Markes International Unity 2 User Manual
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Markes International Unity 2 User Manual

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QUI-1057
Version 2.0 – February 2014
User manual
UNITY 2™
Markes International Ltd
T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com
www.markes.com

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  • Page 1 QUI-1057 Version 2.0 – February 2014 User manual UNITY 2™ Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com www.markes.com...

  • Page 2: Table Of Contents

    Primary (tube) desorption ..........15 2.2.5 Pre trap fire purge ............. 16 2.2.6 Secondary (trap) desorption ..........17 Insertion and removal of a sample tube in UNITY 2 ....18 2.3.1 Insertion................18 2.3.2 Removal ................18 Desorb and split flows ..............18 2.4.1...
  • Page 3 GC system detection limits ..........20 2.4.10 Calculating analyte masses in the sample tube ..... 21 2.4.11 Calculating splits/split modes ......... 21 2.4.12 UNITY 2 systems with Electronic Carrier Control (ECC) .. 22 2.4.13 UNITY 2 systems configured with Electronic Mass Flow Control............... 22 3.
  • Page 4 Windows Vista ..............47 3.7.3 Windows XP ............... 47 4. Accessing product and support information ........48 Markes International Limited - Home Page and facilities.... 48 Consumables and Spares .............. 48 Applications library ................. 48 Technical support ................48 5. Technical Support ................49 Routine maintenance schedule ............

  • Page 5: Preface

    Page 5 1. Preface This manual provides detailed instructions on the use of the UNITY 2. It is suitable for users with little or no prior experience of the system and details the software/hardware interface and procedure for first sample runs.

  • Page 6: Labels/Symbols

    1.4.3 High temperatures  Several parts of the UNITY 2 Several parts of the UNITY 2 can be operated at high temperatures high temperatures. Contact with these zones whilst the system is in operation these zones whilst the system is in operation can cause serious burn injury. These can cause serious burn injury.

  • Page 7: Hydrogen Gas Safety

     For further advice on the use of hydrogen as a carrier gas, please contact Markes International Technical Support. 1.4.5 Cleaning and decontamination Please consult Markes International or your local agent for information on decontamination or the use of cleaning agents NOTE: Incorrect cleaning/decontamination could result in damage to the instrument. Environment operating conditions The instrument should be protected from conditions that could cause exposure to frost, dew, percolating water, rain, excessive direct sunlight, etc.

  • Page 8: Altitude

    <40 A (cold start) Technical support contact details In the first instance please contact your distributor. If they are unable to resolve your query, please contact Markes International (details below). Address: Gwaun Elai Medi-Science Campus, Llantrisant, RCT, UK, CF72 8XL Website: www.markes.com...

  • Page 9: Instrument Familiarisation

    QUI-1057 Page 9 2. Instrument familiarisation Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com www.markes.com...

  • Page 10: Hardware

    2.1.1 Sample tubes UNITY 2 is compatible with industry standard sample tubes - 3.5 inches (89 mm) long by ¼-inch (6.4 mm) O.D with 5 mm (stainless steel and coated steel) or 4 mm (glass) I.D. Sorbent is retained in stainless steel (or coated steel) tubes using stainless steel (or coated steel) gauzes and a gauze retaining spring.

  • Page 11: Trap Filters And Seals

    2.1.6 Trap filters and seals As with the sample tube, the cold trap is sealed into the gas flow path of UNITY 2 via O-rings, which seal on the outer wall of the trap tube. At the cool non-valve end of the trap, the O-ring is backed up with a porous PTFE filter to prevent contamination of the pneumatics in the event of sorbent particles migrating out of the trap.

  • Page 12: Sequence Of Operation

    Page 12 Sequence of operation When a tube is placed and sealed into the flow path of UNITY 2 for conventional 2(3) stage desorption, it undergoes the following sequence of operations: standby, leak test, prepurge, primary desorption, pre trap fire purge and secondary desorption.

  • Page 13: Leak Test

    If the measured pressure drops by more than 5% in 30 seconds this is classified as a leak in the sample flow path and UNITY 2 status changes to Tube Leaked.

  • Page 14: Prepurge

    There is also the option in this step to perform an elevated temperature purge. See Section 3.6.4. Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com www.markes.com...

  • Page 15: Primary (Tube) Desorption

    Note that the tube desorption time is measured from the beginning of tube oven heating and not from the time at which the sample tube reaches the desorption temperature. Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com www.markes.com...

  • Page 16: Pre Trap Fire Purge

    It may also be used to dry purge the cold trap prior to injection when direct desorbing solid or humid samples. This pre-trap fire purge time can be adjusted in the TD method. Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com www.markes.com...

  • Page 17: Secondary (Trap) Desorption

    The flow through the cold trap at this stage is determined by the column flow and any outlet split. NOTE: the flow path of UNITY 2 remains in the trap desorption configuration until the trap has cooled below 50°C.

  • Page 18: Insertion And Removal Of A Sample Tube In Unity 2

    (see section 3.2). Place the tube horizontally in the tube oven, such that it is clear of the seals at both ends. Operate the lever towards the rear of the instrument to seal the tube into the UNITY 2 flow path.

  • Page 19: The Set Gas Flow Function

    The UNITY 2 flow path will then alter so that there is no the question in the box. The UNITY 2 flow path will then alter so that there is no split flow, only the desorb split flow, only the desorb flow, to be adjusted and measured.

  • Page 20: To Exit The Set Gas Flows Function

    2.4.7 Sample splitting UNITY 2 may be set up to offer sample splitting between zero (splitless) and 10,000:1 (double split). The split that is required for a particular analysis will be dependent on the analyte mass in the sample tube, the analytical column capacity and the sensitivity of the GC detector selected.

  • Page 21: Calculating Analyte Masses In The Sample Tube

    Unusually among thermal desorbers, During tube desorption the desorb flow must splitless UNITY 2 can operate in splitless mode be set to at least 10 ml/min to provide in conjunction with narrow bore (0.32 enough flow through the sample tube for mm ID) columns and MS detectors as efficient thermal desorption.

  • Page 22: Unity 2 Systems With Electronic Carrier Control (Ecc)

    2.4.12 UNITY 2 systems with Electronic Carrier Control (ECC) When installed with certain models of commercial GC(-MS), UNITY 2 systems can be configured with electronic control of the carrier gas as it leaves the cold trap and enters the fused silica (or length of analytical capillary column) inside the transfer line.

  • Page 23: Software

    Windows is strongly recommended. In general, a PC with sufficient resources to run 32-bit Windows should have enough performance to control UNITY. Other Windows software may be active on the PC at the same time as UNITY 2 software, for example data handling software, word processing and spreadsheet functions.

  • Page 24: External Ready Signal

    When the GC comes ready it will provide a signal to UNITY 2 via the Interface Harness and the GC indicator on the status bar will change from a cross to a tick. UNITY 2 checks this signal, to ascertain whether the Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com...

  • Page 25: Toolbar Functions

    ( ) at the top left-hand side of the toolbar. This brings up the directory (nominated under Options, see Section 3.4.1) containing UNITY 2 method files. Select the required file name and click OK or double-click on the required file name to access it.
  • Page 26 It is the active method that is printed. Copy method Ensure that the UNITY 2 method you wish to copy is the active method. Clicking parameters on it with the left hand mouse button will make it active if necessary.

  • Page 27: Method Linking

    - along with the GC column - prior to analysing a new sample. UNITY 2 schematic This is accessed using the status icon ( ) or by selecting View > Status Show.
  • Page 28 After a method has been run the next method in the sequence is downloaded to UNITY 2 and run. The After a method has been run the next method in the sequence is downloaded to UNITY 2 and run. The After a method has been run the next method in the sequence is downloaded to UNITY 2 and run.

  • Page 29: The Trap Heat Method

    ) on the toolbar. The following dialogue box then appears. Once Trap Heat has been selected, UNITY 2 will ask you to confirm that the default method is that which Once Trap Heat has been selected, UNITY 2 will ask you to confirm that the default method is that which Once Trap Heat has been selected, UNITY 2 will ask you to confirm that the default method is that which you wish to use.

  • Page 30: Schematic Display Of Unity 2 Status

    Schematic display of UNITY 2 status A simple schematic illustrating the status of UNITY 2 A simple schematic illustrating the status of UNITY 2 can be displayed on the screen at all times during can be displayed on the screen at all times during system operation.

  • Page 31: Configuration

    The configuration page contains the current instrument configuration settings. The configuration page contains the current instrument configuration settings. Instrument Configuration For UNITY 2 operation the Instrument Configuration will be set to UNITY (manual). For UNITY 2 operation the Instrument Configuration will be set to UNITY (manual). Communications Port The communications port determines serial port number (e.g.

  • Page 32: Gc Interface

    UNITY 2 flow path. sets the time taken to release the carrier gas pressure in the tube at the end of tube desorption. The default is 0.3 min.

  • Page 33: Methods

    NOTE: Carrier type only needs to be set when using MFCs. The carrier gas pressure as measured by the pressure transducer, within the UNITY 2, can be displayed in either psi or kPa depending upon preference, and is selected here.
  • Page 34 Page 34 Paths – Method Dir Set by default to the directory where UNITY 2 is installed. To change this directory double click on the current path and select the new path from the directory. Paths – Show Full Path If selected then the active window bar will show the full path and file name of the method in the active window bar, if it is not selected then the active window bar will only display the file name for that method.

  • Page 35: Reporting

    UNITY would have been triggered to start). Unity Deviation Displays any error messages encountered during operation (e.g. Tube Leaked) Injection Count Displays the number of times a given sample has been analysed. Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com www.markes.com...

  • Page 36: Unity 2 Method Options

    3.5.1 Split on or off in standby When UNITY 2 is in standby state, i.e. not being used overnight or at weekends, it is usual to have the split turned off in order to save expensive carrier gas (8 hours overnight at 50 ml/min would use ~24 litres of carrier gas).

  • Page 37: Desorption Modes

    Tenax tube shipped with UNITY 2, will require conditioning prior to use. There are several points to note when conditioning sample tubes using UNITY 2 as opposed prior to use. There are several points to note when conditioning sample tubes using UNITY 2 as opposed prior to use.

  • Page 38: Standard 2(3) Stage Desorption

    Min Carrier Pressure Set a minimum carrier gas pressure just below that at which you normally operate UNITY 2 and the GC analytical column. If the carrier gas pressure drops below this minimum pressure, UNITY 2 status will change to Low Carrier Pressure and UNITY 2 will become Not Ready.
  • Page 39 Typical elevated temperature purge settings are 5-15 minutes at 50-100°C. Trap Desorb Set the Trap Low temperature by clicking in the box and typing in the required value. Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com www.markes.com...
  • Page 40 120°C and 150°C. For ease of use, extended system lifetime and trace level operation a lower Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com www.markes.com...
  • Page 41 The GC Cycle Time = GC Run Time + GC Cool Down Time + Equilibration (if appropriate). If a GC Cycle Time is entered, UNITY 2 will calculate the time at which it can begin the next tube desorption stage such that at the end of that tube desorption and at the time the trap is ready to heat, the GC will have just come ready from the previous analysis.

  • Page 42: Sample Tube Prepurge

    Further information on selecting and setting split flows is given in Section 3.4. Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com...

  • Page 43: Sample Tube Prepurge At Elevated Temperature

    3.6.5 SecureTD-Q™ - Re-collection for repeat analysis UNITY 2 facilitates the quantitative re-collection of the split portion of a sample onto a clean sorbent tube thus facilitating repeat analysis. This is of real benefit in situations where it is not possible, or prohibitively expensive, to collect replicate samples.

  • Page 44: Cold Trap Conditioning

    Trap Heat function on UNITY 2 (see Section 2.3.2.). As with tube conditioning it is essential to check the maximum isothermal temperature of the sorbent in the trap and never to set the trap temperature more than 10°C below this.

  • Page 45: Unity 2 Parameter Specifications

    QUI-1057 Page 45 3.6.7 UNITY 2 parameter specifications Parameter Range Mode Standard 2(3) Stage Thermal Desorption Tube Conditioning Split on in standby Yes/No Ambient temperature carrier gas purge Time settable between 0.0 and 99.9 minutes in 0.1 minute increments Split on during tube purge...

  • Page 46: Uninstalling Unity 2 Software

    Page 46 Uninstalling UNITY 2 software When new UNITY 2 software is issued it is important that any previous installations of software are completely removed prior to installing the new version. In order to ensure that the PC system is correctly purged of all relevant files it is necessary to follow these instructions fully.

  • Page 47: Windows Vista

    4. Click on Add/Remove and follow the on screen prompts (when asked to remove shared files click yes). The Markes TD software should now be uninstalled. Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com www.markes.com...

  • Page 48: Accessing Product And Support Information

    Alternatively contact Markes International Ltd. direct on: Email enquiries@markes.com +44 (0) 1443 231531 Technical support In the first instance please contact your local Markes International sales office. Alternatively, contact Markes International Ltd. direct on Email: support@markes.com Fax: +44 (0) 1443 231531...

  • Page 49: Technical Support

    QUI-1057 Page 49 5. Technical Support Routine maintenance schedule A routine maintenance kit is available for UNITY 2 (RMK-0001-2S) containing all UNITY 2 consumables that are required for an annual service. UNITY 2 ITEMS Frequency Check Oxygen / organics trap - replace if necessary...

  • Page 50: Lifespan Of Tubes

    A gauze retaining spring is then inserted using the TubeMate to hold the gauze in place. Tubes should be impedence tested prior to use A range of pre-packed sorbent tubes is available from Markes International (see relevant Accessories for Thermal Desorption catalogue or contact Markes on consumables@markes.com...

  • Page 51: Conditioning Tubes

    Tubes should be cleaned using the dedicated tube conditioning mode on UNITY or using the TC-20 Multi tube conditioning rig. See Application information (TDTS 5 / TDTS19) for further details. Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com www.markes.com...

  • Page 52: Long Term Storage Of Clean And Sampled Tubes

    The tube O-ring seals (U-COV10 (pk 10), U- COV100 (pk 100)) are found at either end of the tube sealing mechanism. UNITY should be switched off before O-rings are removed or replaced. Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com www.markes.com...

  • Page 53: Changing The Charcoal Split Tube Filters

    Therefore the filters will require changing at routine intervals. SERUTD-5065 Split Filter Tube Packed with Charcoal (UNITY 2) SERAAA-1600 Split Filter Tube, Glass, Packed with Charcoal (Air Server systems) It is suggested that the filters are repacked with conditioned charcoal every three months. Charcoal filters are loaded in the same manner as tubes, with the grooved end (or fritted end of the glass tube) facing the back of UNITY.
  • Page 54 C-DL1P0 Cap, DiffLok, inert coated / st. st, pk 100 pairs 2.7 Changing the nozzle seals (UltrA) NOTE: Before proceeding ensure that UltrA and UNITY 2 are switched off by closing down the software and switching off the main power switch at the back of the instruments.

  • Page 55: Cold Trap

    Markes International Ltd. Empty trap tubes (U-T7EMP-2S) are also 2S) are also available for the user to pack as required. The UNITY 2 cold trap available for the user to pack as required. The UNITY 2 cold trap is constructed of quartz.

  • Page 56: Removing / Replacing A Cold Trap

    The carrier gas supply and See video tutorials for animated cold trap removal compressed air to the instrument and the instrument itself must be turned off before starting. Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com www.markes.com...
  • Page 57 QUI-1057 Page 57 Remove the front top cover from UNITY 2 1. Pull the cover back 2. Lift up Loosen the steel fitting attached to the Loosen the steel fitting attached to the cold trap Keep a firm hold of the trap pneumatics assembly during these steps –...
  • Page 58 If in doubt practice with the trap alignment tool supplied in the shipping alignment tool supplied in the shipping kit. NEVER SWITCH UNITY 2 ON WITH THE TRAP ALIGNMENT TOOL INSTALLED. Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com enquiries@markes.com...
  • Page 59 THE END OF THE QUARTZ COLD TRAP Apply gentle steady pressure to push the trap into the sealing O-ring located inside the steel trap connector. Retighten the screw firmly Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com www.markes.com...
  • Page 60 Refit the front cover Turn on the carrier gas, compressed gas and instrument power. Restart the software. Leak test around the cold trap with a helium leak detector. Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com www.markes.com...

  • Page 61: Removing / Replacing A Broken Cold Trap

    Remove the split tube and any sample tubes / Remove the split tube and any sample tubes / interconnects. Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com enquiries@markes.com www.markes.com...
  • Page 62 1. Loosen the 4 screws highlighted 2. Slide the whole assembly back to allow access to the brass connector and hold in position by tightening one of the rear screws. Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com www.markes.com...
  • Page 63 2. Loosen the screw holding the heated valve assembly in place and slide forwards again. 3. Retighten the 4 screws. 4. Reattach the thermocouple and heater connectors. Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com www.markes.com...
  • Page 64 Loosen the 4 screws again and ensure the assembly is pushed up against the cold trap box. Reinstall a new cold trap as shown in Section 4.2 Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com www.markes.com...
  • Page 65 Repeat until no leak is detected. DO NOT OVERTIGHTEN OR YOU RISK DO NOT OVERTIGHTEN OR YOU RISK BREAKING THE COLD TRAP AGAIN. BREAKING THE COLD TRAP AGAIN. Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com enquiries@markes.com www.markes.com...
  • Page 66 (see Section 3.2) Loosen the thread on the steel connector and remove the cap Replace the O-ring (U-COV06). Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com www.markes.com...

  • Page 67: Trademarks

    QUI-1057 Page 67 6. Trademarks UNITY 2™, U A™, U A 50:50™, Air Server™ and SecureTD-Q™ are all trademarks of Markes International Ltd., UK Windows® is a registered trademark of Microsoft Corporation, USA. Markes International Ltd T: +44 (0)1443 230935 F: +44 (0)1443 231531 E: enquiries@markes.com...

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