or repeat to discharge Repeat Pressure released Wobbleposition...

Page 78: ...section 6 2 6 If solvent flows into the vials the cell sample inside the cell the filter or frit was blocked If solvent does not flow into the vial the SpeedExtractor is blocked and further steps are...

Page 79: ...y the blocked part The flow test in the service menu allows locating the blockage within the instrument See section 8 2 4 Error 41 PositionXclogged pressrepeatto discharge or relieve the pressure manu...

Page 80: ...wise is sufficient Suck up a solvent using a plastic syringe until the pump stops producing bubbles Empty the syringe attach it again start the pump and watch to see whether the pump sucks regularly a...

Page 81: ...ve holder using a 1 4 and 8 mm spanner wrench and take off the capillary Unscrew the fittings of the pump inlet lines Unscrew the four nuts from the head using a 3 mm allen wrench Carefully remove the...

Page 82: ...lative back pressures of the line exceed 10 bar the line is either contaminated with sample or par ticles of the septa see sections 7 2 3 and 7 2 4 or are deformed Check the needles first and clean or...

Page 83: ...the solvent valves Press NEXT to get to the MEDIA VALVE display Press the down button to activate CALIBRATE and confirm with SELECT You will hear the rotating valve finding the correct start position...

Page 84: ...s media valve posi tionvalvesandoutletvalveareshowninaseparatesubmenu It ispossibletoopenorcloseeachvalveseparatelytochecktheir function Tocheckwhetherthevalve isoperatingortocalibrate the rotary valv...

Page 85: ...h are helpful in case of troubleshooting Tochecktheversionofthe instrument firmware etc 8 2 1 Checking the valves Go to SERVICE FUNCTIONS VALVES Depending on the type of mixer 2 or 4 solvent valves wi...

Page 86: ...BRATE to calibrate the pressure sensors to 0 bar Therefore the instrument must not be under pressure so open the heater and the positions valve before calibration Press NEXT to enter the TEMPERATURE S...

Page 87: ...g extraction was caused by the cell containing the sample If pressure builds up a part inside the SpeedEx tractor is blocked Release the pressure manually and continue with test 2 Test 2 Into vial wit...

Page 88: ...elease the pressure manually The top cover plate can be exchanged or cleaned by the operator If parts before the top cover plate are blocked the service techni cian has to exchange or clean these part...

Page 89: ...e is set to 100 to get rid of any solvent possibly leaking from the system NOTE It is not advisable to change this setting as it has an impact on the actual temperature of the heating block Go back to...

Page 90: ...nsive 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 co...

Page 91: ...8 Troubleshooting 90 SpeedExtractor E 916 E 916XL E 914 Operation Manual...

Page 92: ...ds and dusty and hazardous resi dues before packaging the instrument WARNING Death or serious poisoning by contact or incorporation of harmful substances Wear safety goggles Wear safety gloves Wear a...

Page 93: ...n 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 l...

Page 94: ...equipment has not been used in the laboratory and is new was not in contact with toxic corrosive biologically active explosive radioactive or other dangerous matters is free of contamination The solv...

Page 95: ...9 Shutdown storage transport and disposal 94 SpeedExtractor E 916 E 916XL E 914 Operation Manual...

Page 96: ...5 Extraction cell E 916XL 60ml 11069535 Extraction cell E 914 10 mL 11067988 Extraction cell E 914 20 mL 11067989 Extraction cell E 914 40 mL 051234 Extraction cell E 914 80 mL 051233 Extraction cell...

Page 97: ...h Retaining plate for Syncore Analyst vessels for E 916 1 11057054 p Polyvap vessel wide necked 12 040907 i Caps and septa for narrow necked vials 100 11056535 j Septa for narrow necked vials 100 049...

Page 98: ...e 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 Accessories rela...

Page 99: ...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...

Page 100: ...E 914 2 053674 f Top filter for E 916 cellulose 100 049572 f Top filter for E 916XL cellulose 100 11069533 f Top filter for E 914 cellulose 100 051249 6 Top filter for E 916 glass fiber 100 11057189...

Page 101: ...ing 1 8 green 10 053663 d 1 4 UNF 28 ferrules 1 8 green 10 053664 e 1 4 UNF 28 fitting 1 16 gray 25 044816 f 1 4 UNF 28 ferrules 1 16 gray 25 044269 g 1 4UNF 28blindfitting1 8 blue 10 053665 h Fitting...

Page 102: ...r no f f Check valves 1 053610 Piston seal black PTFE 1 053612 Piston seal white 1 11056588 b a Further accessories Item PU Order no a 4 port solvent mixer 053381 b Small cooling unit for viscous samp...

Page 103: ...latingChillerF 105 115V 1 11056462 11056463 RecirculatingChillerF 108 230V RecirculatingChillerF 108 115V 1 11056464 11056465 Accessories related with the process workflow evap oration to defined resi...

Page 104: ...duct Qty Order no Product Qty Order no IQ OQ reference set EN 1 11055354 Operation manual EN 1 093218 IQ OQ documentation EN 1 11056092 Operation manual GE 1 093219 Repeating OQ 1 11056093 Operation m...

Page 105: ...10 Spare parts 104 SpeedExtractor E 916 E 916XL E 914 Operation Manual...

Page 106: ...cause harmful interference in which case the user will be required to correct the interference at his or her own expense Fran ais Cet appareil a t test et s est av r conforme aux limites pr vues pour...

Page 107: ...i com cn zh Indien BUCHI India Private Ltd IN Mumbai 400 055 T 91 22 667 75400 F 91 22 667 18986 india buchi com www buchi com in en Indonesien PT BUCHI Indonesia ID Tangerang 15321 T 62 21 537 62 16...

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