SpeedExtractor E-916 / E-914
Operation Manual
093218F en
Imprint
Product Identification:
Operation Manual (Original), SpeedExtractor E-916 / E-914
093218F en
Publication date: 05.2019
BÜCHI Labortechnik AG
Meierseggstrasse 40
Postfach
CH-9230 Flawil 1
E-Mail: quality@buchi.com
BUCHI reserves the right to make changes to the manual as deemed necessary in the light of experience; especially in respect to structure, illustrations and technical detail.
This manual is copyright. Information from it may not be reproduced, distributed, or used for competitive purposes, nor made available to third parties. The manufacture of any component with the aid of this manual without
prior written agreement is also prohibited.
Table of contents
Table of contents
1 About this manual .............................................................................................................................................................. 5
1.1 Reference documents ......................................................................................................................................... 5
1.2 Trademarks .............................................................................................................................................................. 5
1.3 Abbreviations ......................................................................................................................................................... 6
2 Safety ...................................................................................................................................................................................... 7
2.1 User qualication .................................................................................................................................................. 7
2.2 Proper use ................................................................................................................................................................ 7
2.3 Improper use .......................................................................................................................................................... 7
2.4 Safety warnings and safety signs used in this manual ............................................................................ 8
2.5 Product safety ......................................................................................................................................................10
2.5.1 General hazards .....................................................................................................................................10
2.5.2 Warning labels on housing and assemblies ................................................................................11
2.5.3 Personal protective equipment .......................................................................................................11
2.5.4 Built-in safety elements and measures .........................................................................................12
2.6 General safety rules ............................................................................................................................................13
3 Technical data .................................................................................................................................................................... 15
3.1 Scope of delivery .................................................................................................................................................15
3.2 Instrument congurations ...............................................................................................................................15
3.3 Materials used ......................................................................................................................................................18
3.4 Technical data overview ...................................................................................................................................18
4 Description of function .................................................................................................................................................. 21
4.1 Functional principle ...........................................................................................................................................21
4.2 Overview of the instrument ............................................................................................................................ 21
4.3 Overview of the extraction process ............................................................................................................. 23
4.4 Schematic representation of the process ..................................................................................................24
4.5 Controls and connections ................................................................................................................................25
4.5.1 Instrument controls ..............................................................................................................................25
4.5.2 Main displays of the instrument ......................................................................................................26
4.5.3 General information on buttons ......................................................................................................29
4.5.4 Rear connections ................................................................................................................................... 30
4.5.5 Side connections ................................................................................................................................... 30
5 Putting into operation .................................................................................................................................................... 31
5.1 Installation site .....................................................................................................................................................31
5.2 Electrical connections ....................................................................................................................................... 32
5.3 Gas and solvent connections..........................................................................................................................33
5.4 Dehydration ..........................................................................................................................................................34
5.5 Functional test .....................................................................................................................................................34
2 SpeedExtractor E-916 / E-914 Operation Manual
Table of contents
6 Operation ............................................................................................................................................................................35
6.1 Method development .......................................................................................................................................35
6.2 Preparing the instrument ................................................................................................................................36
6.2.1 Solvent reservoir ....................................................................................................................................36
6.2.2 Modifying the SOLVENT LIST ............................................................................................................37
6.2.3 Preheating the instrument ................................................................................................................38
6.2.4 Activating/deactivating positions ...................................................................................................39
6.2.5 Leak test ....................................................................................................................................................40
6.2.6 Flushing the instrument .....................................................................................................................43
6.2.7 Activating the EcoMode .....................................................................................................................44
6.3 Preparing the sample ........................................................................................................................................45
6.3.1 Sample preparation ..............................................................................................................................45
6.3.2 Extraction cell selection ...................................................................................................................... 46
6.3.3 Packing of the cells ...............................................................................................................................46
6.4 Extraction process ..............................................................................................................................................49
6.4.1 Placing the cells and bottles/vials into the instrument ...........................................................49
6.4.2 Stages of an extraction cycle ............................................................................................................ 50
6.4.3 Creating new methods ........................................................................................................................51
6.4.4 Summary of operating parameters ................................................................................................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 Creating a report (optional) ............................................................................................................................59
7 Maintenance ....................................................................................................................................................................... 61
7.1 Daily maintenance ..............................................................................................................................................61
7.2 Periodic maintenance .......................................................................................................................................62
7.2.1 Sealing system........................................................................................................................................62
7.2.2 Replacing the cup seals ......................................................................................................................62
7.2.3 Tube connections and needles ........................................................................................................63
7.2.4 Septum ...................................................................................................................................................... 65
7.3 Pump maintenance ............................................................................................................................................66
7.3.1 Connections ............................................................................................................................................66
7.3.2 Back washing ..........................................................................................................................................67
8 Troubleshooting................................................................................................................................................................69
8.1 Malfunctions and their remedy ..................................................................................................................... 69
8.1.1 Action in case of a re ..........................................................................................................................69
8.1.2 General malfunctions and their remedy .......................................................................................69
8.1.3 Handling and resolving blockages ................................................................................................. 74
8.1.4 The pump is not aspirating properly .............................................................................................79
8.1.5 Replacement of check valves ............................................................................................................80
8.1.6 Precipitation in the outlet lines ........................................................................................................81
8.1.7 Malfunctions of the rotating valves ................................................................................................82
8.1.8 Upgrading a 2-port mixer to a 4-port mixer ................................................................................82
3 SpeedExtractor E-916 / E-914 Operation Manual
Table of contents
8.2 Description of the service menu ................................................................................................................... 83
8.2.1 Checking the valves .............................................................................................................................84
8.2.2 Checking the sensors ........................................................................................................................... 85
8.2.3 Running the pump ...............................................................................................................................85
8.2.4 Inspecting the lines (ow test) ......................................................................................................... 86
8.2.5 Moving the cell and vial lift ...............................................................................................................88
8.2.6 Changing the fan performance........................................................................................................88
8.2.7 Displaying the operating hours .......................................................................................................88
8.2.8 Unit information ....................................................................................................................................88
8.3 Customer service.................................................................................................................................................89
9 Shutdown, storage, transport and disposal ............................................................................................................91
9.1 Storage and transport ....................................................................................................................................... 91
9.2 Disposal ..................................................................................................................................................................92
9.3 Health and safety clearance ............................................................................................................................93
10 Spare parts .......................................................................................................................................................................... 95
11 Declarations and requirements .................................................................................................................................105
11.1 FCC requirements (for USA and Canada) ................................................................................................105
Read this manual carefully before installing and running your system and note the safety precautions in chapter 2
in particular. Store the manual in the immediate vicinity of the instrument, so that it can be consulted at any time.
No technical modications may be made to the instrument without the prior written agreement of BUCHI. Unauthorized modications may aect the system safety or result in accidents.
This manual is copyright. Information from it may not be reproduced, distributed, or used for competitive purposes, nor made available to third parties. The manufacture of any component 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. If you need another language version of this manual, you can download available versions
at www.buchi.com.
4 SpeedExtractor E-916 / E-914 Operation Manual
1 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 chapter2.
1.1 Reference documents
For information on complementary BUCHI devices, please refer to the corresponding manuals:
Complementary devices
Multivapor P-6 / P-12, Operation Manual
Vacuum Controller, Operation Manual
Vacuum Pump, Operation Manual
Syncore Platform, Operation Manual
Syncore Accessories, Operation Manual
1 About this manual
NOTE
• All manuals are available via www.buchi.com
• For download a free online registration is required
1.2 Trademarks
The following product names and any registered and unregistered trademarks mentioned in this
manual are used for identication purposes only and remain the exclusive property of their respective
owners:
• SpeedExtractor is a registered trademark of BÜCHI Labortechnik AG
• ASE is a registered trademark of Dionex Corporation
5 SpeedExtractor E-916 / E-914 Operation Manual
1.3 Abbreviations
Process-related
ASE Accelerated Solvent Extraction
PSE Pressurized Solvent Extraction
Materials and chemicals
FEP Combination of tetrauoroethylene and hexauoropropylene
FFPM Peruoro caoutchouc
PTFE Polytetrauoroethylene
POM Polyoxymethylene (commercialized as Delrin® by DuPont)
PEEK Polyether ether ketone
THF Tetrahydrofurane
Miscellaneous
FW rm ware
qty quantity
DT Temperature dierence
Dp Pressure dierence
1 About this manual
6 SpeedExtractor E-916 / E-914 Operation Manual
2 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.
2.1 User qualication
The instrument may be used only by laboratory personnel or other persons who on account of instruction or professional experience have an overview of the dangers that can develop when operating the
instrument.
Personnel without such instruction or persons who are currently being trained require careful supervision.
The present Operation Manual serves as a basis for instruction.
2 Safety
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 of heating under pressure. The pressure is
typically applied by the HPLC pump.
2.3 Improper use
Applications beyond those described above are improper. Furthermore, applications that do not
comply with the technical data are also considered improper. The operator bears the sole risk for any
damage caused by such improper use.
The following applications are expressly forbidden:
• Use of solvents with an self ignition point between 40 to 220°C.
• Use of the instrument in rooms that require ex-protected instruments.
• Use as a calibrating instrument for other instruments.
• Preparation of samples that can explode or iname due to shock, friction, heat, or spark formation.
• Use in high pressure situations, i.e. > 200bar.
• Use in conjunction with solvents that have a low self ignition point or contain peroxides, such as
diethyl ether or THF.
• Use of cells, seals, hoses, and tubes other than the originals from BUCHI.
7 SpeedExtractor E-916 / E-914 Operation Manual
2.4 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.
For your safety it is important to read and fully understand the table below with the dierent signal
words and their denitions!
Sign Signal word Definition Risk level
!
DANGER
Indicates a hazardous situation which, if not avoided, will result in
death or serious injury.
2 Safety
★★★★
WARNING
!
CAUTION
!
NOTICE
no
Supplementary safety information symbols may be placed in a rectangular panel on the left to the
signal word and the supplementary text (see below example).
Space for
supplementary
safety
information
symbols.
Table of supplementary safety information symbols
The reference list below incorporates all safety information symbols used in this manual and their
meaning.
Indicates a hazardous situation which, if not avoided, could result
in death or serious injury.
Indicates a hazardous situation which, if not avoided, may result
in minor or moderate injury.
Indicates possible property damage, but no
practices related to personal injury.
!
SIGNAL WORD
Supplementary text, describing the kind and level of hazard/risk seriousness.
• List of measures to avoid the herein described, hazard or hazardous situation.
• ...
• ...
★★★☆
★★☆☆
★☆☆☆
(property damage only)
Symbol Meaning
General warning
Electrical hazard
Harmful to life-forms
8 SpeedExtractor E-916 / E-914 Operation Manual
Symbol Meaning
Fire hazard
Hot item, hot surface
Device damage
Inhalation of substances
2 Safety
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.
NOTE
Useful tips for the easy operation of the instrument/software.
9 SpeedExtractor E-916 / E-914 Operation Manual
2.5 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.
2.5.1 General hazards
The following safety messages show hazards of general kind which may occur when handling the
instrument. The user shall observe all listed counter measures in order to achieve and maintain the
lowest possible level of hazard.
Additional warning messages can be found whenever actions and situations described in this manual
are related to situational hazards.
2 Safety
!
WARNING
Death or serious injuries by formation of explosive atmospheres inside the instrument.
• Before operation, check all gas connections for correct installation
• Regularly discharge the waste bottle to avoid overow
• Check for proper system tightness
!
DANGER
Death or serious injuries by use in explosive environments.
• Do not store or operate the instrument in explosive environments
• Provide sucient ventilation and make sure to directly withdraw fumes
!
WARNING
Death or serious burns by ammable vapors.
• Remove all sources of ammable vapors
• Do not store ammable chemicals in the vicinity of the device
!
CAUTION
Risk of burns by hot heating block and extraction cells.
• Do not touch hot parts or surfaces
• Let the system and inserted extraction cells cool down safely
• Do not move the instrument or parts of it when hot
10 SpeedExtractor E-916 / E-914 Operation Manual
2 Safety
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
Risk of instrument damage by wrong mains supply.
• External mains supply must meet the voltage given on the type plate
• Check for sucient 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 Location
NOTICE
NOTICE
Hot item, hot surface Sticker/label, located at the heating block
2.5.3 Personal protective equipment
Always wear personal protective equipment such as protective eye goggles, protective clothing and
gloves. The personal protective equipment must meet all requirements of the supplementary data
sheets for the chemicals used.
!
Serious chemical burns by corrosives.
• Observe supplementary data sheets of all used chemicals.
• Handle corrosives in well ventilated environments only.
• Always wear protective goggles.
• Always wear protective gloves.
• Always wear protective clothes.
• Do not use damaged glassware.
WARNING
11 SpeedExtractor E-916 / E-914 Operation Manual
2.5.4 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
200bar±20bar.
• 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.
• The presence of extraction cells in the heating block is checked in the tightness test at the beginning of each extraction process.
2 Safety
Seismic tie-down
In earthquake-susceptible regions the instrument
should be tied down by the ventilation slot on the
rear of the instrument.
12 SpeedExtractor E-916 / E-914 Operation Manual
2.6 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.
Duty of maintenance and care
The operator is responsible 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 consumables and spare parts for maintenance to assure good system performance,
reliability and safety. Any modications of spare parts or assemblies are only allowed with the prior
written permission of the manufacturer.
Modications
Modications to the instrument are only permitted after prior consultation and with the written approval
of the manufacturer. Modications and upgrades shall only be carried out by an authorized BUCHI
technical engineer. The manufacturer will decline any claim resulting from unauthorized modications.
2 Safety
13 SpeedExtractor E-916 / E-914 Operation Manual
2 Safety
14 SpeedExtractor E-916 / E-914 Operation Manual
3 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.
3.2 Instrument congurations
The SpeedExtractor is available in 18 dierent congurations diering in the number of positions (E-916:
6 positions, E-914: 4 positions), the type of solvent mixer (2 ports or 4 ports), and the size of the extraction
cells (E-916: 10 – 40mL, E-914: 10 – 120mL). The SpeedExtractor E-914 is available with and without pedestal (the pedestal allows to accommodate large volume collection recipients).
3 Technical data
E-914 without and with pedestal
15 SpeedExtractor E-916 / E-914 Operation Manual
3 Technical data
1 1
5 1
c
Number of positions
4 E-914: 4 positions
5 E-914: 4 positions mounted on pedestal
6 E-916: 6 positions
Size of extraction cells
01 10mL (E-916 only)
02 20mL (E-916 only)
04 40mL
08 80mL (E-914 only)
12 120mL (E-914 only)
Number of solvent ports
2 Ports
4 Ports
d
e
f
i
p
j
q
b
k
r
s
m
l
t
053691 053690
a
h
g
n
o
List of loose parts
Position Item PU Universal Order no. E-914 Order no. E-916
a
b
c
d
e
f
g
h
i
FEP tube D3.2/1.6, 5m 2 110556 0 4
FEP waste tube 1/16", 0.5m 4/6 053303
Solvent bottle 1 L 1 053203
Quartz sand 0.3–0.9mm, 2.5kg 1 037689
Extraction Record demo license 1 053074
Extraction cell carrier 1
Solvent lter 4 044340
Turix wrench 1 044349
Allen wrench 3mm 1 000610
16 SpeedExtractor E-916 / E-914 Operation Manual
c
3 Technical data
d
e
f
i
p
j
q
b
k
r
s
l
t
m
053671 053669
051249 049572
1
110 55342
053038 053037
a
h
g
n
o
List of loose parts
Position Item PU Universal Order no. E-914 Order no. E-916
j
k
l
m
n
o
p
p
q
q
r
s
s
t
t
Spanner wrench 1/4" 1 053204
Spanner wrench 8/10mm 1 053608
Torx screwdriver TX20 1 053668
USB cable 2.0 A-B, 4.5m 1 049226
Plug screws 2 053209
Metal frit 25 049568
Cup seals, top 12
Cup seals, bottom 12 053670
Cellulose lter, top 100
Glass ber lter, bottom 100 110 5 59 32
Swagelok nut and ferrules 1/8"
UNF-28 Fitting 1/8", green 10 053663
UNF-28 Ferrule 1/8", green 10 053664
UNF-28 Fitting 1/16", gray 25 044816
UNF-28 Ferrule 1/16", gray 25 044269
Supporting ring PEEK 2 053667 053666
Filter hook 1 053316
Plunger 1
Syringe 60mL 1 034882
Brush small 1 053256
Brush large 1 053257
Gripper extraction cell 1
Bit wrench 1 052783
Extruder rod 1 1105528 4
Tub e cutter 1 019830
17 SpeedExtractor E-916 / E-914 Operation Manual
053026 053030
3.3 Materials used
Materials used
Component Material designation
Housing SpeedExtractor Stainless steel
Lines to pump FEP
Solvent valve 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 block Aluminum
Heating block cover PTFE
Cup seals PTFE
Extraction cells Stainless steel
Lines to waste FEP
Needles Stainless steel
Collection vials Glass
Septa for vials Silicon, PTFE
Collection unit Stainless steel, POM
Pump PTFE, ceramic, stainless steel
Protective shield Glass, POM
3 Technical data
3.4 Technical data overview
Technical data of the SpeedExtractor
Description
Dimensions (W×H×D)
Weight
Connection voltage
Max. power consumption
Mains connection
Frequency
Fuse
Interface
Installation category
Degree of protection
Pollution degree
Temperature control range
Temperature accuracy
Technical data
670×725×500mm
90kg
100 – 240VAC ±10%
max. 1750W
3-pole (P, N, E) via power cord
50/60Hz
14 A/240V
USB 2.0
II
IP21
2
30 – 200°C
±3°C
18 SpeedExtractor E-916 / E-914 Operation Manual
Technical data of the SpeedExtractor
Description
Pressure range
Pressure accuracy
Primary pressure nitrogen connection
Flow rate pump
Precision ow rate
Precision mixer
Extraction cell size
Environmental conditions
Temperature
Altitude
Humidity
Noise level
3 Technical data
Technical data
50 – 150bar
±5bar
6 – 10bar
1 – 50mL/min
±2%
±2% (±5% for isopropanol)
E-916: 10, 20, 40mL; E-914: 10*, 20*, 40, 80, 120mL
For indoor use only
5 – 40°C
up to 2000m
maximum relative humidity 80% for temperatures
up to 31°C, and then linearly decreasing to 50%
at 40°C
<70dB
*Accessories
19 SpeedExtractor E-916 / E-914 Operation Manual
3 Technical data
20 SpeedExtractor E-916 / E-914 Operation Manual
4 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. In order to maintain the solvent in a liquid state during the
extraction process, the solvent inside the extraction cell is put under pressure. Generally, to achieve
high recoveries multiple extraction cycles are applied. Once the extraction step is nished, the extracts
are cooled down in a cooling unit and ushed into collection vials which then can easily be evaporated
in parallel using the Multivapor™ P-6 or Syncore Analyst R-12. Hence the whole process workow can
be performed in parallel with up to 6 samples.
4 Description of function
The SpeedExtractor E-916 accommodates 6 samples with a maximum volume of 40mL, whereas the
E-914 can be used for up to 4 samples with a limited maximum volume of 120mL. The total volume of
the collection recipients are from 60 mL vials to 240mL bottles. Using a specially designed rack, it is
also possible to use large volume round bottom asks to collect the extracts.
Typical applications are carried out in environmental substances (environmental pollutants such as those
listed in EPA Method 3545A for instance), food (recovery of fat from meat, oil seeds, feeds, dairy products, snack foods, etc.), pharmaceuticals (extracting analytes from natural products, drugs from drug
formulations, pharmaceutical additives from feeds) and polymers (monomeric compounds, oligomers
or additives).
4.2 Overview of the instrument
e
g
d
a
h
b
f
c
21 SpeedExtractor E-916 / E-914 Operation Manual
N
2
j
i
4 Description of function
a Main power switch
The instrument is protected by a 14 A (240V) 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 dierent solvents, with the 4-port mixer up to 4 dierent solvents can be connected allowing
any user-dened solvent ratios.
c Solvent pump and solvent mixer
A self-priming HPLC pump transfers the extraction solvent from dierent solvent reservoirs to the mixer
and from there into the extraction cell. With the control panel arbitrary solvent ratios can be chosen.
d Heating block
The heating block accommodates 6 or 4 extraction cells and guarantees an accurate and uniform
heat distribution across all extraction positions independent of the placement. The whole block is easily pulled out horizontally facilitating the accommodation of the extraction cells. Magnetic connections
on the heating block and on guide rail make sure that the heating block is correctly placed in a dened
middle position, ready for operation. The protection shield protects the operator from hot surfaces and
movable parts during operation.
e Extraction cells
The extraction cells are tailored to the dimensions of the holes in the heating block guarantying an efcient and accurate heat transfer into the sample. The sample volume of the cells diers from 10–40mL
for the E-916 and from 10 – 120mL for the E-914.
f Collection rack
Up to 6 collection vials are loaded into the collection unit. After extraction, the extracts containing the
analytes are collected in these bottles. Dierent collection units and adapters are available to accommodate small vials up to large volume round bottom asks. See chapter 10.
g Control panel
The control panel containing a liquid crystal display (LCD) and membrane keypads allows to program
the full extraction process. Detailed schematic representations inform the operator about the current
stage of the process as well as possible errors.
h Nitrogen inlet
The nitrogen gas inlet connection is located on the right hand side next to the solvent connections. It
is used to get rid of residual solvent by ushing the lines and cells thoroughly with nitrogen and/or to
inerting the system. Inerting the receiving vials is for the stability of some analytes benecial. Nitrogen
pressure of 6 – 10bar is required for proper operation. To avoid any contamination by ushing with
nitrogen 5.0 quality (i.e. vol.-% > 99.999) is recommended for trace analysis and 4.5 (i.e. vol.-% >
99.995) for other applications.
i Waste outlets
An 18-port valve located between the heating block and the collection rack allows collecting the
extract leaving the extraction cells either in the collection bottle or a waste bottle. The latter is in particular benecial when the solvent is changed or the lines are ushed upon contamination. The number
of waste outlets is determined by the instrument conguration! The E-916 features 6, the E-914 only 4
outlet ports.
j Exhaust
The collection vials are sealed by septum. A stainless steel needle pierces this septum allowing the
extract to ow from the extraction cell into the collection bottle. To compensate the pressure a second
needle connects the collection bottle with an exhaust joint situated on the rear of the instrument.
22 SpeedExtractor E-916 / E-914 Operation Manual
4.3 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 lling 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).
• Placing the collection vials in the collection tray (see section 6.4.1).
• Placing the extraction cell into the preheated heating block (see section 6.4.1).
Phase 2: Extraction cycles
• Start extraction method (see section 6.4.8).
An extraction cycle involves three steps with a user-dened time period (except for HEAT UP):
In a rst HEAT UP step the pressure and temperature inside the extraction cell is slowly increased to
the set parameters of extraction program.
During HOLD step these parameters remain constant. This corresponds with the literal extraction step
at constant temperatures and pressures. After this step the outlet valve opens and the liquid extract
is DISCHARGEd and collected in collection vials or a waste bottle by means of pressure compensation. All three steps are repeated several times according to the extraction program. A complete run
may consist of 1 – 10 extraction cycles. The presence of extraction cells is checked in the TIGHTNESS
TEST at the beginning of each extraction process.
4 Description of function
The HEAT UP step is not accessible by the user but is determined by the instrument software. The
absolute time of this period depends on the temperature, pressure, size of the extraction cell and type
of sample. Additional time is needed to ll the extraction cell. The HOLD and the DISCHARGE time
can be dened by the user individually for each cycle.
The actual time used for a complete process is shown in the STATUS menu and/or recorded by
SpeedExtractor Record software, where it can be exported to a report and printed out.
Phase 3: Flushing the lines and unloading the heating block
• Flushing the lines with fresh solvent and collecting the liquid in the collection vials (see section 6.4.2).
• Flushing with nitrogen to remove residual solvent (see section 6.4.2).
• Unloading the heating block (see section 6.4.9).
NOTE
Preheating the instrument to the temperature of operation prior to loading it with the extraction
23 SpeedExtractor E-916 / E-914 Operation Manual
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. In order to achieve reproducible results, it is recommended that the same procedure always be followed. As the time used to reach the set temperature is depending on the absolute
set temperature, it is suggested that the extraction cells never be placed in the heating block until the
instrument is ready and to start the extraction process right away. This procedure guarantees that
the sample is not unnecessarily exposed to the hot environment and that this time period before the
actual process starts does not signicantly inuence the recovery of the extraction process.
In addition, placing extraction cells in all positions is highly recommended even though not all positions are used. This improves the heat uniformity of the heating block. It is possible to deactivate the
positions with the empty cells to avoid needless solvent consumption.
4.4 Schematic representation of the process
4 Description of function
The following illustration provides a schematic representation of the pathways of the dierent media
for the E-916. Up to four dierent solventsa and nitrogenb are connected to the E-916. A media
valvef switches between solvent and nitrogen. The mixerd mixes the solvents that are selected
with the help of the solvent valvesc.
The pumpe transfers the solvent mixture to dividerg where it is equally distributed to each of the
activated positions. Once the system is sealed by closing the extraction cellsl with the upper and
lower tightening device that holds the cup sealsk andm, the outlet valveo is closed in order to
increase the pressure inside the system. The pressure of each position is displayed by the pressure
sensorsj. When the set pressure is reached (at the end of the heat-up step) the position valvesi
are permanently closed, and the sample is extracted (hold step). In the discharge step the outlet
valveo opens, the hot mixture is cooled down by the cooling unitsn and nally transferred to the
collection vialsp. Pressure compensation is achieved by the lines to the exhaustq. In case of an
overpressure, the outlet valve opens and releases solvent into the collection vials. Residual solvent
is optionally ushed with fresh solvent. An additional thorough ushing step with nitrogen removes
residual solvent in the lines. In addition, another optional ushing with solvent into waste instead of the
collection vials is possible by setting the outlet valve to waster. This is usually done to prepare the
system for another run with a dierent solvent. For a thorough description of each step please refer to
section 6.4.
24 SpeedExtractor E-916 / E-914 Operation Manual
r
N
h
n
4 Description of function
a Solvent reservoirs (3 and 4 optional)
b
2
a
b Nitrogen tank
c Solvent valves
d Mixer
e Pump
c
f Media valve
g Divider
f
e
d
h Overpressure valve
i Position valves
j Pressure sensors
j
g
k Upper cup seals
l Extraction cells
i
m Lower cup seals
n Cooling units
j
k
l
o Outlet valve
p Collection vials
q Exhaust
r Waste
m
o
q
4.5 Controls and connections
4.5.1 Instrument controls
a
b
c
d
e
p
a Display to view the instrument software.
b Function buttons to operate the instrument soft-
ware.
c START button to start an extraction.
d The STOP button comprises 3 functions:
• press once: pause the process and continue by
pressing START again
• press twice: interrupts the process and continues
with ushing using solvent and gas
• press three times: stops the process immediately,
i.e. the system remains at the very position of the
process
For more information see section 6.4.8.
e Selection knob to dene values within the instru-
ment software.
25 SpeedExtractor E-916 / E-914 Operation Manual
NOTE
The START and STOP buttons are used only for the extraction method but have no eect on functions such as preheat, leak test, or ush. All functions apart from extractions are initiated by function
buttonsb.
4.5.2 Main displays of the instrument
4 Description of function
A
B C D
A The main display shows the most important parameters of the extraction process, such as the
activated positions in the heating block, the maximum pressure at the position valves, the temperature of the heating block, the number of extraction cycles, as well as the current cycle and the time
remaining to the end of the process. The status and total remaining time are also shown in the main
display. With the 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 instrument. The valves open and close according to the stage of the method and the number of activated positions. As the name already indicates, this menu is very benecial to get a quick
overview of the current status of operation.
C EXTRACTION is used to edit and save a new method or to open or delete an existing method. It
also includes two functions that are required prior to operation: activation of the extraction positions
(OCCUPIED POSITIONS) and preheating of the instrument to the operating temperature (PREHEAT).
D MENU involves all functions that are not directly involved in an extraction method but are typically
used at start-up, during maintenance, and service, and for product information.
These four main displays contain the following elements:
26 SpeedExtractor E-916 / E-914 Operation Manual
4 Description of function
c
f
g
i
k
l
a b
i
h g f
j
o
d
n
j
m
a Current extraction cycle/total extraction cycles
b Name of the current extraction method. When the name is
d
e
h
b
e
c
a
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.
e System symbols like HEATING ( ), PUMPING ( ) or PC
CONNECTION ( ) are reversed or in case of PUMPING rotating when being active.
f Extraction positions. When the symbol is crossed out the cor-
responding position is deactivated (see section 6.4.2).
g Temperature of the heating block.
h Maximum pressure.
i Function buttons for the STATUS, EXTRACTION and MENU
submenus.
j To skip extraction steps or to stop running leak test
a Solvent reservoirs (2 or 4 ports depending on the mixer)
b Nitrogen tank
c Solvent valves
d Mixer
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 waste or collection vials
m NEXT opens a submenu where the progress of extraction run is
shown (see below).
n Waste bottle
o Collection vials
a Remaining time to nish the current extraction cycle.
a
b
c
d e
a
b
c
d
e
f
27 SpeedExtractor E-916 / E-914 Operation Manual
b Remaining time for the next manual override, i.e. exchange
of the collection vials. This only applies to methods where the
function VIAL CHANGE is activated (see section 6.4.3).
c Total remaining time to nish the extraction run.
d BACK goes to the previous STATUS overview.
e END goes back to the main display.
a Denition of the number of positions (see section 6.2.4).
b Heating up the instrument to operation temperature (see sec-
tion 6.2.3).
c Editing an existing (or default) extraction method (see section
6.4.3).
d Open an existing extraction method (see section 6.4.6).
e Save a previously edited extraction method (see section 6.4.3).
f Delete an existing extraction method (see section 6.4.3).
4 Description of function
a
b
c
d
e
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, ow rate and solvent mixtures are
dened in submenus (see section 6.2.6).
c Dening instrument settings like language, contrast of the dis-
play, acoustic signals, preheat demand when the instrument is
turned on.
d SOLVENT LIST shows the default solvent list which includes the
10most frequently used solvents. This list can be edited and
modied as needed (see section 6.2.2).
e The SERVICE FUNCTIONS submenu provides access to
main instrument components for rst 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 collection rack as well as all pressure sensors
are listed. The pump can be directly operated with dierent
ow rates. With the help of a ow test faulty lines can easily be
located. The lift of the heating block and collection rack can
be driven independently. The performance of the fan can be
changed. Information about instrument and operating hours are
shown. For further information see section 8.2.
NOTE
Some submenus contain hidden lines as it is not possible to
show all information on the display. In this case a scroll bar
on the right hand side indicates the presence of hidden lines.
Move down with down button to get access to this information.
28 SpeedExtractor E-916 / E-914 Operation Manual
4.5.3 General information on buttons
The following control buttons are available in the software for navigation and input conguration:
Open the extraction menu
Open the menu functions like leak test, instrument settings etc.
Open the status menu
Get back to the previous screen
Get on to the next screen or entries of a screen
Leave the current screen and get back to the main display
Get back to the start screen without saving possible settings
Backward button to move backward within the submenu structure
Forward button to move forward within the submenu structure
Move up within the entries of a screen
4 Description of function
Move down within the entries of a screen
Arm a screen message
Negate a screen message
Switch on the position or function
Switch o the position of function
Switch on all extraction positions
Copy the entry of currently active parameter of the extraction method to the LEAK
TEST or copy the entries of an extraction cycles
Paste the entries of a copied extraction cycle to a new cycle
Start process except for the extraction process (leak test, ush etc.)
Open the solvent list to select a default solvent
Edit the name of a solvent in the solvent list or the entries of an extraction cycle
Delete all characters of an entry when naming a solvent/program
Conrm the selection of a character when naming a solvent/program
Save a solvent/program under the entered name
Load the predened solvents by replacing the rst 10 entries of the list
Move lift (heating block or rack) up
Move lift (heating block or rack) down
Stop moving the lift
Skip an extraction step or stop the running leak test
29 SpeedExtractor E-916 / E-914 Operation Manual
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