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AZURA DAD 6.1L, DAD 2.1L, MWD 2.1L user manual

1. Serious or moderate injuries can occur CAUTION Moderate injuries can occur Device defects can occur Decontamination Contamination of devices with toxic infectious or radioactive substances poses a hazard for all persons during operation repair sale and disposal of a device DANGER Health danger if getting in contact with toxic A infectious or radio active substances Before disposing of the device or sending it away for repair you are required to decontaminate the device adequately All contaminated devices must be properly decontaminated by a specialist company or the operating company before they can be recommissioned repaired sold or disposed of All materials or fluids used for decontamination must be collected separately and disposed of properly Symbols and Signs The following symbols and signs can be found on the device in the chromatography software or in the user manual Warning Signs Electric shock hazard Toxic substances hazard UV light hazard eye injuries can occur Burn hazard hot components KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 14 Mandatory Signs CE Mark Installation Device Data KNAUER Installation General warning sign Moderate injuries can occur General warning sign Device defects can occur Electrostatic discharge hazard damages to system device or components can occur Obey maximum load for leak tray during
2. if there are devices set up on both sides At least 15 cm on the rear panel for the fan Setup Before you set up the device find a suitable place according to the requirements and remove the packaging as described in the following section Unpacking Prerequisite Check packaging for damage caused during transportation Tool Utility knife CAUTION Damage to the device by lifting on protruding housing parts Lift the device on the side of the housing only Process Set up the package in such a way that you can read the label Using the utility knife cut the adhesive tape and open the packaging Remove the foam insert Take out the accessory kit and the manual Open the accessory kit and check the scope of delivery In case any parts are missing contact the Technical Support Clasp the device from below lift it out of the packaging and place it on its feet Do not hold onto the front cover Check the device for signs of damage that occurred during transport In case you notice any damage contact the Technical Support Place the device in its site of operation and remove protec tive foil KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 17 Next steps Note Prerequisites Note Practical Tip Procedure Next Steps Prerequisites Auxiliary Material KNAUER Installation Store packaging and keep the included packing list for repeat orders The test cell
3. transportation installation and operation Wear protective gloves to avoid skin irrita tions A device or system marked with CE fulfills the product specific requirements of Euro pean directives This is confirmed in a Declaration of Conformity Testing seals in Canada and the USA at nationally recognized testing centers NRTL The certified device or system has successfully passed the quality and secu rity tests This chapter describes all preparatory steps prior to the start up If you encounter difficulties during installation contact the Technical Support Contact Data Transport Carefully prepare the device for transport or storage If you want to return your device to KNAUER for repairs enclose the Service Request Form which can be downloaded from our website For a secure transport note the weight and dimensions of the device see Technical Data DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 15 Lifiting Earthquake Areas KNAUER Installation CAUTION Damage to the device by lifting on protruding housing parts Lift the device on the side of the housing only Clasp the device at its side panels and lift it out of the packaging Do not hold onto front cover or leak tray Operating Environment Only if the requirements for ambient conditions of the operating environment are met can the intended use be ensured You will find the ambient conditions under Technical Data a
4. 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 64 Index L lamp replace 49 lamps 8 LAN 20 40 port 23 problems 40 router 23 settings 21 setup 22 leak 12 management 8 19 remove 52 sensor 52 LED 31 Legal Information 57 location 32 Luer lock cannula 58 M maintenance 45 contract 46 intervals 46 mandatory signs 14 mirror 8 Mobile Control 30 46 mobile phase 59 modifiers 9 O OpenLAB 30 operating environment 15 operating hours 46 operating ranges 6 operation 29 Control Unit 30 software 30 optimize 32 wavelength 35 optional accessories 9 OQ 39 order numbers 60 P packing list 17 path length 34 peak broadening 33 PEEK 9 fittings 19 pin header Autozero 26 connect 26 connectors 24 Start IN port 25 port LAN 23 power connect 27 disconnect 15 plug 15 strip 12 supply 12 power supply cable 12 pressure maximum 35 problems 41 further measures 41 professional group 11 R rear view 6 reference wavelength 35 36 default 36 refractive index 35 remote connector pin header 24 remote operation 35 repeat orders 59 accessories and spare parts 60 device 60 fiber optics 62 flow cell 61 re set 32 response time 37 59 router LAN 23 S safety 11 safety equipment 11 salts 9 sample 59 selectivity 36 self validation 30 sensitivity 33 35 36 service 46 setup 16 side view 7 signal level 38 signal wavelength 35 36 software 46 solvent flammab
5. DAD 6 1L AZLO2 standard deuterium lamp for DAD 2 1L A5193 and MWD 2 1L A9846 1 P6431 P6432 P6424 P6425 A9842 A9843 A9844 A9853 5 AZDOO FZAO2 DAD 6 1L DAD 2 1L MWD 2 1L accesso FDC ries kit AZURA tool kit corrugated hose 16 cm PE grey funnel exhaust capillary guide top capillary guide bottom kit LightGuide flow cells 1 16 kit UV flow cells 1 16 kit UV flow cells 1 8 mounting bracket for flow cells Control Unit CU 2 1 AZURA accessories kit A1033 DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 61 Accessories and Spare Parts Flow Cells Technical Data Order Number 10 mm AMC19 1 16 2 ul 0 8 ul dispersion vol PEEK quartz Teflon 5 ml min 100 bar KNAUER LightGuide Flow Cell Cartridge path length connection volume wetted parts max flow rate max pressure KNAUER LightGuide High Sensitivity Flow Cell Cartridge path length connection volume wetted parts max flow rate max pressure 50 mm AMD59 1 16 6 ul 2 ul dispersion vol PEEK quartz Teflon 5 ml min 100 bar Flow Cells with Fiber Optics Note Flow cells with fiber optics are connected to the devices via a fiber optics adapter The fiber optic cables must be ordered sep arately Technical Data path length 10 mm A4074 connection 1 16 volume 10 ul wetted parts SS quartz PEEK max flow rate 20 ml min max pressure 300 bar path length 3mm A4044 connect
6. can not for operation be processed activate service mode Invalid command Check the cable connections Change the entry Wrong command was transmitted to the device Check if the command is valid Invalid parame Correct command incorrect parame ter s ters Check if the parameters are valid L Lamp cover open The lamp cover was mounted incor rectly or the micro switch is malfunc tioning Mount the lamp cover In case the sys tem message repeats itself inform the Technical Support of KNAUER Lamp not installed GLP data can not be read and lamp operation can not be executed as the lamp D2 or halogen has not been installed KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 44 Troubleshooting System Message Problem and Solution Lamps off Command can not be executed as the lamps are being switched off Lamp supply is not Power supply of lamp has not been available installed or does not react Lamp supply tem The upper temperature limit for perature limit power supply of lamp was exceeded exceeded Lamp unit tem The upper temperature limit for lamp perature limit unit was exceeded exceeded Lamp unit tem Temperature sensor of lamp unit was perature sensor not found or does not react failed Leak sensor failed Switch the device off and then on If the leak sensor is still not present contact the Technical S
7. chemically compatible with the solvents and sample you are working with Stainless steel and metal free flow cells are available The metal free variants are bio inert Pressure Stability The different flow cells can withstand various maximum pres sures The upper pressure limits of the flow cells are 30 bar 100 bar or 300 bar The flow cell should not be subjected to the maximum pressure for a long period of time Connection Undesired effects like the loss of resolution in the chromato gram may be prevented by ensuring a correct connection to the flow cell and the removal of any dead volume Remote Operation Fiber Optics If the flow cell must be positioned outside of the detector e g In an explosion proof room at higher temperatures such as in an oven or in an environment with radioactive substances the devices can be optionally equipped with fiber optic connectors Remote flow cells are recommended for preparative applications high flow rates in order to protect sensitive optical compo nents from potential leakages For detectors with fiber optic cables the light intensity does not depend just on the lamp and the cell but also on the quality condition of the fiber optic cables the quality of the connec tions the length of the fiber optic cables the number of bends and the bending radius Sensitivity is typically reduced to half that of an equivalent stan dard cell when working with standard length fiber op
8. or bending it The flow cells with fiber optics are connected via an adapter No flow cell or test cell is installed Screw type cap fittings for the fiber optics DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 18 Installation WARNING AN Irritation of retina through UV light Concen trated UV light can leak out from the flow cell or the fiber optic connectors Switch off the device or the lamps Note Fiber optical connectors like all other optical parts should never be touched without wearing gloves because otherwise contami nations may reduce light intensity Contaminated parts may be cleaned with a soft cloth and isopropanol Remove the cap fittings from the adapter Place the adapter into the opening and slide to the back until it Fig 7 fiber optics adapter clicks into place inside the device Remove the screw type cap fittings from the fiber optics Manually screw the cap fitting on the fiber fiber optics to the optics adapter Remove the cap fittings from the flow cell Manually screw the fiber optics to the flow cell Fig 9 X fitting of the fiber optics on the flow cell Next Steps Connect the capillaries Connecting the Capillaries Capillaries connect the detector with the column and guide liq uids For the flow cell connectors we recommend PEEK capillar ies and PEEK fittings Prerequisites The flow cell was inserted Screw type cap fittings
9. programming wake up IP 20 IP protection class Technical parameters GLP function Detailed report about lamp recogni tion operating hours lamp operating hours number of lamp ignitions Mobile Control or Control Unit optional display Ambient Conditions temperature range 4 40 C 39 2 104 F KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 56 Disposal air humidity below 90 non condensing height above sea maximum 2000 meters level power supply 100 240 V 50 60 Hz 75 W General Disposal AVV Marking in Ger many WEEE Registration Solvents and Other Operating Materials KNAUER dimensions 361 mm x 158 mm x 523 mm widthx height x depth weight 12 2 kg yes leak sensor Conditions for Specification Technical data has been determined in accordance with the ASTM standard E1657 98 Standard Practice for Variable Wave length Photometric Detectors Used in Liquid Chromatography Reference conditions test cell at wavelength 254 nm 8 nm with reference wavelength 360 nm 30 nm time constant 2 s data rate 1 Hz Linearity Linearity is measured with caffeine at 274 nm 8 nm and time constant 2 s with a flow cell path length 10 mm Performance tests should be done with a completely warmed up optical unit gt 2 hours ASTM measurements require that the detector should be turned on at least 24 h before start of test ing ASTM drift tests require a tem
10. retention in which the interactions between the solute an dthe surface of an adsorption adsorbent dominate analytical Qualitative analysis of samples in HPLC backflush Useful in chromatography to remove com ing pounds that are held strongly at the head of a column calibration A process for correcting measuring values by the value that a measuring device deviates from the standard capillary Tubing to connect various parts of the chro matograph in order to direct flow to the proper place carrier Refers to the support that is used to attach the active ligand usually by a covalent bond chromato A plot of detector signal output versus time or gram elution volume during the chromatographic process column The tube and stationary phase through which mobile phase flows resulting in a chromato graphic separation correction factor that arithmetically corrects device factor related deviations from measuring values dead vol Dead volume is extra volume experienced by ume solutes as they pass through a chromato graphic system in particular any unswept vol ume exposed to the mobile phase flow degassing The process of removing dissolved gas from the mobile phase prior or during use detector device measuring the composition or the quantity of a substance gradient A process to change solvent strength as a func tion of time normally solvent strength increases thereby eluting progressively more
11. selecting the signal and reference wavelengths the respective bandwidths must also be selected see the following section Bandwidth The bandwidth defines the total number of wavelengths actually registered by the photodiode when a specific wavelength is set For example a wavelength set at 254 nm width a bandwidth of 4 nm results in average absorption of 252 256 nm Raw data Fig 29 bandwidth The selection of bandwidth is a balance between sensitivity and selectivity Narrow bandwidths increase selectivity whereas broad bandwidths increase sensitivity By default see Resetting the Device on page 32 the band width for the signal wavelength is set to 8 nm and for the refer ence wavelength the bandwidth is set to 30 nm Spectral Range When measuring with chromatography software the spectral range selected for a given measurement influences the required disc space The disc space is necessary to save generated data A narrow spectral range reduces disk space The range how ever should be wide enough to ensure the detection of all com DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 37 Response Time Time Constant Data Rate Default Data Rate Optimizing the Data Rate KNAUER Optimizing the Detector ponents Also the spectral range always must include the signal wavelength and the reference wavelength when applicable Time Constant amp Data Rate The time constant influences
12. the computer or tablet to a wireless LAN router Data transfer between device and app is actualized through DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 31 O Left LED Center LED Right LED Switch Standby but ton Standby Note Left LED Center LED KNAUER Operation wireless LAN You find a detailed description on the Mobile Con trol in its accompanying user manual Meaning of the LEDs There are three LEDs and a switch on the front of the device D Oo Fig 23 LEDs and switch standby button on the front of the device The LEDs can have different colors depending on the operating conditions To start the standby keep the standby button pressed for 5 seconds Malfunctioning system after repeated standby possible After repeatedly using standby restart the device using the power switch to reset the device s data storage red Error Message Check the sys tem Shortly press the switch to deactivate the error message green 3D data are acquired does not light The lamp has been switched off flashes green The lamp lamps Wait until the are initializing or lamp is running the validation is or the valida progressing tion is finished green The deuterium lamp is active DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 32 Optimizing the Detector Right LED green The device has been switched on flashes green The device not Wait until the r
13. the depressor tool D into the opening on the upper side Continue pushing the depressor tool down and lead the cable into the front end of the terminal strip Remove the depressor tool Check whether the cables Fig 20 terminal strip are tightly attached Plug the terminal strip onto the multi pin con nector Next steps Finish the installation and perform the initial startup Integrator Connector The integrator output supplies the current signal value as an analog voltage max 5 V The integrator output is connected to other instruments with the analog connection cable or other special connection cables For details on the integrator connector see the list below non bipolar 4 channel Oto5V DAC 16 bit scalable Adjustable to offset Power Connection Note The nominal capacity of the connected devices must be maximum 50 of the power supply to account for larger inrush currents when switching on the modules The maximum power input is 75 W Prerequisites The electrical power supply at the installation site must be connected directly to the nearest main power line The power must be free from ripple residual current voltage peaks and electromagnetic interference The connectors for the mains voltage are grounded accord ingly The device receives sufficient power with reserve capacity KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 28 Power Cab
14. the response time of the detector The response time determines how quickly the detector responds to a change in signal A good rule of thumb for selec tion of the time constant is that it should be no larger than i of the baseline peak width of the first peak of interest in seconds Increasing the time constant allows more averaging of the signal also known as digital filtering and results in less baseline noise However increasing the time constant too much may result in broad peaks reduced peak heights and asymmetric peak shapes Therefore a compromise has to be found Using the time constant a signal smoothing can be achieved The larger this value is set the more the signal will be smoothed In general the best time constant is the reciprocal of the data rate see table below If increased sensitivity is desired or if the baseline noise is interfering with integration the time constant should be increased If resolution is compromised it should be decreased It is recommended to set the time constant and data rate in rela tion to peak width Wd 8 ORE The data rate or sampling rate is the number of data points per second Hz at which the detector transmits data to the com puter The default data rate setting for the detectors is 1 Hz see Resetting the Device on page 32 The maximum data rate digital signal is 100 Hz Lower data rates store average data points A 50 Hz data rate averages 2 points A 10 H
15. to be separated in the chromatographic col umn solvent The liquid used to dissolve a sample for the injection into a chromatography column or CE capillary stationary The immobile phase involved in the chromato phase graphic process It is the liquid or the liquid film on the surface of the packing material Accessories and Spare Parts Note For repeat orders of spare parts use the enclosed packing list Contact the Technical Support in case there are any questions on Spare parts or accessories Further Information Further information on spare parts and accessories can be found online www knauer net KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 60 Accessories and Spare Parts DAD 6 1L DAD 2 1L MWD 2 1L User Manual Operation Qualifica tion Installation Qualifica tion Lamps Drainage System Waste Tubing Kit Mounting Bracket Control Unit Accessories Kit Tools KNAUER Device Order Number diode array detector DAD 6 1L with test ADC11 cell diode array detector DAD 2 1L with test ADCO1 cell multi wavelength detector MWD 2 1L with ADBO1 test cell upgrade MWD 2 1L to DAD ADB01 UMBAU Accessories and Spare Parts Order Number V6700 VOQDAD61L VOQDAD21L VOQMWD21L VIQDAD61L VIQDAD21L VIQMWD21L AZLO1 user manual EN DE DAD 6 1L DAD 2 1L MWD 2 1L DAD 6 1L DAD 2 1L MWD 2 1L high intensity deuterium lamp for DAD 6 1L halogen lamp for
16. 750 mm 2 x fiber optics custom made 1 x fiber optics 400 mm 1 x fiber optics 750 mm KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 63 Index Index A absorption 35 36 57 58 accessories 10 adapter 17 additives 9 ambient conditions 15 47 52 53 54 55 analog port 27 analytical 58 AVV marking 56 B backflushing 58 bandwidth 36 default 36 Beer Lambert law 34 C capillary 18 58 fitting 19 lock ring 19 pre installed 29 torque 19 care 46 chromatogram 58 ClarityChrom 30 clean 46 conditions for specification 56 contact data 46 control 20 30 Control Unit 20 LAN 20 Control Unit 20 30 46 cutoff 35 D D2 lamp replace 49 data rate 8 37 default 37 optimize 37 dead volume 35 decommissioning 47 decontamination 13 default settings 32 degasser 58 detector 58 optimize 32 KNAUER rear view 7 technical data 52 device overview 6 disposal 56 drift 35 E eluents 9 F features 7 fiber optics 17 62 adapter 17 flow cell 17 fittings 47 flow cell 8 clean 48 connection 35 fiber optics 61 insert 17 material 35 path length 34 pressure stability 35 rinse 48 select 33 volume 33 flow cell cartridges 8 front view 6 functionality tests 39 G general 39 glossary 57 GLP data 8 gradient 58 GROUND see spring strip 26 H halogen lamp replace 49 HPLC glossary 57 installation 14 site 15 integrator 27 intended use 6 IQ 39 isocratic 58 DAD
17. Acknowledge the error message via Mobile Control Con trol Unit the software or the standby switch without soft ware control Next Steps Bring the device into operation Technical Data DAD 6 1L Detection detector type diode array detector number of diodes 1024 resolution of diodes 0 8 nm diode detection channels 8 digital 4 analog light source high intensity deuterium Dz lamp and halogen lamp with integrated GLP chip wavelength range 190 1000 nm spectral bandwidth lt 3 5 nm at Ha line FWHM Note digital bandwidth 1 32 nm wavelength accu 1 nm racy wavelength verifica internal holmium filter and deuterium tion lines wavelength preci lt 0 5 nm sion noise 3 5 pAU at 254 nm drift 300 uAU h at 254 nm linearity 2 0 AU at 274 nm time constants 0 0 0 1 0 2 0 5 1 0 2 0 5 0 10 05 integration time automatic 5 1000 ms KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 53 Technical Data Communication maximum data rate 100 Hz LAN 12 5 Hz analog inputs Error IN Start IN Autozero 0 10 V Analog IN outputs Events 1 2 Error OUT 5 V Valve 24 V Valve OUT control digital LAN DHCP remote connector manual Mobile Control or Control Unit optional IP protection class IP 20 Technical Parameters GLP function Detailed report about lamp recogni tion operating hours lamp operating hours number of lamp ignitions display Mobile Cont
18. CC SAU Sorge 47 Disconnecting the Power Supply 20 2 eee eee ee eee eee 47 KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 5 Table of Contents Cleaning the Flow Cell scada nie A pees en es 48 RINSING the FIOW Cell 225 opus a Besos eee es 48 Replacing the FHlowW C ellssoaia ctas a om hcg tring eae She BEES gee oe 48 Replacing Ne Lamps 4424 ch0ne dre Ree der idu dee o ee e sak ae 49 Removing the Deuterium or Halogen Lamp o o oo ooooomo o o 49 Installing the Deuterium or Halogen Lamp oo ooooomooo oo 50 REMOVING Me LeaKk s oce rio ooh bo ebbe ea ADDE RO Slut USUS 52 Technical Data 4 99 1 21 3 29 NUI Eo uideri eu de 52 DAD STE xod rr PET S d HERO SS ded edd me asias 52 DADE2 E ts E S lo dear ack Saepe 53 MWD Z DT 55 Conaltions FOr Specifications ess aea a ete be a as 56 DIPO ale e wel oes crane E qua E wins euet ans E bad 56 Legal INtOrMatON 42 599 3 279 809 370 vts ainia lia 57 Waranty Conditions oor taii hrs bett ON e dove acer eee ks dios 57 Transport Damage 354 hice mcs emo dedii ue rm EUR as 57 HPEC CIOS ai V ai iia ind sudo math dur dau aS 57 Accessories and Spare PartS oooooooooocmo morro roo 59 DEVIC cose aede ARR bc UPON Mb En we ee ea eee Ge aa 60 Accessories ard Spare Parts xut pato fae enu ace tior dedos e 60 FOW CONS ecos tai sd UTR S actio Mudo queer EPOR e Reg oe ao e da 61 Flow Cells with Fiber Optics tox semen Rs dede EE 61 Fiber ODUG Cables
19. D 2 1L user manual V6700 version 2 1 20 Installation 2 Push the long ending of the first nozzle into the hose Abb 13 Hose and nozzle Connect the nozzle and the funnel Push the other end of the hose onto the noz zle of the leak tray on Fa k pa E wo ie e 4 La Abb 14 Hose connected to device 5 For the bottom device push the short end of the nozzle into the opening in the collec tion point of the leak tray Connect the hose to Abb 15 Leak tray with nozzle the nozzle and lead the second ending to the waste bottle Place the waste bottle below the bottom device Next steps Attach the front cover Control The detector can be operated in two ways via remote connector as part of a LAN via the LAN connector of the router All connectors for external control are located on the rear side of the detector The detector can also be controlled via Control Unit or Mobile Control The Control Unit connector is located on the side of the device KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 21 Legend integrator outlets LAN connector service interface multi pin connector USB port for the Control Unit Note Process KNAUER Installation Q0 Fig 16 connectors on rear side Fig 17 USB port for the Control Unit Connecting the Device to the Computer This section describes ho
20. Defective power cables are not to be used to connect the device and the power sup ply system self ignition point Only use eluents that have a self ignition point higher than 150 C under normal ambient conditions power strip If several devices are connected to one power strip always consider the maxi mum power consumption of each device power supply Only connect devices to voltage sources whose voltage equals the device s volt age toxicity Organic eluents 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 Where is use of the Never use the system in potentially explosive atmospheres with device prohibited out appropriate protective equipment For further information contact the Technical Support of KNAUER Decommissioning the At any time take the device completely out of operation by Device Securely either switching off the power switch or by pulling the power plug Opening the Device The device may be opened by the KNAUER Technical Support or any company authorized by KNAUER only Definition of Personal and Material Damage Possible dangers related to the device are divided into personal and material damage in this user manual KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 13 Symbols and Signs Category Explanations DANGER Lethal or very serious injuries can occur WARNING
21. ID are less affected by the volume of the flow cell The flow rate should also be taken into consideration A lower flow rate increases the axial and longitudinal diffusion and adds to a broadened flow profile which may lead to a peak broaden ing Path Length As described by the Beer Lambert law the path length of a flow cell affects the light intensity that is detected A logT log 2 g xdxc O Fig 26 Beer Lambert law measured absorption at a given wavelength transmittance defined as the quotient of the light intensity 1 after passing through the sample and the initial light intensity 75 before passing through the sample E molar absorptivity coefficient wavelength and tem perature dependent CE path length analyte concentration temperature dependent For the same concentration the peak height will be higher if the path length is longer Path lengths of 3 mm 10 mm and 50 mm are available for the detectors A longer path length therefore increases the sensitivity of a method see figure 27 The limit of detection is inversely proportional to the path length DAD 6 1L 50 mm 6 yl LightGuide Cartridge DAD 6 1L 10 mm 2 pl LightGuide Cartridge path length comparison DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 35 Signal Wavelength Baseline Correction Reference Wavelength KNAUER Optimizing the Detector Wetted Parts The flow cell materials must be
22. and PEEK capillaries are color coded according to their inner diameter Wim 0 INN red marker PEEK 0 1 mm blue marker PEEK 0 25 mm orange marker PEEK PEEK capillaries are not suitable for use with pure acetonitrile Acetonitrile can cause capillaries to crack or rupture In this chapter you find the information relevant for operating the detector Initial Start Up Use this checklist to determine whether the detector is ready for initial start up Device is positioned in the correct location The power plug has been connected If the device is part of an HPLC system you should also note the following he network connection to the router is established he chromatography software has been installed by KNAUER or a company authorized by KNAUER A flow cell was inserted The capillaries have been connected Switch On Installation has been completed A flow cell was inserted CAUTION Possible damage to the device caused by con densed water Allow device to acclimate for 3 h before it is con nected to power supply and taken into operation DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 30 Procedure Result Next Steps Note KNAUER Operation 1 On the rear of the device plug the power cable into the power E connector 2 Plug in the power sup ply Fig 22 power switch with 3 On the rear of the female connector at the device switch on t
23. and cap fittings were removed Procedure Attach the capillaries with screw fittings Note The KNAUER LightGuide flow cell cartridges have unisex input and output connections KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 19 Installation CAUTION Damage to the flow cell caused by strongly tight ened fittings Check the torque of screw fittings 5 Nm for stainless steel fittings 0 5 Nm for PEEK fittings Procedure Process Push the capillary through the fitting Slide the lock ring over the tubing Note that the tapered end of the lock ring has to point to the seal ring Attach the seal ring Fasten the capillary at the flow cell finger tight flow cell with capillary Next Steps Bring the device into operation Using the PEEK Fittings PEEK fittings withstand a maximum pressure of 400 bar Note the torque of 0 5 Nm Connecting the Leak Management The leak management consists of the leak sensor and the drain age system The drainage system ensures that escaping liquids flow into a waste bottle If there is too much liquid the red LED starts flashing Both the device and the data acquisition via chro matography software are stopped Prerequisite The front cover has been removed 1 Carefully push the fun nel into the center opening of the capillary guide Abb 12 Funnel and capillary guide KNAUER DAD 6 1L DAD 2 1L MW
24. ccessories Kit DAD 6 1L AZURA DAD 2 1L detector with test cell power cable user manual German English Installation Qualification Accessories Kit DAD 2 1L AZURA MWD 2 1L detector with test cell power cable user manual German English Installation Qualification Accessories Kit MWD 2 1L AZURA KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 11 Safety for Users Safety for Users Professional Group Safety Equipment What must be taken into account KNAUER The user manual addresses persons who are qualified as chemi cal laboratory technicians or have completed comparable voca tional training The following knowledge is required Fundamental knowledge of liquid chromatography Knowledge regarding substances that are suitable only to a limited extent for use in liquid chromatography Knowledge regarding the health risks of chemicals Participation during an installation of a device or a training by the company KNAUER or an authorized company If you do not belong to this or a comparable professional group you may not perform the work described in this user manual under any circumstances In this case please contact your supe rior When working with the device take measures according to lab regulations and wear protective clothing Safety glasses with side protection Protective gloves ab coat All safety instructions in the user manual The environmental in
25. ces for sending start control and error signals to external devices 56 Error OUT m C z LLI LLI Valve OUT EN Valve 24V Az O 12345678 9101112 Fig 19 relation between display and terminal strip ED Autozero DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 25 Installation Connections to the Terminal Strip m EV 1 Event 1 Relay Contact The contact is on a floating basis Its setting depends on the settings in the Control Unit Mobile Control or soft ware Steady rate signal passive open relay contact 0 active closed relay contact e Pulse Closed relay contact for at least 1000 ms Permissible load of the relay contact 1 A 24 V DC EV 2 Event 2 TTL Output Levels passive 5 V active 0 V Pulse QV for at least 1000 ms Error OUT TTL Output Levels passive 5 V active O V e Output is active until the Error con dition has been eliminated Error IN TTL Input Low active Secure switching threshold at least 10 mA After receiving a signal short circuit to ground from an external device an error message appears and the device stops Start IN TTL Input Low active Secure switching threshold at least 10 mA After receiving a signal short circuit to ground from an external device the device starts If controlled with soft ware an electronic trigger is send through the LAN KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manua
26. ch off the device and pull the power plug DANGER High voltages pose a life threatening risk Before opening the device turn off the device and pull the power plug KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 46 Hotline Europe E mail Operating Hours KNAUER Maintenance and Care Users may perform the following maintenance tasks themselves Regularly check the operating hours of the lamp Inspect the installation of the flow cell Replace the flow cell Replace the lamp Proper maintenance of your HPLC device will ensure successful analyses and reproducible results You find the order numbers for the desired spare parts at the end of this manual see Accessories and Spare Parts on page 59 Contacting the Technical Support If you have any technical questions regarding KNAUER hardware or software please use one of the contact options below Technical Support hotline Languages Available by telephone in German or English 8 am to 5 pm CET Phone 49 30 809727 111 Telefax 49 30 8015010 supportOknauer net Maintenance Contract The following maintenance work on the device may only be per formed by KNAUER or a company authorized by KNAUER and is covered by a separate maintenance contract e Opening the device or removing housing parts Maintenance Intervals Using the Control Unit Mobile Control or software you can read out the operating hours of the detect
27. commended operating time of the deuterium lamp is 2000 hours he recommended operating time of the halogen lamp is 1000 hours Fig 32 overview deuterium lamp and halogen lamp Removing the Deuterium or Halogen Lamp The device is switched off The lamp has cooled down Allen screwdriver 2 5 mm If the device is still in operation the integrated security switch turns off the lamp automatically on opening the lamp cover An error message is displayed Additionally the red LED lights up and the center LED doe not light DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 50 Maintenance and Care DANGER AN High voltages pose a life threatening risk Do not change lamps if the lamp area is not voltage free Check the status of the lamps in the software and on the LEDs WARNINC Burn hazard from hot lamp Switch off the lamp meanwhile the device remains switched on for further 15 minutes oth erwise the lamp can not cool down Afterwards switch off the device and pull the power plug Deuterium Lamp Loosen the screws D and of the lamp cover Remove the lamp cover Loosen the lock ring 3 or 4 of the lamp plug and pull out the plug Using the screw driver loosen the two screws or O Remove the lamp Fig 35 screws on the lamp socket Next Steps Insert a new lamp Installing the Deuterium or Halogen Lamp Removing the lamp cover switches off t
28. contact the Technical Support of the manufacturer Suitable Eluents acetate buffer solutions acetone at 4 C 25 C 39 2 C 77 0 F acetonitrile benzene chloroform ethyl acetate ethanol formiate buffer solution isopropanol carbon dioxide liquid 99 999 96 CO methanol phosphate buffer solutions 0 5 M toluol ammoniated dilute solution acetic acid 0 1 1 96 at 25 C sodium hydroxide 1 M water 1 valid for the specified temperature range 2 notrecommended in combination with PEEK small parts and PEEK capillaries Less Suitable Eluents diethylamine 0 1 96 DEA dimethyl sulfoxide DMSO slightly volatile eluents methylene chloride tetrahydrofuran THF phosphoric dilute acid triethylamine 0 1 TEA trifluoroacetic acid 0 1 TFA DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 10 Scope of Delivery 1 not recommended in combination with PEEK small parts and PEEK capillaries Unsuitable Eluents halogenated hydrocarbons e g Freon concentrated mineral and organic acids concentrated bases eluents containing particles perfluorinated eluents e g Fluorinert amp FC 75 FC 40 perfluorinated polyether e g Fomblin Scope of Delivery Note Only use original parts and accessories made by the manufac turer or a company authorized by the manufacturer DAD 6 1L detector with test cell power cable user manual German English Installation Qualification A
29. cting the Device to the Computer l l 21 Configuring the LAN Settings llle 21 Connecting Me CADDIES s ord oe tue sarao roads 22 Contiguring he ROUEN cuts aber eet Sood ets 23 Integrating the LAN into a Company Network less 23 Controlling Several Systems Separately in a LAN 23 Using Remot Control adag e yates Eat edt eee ee ees 24 Connections to the Terminal Strip o oo oooooooooooo oo 25 Connecting Cables to the Terminal Strip o oo ooooo o 26 Integrator Connector seres laos eoe dati Ca d peda 27 KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 4 Table of Contents POWER Cor necHlolbi s 4 a deba asadas 27 Integrating the Detector into the SysteM oo oo ooooooo leen 28 Pre Installed Capillaries 3 ptor vi SEO ETE a eux Seir d aC aor 29 Operadlo PP iaa ess 29 IMA Star m pa et prada ee dette tata Aroa aos 29 INACIO eta aaa rrr 29 ODSI ALIOD aq Sos aio Cord tacita cerda carr soeces 30 Operating with Chromatography Software oo ooooooo ooo o 30 Operating with Control Unit llle 30 Operating with Mobile Control o o o oooooooooooo oo 30 Meaning or e LEDS s sa soot ac RR dao 31 Resetting the DEVICE sende ss ek P Bog l ace S names aet sU dah eR e deu Rebus 32 Optimizing the Detector session 32 LOCALO DECR ES ENN ty a ES EIL S LOL ETT 32 Wal MiS ep uM anto ee etri e unns uita ring
30. d changes are made to the device During the warranty period any components with material or design related defects will be replaced or repaired by the manu facturer free of charge This warranty excludes the following accidental or willful damage damage or errors caused by third parties that are not contrac tually related to the manufacturer at the time the damage occurs wear parts fuses glass parts columns light sources cuvettes and other optical components damage caused by negligence or improper operation of the device and damage caused by clogged capillary packaging and transport damage In the event of device malfunctions directly contact the manu facturer KNAUER Wissenschaftliche Gerate GmbH Hegauer Weg 38 14163 Berlin Germany Phone 49 30 809727 111 Telefax 49 30 8015010 e mail info knauer net Internet www knauer net Transport Damage The packaging of our devices provides the best possible protec tion against transport damage Check the devices for signs of transport damage In case you notice any damage contact the Technical Support and the forwarder company within three workdays HPLC Glossary In the following chapter you find abbreviations and terminology that is used in HPLC absorption The process of retention in which the solute partitions into a liquid like coating DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 KNAUER 58 HPLC Glossary A process of
31. e ded erus aote 33 Selecting Ne FlOW Cell veces ERR RENI QUE E M Merxsuts xe 33 FIOW Cell Volum 26 s Stu aate wee ee als Docta aN 33 A A 3 a eens Soe ESSE IM fud oed its 34 WAIE PES 2 4 na up Grp ded dep uh Vo RODEO A quw eve acq 35 Pressure STADI maiman a Ea y e arte oo agii ai ad ot Dee ed Gap ae a 35 CODD EO NE don does ane ant eats teh a Sar E A ira dL Denia ut ecos 35 Remote Operation Fiber Optics ooooooocooooooomo ooo 35 Selecting the Wavelength vado sie A 35 Banawidt are oe casks oe ee OU ae Pee oe aoe aa ee eee 36 Neroni Range 20 ebexeat benno ERNE gen Baek e ead eens 36 Time Constant amp Data Rate ee ee ene 37 tegration TIBI naaa erat salt qe Set atch o e ci ias 38 Subtraction of the Baseline Chromatogram 020e ee eee 38 Generals sul cares Os e Bees sa Bi ees oS 39 FUNCUONGAIILY Tests i25 dir aa 39 Troubleshooting 24 iia aa 40 A O eee ONE 40 Possible Problems and Rectifications ooooooooooo momo 41 SYSE MESSIES taria ass 41 Maintenance and Care ooooooooooooomo ooo ooo 45 Contacting the Technical Support o o ooooooocooonoooooo ooo 46 Maintenance Contracts evi ctade mal qae Sco bw A RIS DA TR 46 Maintenance Intervals i4 3 s mE A A AA 46 Cleaning and Caring for the Device llle 46 CHECKING the FIEBETGS rasca des eh ecco e aaa BERS Ai 47 DECOMMISSIONING 55s uet Foe X Sane dela RE aS os RR 47 STORAGE axis sequ ug PENNE Na Rd N
32. e device matches the port in the chromatography software Possible Problems and Rectifications Baseline drift Maintain constant temperature condi tions during the measurement Device cannot be Inspect the power cable to ensure that switched on it is plugged into the power supply Device cannot be 1 Insert the test cell calibrated 2 Inspect the calibration with a weak absorbing eluent Baseline noise Inspect the flow cell assembly Exchange the defective flow cell Inspect the service life of the lamp on the display Reduce the air in the flow cell by using a degasser The relationship of Flush the flow cell the signal to the Replace the lamps light path reference is very low Further Measures Install the maintenance software service tool Save device information and send to manufacturer Inform the Technical Support of KNAUER System Messages If other system messages are displayed besides those listed below please turn the device off and then on Inform the Tech nical Support of the manufacturer in case the system message repeats itself The system messages are in alphabetical order System Message Problem and Solution Ambient tempera Temperature sensor on the mainboard ture sensor failed was not found or does not react C Cannot initialize Check cables and connections in local LAN area network KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 42 Tro
33. eady for opera device is ready tion for operation The device is in Press the standby standby but ton to end the standby Resetting the Device Using the Control Unit you can re set the detector to its default settings Reference correction Reference channel enabled for channel 1 WL 360 nm BW 30 nm ke Optimizing the Detector In this chapter you find information on how to optimize your detector Location In order to ensure thermo stability and to prevent drift effects note the following aspects Protect the detector against strong ventilation Protect the detector against direct sunlight Note the space requirements Avoid vibrations KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 33 Optimizing the Detector Warm Up Time The recommended warm up time for the detectors is 30 min utes This recommendation is applicable after turning the detec tor on as well as and after turning the lamp s on o Device working temperature Room o temperature Te 100 ES 150 15 200 225 250 756 300 25 0 175 400 425 45 Minutes Fig 24 cold start temperature profile Selecting the Flow Cell Several different flow cells are available for the detector see Flow Cells on page 61 Note that the detector is shipped with a test cell A flow cell must be ordered separately Signal sensitivity peak broadening and response can all be affected by the choice of
34. ed spectral range or the selected path length bandwidth WL validation Wavelength accuracy test failed failed Restart the validation Holmium oxide and or Ha Hg lines do not meet the specifications In case the system mes sage repeats itself inform the Techni cal Support of KNAUER Maintenance and Care Opening the Module In this chapter you find the information relevant for maintenance care and storage Additionally you find instructions for maintenance tasks that may be performed by the customer In case there are any maintenance tasks on that you do not find instructions here contact your supplier or the Technical Support Organic eluents are toxic above a certain concentration Ensure that work areas are always well ventilated When performing maintenance tasks on the device always wear safety glasses with side protection protective gloves and an overall All wetted components of a device e g flow cells of detectors have to be flushed with isopropanol first and water second before being maintained disassembled or disposed The device may only be opened by the Technical Support of KNAUER or any company authorized by KNAUER WARNING AN Irritation of retina through UV light Concen trated UV light can leak out from the flow cell or the fiber optic connectors Switch off the device or the lamps CAUTION Performing maintenance tasks on a switched on device can cause damage to the device Swit
35. en applied to the rear panel Berlin 2014 10 01 Alexanda Knauer CEO and owner part of V6700 O KNAUER Wissenschaftliche Ger te GmbH All rights reserved Technical data are subject to change without prior notice Check our website for latest updates and changes Translation of the original German edition version 2 1 Last update 2015 07 08 Printed in Germany on environmentally friendly paper from susta inable forests AZURA are registered trademarks of KNAUER Wissenschaftliche Gerate GmbH See up to date manuals online www knauer net downloads HPLC SMB Osmometry KNAUER Phone 49 30 809727 0 Wissenschaftliche Gerate GmbH Telefax 49 30 8015010 Hegauer Weg 38 E Mail info knauer net 14163 Berlin Germany Internet www knauer net lh KNALIER KNAUER 2014 V6700 0 02 08 14 Gr
36. ep if the problem is solved If the problem cannot be located call the Technical Support 1 Check the status of the LAN connection in the Windows task bar a Connected hal Connection not established If no connection was established test the following Is the router switched on Is the patch cable connected correctly to the router and the computer Check the router settings Is the router set to DCHP server Is the IP address range sufficient for all the connected devices Check all connections Are the patch cable connected to the LAN ports and not the WAN port Are all cable connections between devices and router cor rect Are the cables plugged in tightly If the router is integrated into a company network pull out the patch cable from the WAN port Can the devices communicate with the computer even though the router is disconnected from the company net work In case you own a Control Unit check the settings in the menu Setup Network Is LAN DHCP set for controlling Did the device receive an IP address Turn off all devices router and computer Firstly turn on the router and secondly turn on the devices and the com puter Has this been successful DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 41 Troubleshooting Replace the patch cable to the device with that no connec tion could be established Has this been successful Make sure that the IP port of th
37. erating hours number of lamp ignitions Mobile Control or Control Unit optional display Ambient Conditions temperature range 4 40 C 39 2 104 F air humidity below 90 96 non condensing height above sea maximum 2000 meters level General power supply 100 240 V 50 60 Hz 75 W dimensions 361 mm x 158 mm x 523 mm widthx height x depth weight 12 2 kg leak sensor yes KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 Technical Data MWD 2 1L 55 Detection detector type multiwavelength detector 8 digital 4 analog detection channels light source deuterium D gt lamp with integrated GLP chip wavelength range 190 700 nm spectral bandwidth lt 8 nm at H line FWHM Note digital bandwidth 1 32 nm wavelength accu 1 nm racy wavelength preci 0 1 nm sion internal holmium filter and deuterium lines 5 AU at 254 nm 400 uAU h at 254 nm gt 1 6 AU at 274 nm 0 0 0 1 0 2 0 5 1 0 2 0 5 0 10 0 s wavelength verifica tion noise drift linearity time constants integration time automatic 5 1000 ms 100 Hz LAN 12 5 Hz analog Error IN Start IN Autozero 0 10 V Analog IN Events 1 2 Error OUT 5 V Valve 24 V Valve OUT 4x0 5 V 16 bit Communication maximum data rate inputs outputs digital LAN DHCP remote connector manual Mobile Control or Control analog outputs control Unit optional
38. flow cell Volume path length as well as wetted parts required pressure range flow cell connection and remote operation are further factors that need considering when selecting a flow cell Flow Cell Volume Depending on your instrument setup column and sample s one flow cell volume may be more appropriate that another If the volume is too large two adjacent peaks may get mixed in the cell If the volume is too small the noise may be higher and the signal may be too small due to less light reaching the photo diodes Ideal flow cell volume therefore is a compromise between peak broadening and sensitivity see figure 25 g B 50 mm LightGuide Cartridge 6 pl illuminated volume 50 mm flow cell 12 pl illuminated volume E BS 8 P 8 dg P P P a cV GER A AME A EM A A A ees NEW A B b Fig 25 volume comparison KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 34 KNAUER Optimizing the Detector A good rule of thumb is that the flow cell volume should not be more than 1 3 of the peak volume of your separated sample To determine the volume of your peaks take the peak width as reported in the integration results multiply it by the flow rate and divide it by 3 Cartridge flow cells with volumes of 2 ul 6 ul and 10 ul are available for the detectors Narrow bore columns 2 1 mm ID are suitable for flow cells with smaller volumes Columns with with a larger inner diameter gt 3 0 mm
39. he device KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 51 Maintenance and Care Prerequisites The device is switched off The lamp cover has been removed The old lamp has been removed Tools Allen screwdriver 2 5 mm Note You can clean the lamp thoroughly with a lint free cloth and iso propanol CAUTION Damage to the lamp and inaccurate measuring results due to residue possible Do not touch the glass body with your hands Wear gloves Use a clean soft cloth Hold the lamp at the lamp socket and guide the glass body into the lamp pod O The bolt of the lamp pod deuterium lamp deuterium lamp sits i in a notch in the lamp socket Insert the halogen lamp G into the Fig 37 lamp pod halogen lamp lamp pod at a slight angle Using the screw driver tighte the 4 two screws or i P on the lamp socket m O 6 Connect the plug PET x ES or and tighten SE CR the lock ring installing the deuterium Attach the lamp cover and fix it with the screws and O Fig 39 lamp cover Next Steps Bring the device into operation KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 52 Technical Data Removing the Leak Prerequisites If the leak tray is filled with liquid the leak has to be removed Auxiliary Material Cloth for drying the leak sensor Procedure Process Remove the leak Dry the leak tray
40. he rear panel detector using the power switch D The detector starts its self validation If the self validation has been successfully completed the LEDs on the right and in the center light up green Bring the detector into service Operation There are several options for controlling the device with chromatography software with Control Unit with Mobile Control It is not possible to use 2 control methods simultaneously If the device is connected to the software it cannot be controlled via Control Unit or Mobile Control The device status can however be monitored Operating with Chromatography Software To control the device with software you have to establish a con nection between the LAN port and a computer Devices can be controlled with e g OpenLAB EZChrom edition version A 01 05 A 04 05 or higher or ClarityChrom version 5 0 3 or higher DAD 6 1L or version 5 0 5 or higher DAD 2 1L MWD 2 1L You find a detailed description on chromatography software in the corresponding user manual Operating with Control Unit The Control Unit is an optional accessory To control the device using the Control Unit connect the cable of the Control Unit to the device You find a detailed description on the Control Unit in its accompanying user manual Operating with Mobile Control The Mobile Control is an app which can be installed on your computer or tablet To control the device using the Mobile Con trol connect
41. highly retained analytes isocratic mode of sample separation where the compo sition of a solvent remains constant LightGuide KNAUER LightGuide flow cell cartridges com bine a maximum light transmission using total reflection with a minimum cell volume to offer an ideal signal to noise ratio Luer Lock a standardized connector between syringes and cannulas DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 KNAUER 59 Accessories and Spare Parts mobile The fluid that moves solutes through the col phase umn packing The adsorbent gel or solid support used in the chromatography column preparative Isolating the maximum amount of a substance in a short amount of time in a required purity response Time for a detector to respond to 90 of the time incoming solute amount The response time is generally taken as 2 4 times the time constant retention The time required from an injection of a sub time stance until the maximum concentration of a substance becomes visible sample A mixture of different components which are to be separated via chromatography The com ponents are moved by the mobile phase and dissolved from the column sample A loop which is separate from a chromato loop graphic system and which the sample is injected to After a switch is actuated the sol vent flow passes the loop and the sample is flushed onto the column solute The dissolved component of a mixture that is
42. ility 12 line 12 KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 65 Index self ignition point 12 toxicity 12 tray 12 space requirements 15 16 spare parts 10 59 standby 31 Start IN see pin header 25 start up 29 storage 45 47 subtraction 38 system messages 41 T technical data detector 52 Technical Support 46 test Installation Qualification 39 Operation Qualification 39 time constant 37 transport damage 57 troubleshooting 40 LAN 40 U unpacking 16 USB 7 W warm up time 33 warning signs 13 warranty 57 wavelength cutoff 35 select 35 KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 ll KNIALIEFI Declaration of Conformity Producer Model Type Reference Machinery EMC Disposal Safety C revision 02 Date KNAUER Wissenschaftliche Ger te GmbH Hegauer Weg 38 14163 Berlin Germany Detector 1 DAD 6 1L Product No EDC11 2 DAD 2 1L Product No EDCO1 3 MWD 2 1L Product No EDBO1 The product complies with the following standards Machinery Directive 2006 42 EC EMC Directive 2004 108 EC IEC 61000 3 2 2012 IEC 61326 1 2011 ROHS directive 2011 65 EU WEEE directive 2012 19 EU Low Voltage Directive 2006 95 EC IEC 61010 1 2010 IEC 61010 2 081 2001 Al Canada CSA C22 2 No 61010 1 3rd Edition 2012 USA UL 61010 1 3rd Edition 2012 The product was tested with a typical configuration The mark of conformity has be
43. ion 1 16 volume 2 ul wetted parts SS quartz PTFE max flow rate 50 ml min max pressure 300 bar path length 3mm A4047 connection 1 16 volume 2 ul wetted parts PEEK quartz PTFE max flow rate 50 ml min max pressure 30 bar path length 0 5 mm A4089 connection 1 16 volume 3 ul wetted parts SS quartz PTFE max flow rate 250 ml min max pressure 200 bar KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 62 Accessories and Spare Parts Technical Data path length connection volume wetted parts max flow rate max pressure path length connection volume wetted parts max flow rate max pressure path length connection volume wetted parts max flow rate max pressure path length connection volume wetted parts max flow rate max pressure Fiber Optics Adapter Order Number 0 5 mm 1 16 3 ul PEEK quartz PTFE 250 ml min 100 bar 0 5 1 25 2 mm 1 8 1 7 4 3 6 8 yl SS quartz PTFE 1000 ml min 200 bar 0 5 1 25 2 mm 1 8 1 7 4 3 6 8 yl PEEK quartz PTFE 1000 ml min 100 bar 0 5 1 25 2 mm 1 4 1 7 4 3 6 ul SS quartz PTFE 10000 ml min 200 bar required for the connection of fiber optics AMKX8 Fiber Optics Adapter including fiber optics adapter fiber optic AMKX8KIT Kit cables and mounting bracket Ideal for semi preparative and preparative remote flow cells Order Number A0740 A0743 A0911 A0742 Fiber Optic Cables 2 x fiber optics
44. is used during operation qualifications and must be stored Inserting the Flow Cell Before taking a flow cell filled with solvent into operation please make certain that the used eluent is miscible with that one used previously Otherwise purge the flow cell with a medium misci ble with both the eluents No flow cell or test cell is installed The device is switched off Pay attention to the compatibility of the flow cells Unscrew the capillary for easier handling WARNING Irritation of retina through UV light Concen trated UV light can leak out from the flow cell or the fiber optic connectors Switch off the device or the lamps Place the flow cell into the opening and slide to the back until it clicks into place inside the device Fig 6 flow cell Connect the capillaries Inserting the Flow Cell with Fiber Optics KNAUER fiber optic cables are extremely robust and solarization proof Nevertheless fiber optic cables are sensitive to bending The minimum bending radius is 100 mm short term 70 mm Observe the following regarding the use of fiber optics UV light will cause the fiber optic to become blind with time solarization making them no longer suitable for use Do not touch the ends of the fiber optic with your fingers as this could falsify the measurement Handle the fiber optic with care avoid impacts or hard actions Move the fiber optic carefully without using pressure
45. ise ration Adapters for fiber optics are optionally available Fiber optics allow separating the flow cell from the detector This way work ing with dangerous explosive or toxic materials becomes safer Remote flow cells are recommended for preparative applications high flow rates in order to protect sensitive optical compo nents from potential leakages The detector measures with a maximum data rate of 100 Hz During the measurement approx 100 spectra per second are recorded Integrated leak management drains liquids from leaks The Mobile Control the Control Unit and the different software products ClarityChrom or OpenLAB can be used to display or read GLP data like operating hours lamp operating hours number of lamp ignitions etc You find a detailed description on how to display or read out GLP data in the respective user man uals DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 9 Upgrade MWD 2 1L Optional Accessories KNAUER Intended Use The multiwavelength detector can be upgraded to a diode array detector The following optional accessories are available Mobile Control app Control Unit Eluents Even small quantities of other substances such as additives modifiers or salts can influence the durability of the materials The list of selected solvents was compiled based on research in the pertinent literature and is only a recommendation by KNAUER If there is any doubt
46. l V6700 version 2 1 26 Installation Connection Function Autozero TTL Input Low active Secure switching threshold at least 10 mA A signal short circuit to ground sets the measuring signal to zero 5 V Provides a voltage of 5 V with respect to GND This makes it possible to sup ply a load that is switched by an EVENT Protection 5 V 50 mA GND Reference point of the voltage at the signal inputs 24 V Valve Event controlled switching of 24 V against GND Protection 24 V 200 mA Valve OUT Output is active until the valve condi tion has been eliminated GND Reference point of the voltage at the signal inputs Connecting Cables to the Terminal Strip To control one device through another you use the multi pin connector To use remote control you have to connect cables to the terminal strip everything comes included with delivery The single ports are used to exchange control signals Prerequisites The device has been turned off The power plug has been pulled Tools Depressor tool CAUTION Short circuit hazard Turn off the device before connecting it to the multi pin connector Pull the power plug CAUTION Electrostatic discharge can destroy the electronics Wear a protective bracelet against electrostatic discharge and ground KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 27 Installation Place the terminal strip amp on a suitable surface Push
47. le Power Plug Next Steps Procedure Capillary Layout KNAUER Installation The device is intended for use with AC power networks of 100 240 V Only the supplied power cable is to be used to connect the device to the mains supply Replace defective power cables only with accessories from KNAUER Only use power cables with a permission for use in your country In case of queries contact the Technical Support CAUTION Electric hazard if the device is turned on while connecting or interrupting the power connec tion Switch off the device beforehand Make sure that the power plug on rear of the device is always accessible so that the device can be disconnected from the power supply Finish the installation and connect the device to the mains Integrating the Detector into the System To integrate the detector into a system note the ambient condi tions found in the section Technical Data as well as the ambient conditions of other devices to be integrated into that system The detector is integrated into the HPLC flow system by con necting the capillary to the flow cell and the HPLC system Stainless steel fittings are tightened with 5 Nm PEEK fittings are tightened with 0 5 Nm Fig 21 installation for detector DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 29 Note Operation Prerequisites KNAUER Operation Pre Installed Capillaries Pre installed stainless steel
48. light falls onto a geometric array of 1024 DAD 6 1L or 256 DAD 2 1L MWD 2 1L separate photodiodes the photodiode array The optical system of the AZURA DAD 6 1L is depicted in figure 4 An active temperature control with 0 5 C sensitivity ensures baseline stability for minimal baseline drift DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 8 Legend D deuterium lamp halogen lamp flow cell diode array sensor diffraction grating mirror Lamps DAD 6 1L DAD 2 1L MWD 2 1L Mirror DAD 6 1L Flow Cell KNAUER LightGuide Flow Cell Cartridges Data Rate Leak Management GLP Data KNAUER Intended Use Fig 4 optical system DAD 6 1L The lamps can be exchanged quickly and easily without the need of a service technician 2 light sources a deuterium lamp and a halogen lamp cover the entire UV Vis wavelength range 1 deuterium lamp covers the UV wavelength range Maximum light intensity is provided by effectively mixing the light sources from the deuterium and halogen lamp with a mir ror using Polka Dot technology Various types of flow cells are available to the user and allow a variety of applications Flow cell cartridges with standard and KNAUER LightGuide technology are available see Flow Cells on page 61 KNAUER LightGuide flow cell cartridges combine a maximum light transmission using total reflection with a minimum cell volume to offer an ideal signal to no
49. ll KNALIER feura Detector DAD 6 1L DAD 2 1L MWD 2 1L User Manual V6700 3 Table of Contents Table of Contents Note For your own safety read the manual and always observe the warnings and safety information on the device and in the manual Intended Use aa O Na 6 DEVICE VET VIO WW Faan eund o is a 6 a AU M C T ts e pita Mae pap leek 6 Rear VEW ado DAA RR a 6 SIGS VIEW rebasa ata EE 7 A e AN 7 a suecas dancer ya E ro Whee gon deca es 9 Scope ol DellVeby uide a gue A a des 10 Safety for USES coe ee aa A EE REUS OE SEE S adds 11 Definition of Personal and Material Damage llle 12 DECONTAMINAUION bus vrs rut IPEA SU Orto d utr doe d 13 Symbols ANG SIGNS s ese 5 ase carere ud aes SO AER MORE A E 13 e AAA O dur NE pta sine ya Ger DEIN dre 14 Gron ewm Cr 14 lien A PvP 14 Operating ENVIrONMEN ss sa ico ai dett ug eiii ded acier ERU iii dodo 15 space Requirements atestado 15 Sta AION d 0 3 8 20 FS ER yor a hess sn AL oS 15 Space Requirements are os eh tet eee AA IE ee eS 16 SUID wate eee a eee rae PITE eee 16 UNPACKING Mc PPP 16 Inser ng the Flow ell s etes aeo etat es EA Cn Sea te laa wen ERE ee ERES 17 Inserting the Flow Cell with Fiber Optics o oo oooooooo ooo 17 Connecting he Capilares 2 3s 09m aede EORR SERERE Re ee ems 18 Using the PEEK HUMOS ce uet EOD SUE aia RE en ee ACRI m eR 19 Connecting the Leak Management leeren 19 COMMON A E d denn eee ES 20 Conne
50. lowing confirmation of flawless condition at delivery check if the delivery is complete certification on the functionality of the device The Operation Qualification includes an extensive functionality test and must be purchased from the manufacturer Contact the KNAUER Sales Department to request an offer The Operation Qualification is a standardized KNAUER document and includes the following definition of customer requirements and acceptance terms documentation on device specifications device functionality check at installation site To make sure that the device operates within the specified range you should test the device using the Operation Qualifica tion at following intervals Average Useful Life 1 to 5 days week Every 6 months More than 5 days week or 24 hours day Every 3 months Operation with buffer solutions or other Every 3 months salt solutions The test can be carried out either by the Technical Support of KNAUER or from a provider authorized by KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 40 Troubleshooting Troubleshooting First Measures KNAUER Check all cabling Check all screw fittings 1 2 3 Check whether air has gotten into the supply lines 4 Check device for leaks 5 Pay attention to system messages LAN Go through the following steps in case no connection between the computer and the devices can be established Check after each st
51. n Properties Select Internet Protocol version 4 TCP IPv4 Click on the button Properties QV Un BR W N Check the settings in the tab General The correct settings for the DHCP client are a Obtain IP address automatically b Obtain DNS server address automatically 7 Click on the button OK Connecting the Cables A router has several LAN ports and one WAN port that can be used to integrate the LAN into a wide area network WAN e g a company network or the Internet In contrast the LAN ports serve to set up a network from devices and a computer To avoid interference we recommend operating the HPLC system separately from the company network You will find patch cables for each device and the router in the accessories kit To connect the router to a WAN an additional patch cable is required which is not supplied within the scope of delivery Modules WAN port Router Workstation LAN ports Fig 18 Cabling system LAN KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 23 Prerequisite Procedure Procedure Result Prerequisite Procedure Note Procedure KNAUER Installation The computer has been switched off There is a patch cable for each device and the computer 1 Use the patch cable to connect the router and the computer Repeat this step to connect all devices 2 Use the power supply to connect the router to the mains power system Config
52. nalysis food analysis pharmaceutical analysis environmental analysis Device Overview Front View On the front of the device there are the flow cell and the removable lamp cover for lamp replacement Fig 1 front view example DAD 6 1L Rear View On the back of the detector the connectors for LAN and power plug are located as well as the serial number of the device and the power switch on off Please note that the service interface is solely used for repair and maintenance tasks performed by service technicians DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 7 Intended Use Legend device information integrator outlets LAN connector service interface multi pin connector fan connection and power switch Legend USB port for the Control Unit Optical Module KNAUER Fig 2 rear view example DAD 6 1L Side View On the side of the detector you find the connector for the oper ating panel Control Unit see Operating with Control Unit on page 30 Fig 3 USB port for the Control Unit Features In an HPLC system the detector serves to detect substances in liquids and show their concentration The sensitivity of the detector depends on the installed flow cell The detectors measure the light absorption of the sample in the ultraviolet and visual spectra The entire spectrum permeates the sample and afterwards is split up by a grate The split
53. nd below CAUTION Defect of the device due to overheating possible Set up the device in such a way that it is pro tected against exposure to direct sunlight Keep at least 15 cm clear at the rear and 5 10 cm at each side for air circulation Space Requirements Position the device on a level and even surface Protect the device against direct exposure to sunlight Set up the device at a location not exposed to air drafts A C systems Do not set up the device in the vicinity of other machines that cause floor vibrations Lateral distance to other devices At least 5 cm if another device is set up on one side At least 10 cm if further devices are set up on both sides Leave the power plug on the rear of the device accessible to be able to disconnect the device from the mains Installation Site air humidity below 90 96 non condensing temperature range 4 40 C 39 2 104 F Avoid sources of high frequencies near the device High fre quency sources may compromise measuring values If you are located in an earthquake area use the bore holes D in the side panels to secure the device The bore holes are located on either right or left side panel DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 16 Installation Fig 5 bore holes of device Space Requirements Side clearance to other devices At least 5 cm if there is another device on one side At least 10 cm
54. or You find a detailed description on how to read out GLP data in the respective user manuals 1000 Replace halogen lamp DAD 6 1L Replace deuterium lamp Cleaning and Caring for the Device CAUTION Intruding liquids can cause damage to the device Place solvent bottles next to the device or in a solvent tray Moisten the cleaning cloth only slightly All smooth surfaces of the device can be cleaned with a mild commercially available cleaning solution or with isopropanol DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 47 Maintenance and Care Prerequisites Auxiliary Material Procedure Next Steps Prerequisites Procedure KNAUER Checking the Fittings Check if all fittings are tight In case you find fittings that are not tight tighten them up Stainless steel fittings PEEK fittings Decommissioning The detector is designed for the use of different solvents In case the detector has not been used for several weeks solvent resi dues may cause damage We therefore recommend to Flush the flow cell and the capillaries Completely remove used solvents Fill the flow cell and the capillaries with isopropanol Before storage close the open connectors of the flow cell with hole plugs The detector has been flushed hole plugs and or cap fittings Process 1 Unscrew the eluent supply lines and close the open con nectors with hole plugs 2 Disconnec
55. orm the Technical Support of KNAUER The lamp unit has to be replaced No lamp ignition when starting the device or the manual validation Data acquisition No entries are possible First stop active acquiring measurement data after wards you can make a new entry KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 43 Troubleshooting System Message Problem and Solution E Error input acti External error outside the device vated Check the external devices and cable connections Check the system to locate and remove the error H HAL lamp does not Switch the lamp on In case the error start DAD 6 1L shows again restart the device In case no improvement shows replace the lamp Instrument busy 3D data is being collected while scan ning leak sensor or cover are process ing earlier inputs Wait until the device has completed the process Instrument in Command not allowed during standby mode standby mode 12C lamp s opera Connecting error between power tion failed source of lamp and I2C 12C operation Connecting error for power source of failed leak sensor or lamp at firmware upload or via EEPROM I2C Instrument in Command can not be executed in standalone mode local operation only in remote opera tion Instrument remote This entry is not executable Quit soft controlled ware Insufficient access Data on lamp power supply
56. perature change below 2 C hour over a one hour period Hand in old devices or disassembled old components at a certi fied waste facility where they will be disposed of properly According to the German Abfallverzeichnisverordnung AVV January 2001 old devices manufactured by KNAUER are marked as waste electrical and electronic equipment 160214 KNAUER as a company is registered by the WEEE number DE 34642789 in the German Elektroaltgerateregister EAR The number belongs to category 8 and 9 which among others comprise laboratory equipment All distributors and importers are responsible for the disposal of old devices as defined by the WEEE directive End users can send their old devices manufactured by KNAUER back to the dis tributor the importer or the company free of charge but would be charged for the disposal All solvents and other operating materials must be collected sep arately and disposed of properly All wetted components of a device e g flow cells of detectors or pump heads and pressure sensors for pumps have to be flushed first with isopropanol and then with water before being maintained disassembled or disposed DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 ae Legal Information Legal Information Warranty Conditions The factory warranty for the device is valid for 12 months after the date of dispatch All warranty claims shall expire in the event that any unauthorize
57. rol or Control Unit optional Ambient Conditions 4 40 C 39 2 104 F below 90 96 non condensing height above sea maximum 2000 meters level General 100 240 V 50 60 Hz 75 W 361 mm x 158 mm x 523 mm widthx height x depth DAD 2 1L Detection diode array detector resolution of diodes 2 nm diode detection channels 8 digital 4 analog light source deuterium D gt lamp with integrated GLP chip wavelength range 190 700 nm spectral bandwidth lt 8 nm at H line FWHM Note digital bandwidth 1 32 nm KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 54 Technical Data wavelength accu 1 nm racy wavelength preci 0 1 nm sion internal holmium filter and deuterium lines 5 UAU at 254 nm 400 uAU h at 254 nm 1 6 AU at 274 nm 0 0 0 1 0 2 0 5 1 0 2 0 5 0 10 05 wavelength verifica tion noise drift linearity time constants integration time automatic 5 1000 ms 100 Hz LAN 12 5 Hz analog Communication maximum data rate Error IN Start IN Autozero 0 10 V Analog IN Events 1 2 Error OUT 5 V Valve 24 V Valve OUT 4x0 5 V 16 bit inputs outputs digital LAN DHCP remote connector manual Mobile Control or Control analog outputs control Unit optional programming wake up IP 20 IP protection class Technical parameters GLP function Detailed report about lamp recogni tion operating hours lamp op
58. ros aa oes a a ar os 62 ho qe ree eo cae de een ap 63 Declaration of Conformity 0 cc eee eee eee ee 66 An alle die es betrifft Wenn Sie ein franzosischsprachiges Benutzerhandbuch zu die sem Produkt wunschen senden Sie ihr Anliegen und die ent sprechende Seriennummer per E Mail oder Fax an KNAUER support knauer net 49 30 8015010 Vielen Dank To whom it may concern In case you prefer a French language user manual for this pro duct submit your request including the corresponding serial number via email or fax to KNAUER support knauer net 49 30 8015010 Thank you A qui que ce soit Si jamais vous pr f riez un manuel en francais pour ce poduit contacter KNAUER par email ou par fax avec le no de s rie support knauer net 49 30 8015010 Merci beaucoup KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 6 Intended Use Note Description Operating Ranges Legend O leak tray capillary guide lamp cover serial number leak management switch standby key status LED flow cell RS 232 Service Interface KNAUER Intended Use Only use the device for applications that fall within the range of the intended use Otherwise the protective and safety equip ment of the device could fail The detector can be used for analytical semi preparative and preparative applications The device can be used in the following areas biochemical analysis chemical a
59. se compressed air for drying 1 Fill the syringe with eluent 2 Inject it into the inlet of the flow cell and allow it to act for 5 minutes 3 Repeatedly flush with syringe and water 4 Remove the flow cell from the detector and use a nitrogen stream to dry it Check if the baseline noise has disappeared Replacing the Flow Cell UV light will cause the flow cells to become blind with time solarization making them no longer suitable for use The man ufacturer recommends replacing the flow cell after about 6000 operating hours The capillaries are disconnected The device is switched off WARNING AN Irritation of retina through UV light Concen trated UV light can leak out from the flow cell or the fiber optic connectors Switch off the device or the lamps DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 49 Procedure Next Steps DAD 6 1L DAD 2 1L MWD 2 1L DAD 6 1L Legend deuterium lamp con nector halogen lamp connec tor DAD 6 1L halogen lamp DAD 6 1L deuterium lamp Prerequisites Tools Note KNAUER Maintenance and Care 1 Press the release lever down 2 Theflow cell is being released and can be pulled out Push in the new flow Fig 31 releasing the flow cell cell until it locks into place Connect the capillaries Replacing the Lamps Replace the lamp if it malfunctions or its intensity is low he re
60. stallation and connection specifica tions in the user manual National and international regulations pertaining to labora tory work Original spare parts tools and solvents made or recom mended by KNAUER Good Laboratory Practice GLP Accident prevention regulations published by the accident insurance companies for laboratory work Filtration of substances under analysis Use of inline filters Once they have been used never re use capillaries in other areas of the HPLC system Only use a given PEEK fitting for one specific port and never re use it for other ports Always install new PEEK fittings on each separate port Follow KNAUER or manufacturer s instructions on caring for the columns More safety relevant information is listed in alphabetical order in the following table DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 12 Safety for Users 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 solvent tray Risk of electrical shock or short circuit if liquids get into the device s interior For this reason place all bottles in a solvent tray solvent lines Install capillaries and tubing in such a way that liquids cannot get into the interior in case of a leak leaks Regularly check if any system compo nents are leaking power cable
61. t number for each device must be changed and this same number must be entered into the device configu ration of the chromatography software We recommend to use the same port number for all devices in the same system The port is set to 10001 at the factory You must use the same numbers in the device configuration of the chromatography software as in the device otherwise the connection fails 1 Find out port number and change it on the device DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 24 Result KNAUER Installation 2 Enter the port number in the chromatography software The connection is established Using Remote Control On the rear panel of the detectors an electrical connector socket is located which serves to send or receive signals from other instruments For example start signals from an injection valve or an autosampler can be put to the START input All voltages have to be mounted between GROUND and the corresponding event CAUTION Electrostatic discharge can destroy the electronics Wear a protective bracelet against electrostatic discharge and ground For test purposes or in some other cases it can make sense to manually enter these signals sending control signals Events to external devices opening and closing contacts activating 500 ms pulses The following remote signals can be received and sent for receiving start control and error signals from external devi
62. t the detector from the system and close the open connector of the flow cell with a hole plug Select a storage location according to the requirements which are listed in the according chapter of this manual Storage Pay attention that all hoses and capillaries have been emptied or filled with flushing solution e g isopropanol before storage To prevent algae formation do not use pure water Close all inputs and outputs with cap fittings Pay attention to the ambient conditions for storage see Techni cal Data on page 52 Disconnecting the Power Supply The device has been switched off Process 1 Pull the power plug out of the socket and afterwards out of the device 2 Pack the power cable together with the device DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 48 Next Steps Tools Procedure Next Steps Prerequisites KNAUER Maintenance and Care Disconnect further electrical connections Remove the flow cell and pack the device for transport or storage Cleaning the Flow Cell Increased noise of the baseline and reduced sensitivity can be a result of a dirty flow cell Often it is sufficient to rinse the flow cell to restore optimal sensitivity Rinsing the Flow Cell The following solvents are recommended for rinsing dilute HCI 1 mol L 1 mol L NaOH aq Ethanol Acetone Syringe CAUTION Contamination of the flow cell caused by oil drops Do not u
63. the special range see section When a narrower spectral range is selected the signal intensity will be increased This increase is limited however by the data rate Subtraction of the Baseline Chromatogram The baseline subtraction can eliminate the effects of drift that result from solvent gradient or flow programming The base line profile is subtracted from the measured chromatogram This results in a mathematically reprocessed chromatogram with an ideally flat baseline KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 39 Functionality Tests General The performance of the detector is largely dependent on the performance of the HPLC system Noise can be related to pump stability the flow cell cleanli ness lamp quality mobile phase composition and other fac tors Drift is usually related to long term changes in the environ ment such as detector warm up or fluctuations in tempera ture and mobile phase composition Functionality Tests Installation Qualification IQ Operation Qualification OQ Test Intervals Execution KNAUER The customer may request the Installation Qualification which is free of charge In case of a request the Technical Support of KNAUER or from a provider authorized by KNAUER performs this functionality test during the installation The Installation Qualification is a standardized document that comes as part of the delivery and includes the fol
64. tic cables 750 mm Overall sensitivity is inversely proportional to the length of the fiber optic cables Temperature changes around the cables may cause additional drift Selecting the Wavelength Wavelength selection can influence the sensitivity selectivity and linearity of a measurement The measurement wavelength can be selected within the range from 190 1000 nm for the DAD 6 1L or 190 700 nm for the DAD 2 1L and MWD 2 1L in 1 nm steps The best wavelength for a given measurement sig nal wavelength is that which fives the maximum absorption above the UV cutoff of the mobile phase In cases where there are multiple components with different absorbance maxima a compromise wavelength must be chosen where all components absorb In order to minimize baseline drift due to refractive index effects a reference wavelength can be set in order to correct the base line see figure 28 The reference should be set in the same spectral region as the signal wavelength UV or Vis but at a wavelength at which the analyte has no absorbance DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 36 Default Reference Wave length Default Bandwidth KNAUER Optimizing the Detector By default the reference wavelength 360 nm is activated This is a suitable value for most applications Without baseline correction With baseline correction a CEREREM CORN comparison with and without baseline correction When
65. ubleshooting System Message Problem and Solution Instrument not vali Data acquisition or simple scans can dated not be executed if the system has not been validated Cannot proceed Manual validation is not possible while D2 lamp heating lamp is heating up Wait until deute rium lamp has initialized and continue afterwards Cannot proceed Manual validation is not possible while D2 lamp off lamp is switched off Switch the lamp on In case the error shows again restart the device In case no improvement shows replace the lamp Cannot proceed Validation failed because of exceeded Low light integration time The operating time of the lamp has been exceeded Replace the deuterium lamp Flow cell is dirty Clean the flow cell Error state of the optical system Inform the Technical Support of KNAUER D2 lamp failed Manual validation is not possible with out deuterium lamp Communication Communication via RS 232 is inter buffer overflow rupted Communication Timeout Connecting error RS 232 timeout 5 s leak sensor 0 5 s or any hard ware component lamp power con nection EPROM I2C with GUI CRC failure Correct input connection interrupted currently inactive D D2 lamp operation Restart the device If the error occurs failed again replace the lamp D2 lamp does not Switch off lamp and turn on again In start case the system message repeats itself inf
66. upport of the manufacturer Leak sensor was not found or does not react Leak was detected Switch off the device Remove the leak and start the device afterwards No D2 lamp Check if the deuterium lamp was detected installed correctly Z Not available for 3D data acquisition or simple scans via this communication RS 232 are not possible mode R Recommended D2 The recommended operating time of lamp life exceeded the deuterium lamp of 2000 hours was exceeded Replace the lamp Recommended The recommended operating time of HAL lamp life the halogen lamp of 1000 hours was exceeded exceeded Replace the lamp S Shutter position Malfunction of cover motor failed Spectrum buffer The internal 3D data buffer was used overflow up because of a LAN connection error Spectrum output 3D data acquisition can not be busy or not ready started Wait until data transfer is fin ished and continue afterwards Temperature con The upper temperature limit of the trol failed lamp unit was exceeded Time already Correct the time entry exists KNAUER DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 45 Maintenance and Care System Message Problem and Solution Wake up time Wakeup time is in the past Specify already passed new time WL BW out of Selected path length and bandwidth spectral range exceed the spectral range Expand the select
67. uring the Router The router is preset at the factory You will find a label at the bottom side of the router on which IP address user name and password are printed These information help to open the router configuration 1 To open the router configuration start your Internet browser and enter the IP address not for all routers 2 Enter user name and password 3 Configure the router as DHCP server 4 In the router configuration check the IP address range and make changes if necessary Once the router has assigned IP addresses to all devices the chromatography software can be used to remotely control the system Integrating the LAN into a Company Network A network administrator can integrate the LAN into your com pany network In this case you use the WAN port of the router There is a patch cable for the connection 1 Check that the IP address range of the router and of the com pany network do not overlap 2 In case of an overlap change the IP address range of the router 3 Use the patch cable to connect the router WAN port to the company network 4 Restart all devices including the computer Controlling Several Systems Separately in a LAN Devices connected to a LAN communicate through ports which are part of the IP address If more than one HPLC system is con nected to the same LAN and you plan on controlling them sepa rately you can use different ports to avoid interference Therefore the por
68. w to set up an HPLC system in a local area network LAN and how a network administrator can inte grate this LAN into your company network The description applies to the operating system Windows and all conventional routers To set up a LAN we recommend to use a router That means the following steps are required 1 On the computer go to the control panel and check the LAN properties 2 Hook up the router to the devices and the computer 3 On the computer configure the router to set up the network 4 Install the chromatography software from the data storage device 5 Switch on the device and run the chromatography software Configuring the LAN Settings The LAN uses only one server which is normally the router from that the devices automatically receive their IP address DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 22 Installation Prerequisite In Windows power saving hibernation standby and screen saver must be deactived n case you use an USB to COM box the option Allow the computer to turn off ths device to save power in the device manager must be deactivated for all USB hosts Only for Windows 7 For the network adapter the option Allow the computer to turn off this device to save power in the Device Manager must be deactivated Procedure 1 In Windows 7 choose Start gt Control Panel gt Network and Sharing Center Double click on LAN Connection Click on the butto
69. z data rate averages 10 points The analog data rate is fixed at 12 5 Hz The optimal data rate depend on your application Too few points across a peak short data rate decrease detail and com promise reproducibility Too many points high data rate intro DAD 6 1L DAD 2 1L MWD 2 1L user manual V6700 version 2 1 38 Optimizing the Detector duce noise into the system and the resulting files can become very large Some general considerations are listed below Each peak should be defined by 20 30 data points For chro matograms with co eluting peaks or low signal to noise ratios 40 50 data points per peak are recommended If all peaks are relatively wide select a slower data rate If any peaks of interest are less than a few seconds select a faster data rate If the data rate is too slow the start and end points of the peaks are not accurately determined If the data rate is too fast data files may occupy excessive disk space and post run analyses may require more processing time Fig 30 noise with different data rates Integration Time Signal Level The integration time influences the intensity of the signal and therefore the sensitivity of the measurement The larger the inte gration time the higher the intensity of the signal until the max imum sensor counts are reached The integration time is automatically calculated by the software before the start of a measurement The calculations are in relation to

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