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Knauer BlueShadow Series, Manual

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57

Index

Index

A

Abbreviations

 

52

AC system

 

10

Accessories

 

24

Accumulation of a sample

 

15

Adapter plate

 

27

Ambient conditions

 

25

, 

50

ambient conditions

 

48

Application examples

 

10

Assistant, see Multifunction module

 

31

B

Backflushing

 

13

Backflushing of a column

 

13

Backflushing of a precolumn

 

14

Biconical seal

 

29

Binary code

 

35

Buttons

 

25

, 

37

C

Care

 

44

, 

48

Ccolumn holder

 

29

Chromatography software

 

32

, 

36

Cleaning

 

48

Column selection

2-channel valve

 

12

3-channel valve

 

11

Command lines

 

40

Connector strip

 

40

Contact address

 

24

Control

analog

 

39

Binary

 

40

Customer services

 

24

D

Data transfer

Interfaces

 

32

Dead volume

 

23

Declaration of conformity

 

54

Decontamination

 

48

Device

Front view

 

25

Device overview

 

9

Device safety

 

21

Device, front view

 

25

Devices

Back side

 

26

DIP

Switch

 

42

DIP configuration

 

42

Disconnecting from power supply

 

25

Disk springs

Pressure stability

 

47

Display

 

25

Disposal

 

48

Drived, see Valve drives

 

6

Dynaseal

 

29

E

Electrical connections

 

33

Environmental protection

 

48

Exploded view of an electrical valve

 

27

Explosion hazard

 

10

F

Filter

 

23

Flammability

 

21

Flashpoint

 

22

Flat ribbon cable

 

40

G

Gradient grade, filtered solvents

 

23

Ground connection

 

26

grounding the device

 

26

H

Hotline

Europe

 

24

I

Injection valves

 

6

, 

7

Installation

 

24

Installation site

 

25

Interface Box

 

41

Interfaces

Data transfer

 

32

K

Keyboard of the device

 

37

L

Laboratory regulations

 

21

Laboratory use

 

10

LAN

 

32

Leaks

 

21

Legal information

 

53

Summary of Contents for BlueShadow Series

Page 1: ...BlueShadow Valves and valve drives Manual V7695A HPLC ...

Page 2: ...13 Backflushing of a precolumn 14 Accumulation of a sample 15 Precleaning of a sample by a precolumn 16 Precleaning of a sample 17 Alternating precleaning of a sample 18 Symbols and labels 20 Safety 21 Laboratory regulations 21 Solvents 21 PEEK connections 22 Protective measures 22 Power supply and mains connection 23 Target group 23 To what should the user pay particular attention 23 What experti...

Page 3: ...the valve 36 Control of the valve with chromatography software 36 Operating the valve drive manually 36 The keyboard for operating the device 37 Setting the position of the valve 37 Set the position manually on the valve 38 Filling the sample into the sample loop 38 Injecting the sample 39 Operating the valve drive externally 39 Analog control 39 Binary control 40 Connecting the flat ribbon cable ...

Page 4: ...50 Ambient conditions 50 Valve drive 50 Valve 51 Electrical valves 51 Manual valves 51 Abbreviations and terminology 52 Legal information 53 Warranty conditions 53 Manufacturer 53 Declaration of conformity 54 Table of Figures 55 Index 57 ...

Page 5: ...hannel valves Overview valves and valve drives Valves and valve drives are always completely assembled and tested when they leave the factory The following components may be included Fig 1 Overview valves and valve drives Main areas of application Main areas of application for multichannel valves are the injec tion or column switching the column backflushing sample accumulation or the alternating ...

Page 6: ...s with 2 channels The structure of the rotor seal in the inside of the injection valve specifies whether the valve can be operated as a 2 or 3 channel valve Fig 3 Injection valves 6P 2C and 6P 3C Legend A Position number B Connection between the central connection and the individual positions 1 6 C Adapter plate for mounting on the valve drive 4 6 2 5 3 1 A B C Legend A Position number B 6 Ports w...

Page 7: ...ltiposition valve gives the start signal for a measurement to the entire analytical system or a detector Hand operated valves For hand operated valves a mounting of a mounting plate or a universal angle on the housing of a valve drive is advisable Electrical valve drives Electrical valve drives for the injection or multiposition valves synchronize the sample injection in the analytical system The ...

Page 8: ...ri cal drives can be queried by the technical support of the manufacturer Valve Switch posi tions Operating mode 6V injection valve 2 6P 3C 6 ports 3 channels 6P 2C 6 ports 2 channels 6V Multiposition valve 6 7P 1C 7 ports 1 channel 12V Multiposition valve 12 13P 1C 13 ports 1 channel 16V Multiposition valve 16 16P 1C 16 ports 1 channel 4 6 2 5 3 1 ...

Page 9: ...Risk of explosion Never use the device in poten tially explosive atmospheres without appropri ate protective equipment and approval by a notified body Inform the technical service department of the manufacturer Application examples Abbreviations Connections and channels of an injection or multiposition valve are described by abbreviations Example 6P 3C valve That is an injection valve with 6 conne...

Page 10: ... the detector Fig 5 Column selection injection from the 6P 3C valve on column A Note Make sure there is no pressure when switching between the columns so that the columns are not damaged From the injection valve the sample is injected via the channel 2 3 onto the column B From connection 5 the components of the sample are forwarded separate to the detector Fig 6 Column selection injection from the...

Page 11: ...t columns The sample is separated on the precolumn The further separa tion can be carried out on column 1 and be continued on col umn 2 after switching over Fig 7 Column selection with a 2 channel valve Legend A Detector B Column 1 C Precolumn D Injection valve E Column 2 Injection Detector 6 1 2 3 4 5 after switching Column A Precolumn Column B ...

Page 12: ...3 The quicker part of the substances is separated through the channels 6 1 and 5 4 and flushed to the detector Fig 8 Backflushing injection from the 6P 3C valve on the column Note Make sure there is no pressure when switching between the columns so that the columns are not damaged After switching over the valve to the channel 2 1 heavily retarding substances are eluted in opposite direction fluid ...

Page 13: ...th sample through the channel 2 3 From the channel 6 1 the quickly dissolved substances on the column are measured the heavily retarding substances remain on the precolumn Note The eluent flushes the precolumn after switchover in opposite direction Fig 11 Backflushing precolumn switchover of the 6P 3C valve After switching over the valve to the channel 2 1 the late elut ing substances are flushed ...

Page 14: ...lvent A through the channel 2 1 From channel 4 3 the eluent is fed through the detector A into the waste container Note Make sure there is no pressure when switching between the columns so that the columns are not damaged After switching over the valve to the channel 5 4 a solvent B are flushed back in opposite direction through the precolumn The accumulated sample is flushed through channel 1 6 o...

Page 15: ...fer ent precolumns Fig 14 Precleaning of a sample by a precolumn After the injection of the sample on the precolumn it is heavily retarded Fig 15 Precleaning of a sample Switching over to main column After switching over the valve on the channel 2 3 the sample is flushed with a second solvent in the main column Injection on precolumn 1 2 3 4 5 6 Injection Precolumn Detector Column Switchover of th...

Page 16: ...rnating on two precolumns and analyze all substances from both precolumns The sample is precleaned on precolumn 1 and the weak retard ing substances are flushed directly on the analytical column and separated there After switching over the valves precolumn 1 is cleaned and the sample is precleaned on precolumn 2 and flushed to the analyti cal column to be separated there Note Make sure there is no...

Page 17: ...lves can be connected with each other to preclean sample alternating on different precolumns for the analysis Fig 17 Alternating sample precleaning sample is filled in the precolumn B Precolumn B is filled with sample by pump A and flushed directly to the analytical column Simultaneously precolumn B is prepared by pump B with a second solvent The solvent is fed through detector B to the waste cont...

Page 18: ...and precolumn A is filled with sample After switching over the valve precolumn B is cleaned in oppo site direction for the next analysis The sample from precolumn A is flushed in opposite direction with the first solvent into the analytical column Switchover of the direction of flow Pump B Eluent B Pump A Eluent A Waste Detector B Detector A Precolumn B Precolumn A Column Injection ...

Page 19: ...aphy column Filling for example a sample loop with sample L Load Ground connection for grounding the device Connection to the power supply with direct current 24 V and 1 5 A CE Conformité Européenne mark for equipment that complies with the per tinent EU directives and comes with a declaration of conformity from the manufacturer Marking for devices that comply with the canadian requirements for la...

Page 20: ... for laboratory work Solvents Flammability Organic solvents are highly flammable Since capillaries can detach from their screw fittings and allow solvent to escape it is prohibited to have any open flames near the analytical system Leaks and clogged capillaries Regularly check for leaks and clogged capillaries test back pressure without column Suitable Solvents Solvents suitable for use in HPLC Ac...

Page 21: ...o avoid damage from leaks always place solvent bottles in a solvent tray on the device Self ignition point Only use solvents that have a self ignition point higher than 150 C under normal ambient conditions Toxicity Organic solvents are toxic above a certain concentration Ensure that work areas are always well ventilated Wear protective gloves and safety glasses when working on the device PEEK con...

Page 22: ...ck for clogged capillaries test back pressure without column Using filtered solvents 1 Use ultra pure filtered solvents for HPLC gradient grade 2 Filtration of substances under analysis 3 Use of inline filters The device open may only be opened by the technical service department Note Only allow the technical service department of the manufacturer or a company authorized by the manu facturer to op...

Page 23: ...hecking the scope of delivery 1 Check whether the device and accessories are complete 2 If a part is missing inform the technical service department of the manufacturer Technical customer services of the manufacturer Technical customer services Europe Languages German and English Available by telephone 8 am to 5 pm CET Telephone 49 0 30 809727 0 Fax 49 0 30 8015010 E mail contact E mail info knaue...

Page 24: ...on of the position of the valve is visi ble on the device s front side the injection or multiposition valve and the buttons for operating the device Device display and buttons The display indicates the status of the valve in the position indi cator 1 Press the button to increase the position or start the filling of the sample loop by pressing the LOAD L button 2 Press the button to reduce the posi...

Page 25: ...tart signal for a measurement to the entire analytical system or a detector Electrical valves Electrical valve The electrically operated 7P 1C valve differ only in the material and some internal dimensions of components The valve body contains a rotor in its housing This rotor is preset by disk springs for a certain pressure resistance The rotation of the electrical valve can be set 360 in a preco...

Page 26: ...y around The openings for the countersunk screws point to the front 2 Fasten the adapter plate with two Phillips head screws M3 Tighten the Phillips head screw firmly Fig 22 Back side of the electrical valve adapter plate for mounting Legend A Axial plate B Axial needle bearing C Compensation plate D Disk spring E Rotor F Rotor seal G Seal ring A B C D F E G Legend A Back side of an elec trical va...

Page 27: ...e bottom of the device to make sure that the electrical control of the valve drive has been set correctly 2 Switch on the valve drive The initialization of the valve drive causes the markings on the drive axle to be on top 3 Port 1 of the injection valve has to point up Plug the injec tion valve on the drive axle on the valve drive 4 Screw the injection valve to the adapter plate with Allen screws...

Page 28: ...olumn holder Connecting capillary with valve and seal Biconical seal or Dynaseal You can use two seal types to connect the steel or PEEK capillary with the valves biconical or Dynaseal Note For pressures 50 bar you should always use a Dynaseal Legend A Valve drive B Mounting plate C Electrical injection or multiposition valve D Side holder for valves E Column holder A B C D E A Biconical seal B Cu...

Page 29: ... the syringe connection is available as PTFE or Teflon tube The sample loop is filled with a syringe or a feed pump It is necessary for this to insert a needle seal in the syringe connection and to fixate it with a biconical seal 1 Insert the needle seal in the syringe connection and put a biconical seal on the tip to seal off the needle seal 2 Screw on the syringe connection with installed needle...

Page 30: ...already permanently assembled in the factory This multifunction module carries as an order name the product name Assistant Note Explanations on the mechanism and handling of the multifunction module Assistant are described in a separate information sheet and added to the devices Legend A Injection valve B Syringe connection C Needle seal D Sample loop E Metal cannula with luer lock F Glass syringe...

Page 31: ...rea network LAN is automatically recognized by the chromatography software Device status When used in a local area network LAN the system status of the valve can be checked using the chromatography software LAN setting Ex works the valve is set to DHCP Dynamic Host Configuration Protocol This means that the valve is automatically assigned an IP address within the local network Interfaces for data ...

Page 32: ...r nal devices Use the LAN connection to connect the valve with external devices within a network Alternatively connect the valve via the communication inter face RS 232 port to a computer Caution Electrostatic discharge can damage the electron ics of the valve Never touch the electric contacts of the Remote terminal strip Remote terminal strip For receiving start control and error signals from ext...

Page 33: ...inary input is inactive during the change of the valve position This can be used to control further external devices Signal Explanation GROUND Ground connection for start and error sig nals HOME POS 1 Connection for short circuit for creating a switch signal Valve drive is set to position 1 FORWARD LOADING Connection for short circuit for creating a switch signal example for output LOADING Set the...

Page 34: ...o that the valve can be set externally in the correct position nominal position Position BIN 0 20 1 BIN 1 21 2 BIN 2 22 4 BIN 3 23 8 Result binary 1 0 0 0 0 0 2 1 0 0 0 1 3 0 1 0 0 2 4 1 1 0 0 3 5 0 0 1 0 4 6 1 0 1 0 5 7 0 1 1 0 6 8 1 1 1 0 7 9 0 0 0 1 8 10 1 0 0 1 9 11 0 1 0 1 10 12 1 1 0 1 11 13 0 0 1 1 12 14 1 0 1 1 13 15 0 1 1 1 14 16 1 1 1 1 15 ...

Page 35: ...2 Wait until the pump has completed the self test The valve is ready for operation Control of the valve with chromatography software The valve can be used with a computer and a chromatography software This information is described in the manual for the chromatography software Valves and valve drives can also be operated without software Manually by buttons of the membrane keyboard Externally and e...

Page 36: ...12 or 16 switch positions have an internal relaying e g from position 6 directly further to position 1 or back These so called 360 valves can therefore be set by one of the two buttons or in any desired position Setting the position of the valve Changing of the position of the valve can be carried out during running operation In this case the change takes effect immedi ately Set the external posit...

Page 37: ...syringe connection was mounted on the desired connec tion There are no air bubbles in the injection syringe Caution Damages to the valve due to pointed injection syringes Use only injection syringes with luer lock and flat ground cannula Set the valve to L load to be able to fill the sample loop Loading An L for loading is displayed in the display A Fig 33 Display load sample Fig 34 Injection syri...

Page 38: ...o other devices in the HPLC system Communication is possible via the following interfaces LAN RS 232 Remote control WAGO Control via one of these interfaces is executed by a terminal pro gram of a software The electrical valve drives can be controlled analog as well as binary Analog control The technical conditions for the analog and binary control of the valve drives via the interfaces and a term...

Page 39: ...es to the valve flat ribbon cables are connected with a connector strip and con nected to the Remote terminal strip on the device rear of the valve Command Action Comment 1 2 3 6 Valve sets the entered position Only 360 valves 1 2 15 16 01 Valve sets the entered position Only 360 valves H h Valve sets the position 1 Only 360 valves H home position L l Valve sets the position Loading Only injection...

Page 40: ...e terminal strip Remote is designed as a MINI WAGO connection in the construction of an open collector Connect flat ribbon cable to the connector strip Steps Figure 1 Place the connector strip C on a suitable surface 2 Put the stylus A in the opening on the top of the connector strip and press downward 3 Keep the stylus pressed down and insert the cable end B into the front of the connector strip ...

Page 41: ...39 Details of the setting of the DIP switches among the different series of the valve drives DIP Function Comment 1 Specify valve type 2 Specify valve position 3 and 4 Set the port OUT BIN 3 on the back of the device as input or output Set DIP switches 3 and 4 always opposite DIP I 0 V6 V12 V16 1 IN 360 valve 7P 1C 360 valve 13P 1C not permitted OUT 6P 2C 6P 3C not permitted 360 valve 17P 1C 2 IN ...

Page 42: ...nd setting of the DIP switches Drive Valve Mode DIP1 DIP2 DIP3 DIP4 V6 6P 2C Analog OUT OUT IN OUT 6P 3C Analog OUT OUT IN OUT 7P 1C Analog IN OUT IN OUT 7P 1C Binary IN IN IN OUT V12 13P 1C Analog IN OUT IN OUT 13P 1C Binary IN IN OUT IN V16 17P 1C Analog OUT OUT IN OUT 17P 1C Binary OUT IN OUT IN ...

Page 43: ...ps Figure 1 Alternating loosen the three Allen screws A of the valve with a screw driver M3 Hold the housing of valve together when the Allen screws are removed so that the individual parts do not fall out Fig 41 Open the valve housing 2 Take off the top part A The cylinder pins B the inner components and the rotor seal C become visible Fig 42 Remove the top part of the valve 3 Remove the rotor se...

Page 44: ...y 4 Hold the inner com ponents of the valve and turn over the bottom part in order to deposit the inner parts orderly Rotor plate with micro cylinder pins A four disk springs in two groups of two B rotor seal C several sealing disks D inside the valve Fig 44 Inner components of the valve Steps Figure A B C D ...

Page 45: ...46 Maintenance and care Alignment of the rotor seal in the valve Valve type Position of the rotor seal during installation 1 channel 2 channel 3 channel markings rotor with sealing rotor cylindrical pin ...

Page 46: ...o the syringe connection at the valve 4 Screw the screw fit ting A on the valve moderately tight 5 Insert the injection syringe all the way into the new needle seal C Loosen the screw fitting until the injection syringe can still be pulled easily but with noticeable friction straight out Fig 45 Biconical seal needle seal and screw fitting of the syringe connection Fig 46 Schematic display of the s...

Page 47: ...nces poses a hazard for all persons during operation repair sale and disposal of a device DANGER Danger caused by toxic infectious or radio active substances A contaminated device must never be submitted for repairs sold or disposed of Contract a specialist company to decontaminate the device or perform the decontamination yourself if you have the required expertise All contaminated devices must b...

Page 48: ...the motor current is too high Replacing the rotor seals of the valve E2 The change from one valve position to the next take too long Replacing the rotor seals of the valve E3 Switch position of DIP 3 and 4 are not correct Correct DIP switch 3 and 4 E4 Valve position 1 is not recognized Replacing the rotor seals of the valve E5 Switch position of DIP 1 and 2 are not correct Correct DIP switch 1 and...

Page 49: ...ite as of version 3 3 2 plus driver of the manufacturer Update firmware by the techni cal support department of the manufacturer Mains connection 24 V 1 5 A External power supply and power cable 100 240 V 50 60 Hz Integrated power supply on the multifunction module IP protection class IP 20 Weight 1 86 kg approx 5 3 kg multifunction module with pump and valve drive Dimensions length x width x heig...

Page 50: ...or ETFE Sample loops 1 16 made of stainless steel or PEEK Stainless steel 5 10 20 30 50 75 100 200 500 1000 2000 μl PEEK 10 20 50 200 500 μl 1 8 made of stainless steel or PEEK Stainless steel 1 2 11 45 ml PEEK 1 2 11 45 ml Pressure resistance maximum 300 bar 30 MPa for stainless steel capillaries maximum 150 bar 15 MPa for PEEK capillaries Weight 300 g valve Diameter valve 47 5 mm Material Stainl...

Page 51: ... filtered solvents in liquid chromatography Isocratic Sample mixtures separated by constant com position of solvent Channel The connection of two connections on the valve by a special form of rotor seal Solvents Mobile phase eluent or carrier for liquid chromatography Luer lock Standardized connection system between syringes and cannulaes NP Normal phase in adsorption chromatography OQ Comprehensi...

Page 52: ... occurs 3 Wear parts fuses glass parts columns light sources cuvettes and other optical components 4 Damage caused by negligence or improper operation of the device and damage caused by clogged capillaries 5 Packaging and transport damage In the event of device malfunctions contact Manufacturer Wissenschaftliche Gerätebau Dr Ing Herbert KNAUER GmbH Hegauer Weg 38 14163 Berlin Germany Telephone 49 ...

Page 53: ... 2009 A2 2009 EMC standarts 2004 108 EC DIN EN 61326 1 October 2006 Electrical equipment for measurement control and laboratory use EMC requirements DIN EN 61326 1 Corrigendum 2 April 2011 Directives for an environmentally sound use of electrical and electronic equipment RoHS directive 2002 95 EC February 2003 on the restriction of the use of certain hazardous substances in electrical and electron...

Page 54: ...Fig 17 Alternating sample precleaning sample is filled in the precolumn B 18 Fig 18 Alternating sample precleaning precolumn B is purged and precolumn A is filled with sample 19 Fig 19 Device front side of the valve drive with mounted injection valve 25 Fig 20 Rear view of the device with connections 26 Fig 21 Exploded view of an electrical valve 27 Fig 22 Back side of the electrical valve adapter...

Page 55: ...ve drive valve operating mode and setting of the DIP switches 43 Fig 41 Open the valve housing 44 Fig 42 Remove the top part of the valve 44 Fig 43 Deposit the rotor seal true sided with the marking of the position 44 Fig 44 Inner components of the valve 45 Fig 45 Biconical seal needle seal and screw fitting of the syringe connection 47 Fig 46 Schematic display of the syringe connection 47 ...

Page 56: ...e 23 Declaration of conformity 54 Decontamination 48 Device Front view 25 Device overview 9 Device safety 21 Device front view 25 Devices Back side 26 DIP Switch 42 DIP configuration 42 Disconnecting from power supply 25 Disk springs Pressure stability 47 Display 25 Disposal 48 Drived see Valve drives 6 Dynaseal 29 E Electrical connections 33 Environmental protection 48 Exploded view of an electri...

Page 57: ...ice 33 Room ventilation 10 Rotor seal Aligning 46 RS 232 Settings 39 S Safety 21 Sampled Backflushing 14 Samples Accumulation 15 Backflushing 13 Filling in sample loop 38 Precleaning 16 Scope of delivery 24 Seals 29 Dynaseal 29 see technical customer services 24 Selecting a column 11 Selection of a solvent 6 Self ignition temperature 22 Self test 36 Serial number 26 Series 9 Solvent Suitable to a ...

Page 58: ...ration 36 Valve positions Loading and injecting 8 Valves 6 Adapter plate 27 Chromatography software 36 Electrical 26 Exploded view 27 Increasing the pressure stability 47 Manual 26 Manual setting 38 Operation 36 Setting the position 37 W Warnings 21 Warranty conditions 53 ...

Page 59: ...727 0 Telefax 49 0 30 8015010 E Mail info knauer net Internet www knauer net www knauer net Wissenschaftliche Gerätebau Dr Ing Herbert Knauer GmbH All rights reserved The information in this document is subject to change without prior notice Translation of the original German edition of this manual 2011 01 27 Printed in Germany ...

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