Biotage ELSD-1080 Operation Manual

Evaporative light scattering detector
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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

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Summary of Contents for Biotage ELSD-1080

  • Page 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...
  • Page 2 Biotage ELSD-1080 Biotage offices Biotage has offices in Sweden, Wales, Japan and the US. Biotage AB Kungsgatan 76 SE-753 18 Uppsala Sweden Sales: +46 18 56 57 10 (phone) +46 18 56 57 05 (fax) ordermailbox@eu.biotage.com Support: +46 18 56 59 11 1-PointSupport@eu.biotage.com...
  • Page 3 See the “Biotage Terms & Conditions of Sale” document at www.biotage.com. Copyright Biotage Sweden AB, is the owner of copyright on this document and any associated software. Under law, the written permission of Biotage Sweden AB must be obtained before either the...
  • Page 4 Biotage ELSD-1080 This page is intentionally left blank. Publication date: July 2010...
  • Page 5: Table Of Contents

    Cleaning ..............11   Other Precautions ............11   Warning and Caution Messages ........12   CE Compliance ............14   Local Biotage Offices or Distributors ......... 14   General Information ..........15     Introduction ............15    ...
  • Page 6 Power Mode ..........36 3.4.8     Data Output Rate (Hz) ......... 37 3.4.9     Controlling the Biotage ELSD-1080 Detector Using the Standalone   Software Utilities ............37   Control Software-Overview ......37 3.5.1     Control Software-Parameter Settings ....38 3.5.2...
  • Page 7 Biotage ELSD-1080 Real-time Operation ........40 3.6.1     Starting & Stopping Real-time Control ....40 3.6.2     General Considerations .......... 41     Solvent Recommendations ......42 3.7.1     Sample Preparation ........42 3.7.2     Column Considerations ........ 42 3.7.3...
  • Page 8 Biotage ELSD-1080 This page is intentionally left blank. Publication date: July 2010...
  • Page 9: Safety Practices And Hazards

    Biotage assumes no liability for the customer’s failure to comply with these requirements. It is the responsibility of the customer to inform Biotage 1-Point Support Representatives 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.
  • Page 10: Electrical Hazards

    Biotage ELSD-1080 detectors have been carefully designed to operate safely and effectively when using components that conform to the design criteria. Use of non-approved components in the detector may render the system inoperative and/or hazardous.
  • Page 11: Hot Surface Hazards

    Before using any cleaning or decontamination method except those recommended by Biotage, users should check with Biotage that the proposed method will not damage the equipment. See Appendix 3 for detailed recommended procedures. Other Precautions...
  • Page 12: Warning And Caution Messages

    A Caution message is used when failure to observe instructions could result in damage to equipment (supplied by Biotage and/or other associated equipment). Warning Symbols The following is a list of symbols that appear in conjunction with warnings in this manual or on the detector.
  • Page 13 Biotage ELSD-1080 A triangular symbol indicates a warning. The meanings of the symbols that may appear alongside warnings in the documentation or on the detector itself are as follows: Corrosive liquid Electrical shock Explosion hazard Heavy weight Eye hazard Fire hazard...
  • Page 14: Ce Compliance

    Biotage ELSD-1080 CE Compliance Your Biotage ELSD-1080 has been designed to comply with the requirements of the Electromagnetic Compatibility (EMC) Directive and the Low Voltage (electrical safety) Directive (commonly referred to as the LVD) of the European Union. Biotage has confirmed that each product complies with the relevant Directives by testing a prototype against the prescribed EN (European Norm) standards.
  • Page 15: General Information

    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.
  • Page 16: Notes And Hot Tips

    Weight (unpacked) 13 kg (ELSD-1080) Weight (packed) 18 kg (ELSD-1080) PC Control (software) Biotage ELSD Control Software Remote Operation Remote Start Input Safety Features Gas shut off Valve, Leak Detection Table 1. Biotage ELSD-1080 Performance Specifications Publication date: July 2010...
  • Page 17: Unpacking And Installation

    Any damage to the container or detector should be reported immediately to your local distributor, or to Biotage. It is recommended that the shipping container be kept, if possible, for re-shipment or return to a service centre.
  • Page 18: Site Preparation Checklist

    >50 mm. Table 2. Site Preparation Checklist Warning Biotage ELSD-1080 detectors weigh approximately 13 kg (28.7lb). To avoid injury to personnel or damage to equipment, always follow all precautions for lifting heavy objects when moving the detector. It is advisable to locate the system on a sturdy bench.
  • Page 19: Location Of The Detector Module

    The ELSD-1080 detector can be placed within 2 meters of an extraction unit, using the exhaust tube provided. Do’s and Don’ts of ELS Detection 1.
  • Page 20: Solvent Recommendations

    The maximum operating temperature of the detector and the boiling point of the solvent will determine the type of solvents compatible with the Biotage ELSD-1080 detector. High boiling point solvents such as N-Methylpyrrolidone (NMP), Dimethylsulfoxide (DMSO) are not recommended for long-term operation.
  • Page 21: Installation

    Biotage ELSD-1080 Installation Biotage ELSD-1080 detectors must be installed by a field service support representative (FSSR) trained, qualified, or authorized by Biotage. Details for unpacking the detector and what to do in case it has been damaged in transit are outlined in this operation manual in Chapter 1, Section 1.4.
  • Page 22: Extraction

    Biotage ELSD-1080 Extraction The ELSD-1080 detector is provided with tubing for venting the exhaust gases and vapors, and so does not need to be placed in a fume hood. Instead, the exhaust hose provided must be attached to the rear of the unit and vented to a fume hood or other disposal unit.
  • Page 23 Biotage ELSD-1080 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...
  • Page 24 Biotage ELSD-1080 Figure 2. Rear View of Biotage ELSD-1080 1. External Vapor Sensor 6. Mains Switch 2. Serial RS232 connector-24bit 7. Mains Input digital output 8. Fuses 3. Service Connector 9. Gas supply inlet port 4. Service Switch (run/flash) 10. Exhaust port 5.
  • Page 25: Other Connections

    Biotage (Part No. ELSD-0890-0350). Fluid Connection 2.6.1 Inlet The eluent from the Isolera system flow splitter is connected to the central front port of the Biotage ELSD-1080 detector via a low dead volume Valco bulkhead connector. ® Publication date: December 2008...
  • Page 26: Outlet

    Waste tube must NOT be submerged in the liquid. 7. Connect the exhaust hose between the exhaust outlet and a fume hood. 8. For analog data collection, connect the ELSD-1080 detector to the Isolera system using the analog cable provided.
  • Page 27: Connecting The Detector To Your Pc

    Biotage ELSD-1080 10. Turn on the source gas to a pressure of about 60-100 psi. 11. Switch on the Biotage ELSD-1080 detector, and select a desired method (e.g. Method “XXX”). 12. Initiate heating by selecting RUN mode using the arrow keys on the front keypad.
  • Page 28: Biotage Elsd-1080 Software Control

    2.10 Installing the Standalone Software Utilities Two software utilities are provided with your Biotage ELSD- 1080 detector, namely Control and Method Editing software. To install the software utilities, you must have administrator rights for the PC. When you insert the supplied software CD into your CD drive, the CD browser will start automatically.
  • Page 29: System Description And General Operation

    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.
  • Page 30: Theory

    Biotage ELSD-1080 1.Nebulization 2.Evaporation 3.Detection Figure 3. Principles of Operation 3.1.1 Theory There are four main processes by which the path of electromagnetic radiation or light can change direction, when passing through a medium containing a suspended particulate phase. These are shown in Figure 4: Figure 4.
  • Page 31: Operational Parameters

    Biotage ELSD-1080 evaporator temperature is independent of the mobile phase. Consequently, the ELSD-1080 can be set at 30 °C for all types of mobile phase provided the evaporator gas flow is adjusted accordingly.
  • Page 32: Display Screen

    Operating parameters can be altered via the interactive menu bar at the bottom of the display. Figure 5. Biotage ELSD-1080 Display Screen 3.3.2 Keypad The four arrows on the front of the detector are used to navigate within the interactive menu bar.
  • Page 33: Sub-Menu 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.
  • Page 34: Error Conditions

    Software utility (page 39) is required to edit and download the custom methods. In addition to the 10 on-board methods, the ELSD-1080 has a method XXX that allows modification of the ELSD parameters to be made without the need for software control. Method XXX allows the detector to be used in standalone mode via the front screen and keypad.
  • Page 35: Evaporator Temperature

    3.4.2 Evaporator Temperature The evaporator temperature is the most important setting on the ELSD-1080 detector. This should be set according to the volatility of the compound(s) being analyzed. If the compound is non-volatile, e.g. sugars, then the evaporator temperature should be set to 80-90 °C.
  • Page 36: Detector Gain (Pmt)

    Biotage ELSD-1080 temperature is reduced to ambient and sub-ambient temperatures, the gas flow needs to be increased to compensate (e.g. 1.6-1.8 SLM). The evaporation gas range for both models is: 0.9-3.25 SLM (0.05 increments). The default value is 1.6 SLM.
  • Page 37: Data Output Rate (Hz)

    STANDBY mode. 3.4.9 Data Output Rate (Hz) The rate at which the ELSD-1080 outputs data can be selected from the sub-menu screen. A 10Hz output rate is suitable for flash applications (the default value is 10Hz).
  • Page 38: Control Software-Parameter Settings

    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 this feature (TOOLS / Run system test menu option), the software will run the ELSD through a number of internal diagnostic tests, and then compare the results with the expected values set by Biotage.
  • Page 39: Method Editor Software-Overview

    Figure 7. Control Software Main Screen 3.5.5 Method Editor-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.
  • Page 40: Method Editor-Downloading Method Sets

    Biotage ELSD-1080 3.5.6 Method Editor-Downloading Method Sets To download a Method Set to the ELSD-1080, open the desired Method Set to be downloaded. Ensure the Method Editor is configured for the correct communication port for the detector. Ensure that any software session that is currently accessing the detector via the selected COM port is closed down.
  • Page 41: General Considerations

    Figure 8. Biotage ELSD-1080 Front Panel Display During Timetable Operation 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.
  • Page 42: Solvent Recommendations

    – any non-volatilized eluent will increase baseline noise and reduce sensitivity. The ELSD-1080 is a destructive technique and must be placed last when used in series with other detectors. 3.7.1 Solvent Recommendations Any solvent intended for use with the Biotage ELSD-1080 detector should be thoroughly degassed, filtered (0.45 µm) and...
  • Page 43: Transferring Elsd Temperature Methods

    ELSDs to the Biotage ELSD-1080 detector may not provide equivalent performance. As stated in Section 3.4 (page 34), the operating temperatures of the ELSD-1080 detector are set according to the type of analyte and not the mobile phase composition as with other ELSDs.
  • Page 44 Biotage ELSD-1080 This page is intentionally left blank. Publication date: July 2010...
  • Page 45: Routine Maintenance

    (e.g., safety glasses, gloves and protective clothing) according to the safety data sheets when handling solvents. The Biotage ELSD-1080 detector is designed to be a low- maintenance detector and does not generally require regular service. However, should the detector performance deteriorate, we recommend the following procedures to clean the nebulizer and evaporator section without dismantling the unit.
  • Page 46: Information For Service Personnel

    WARNING Information for Service Personnel Please note that the ELSD-1080 detector is double fused. 4.3.1 Heater PCB Fuses There are 3 fuses fitted to the main control PCB, one to protect each of the heater circuits.
  • Page 47: Upgrading The Firmware

    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.
  • Page 48 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. Publication date: July 2010...
  • Page 49: Troubleshooting

    Biotage ELSD-1080 Troubleshooting If a problem is encountered, Biotage advises that a system test be performed via the ELS standalone control software (Section 3.5.3, page 38) to ensure that the detector is working correctly. If there is an error or fault and you follow the recommended course of action and the result is not satisfactory, then please direct the matter to Biotage or your local distributor.
  • Page 50: Detector Errors

    Biotage ELSD-1080 Detector Errors Error Description Suggestions Air temp <= 10 °C inside Environmental temp too cold. enclosure Move to warmer location Air temp > 40 °C temp inside Environmental temp too hot. enclosure Move to cooler location On-board sensor heater failed...
  • Page 51: General Problems

    Biotage ELSD-1080 General Problems Faults or Possible Cause(s) Remedy Problems Baseline noise Poor nebulization of solvent Increase the temperature of the evaporator by 10° intervals until the noise is acceptable Insufficient evaporation Increase the evap gas flow rate Decrease the nebulization...
  • Page 52 Biotage ELSD-1080 Large baseline Inefficient evaporation Increase the evaporator offset temperature and/or gas flow High concentration of non- Use a lower concentration of volatile buffer or stabilizer stabilizer, unstabilized solvent or a more volatile buffer (ammonium acetate or ammonium formate)
  • Page 53 Ensure Switch is in UP position Temperature Temperature probe fault or Check RTD connections error as soon as disconnected Consult Biotage or your local detector powered agent for further advice Display not on, Detector in service mode Ensure service Switch is in but power...
  • Page 54 Biotage ELSD-1080 This page is intentionally left blank. Publication date: July 2010...
  • Page 55: Appendix 1 - Method Record

    Biotage ELSD-1080 APPENDIX 1 – Method Record Chromatography Eluent Eluent Method Evap Date Comments Conditions Flow Number Temp Temp Flow Stored Publication date: July 2010...
  • Page 56 Biotage ELSD-1080 This page is intentionally left blank. Publication date: July 2010...
  • Page 57: Appendix 2 - Spare Parts Listing

    Biotage ELSD-1080 APPENDIX 2 – Spare Parts Listing The following list of spare parts was current at the time of issue of this manual. Please contact your local distributor or Biotage for an up-to-date price list and availability. Description Part Number...
  • Page 58 Biotage ELSD-1080 This page is intentionally left blank. Publication date: July 2010...
  • Page 59: Appendix 3 - Cleaning And Decontamination Procedure

    Identify and if possible correct the source of the leak. Inspect cabling, parts and surfaces to determine whether any damage has occurred. If in doubt, contact the Biotage Service Department for assistance. Allow the interior and exterior of the detector to dry out completely before closing the cover and reconnecting power.

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