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Biotage ELSD-1080

1.

General Information

1.1

Introduction

The Biotage Evaporative Light Scattering Detector (ELSD) is a

unique and highly sensitive detector for semi-volatile and non-
volatile solutes in a liquid stream. It is mainly used as a

concentration detector for liquid chromatography. The solvent
stream containing the solute material is nebulized and carried

by a gas flow through an evaporation chamber. The solvent is
volatilized, leaving a mist of solute particles that scatter light to

a photosensitive device. The signal is amplified and a voltage
output provides the concentration of the solute particles
passing through the light.
Biotage ELSD-1080 detectors may be used alone, or as one of
several detectors in an LC or flash system. As the solvent or

eluent is evaporated in the course of the purification, the ELSD-
1080 detector must be the last in series if used in conjunction

with other detectors. If the ELSD-1080 detector is being used as
the last detector in a series, care must be taken not to exceed

the recommended backpressure in detector cells in other units.
This manual instructs the user in the installation and operation
of the ELSD-1080 detector for stand-alone use.

1.2

Pre-installation Requirements

The Biotage ELSD-1080 operation manual describes the

environmental and operating requirements of the detector. You
must prepare your laboratory according to these instructions

before the detector can be installed. If you have misplaced your
copy, you can obtain a replacement from your local Biotage

office.
You have been provided with this operation manual to help you
set up and operate your ELSD-1080. This operation manual

contains safety practices and hazards information, where to
find information about installing and maintaining detector

components and a brief operation overview.

1.2.1

Conventions

The following conventions have been used throughout the
documentation:

•

Menus, menu options and field names (e.g., choose

Copy

from the

Edit

menu) have been typed in bold.

Bold is also used to signify the buttons appearing

throughout the software (e.g., click

OK

).

•

ALL CAPITALS indicate keyboard commands (e.g., press

the F2 key) and text you must type in from the
keyboard (e.g., type SETUP at the prompt).

Publication date: July 2010

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Содержание ELSD-1080

Страница 1: ...Biotage ELSD 1080 Evaporative Light Scattering Detector Operation Manual v1 0 Installation Category II Pollution Degree 2 Safety Class 1 EN 61010 1 ELSD 1080 July 2010 Ref 6 27400 ...

Страница 2: ...F82 7TS United Kingdom Biotage Japan Ltd Medi Coop BLDG 8 5F 2 4 14 Kichijojihoncho Musashinoshi Tokyo Japan 180 0004 Sales 81 422 28 1233 phone 81 422 28 1236 fax info biotage co jp Support 1 pointsupport biotage co jp Biotage LLC 10430 Harris Oaks Blvd Charlotte NC 28269 U S A Sales 1 704 654 4900 phone 1 800 446 4752 toll free 1 704 654 4917 fax Product_info biotage com Support 1 800 446 4752 p...

Страница 3: ...whole or in part Biotage Sweden AB reserves the right to make changes to the information contained herein without prior notice First published July 2010 in Uppsala SE Comments about this manual should be directed to the Product Manager Biotage by e mail to product_managers biotage com 2010 Biotage Sweden AB Trademarks Biotage and are trademarks owned by Biotage AB Other product and company names m...

Страница 4: ...Biotage ELSD 1080 This page is intentionally left blank 4 Publication date July 2010 ...

Страница 5: ...ions 15 1 2 2 Notes and Hot Tips 16 1 3 Specifications 16 1 4 Unpacking and Installation 17 1 5 Packing List 17 1 6 Site Preparation Checklist 18 1 7 Location of the Detector Module 19 1 8 Do s and Don ts of ELS Detection 19 1 8 1 Pumping Systems 19 1 8 2 Mobile Phase Priming 19 1 8 3 Solvent Recommendations 20 2 Installation 21 2 1 Installation Checklist 21 2 2 Power Connections 21 2 3 Extraction...

Страница 6: ...tions 34 3 3 7 Clearing an Error 34 3 4 Operational Parameters 34 3 4 1 Method 34 3 4 2 Evaporator Temperature 35 3 4 3 Nebulizer Temperature 35 3 4 4 Evaporator Gas Flow 35 3 4 5 Detector Gain PMT 36 3 4 6 Response Time Smoothing 36 3 4 7 Light Source Intensity LED 36 3 4 8 Power Mode 36 3 4 9 Data Output Rate Hz 37 3 5 Controlling the Biotage ELSD 1080 Detector Using the Standalone Software Util...

Страница 7: ...ser 45 4 2 Cleaning Evaporator Tube 45 4 3 Information for Service Personnel 46 4 3 1 Heater PCB Fuses 46 4 3 2 Light Source 46 4 4 Putting the Detector into Storage 46 4 5 Upgrading the Firmware 47 4 5 1 Tools Required 47 4 5 2 Firmware Upgrade Procedure 47 5 Troubleshooting 49 5 1 Troubleshooting an HPLC System 49 5 2 Detector Errors 50 5 3 General Problems 51 APPENDIX 1 Method Record 55 APPENDI...

Страница 8: ...Biotage ELSD 1080 This page is intentionally left blank 8 Publication date July 2010 ...

Страница 9: ...atives if the detector has been used for the analysis of hazardous biological radioactive or toxic samples prior to any detector service being performed or when a detector is being returned to the service center for repair General Operation of the Biotage ELSD 1080 detector involves the use of pressurized liquid and hazardous materials including corrosive fluids and flammable liquids Careless impr...

Страница 10: ...nder the system inoperative and or hazardous It may also invalidate the warranty on the detector Use only related components supplied or authorized by Biotage Voltages above 110 V AC are present within the detector Disconnect the detector from all power sources before removing protective panels to avoid exposure to potentially dangerous voltages ONLY Customer Service Representatives trained qualif...

Страница 11: ...tile and or toxic liquids Wear face protection when you inject samples or perform routine maintenance Never open a solvent line or valve under pressure Stop the pump first and let the pressure drop to zero Use shatterproof solvent reservoirs capable of operating at 50 60 psi Keep the solvent reservoir enclosure closed when the reservoir is under pressure Read and adhere to all NOTES CAUTIONS and W...

Страница 12: ...e mineral acids or bases should be avoided Employ static measuring and static discharge devices e g air ionizers to safeguard against the buildup of static electricity The unit should not be stacked more than two high without additional means of support and suitable precautions should be taken to prevent the units being knocked over Biotage ELSD 1080 detectors weigh approximately 13 kg 28 7 lb To ...

Страница 13: ...ached to the detector When you see this symbol refer to the relevant operation or service manual for the correct procedure referred to by that warning label The following symbols appear on the detector for your information I Mains power on 0 Mains power off Fuse Single phase alternating current Direct current When attached to the rear of the detector indicates that the product complies with the re...

Страница 14: ...panies the product contains a copy of the Declaration of Conformity The Declaration of Conformity is the legal declaration by Biotage that the product complies with the directives listed above and shows the EN standards to which the product was tested to demonstrate compliance It is signed by Biotage Authorized Representative Local Biotage Offices or Distributors We stress the importance of standa...

Страница 15: ...recommended backpressure in detector cells in other units This manual instructs the user in the installation and operation of the ELSD 1080 detector for stand alone use 1 2 Pre installation Requirements The Biotage ELSD 1080 operation manual describes the environmental and operating requirements of the detector You must prepare your laboratory according to these instructions before the detector ca...

Страница 16: ...tor Biotage ELSD 1080 OFF 10 80 C Gas Flow Range 0 9 3 25 SLM with controlled gas shut off valve Operating Pressure 60 100 psi 4 6 7 bar Eluent Flow range 0 2 5 0 mL min Digital Output 10 or 40Hz 24bit Analog Output 0 1V FSD Communication Serial RS232 Remote Start Input Pump Stop 1 Contact closure Power Requirements 90 120V AC or 220 250V AC 50 60 Hz 2A Max Power Consumption 150 W max Dimensions W...

Страница 17: ...ainer be kept if possible for re shipment or return to a service centre Examine the shipping carton for visible signs of exterior damage Unpack the detector and examine it for transit damage Check that all items on the packing list are included Notify your local distributor or Biotage of any damage or missing items 1 5 Packing List Biotage ELSD 1080 Operation Manual ELSD Control Software Mains lea...

Страница 18: ...y Nitrogen 98 purity filtered to 0 2 µm Air can only be used for non flammable solvents The detector is not calibrated for use with gases other than air or nitrogen Nitrogen generator strongly recommended for best performance For operation with other inert gases contact Biotage for advice Extraction requirements The exhaust gases from the detector must be extracted to a fume hood or similar extrac...

Страница 19: ...eate backpressure on the nebulization chamber leading to increased noise 3 When placing more than one detector in series always place the ELSD 1080 detector last 4 Only volatile mobile phase additives can be used the ELSD See Table 5 page 43 The use of non volatile buffers will lead to increased baseline noise levels 1 8 1 Pumping Systems It is recommended to use a high performance pumping system ...

Страница 20: ...h the Biotage ELSD 1080 detector High boiling point solvents such as N Methylpyrrolidone NMP Dimethylsulfoxide DMSO are not recommended for long term operation Greater care and attention to detector cleaning procedures should be exercised with these solvents It is recommended that any solvent be flushed from the detector for overnight and weekend storage 20 Publication date July 2010 ...

Страница 21: ... you for review Unpack the accessories supplied with the detector and check that you have received everything on the packing lists enclosed in the packing crate Install your ELSD 1080 detector To install the ELSD 1080 detector Connect the power and communication cables Connect the gas solvent outlet tubing Connect the solvent inlet tubing to the detector Install the ELSD software driver on the PC ...

Страница 22: ...n dry nitrogen gas between 60 100 psi in pressure For optimum performance a gas pressure of 60 psi is recommended A convenient 4 mm push in connection for the gas source is provided at the rear of the detector For consistent gas flow either a Nitrogen generator or a pressure dampener between the gas regulator and the ELSD is required To prevent against unnecessary gas usage a controlled gas shut o...

Страница 23: ...Biotage ELSD 1080 1 2 3 4 Figure 1 Front View of Biotage ELSD 1080 1 Front screen display 2 Keypad 3 Eluent inlet 4 Solvent waste outlet Publication date July 2010 23 ...

Страница 24: ...Figure 2 Rear View of Biotage ELSD 1080 1 External Vapor Sensor 6 Mains Switch 2 Serial RS232 connector 24bit digital output 7 Mains Input 8 Fuses 3 Service Connector 9 Gas supply inlet port 4 Service Switch run flash 10 Exhaust port 5 Remote Start Input 11 Analog Output 1V ...

Страница 25: ...opping the operation of a pump if the unit reports an error condition The Biotage ELSD 1080 detector is also equipped with one contact closure which is normally open and two TTL logic inputs both active low with internal pull up resistors to 5 V Note Pump stop facility must be employed if the detector is to be left unattended or if units are stacked I O description Pin number Inputs Remote Start 1...

Страница 26: ...nit 3 Attach the 4 mm OD gas tube into the gas inlet port at the rear of the detector see Figure 2 The gas connection is a push in fitting 4 The gas should be dry filtered and have a minimum inlet pressure of 60 psi 60 100 psi is required to achieve the maximum operating detector gas flow rate of 3 25 SLM 5 Connect the solvent waste tube to the waste outlet at the front of the detector and positio...

Страница 27: ...ble offsets and increased noise levels 2 8 Connecting the Detector to Your PC To operate the Biotage ELSD 1080 detector a free Serial RS 232 communications port 1 to 255 is required on your PC Most computers are supplied with at least one serial port as standard but if your PC does not provide a serial port or you are already using the existing serial ports for other devices then there are a coupl...

Страница 28: ...tware CD into your CD drive the CD browser will start automatically If it does not you can launch the browser by running Setup exe from the root directory of the CD Note The Standalone Software utilities are only compatible with Windows 2000 XP Pro 2 10 1 Configuring the Software Utilities On starting the ELSD Control Software or Method Editor program the correct serial port must be configured for...

Страница 29: ... chamber and randomizes the particle plume The Biotage ELSD 1080 detector uses patented gas flow technology in the evaporation zone to aid evaporation at low temperatures By adding a stream of dry nitrogen evaporation gas at the entrance of the evaporator tube less volatile solvents e g water are easily evaporated This evaporation gas is controlled by the user and facilitates sub ambient operation...

Страница 30: ...behave as point sources and Mie scattering becomes predominant Once particle size approaches the wavelength of incident light then reflection and refraction begin to prevail The relative importance of refraction and reflection can be understood by examining the effects of the incident light on a single spherical particle whose equilateral axis lies in the same plane as the photo detector and light...

Страница 31: ...ted technology that reduces the evaporation time of highly aqueous solvents at low temperature and also prevents the evaporation tube becoming saturated which would otherwise preventing further evaporation occurring Using this patented evaporation gas technology a 20 µm droplet of water at 30 C can be dried ca 3x faster than just temperature alone Using the ELSD 1080 water can be evaporated as low...

Страница 32: ... running If the AZ Stop key is pressed during an active timetable the timetable will stop running and the ELSD will revert to STANDBY mode 3 3 3 Main Menu Bar To change the current settings use the arrow keys to navigate across the interactive menu bar until the desired option is flashing Using the up down arrow keys alter the parameter to the desired setting In order to action any changes the cur...

Страница 33: ...e screen 3 3 5 1 STANDBY The STANDBY mode is the ground state of the ELSD 1080 detector which is by default initiated automatically after power on default can be changed using Power Mode page 36 In STANDBY mode the heaters are switched off and the gas manifold valve is closed at power on The STANDBY mode gives the user a control platform in which to set up the operational parameters gas flow nebul...

Страница 34: ...onal state If the problem has not been rectified the ELSD will repeatedly error when RUN mode is selected 3 4 Operational Parameters 3 4 1 Method The Biotage ELSD 1080 detector has the capacity to store 10 custom definable methods in memory These methods comprise evaporator nebulizer temperature and gas flow which can be optimized for specific applications These 10 on board methods are selected us...

Страница 35: ... the ELSD 1080 is 10 80 C 1 C increments The default evaporator temperature is 30 C 3 4 3 Nebulizer Temperature The nebulizer temperature can be used to optimize signal response in addition to evaporator temperature Higher nebulizer temperatures increase peak response but the nebulizer temperature must not exceed the boiling point of the mobile phase The nebulizer temperature range for both models...

Страница 36: ...tted from the detector can be averaged to produce a smoother response The smoothing width is set to the number of data points over which the data is averaged and can be regarded as a digital time constant The smoothing range is settable from 1 50 in increments of 1 which translates to 0 1 5 0 seconds For flash applications a value of 50 5 seconds is satisfactory 3 4 7 Light Source Intensity LED Th...

Страница 37: ...ll as a comprehensive monitoring system Operational parameters can be easily manipulated saved or loaded by using the flexible Methods Editor enabling rapid set up and custom method archiving A general description of the features available through the software utilities is given below but for a more comprehensive guide on how to use the control software please refer to the on line help supplied wi...

Страница 38: ...nu option Once a change has been made the UPDATE button must be pressed in order to download the information to the detector Note The L E D intensity is set for ALL methods used on the detector and is NOT Method specific 3 5 3 Control Software System Test The System Test is used to evaluate the ELSD 1080 performance to ensure it is operating to the high standards set by Biotage When you select thi...

Страница 39: ... Creating Storing Methods To change a custom method on the ELSD 1080 you must first create a custom Method Set FILE New A Method Set comprises 10 custom methods which can be customized using the Method Editor software A description can be entered for each method within the method set in order to distinguish between them Having created a method set the set of methods can be downloaded to the ELSD v...

Страница 40: ...80 Detector During an Injection The Biotage ELSD 1080 detector has the capability to change operational parameters in real time during a sample injection using an on board timetable 3 6 1 Real time Operation The Biotage ELSD 1080 detector can store in memory a series of time based events within a single timetable This timetable allows the operational settings of the ELSD to be changed in real time...

Страница 41: ...ime 2 Total runtime 3 On board Timetable is active Figure 8 Biotage ELSD 1080 Front Panel Display During Timetable Operation 3 7 General Considerations The Biotage ELSD 1080 detector should be thought of as a detector like any other designed for liquid chromatography The main distinguishing feature is the ability to evaporate the solvent from the column eluent Therefore normal system set up precau...

Страница 42: ...hose listed in Table 5 page 43 should be used with the ELSD 1080 detector Tetrahydrofuran THF stabilized with BHT may increase the baseline noise level Where possible unstabilized THF should be used with the ELSD 1080 detector High boiling point solvents such as N methylpyrrolidone NMP and Dimethylsulfoxide DMSO are not recommended for long term operation Greater care and attention to detector cle...

Страница 43: ...6 8 11 3 106 Ion Pair Reagent Pentafluoropropionic acid PFPA 0 6 97 Heptafluorobutyric acid HFBA 0 6 120 Nonafluoropropionic acid NFPA 0 6 140 Tridecafluoroheptanoic acid 0 6 175 Table 5 Volatile Mobile Additives Compatible with ELS Detection 3 7 4 Transferring ELSD Temperature Methods The direct transfer of ELSD operating conditions from other manufacturers ELSDs to the Biotage ELSD 1080 detector...

Страница 44: ...Biotage ELSD 1080 This page is intentionally left blank 44 Publication date July 2010 ...

Страница 45: ...oss of signal increased baseline noise and in the extreme case gas bubbling out of the nebulizer drain tube If this happens then simply turn off the liquid flow increase the gas flow to 2 8 SLM and increase the evaporator to maximum temperature The diffuser will be dried out and the detector ready to use after approximately 1 hour under these conditions Reset the detector to the correct operating ...

Страница 46: ...e light source assembly is a Class 1 L E D product as defined in IEC 60825 1 Ed 1 2 While this is non hazardous it is advisable to avoid staring into the beam 4 4 Putting the Detector into Storage If the detector is to be stored or not used for an extended period of time it is recommended to follow the procedure outlined below 1 Flush the detector with a mixture of Acetone Water 50 50 at 1 ml min ...

Страница 47: ...connected to the unit and turn off the detector 3 Connect the serial cable from the PC the Service port on the rear of the detector 4 At the rear of the detector move the black switch located below the service port to the down position i e FLASH 5 Run the HexTerm exe program 6 Select ELSD 1080 from the drop down menu of available detector models 7 Select the appropriate communication port 8 Turn o...

Страница 48: ... port at the rear of the detector 15 Switch the detector back on and check the correct version of firmware has been loaded by reading the boot up screen on the front panel of the detector Or by choosing the status option for the ELSD 1080 control window within Galaxie 48 Publication date July 2010 ...

Страница 49: ...hich by its very nature is spread throughout the HPLC system but appears as a malfunction of the ELSD 1080 detector To troubleshoot the Biotage ELSD 1080 detector you must be able to separate the performance of the detector within the flash system from its performance outside the flash system This section begins with guidelines for testing the ELSD 1080 detector as a stand alone The troubleshootin...

Страница 50: ...he circuitry wires fan Call service engineer if this happens regularly 18 Nebulizer temperature exceeded threshold after stabilizing Faulty thermocouple or heater control 19 Evaporator temperature exceeded threshold after stabilizing Faulty thermocouple or heater control 20 Light source error Replace light source assembly 21 Evaporator gas flow rate exceeded threshold after stabilizing Check opera...

Страница 51: ...locked or extraction is too strong Use a pulse free pump Increase the back pressure on the pump by fitting a back pressure column between the pump and the injection valve Use a pulse dampener directly after the pump in the system Use a volatile mobile phase as shown Baseline spikes Particulate matter in the gas supply Column shedding Poor nebulization Non volatile additive in mobile phase Filter t...

Страница 52: ...othing Sample precipitation during nebulization Inconsistent pump flow rates Nitrogen is the recommended gas others can be used but may not nebulize as efficiently Change gas to nitrogen or evaluate different nitrogen sources If using bottled gas check that gas regulator is functioning correctly and giving consistent flow Alternatively use a pulse dampener The broader the peaks the higher the smoo...

Страница 53: ...ode Ensure service Switch is in UP position RUN Consult Biotage or your local agent for further advice Evaporator Temperature reads zero at start up and cannot be changed Peltier cooler has not initiated correctly Switch detector off then on at the power socket Consult Biotage or your local agent if problem persists Vapor sensor error occurs but there is no solvent or vapor leak inside unit Solven...

Страница 54: ...Biotage ELSD 1080 This page is intentionally left blank 54 Publication date July 2010 ...

Страница 55: ...Biotage ELSD 1080 Publication date July 2010 55 APPENDIX 1 Method Record Chromatography Conditions Eluent Eluent Flow Method Number Evap Temp Neb Temp Gas Flow Date Stored Comments ...

Страница 56: ...Biotage ELSD 1080 This page is intentionally left blank 56 Publication date July 2010 ...

Страница 57: ...ntainer 500 mL ELSD 0890 0320 RS232 Communication Cable ELSD 0890 0325 Biotage ELSD Mains Lead UK ELSD 0890 0330 Biotage ELSD Mains Lead EURO ELSD 0890 0335 Biotage ELSD Mains Lead US ELSD 0890 0340 I O cable ELSD 0890 0345 Remote Start Cable ELSD 0890 0350 Biotage ELSD Operation Manual ELSD 0890 0355 Biotage ELSD Service Manual ELSD 0890 0360 Biotage ELSD IQ OQ Workbook ELSD 0890 0365 Biotage ELS...

Страница 58: ...Biotage ELSD 1080 This page is intentionally left blank 58 Publication date July 2010 ...

Страница 59: ...high Disconnect the detector completely and remove it to a fume hood if necessary Open the cover of the detector to see if any solvent has contaminated the interior Excess quantities of liquid spilt on or inside the detector should be mopped up using absorbent cloths followed by repeated wiping down with soft cloths moistened with acetone or deionized water as appropriate to the spilt solvent unti...

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