TD-100 TM. Operator Manual. Version 1.1. August QUI-1069 TD-100 Operators Manual

Transcription

1 TD-100 TM Operator Manual Version 1.1 August 2012 QUI-1069 TD-100 Operators Manual

2 Contents 1. Introduction Instrument Technology Instrument familiarisation Hardware TD-100 component illustration Sample tubes DiffLok analytical end caps for sample tubes Optical sensor on main chassis door Tube desorption oven Tube seals The cold trap Cold trap cooling and heating Trap filters and seals Split filters Operation sequence Standby Load tube Leak Test Prepurge Primary (Tube) Desorption Pre-Trap Fire Purge Secondary (Trap) Desorption Inserting sample tubes into TD Capping tubes with DiffLok caps Loading tubes and trays into TD Desorb and split flows Gas flow through the cold trap When should desorb/split flows be measured? Sample splitting Calculating analyte masses in the sample tube Calculating splits/split modes Systems with Electronic Carrier Control (ECC) Software Start up Overview/summary Status bar...18 QUI-1069 TD-100 Operators Manual

3 Checks on external components of the analytical system Toolbar Schematic display of TD-100 status Controlling method The Trap Heat Function The Reset TD-100 icon Operating environment The Sequence Window Sequence Builder Creation of sequences and sets Adding a TD-100 set Viewing & changing parameters for tubes within a set Adding new samples to an existing set Deleting an item Storing and re-calling sequences Sequence recycling Sequence Viewer Sequence reporter (run log) Tube pressure ratio (PR) System Operation Loading a sequence Initiating a sequence Unloading the tube Loading the next tube Stopping a sequence Extending a progressing sequence TD-100 Options Configuration GC Interface Gas & Flow Methods Reporting option TD-100 method options Split on or off in standby Determining the prepurge time Desorption modes Tube conditioning mode Standard 2(3) stage desorption Sample tube prepurge Sample tube prepurge at elevated temperature...44 QUI-1069 TD-100 Operators Manual

4 SecureTD-Q - Re-collection for repeat analysis Cold Trap conditioning TD-100 parameter specifications Tube not found Tray not found Manual Leak Test The Set Gas Flow function Measuring and adjusting flows during Set Gas Flow TD-100 systems configured with Electronic Mass Flow Control To exit the Set Gas Flow function Gas flow constraints - minimum & maximum settings TubeTAG Introduction Placing TAG tubes in sample trays Manual tag read / write Tube information field descriptions Sample Information field descriptions Sequence reports with TAG tubes Tag information/error messages Altering the TubeTAG drop down menus Internal Standard Addition/Dry Purge Accessory (ISDP) Internal standard calibration gas: Gas connections ISDP flow path / sequence of operation Dry purge without internal standard addition ISDP method options Dry Purge Inject standard TD-100 systems and Electronic Mass Flow Control Ensuring split flow stability during trap fire with MFCs Automated SecureTD-Q re-collection operation Adding re-collection to a sequence Sequence of operation with automated Secure TD-Q Setting re-collection split / dry purge flow To exit the Set Gas Flow function Routine maintenance QUI-1069 TD-100 Operators Manual

5 8.1. Autosampler O-ring replacement Split tube O-ring / PTFE filter replacement Replacing a cold trap Cold trap O-ring replacement Accessing product and support information on the World Wide Web Appendix Uninstalling TD-100 software...80 QUI-1069 TD-100 Operators Manual

6 Preface This manual provides detailed instructions on the use of the TD-100. 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. I. Regulatory compliance Our products are thoroughly tested and evaluated to ensure compliance with applicable domestic and international regulations. This system (hardware and software) is CE compliant and meets Electromagnetic Compatibility (EMC) Directive and the Low Voltage Directive. The product has been evaluated to the following safety standards: UL 61010/CSA C22.2 NO UPD 1, IEC II. Warnings If the equipment is not used in a way specified by the manufacturer, the protection provided by the equipment may be reduced. System failures arising from such use may not be covered in standard warranty and service contract documents. Ensure that the plug (electrical isolator) can be easily and quickly accessed during equipment use. III. Technical Specifications Physical Electrical Height (cm/inches): 62/24.40 Maximum Power (W): 650 Width (cm/inches): 40/15.7 Line voltage: * Length (cm/inches): 53/21 Frequency (Hz): Mass (kg/lbs): 39/85.8 Input inrush current (A): <40 Energy (maximum) (BTU.hour -1 ): 191 *automatically selected IV. Environment operating conditions It is advisable to operate the system in a clean laboratory environment, with minimal atmospheric concentrations of organic vapours. Performance can be affected by sources of heat and cold from heating, air conditioning systems, or drafts. Temperature: Recommended operating ambient temperature range is 15 to 30 C. Humidity: Recommended operating humidity range is 5 to 95% non-condensing. NOTE: For storage or shipping the allowable temperature range is -40 to 70 C and the allowable humidity range is 5-95% non-condensing. After instrument exposure to extremes of temperature or humidity, allow 2 hours for return to the recommended ranges. QUI-1069 TD-100 Operators Manual 1

7 Altitude: The recommended operating altitude is up to 8000 ft (2500 m). Higher altitudes pose no safety risk, but instrument performance may be reduced. V. Safety alerts The CAUTION HOT SURFACE symbol indicates a burn hazard. Make sure the instrument is at room temperature before touching, or you may incur burn injuries. The BEWARE OF MOVING MACHINERY symbol indicates that there are mechanical moving parts which may cause physical injury. The LIFTING HAZARD symbol indicates that physical injury may occur if the correct lifting procedure for the instrument is not followed. Ensure that sufficient resources are available for moving and positioning the unit, and that staff are competent in manual handling techniques. VI. Technical support contact details In the first instance please contact your supplier. If they are unable to resolve your query, please contact Markes International on the details below. Address: Gwaun Elai Medi Science Campus, LLANTRISANT, RCT, UK, CF72 8XL Website: enquiries@markes.com Telephone: +44 (0) Fax: +44 (0) QUI-1069 TD-100 Operators Manual 2

8 1. Introduction 1.1. Instrument The TD-100 is a low cost, fully functional thermal desorption (TD) instrument, which allows simultaneous analysis of volatile and semi-volatile organic compounds [(S)VOCs] on one platform. Sample overlap mode means that desorption of a subsequent tube can begin while GC(/MS) analysis of a previous sample continues. This equates to minimised analytical cycle times. With typical GC(/MS) cycle times of 40 minutes, the TD-100 offers unattended processing of 100 tubes over a standard 60-hour weekend. This represents significant revenue potential with minimal labour costs, making it ideal for the analytical chemist/gas chromatographer working in a high-throughput laboratory environment. RFID tube tagging (TubeTAG ) further expands this capacity. This technology enables accurate electronic sample tracking of sorbent tubes from laboratory to field, and also within the laboratory. Electrical cooling replaces liquid nitrogen (cryogen), thus reducing footprint and continuous running costs. Sample re-collection as standard ensures no sample loss during analysis, and assists with method development/validation. Fully automated sample re-collection is offered as an option Technology Thermal desorption is a highly versatile, sensitive and laboursaving sample preparation technique for measurement of volatile and semi-volatile organic compounds [(S)VOCs] in air and materials. It provides the ultimate sample introduction technology for GC(/MS) in a fully automated and labour saving package. It combines selective concentration enhancement with direct extraction into the carrier gas, and efficient transfer/injection. TD is applicable to GC-compatible organics ranging in volatility from acetylene and freons, to high boilers such as n-c40, phthalate plasticisers and benzo-a-pyrene. It also offers quantitative concentration of some inorganic gases including nitrous oxide, SF6, CS2 and H2S. Key applications include: Environmental and workplace air monitoring Civil defence and forensic analysis Materials and materials emissions testing Food, flavour and fragrance profiling Material samples such as polymers, paints, drugs, foods, textiles, etc. can be directly thermally desorbed. Weighed samples are heated in a stream of carrier gas, allowing volatiles to be extracted into the gas flow, refocused and injected into the GC(/MS) analyser as a discrete, concentrated vapour band. Alternatively, vapours in gas or air can be concentrated on- or off-line onto sorbent traps/tubes before TD-GC(/MS) analysis. Several hundred litres of air or gas can be sampled and the vapours transferred/injected into the analyser in as little as 200 µl of carrier gas. Concentration up to 10 6 can be obtained in this way. Thermal desorption is recognised as the technique of choice for air monitoring (workplace and environmental) and is the subject of many international standard methods. Key examples include: EN ISO 16017, ISO , EN (parts 1 & 4), ASTM D6196, US EPA TO-15 (canisters) & TO-17 (tubes), NIOSH 2549, UK Environment Agency guidance on landfill gas (LFGH 04) and US EPA guidance for online ozone precursor monitoring. Markes TD systems are fully compliant with all these standards. Thermal desorption offers significant advantages over solvent extraction (SE). Key benefits include: Greatly improved recovery (>95% vs % with SE Reusable sample tubes No toxic solvent required Reduced analytical interference Typically 1000-fold sensitivity improvement QUI-1069 TD-100 Operators Manual 3

9 2. Instrument familiarisation 2.1. Hardware TD-100 component illustration Sample tubes TD-100 is compatible with industry standard sample tubes 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. Quartz or glass wool is recommended for retaining the sorbent in glass tubes. QUI-1069 TD-100 Operators Manual 4

10 DiffLok analytical end caps for sample tubes The DiffLok analytical end caps used with TD-100 are fitted with patented DiffLok technology which reduces diffusive ingress effectively to zero. This preserves the integrity of both samples and clean desorbed tubes by preventing ingress or loss of volatiles while the tubes are on TD-100. However when a tube is lifted into the TD- 100 desorption oven and sealed into the carrier gas flow path just prior to desorption, the application of pressure to the caps allows carrier gas to flow. Each tube requires two DiffLok caps - a plain stainless steel cap which goes on the cold end or non-sampling end of the tube and an inert coated stainless steel cap (which is blue/pink in colour) which goes on the hot end or sampling end of the tube Note: it is important to keep the hot end and cold end caps separate to ensure good quality analysis. Hot sample gas is desorbed from the tube and passes through the hot end cap into the thermal desorber - this is why the hot end cap is inert coated (as it is part of the sample path). Only carrier gas passes through the cold end cap Optical sensor on main chassis door The main front chassis door on TD-100 is configured with an optical sensor which prevents up and down movement of the main tray stack while the door is opened. Other movements, including further withdrawal of an already active tray, elevation of the active tube, etc., and all analytical desorption steps will continue as normal. In general, if the TD-100 door needs to be opened during a sequence, first examine system status via the Sequence Viewer to check that the system will not need to access a different tray within the period of time that the door needs to be open Tube desorption oven The TD-100 tube desorption oven heats up rapidly (~150 C/min) at the start of elevated temperature purge or tube desorption. It begins to cool at the end of primary (tube) desorption and decreases from 300 C to 50 C within 5 minutes Tube seals Once the sample tube has been moved into position in the tube oven it is sealed into the flow path by temperature resistant Viton O-rings located on sealing nozzles. Each O-ring should last for >1000 tube-sealing operations. In the event of failure, O-rings are readily replaced by the user (see section 8) The cold trap The quartz cold trap contains a 2 mm diameter x 60 mm long bed of sorbent (30 to 100 mg depending on sorbent density) supported by quartz or glass wool. Note that the length of the first plug of glass wool is included in the total 60 mm sorbent bed. The full range of cold traps available can be found in the Markes International thermal desorption accessories and consumables catalogue. Information on replacing a cold trap can be found in section Cold trap cooling and heating TD-100 contains a 2-stage Peltier cell, which uniformly cools the entire 60 mm sorbent bed to a minimum of - 30 C and a maximum of +50 C in ambient temperatures. No liquid cryogen is required. Dry air or nitrogen flows into the cold trap box creating a slight positive pressure and minimising entry of water from the QUI-1069 TD-100 Operators Manual 5

11 laboratory atmosphere. If the cold trap box was not purged, ice would quickly build up around the Peltier cell, which is maintained at sub-zero temperatures throughout TD-100 operation. Note: C2 hydrocarbons (ethyne, ethene and ethane) and the most volatile freons cannot normally be sampled using sorbent tubes at ambient temperatures - breakthrough volumes are too small for practical use,even with the strongest tube sorbents. Once all the target analytes have been collected and focused in the cold trap, the trap oven heats rapidly reaching rates of 100 C/sec for the first critical stages of trap desorption. Uncompromised capillary chromatography is produced without on-column focusing and with desorption flows as low as 2 ml/min. This facilitates splitless operation with high-resolution capillary GC Trap filters and seals As with the sample tube, the cold trap is sealed into the gas flow path of TD-100 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. The user has access to this O-ring seal and filter in the connector (see section 8), but a Service visit is required to access and change the trap O-ring seal in the heated valve. As the cold trap is only changed infrequently, the seals will rarely, if ever, need to be replaced. It is recommended that TD-100 is professionally serviced once per year and that the valve-end seal be changed as part of this annual maintenance operation Split filters There is a split filter tube packed with charcoal (P/N SERUTD-5065) on the split line upstream of the on/off solenoid and needle valve. This prevents the split portion of the sample from contaminating the valves and from reaching the laboratory air. The flow path up to the charcoal filter is heated and constructed of inert, Silcosteel tubing. The split filter itself is the same size as a standard sample tube and may be readily replaced by a clean sorbent tube if the split effluent is to be re-collected for repeat analysis, see section The split filter (or re-collection tube) is sealed into the split flow line using easy-connect, Viton O-ring seals. The sampling end/grooved end of the re-collection tube should point to the rear of the instrument. Conventional charcoal split filters will become contaminated over time and should be reconditioned or repacked when required Operation sequence When a tube is placed and sealed into the flow path of TD-100 for conventional 2(3) stage desorption, it undergoes the following operational sequence: (1) Standby, (2) Tube loaded and sealed into flow path, (3) Leak test, (4) Prepurge, (5) Primary desorption, (6) Pre trap fire purge and (7) Secondary desorption. These sequence steps are illustrated below. QUI-1069 TD-100 Operators Manual 6

12 Standby To GC HV P2 4 Key P1 Pressure and flow Pressure no flow Trap / desorb vent Split vent Load tube A tube cannot be loaded into the TD-100 oven, until it is at or below the Load Temperature. The Load Temperature is set under Options and is recommended to be set at 50 C. Click on View and Options and open the Configurations tab. Once the oven has reached the Load temperature, the tube lift mechanism raises the tube into the oven cradle and the tube is sealed into the carrier flow path. QUI-1069 TD-100 Operators Manual 7

13 Leak Test To GC HV P2 4 Key P1 Pressure and flow Pressure no flow Trap / desorb vent Split vent After the sample tube is loaded the Leak test begins. This has 4 parts: 1) Sample side high pressure (shown) 2) Sample side low pressure 3) Sample side + cold trap + split tube high pressure 4) Sample side + cold trap + split tube high pressure During the high pressure tests the isolated part of the flow path is pressurised with carrier gas. The pressure is then switched off and the pressure monitored (P2). If the measured pressure drops by more than 5% in 30 seconds this is classified as a leak in the sample flow path. During the low pressure tests the flow path is depressurised briefly and the isolated part of the flow path monitored to see if it increases by more than 2 Psi over 30 seconds. A leak during the low pressure tests would indicate an internal leak. If TD-100 fails the low pressure parts of the leak test the system requires the attention of a trained service engineer. QUI-1069 TD-100 Operators Manual 8

14 Prepurge To GC HV P2 4 Key P1 Pressure and flow Pressure no flow Pressure optional flow Trap / desorb vent Split vent Each tube must be purged thoroughly with carrier gas to remove air before heat is applied. Even the smallest trace of oxygen could result in sorbent and possible analyte oxidation, generating artifacts and compromising data quality. Further information about determining the prepurge time can be found in section QUI-1069 TD-100 Operators Manual 9

15 Primary (Tube) Desorption To GC HV P2 4 Key P1 Pressure and flow Pressure no flow Pressure optional flow Trap / desorb vent Split vent At the start of primary (tube) desorption the tube oven begins to heat (either from ambient or from the temperature of the optional elevated temperature purge if selected). 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. QUI-1069 TD-100 Operators Manual 10

16 Pre-Trap Fire Purge HV To GC P2 4 Key P1 Pressure and flow Pressure no flow Trap / desorb vent Split vent Following primary desorption, the heated valve is moved and carrier gas is flushed through the split tube and trap to remove any residual air and water, prior to trap injection. It may also be used to dry purge the cold trap prior to injection when directly desorbing solid or humid samples. QUI-1069 TD-100 Operators Manual 11

17 Secondary (Trap) Desorption To GC HV P2 4 Key P1 Pressure and flow Pressure no flow Pressure optional flow Trap / desorb vent Split vent The final stage is secondary trap desorption. The cold trap is heated at a rate of 100 C/s during the first seconds ensuring rapid desorption of analytes into the carrier gas stream. The flow through the cold trap at this stage is determined by the column flow and any outlet split. Note that the TD-100 flow path remains in the trap desorption configuration, until the trap has cooled back down below 50 C. The sample tube is unloaded once it reaches its Unload temperature, see section QUI-1069 TD-100 Operators Manual 12

18 2.3. Inserting sample tubes into TD Capping tubes with DiffLok caps The caps should be pushed gently onto the correct end of the tube using a turning motion until they reach a natural stop. Do not force the cap further onto the tube once this stop has been reached. A tube correctly capped with a pair of DiffLok caps is 123 mm long, and tubes with correctly fitting caps will fit snugly inside the TD-100 tray, but without any force being required to insert the tube or lift it from the tray. The inert coated (blue/pink coloured) cap should be placed on the sampling (desorption) end of the tube - this is normally the grooved end of stainless or coated steel tubes and, in the case of glass tubes, usually the end closest to the frit (if present) i.e. the end that is nearest the 'M' of 'Mi' Sampling End Loading tubes and trays into TD-100 It is usually easier to withdraw the trays from TD-100 and place them on the bench, before loading them with tubes. However, take care that the trays have been appropriately labelled before they are taken out of the instrument. Each tube position in a tray is numbered (1 at the back to 10 at the front of the tray). There is a notch on the right hand side of each plastic partition between the tubes which will be on the right hand side when the tray is correctly orientated. Tubes should be loaded in the tray such that the sampling (grooved) end of the tube (capped with the blue/pink cap) is also on the right hand side. With the tray orientated such that its label is towards you and tube position 1 is furthest from you, place the capped tubes in the desired positions in the tray with the sampling end on the right as described above. Loaded trays should then be pushed back into the appropriate tray locations in TD-100. QUI-1069 TD-100 Operators Manual 13

19 Note: If the TD-100 autosampler door is opened while a sequence is in progress, it is physically possible to access, remove or add any non-active tray to TD-100. (The active tray will be recessed towards the back of TD-100). Caution: This must be done with great g care. Any attempt to remove the active tray (i.e. the recessed tray) or to push a second tray into the same position in the stack, could result in serious mechanical failure. It is normally advisable to load the complete sequence of tubes and trays into the system before closing the main door and initiating the complete sequence Desorb and split flows Gas flow through the cold trap The TD-100 cold trap operates in backflush mode - the sample gas stream enters and leaves the cold trap through the narrow-bore/restricted end which points to the rear of the instrument. Backflush desorption allows use of a series of 2 or 3 sorbents of increasing strength in the cold trap. This facilitates the analysis of wide volatility range samples. High boiling compounds are retained by and quantitatively desorbed from the first weak sorbent, without ever coming into contact with the stronger sorbents behind When should desorb/split flows be measured? Whenever a needle valve adjustment knob has been moved (deliberately or accidentally). Whenever the GC column has been changed. Whenever the carrier gas pressure to TD-100 has been changed. Measuring the flows is often done at the start of a sequence of analyses to confirm/ensure that no system changes have taken place Sample splitting A sample analysed on the TD-100 can be desorbed splitlessly, transferring all of the sample to the analytical system (GC-MS). However, depending on the analyte mass in the sample tube, it may be necessary to split some of the sample so that the amount of transferred to the GC-MS is reduced, to make it compatible with the analytical column capacity (typically 100 ng per component for a 0.25 mm I.D. column with a 0.25 µm film) and within the linear range of the GC detector (for a modern mass spectrometers in full scan mode is pg per component) Calculating analyte masses in the sample tube In order to determine the required split, it is necessary to have an approximate idea of the mass of analyte which is expected to be retained/collected in the sample tube. For direct desorption of volatiles from materials, the mass of analyte is most easily determined experimentally from control or real-life samples. It can also be calculated from relevant material specifications where appropriate e.g. if the specification for residual chloroform in cough medicine is 1% w/w a 20 mg sample will contain 200 µg of chloroform. For air monitoring applications the calculations are a little more complex as they depend on variables such as diffusive uptake rate, pumped volume and molecular weight (See Mi TDTS 25). QUI-1069 TD-100 Operators Manual 14

20 Calculating splits/split modes Once the expected mass of analyte, the detection limits of the system, and the analytical capacity of the column are all known, then an overall ideal split can be calculated. For example, if the expected mass of analyte on the sample tube is 50 µg and the analytical column capacity is 100 ng, then a total split of at least 1/500 is required to prevent column overload i.e. only 0.2% of the sample must be transferred to the column. One of three different split modes can be utilised: Zero/ splitless Unusually among thermal desorbers, TD-100 can operate in splitless mode in conjunction with narrow bore (0.32 mm ID) columns and MS detectors as the minimum flow required through the cold trap during trap heat is 2 ml/min. During tube desorption the desorb flow must be set to at least 10 ml/min to provide enough flow through the sample tube for efficient thermal desorption. During tube desorption the desorb flow should not far exceed 50 ml/min or there may be a risk of breakthrough from the cold trap. Single During single split operation the split may either be open during tube or trap desorption. The advantages of having the split open on the way into the trap (inlet split) are: During tube desorption the desorb flow must be set to at least 10 ml/min to provide enough flow through the sample tube for efficient thermal desorption. 1. That a relatively fast flow can be used through the tube to facilitate desorption while, at the same time, the flow passing through the cold trap is kept low to aid retention and focusing of analytes. 2. That the cold trap is not overloaded with solvent or analytes. Split discrimination and/or peak splitting may be observed if the trap is allowed to become overloaded with volatile solvent or water. During tube desorption the desorb flow should not exceed 50 ml/min or there may be a risk of breakthrough from the cold trap. During tube desorption the desorb flow should not be less than 2 ml/min to ensure efficient sweeping of analytes onto the trap sorbent. The flow through the trap during trap heat should not exceed 100 ml/min. Double During double split operation the split is open both during tube desorption and trap heat. As above for single split operation. During splitless operation: Flow through tube during tube desorption Flow through trap during tube desorption Flow through trap during trap heat = Desorb Flow = Desorb Flow = Column Flow QUI-1069 TD-100 Operators Manual 15

21 During single split operation: Flow through tube during tube desorption Flow through trap during tube desorption Flow through trap during trap heat = Desorb Flow + Split Flow (if selected) = Desorb Flow = Column Flow + Split Flow (if selected) During double split operation: Flow through tube during tube desorption Flow through trap during tube desorption Flow through trap during trap heat = Desorb Flow + Split Flow = Desorb Flow = Column Flow + Split Flow Systems with Electronic Carrier Control (ECC) When installed with certain models of commercial GC(/MS), TD-100 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. In this case, manual adjustment of the desorb and split flows, as described above, is still required. Key benefits of electronic control of the carrier gas through the column include retention time stability (even when split flows are changed significantly) and pressure programming for enhanced chromatographic performance with higher boiling compounds. For further information see section 6. QUI-1069 TD-100 Operators Manual 16

22 3. Software 3.1. Start up In order for the User Interface (UI) to start up, the software has to detect the two system components, namely the autosampler and trap module. Turn on the mains switch at the rear of the unit. The green light on the trap (small) section will display, whilst the red light will display on the autosampler (large). Double clicking on the desktop TD-100 icon, prompts the UI to first attempt to detect the trap module before beginning firmware download to the autosampler. At this stage, the red light on the autosampler component will turn amber. The conversion to green will indicate software activation. In summary, viewed from the front of the unit, these light colour changes will progress as indicated, with firmware download. Autosampler component Trap component Overview/summary QUI-1069 TD-100 Operators Manual 17

23 The above screen capture shows the main components of the software, namely Method Method page, Flowpath Flowpath schematic (appears after clicking the red bordered icon) and Sequence Sequence page, the details of which are covered separately Status bar The status bar displays all key TD-100 parameters and is always visible and on top of the desktop while the software is open, whether maximised or minimised. The level of information presented for each category may be selected by a right click of the mouse on the appropriate section of the status bar. The parameters shown on the status bar are as follows: Status Shows the overall status of TD-100 as it progresses through the various stages of the sequence - Standby, Leak Test, Trap Heat etc. Elapsed Time Shows the time elapsed since the start of the function currently operating on TD- 100 and should be read in conjunction with the Status parameter. For example if the Status is reading Prepurge and the Elapsed Time is reading 0.3 this tells us that TD-100 is 0.3 minutes (i.e. 18 seconds) into the ambient purge. If the Status is reading Primary Desorb and the Elapsed Time is then it is 4.9 minutes since the start of tube desorption etc. Pressure Shows the pressure of the carrier gas within the TD-100 flow path. Autosampler / Trap Module TD-100 continually monitors the actual temperature of its internal heated/cooled zones (tube oven, cap heater, interface, cold trap, transfer line and heated valve) and compares them to the set values. When first switched on TD-100 status changes to Standby and the display for the temperatures will be highlighted blue until all zones reach the relevant set point. Note: A run may be started when TD-100 is Not Ready and the run will then pause, waiting for the appropriate zone to reach temperature before desorbing the tube. The status will read Equilibrating at this stage. Note: The actual temperature of the tube oven has no effect on the ready status as heat is not applied to the oven until tube desorption starts. QUI-1069 TD-100 Operators Manual 18

24 GC Indicates whether the GC status is ready ( ) or not ready ( ). See section below Checks on external components of the analytical system TD-100 is connected to the GC via the relevant GC Interface Harness. The analytical system should be configured such that all components "downstream" of the GC (e.g. mass spectrometer, data handling system) must be ready before the GC becomes ready. This ensures that no sample is injected from TD-100 onto the GC when the analytical system is not able to analyse the sample and collect the data. When the GC comes ready it will provide a signal to TD-100 via the Interface Harness and the GC indicator on the status bar will change from a cross to a tick. TD-100 checks this signal, to ascertain whether the GC is ready, twice during its operation sequence: Before going to tube desorb Before going to trap heat If TD-100 finds that the GC is not ready, it will indicate as such and display Waiting for GC on the status bar. TD-100 will continue to wait until it receives an external ready signal from the GC system before proceeding to either of these two stages. QUI-1069 TD-100 Operators Manual 19

25 3.4. Toolbar The main TD-100 software toolbar is shown below, with the icons explained in the table. (1) (2) (3) (4) (5) (6) (7) (8) (9) (10) (11) (12 12) (13 13) (14 14) ) (15( 15) (16 16) (1) Generating a new method / sequence ( ) New methods / sequences are generated by either selecting File > New, by clicking on the icon, or by pressing CTRL and N. A new method / sequence window will be brought up containing a set of default parameters ready for you to modify. Once the method has been generated it can be named and saved. See below. (2) Opening a stored method / sequence ( ) (3) Saving a method / sequence ( ) Methods / sequences are opened by either selecting File > Open, or by clicking on the icon. This brings up the directory (nominated under Options, see section 3.7) containing TD-100 method and sequence files. Select the required file name and click OK or double click on the required file name to access it. New methods / sequences can be saved by: 1. Clicking on the icon 2. Selecting File > Save 3. Pressing CTRL and S 4. Selecting File > Save As Using the first three routes brings up the Properties dialogue box. Using route 4 brings up the Method File Directory and allows a file name to be entered for the method. The Properties dialogue box then automatically appears with the file name in the appropriate field. The Method Author and Company names will appear in the Method Properties dialogue box, as set up under Options (see section 3.7). If nothing has been entered for these fields under Options the blanks may be filled in at this stage. The Method Name and Notes sections can be used to provide additional information on the method if required. (4) Print (method) ( ) Select File > Print or click on the print icon to print the method. This function will either print the entire method, including properties and gas flows (if entered) as a text string, or will simply print the main method page as it appears on the computer screen. Method print format is selected under Options (see section 3.7). Print Preview under the File menu will display the print format on the screen if needed. It is the active method that is printed. (5) Copy (method Ensure that the method you wish to copy is the active method. Clicking on it with QUI-1069 TD-100 Operators Manual 20

26 parameters) ( ) (6) Paste ( ) the left hand mouse button will make it active if necessary. Select Edit > Copy, or click on the icon (the shortcut CTRL and C can also be used). Copy will put a "text copy" of the active method onto the Windows Clipboard (in English Only), thus allowing you to paste the text string into another application such as a word processor. Paste is activated after Copy has been used and allows for a copy of the active method to be pasted to another method (after THAT method has been made Active). Note: TD-100 does not support pasting from the Windows clipboard i.e. you cannot paste from the Word processor to TD-100 software applications. (7) Start run ( ) Used to start a desorption sequence. This is accessed by clicking the icon or selecting Instrument > Run. (8) Set gas flows ( ) Used to set the split and desorb flows. Accessed by clicking the icon, see section 3.13 (9) Trap heat ( ) Selected either by clicking Instrument > Trap Heat, or by clicking on the icon, see section (10) Exchange split tube ( ) (11) Stop run/sequence ( ) (12) TD-100 schematic ( ) Used to divert any split flow in standby mode so that the split/recollection tube can be removed without loss of carrier gas. Accessed by clicking on the icon. see section The Stop sequence function is used to stop a run or run sequence (see section 3.6.5), exit the Set Gas Flows mode, Exchange split tube mode and Trap Heat procedure. Accessed by the icon. Note: If you stop a run at any point after the tube desorption process has started, then some components will have already passed onto the trap which will therefore need cleaning - along with the GC column - prior to analysing a new sample. Accessed by clicking on the icon or by selecting View > Status > Show, see section (13) Controlling method Used to assign the active method / sequence as the controlling method / sequence by clicking on the icon, see sections & 3.5 ( ) (14) Leak test ( ) A leak test may be carried out manually via the icon. This opens a dialogue box with a button to load a tube then pressurise the flow path and to perform a leak test. The Leak Test function should be used in conjunction with a He leak detector. The Leak Test dialogue box also allows the valves controlling the flow path to be operated independently for assistance with diagnosis of faults, see section 3.12 (15) Edit In standby - Used to load a tube fitted with a TAG for manual read / write operations, see sections & 4. QUI-1069 TD-100 Operators Manual 21

27 ( ) (16) Reset Mechanically reset TD-100, see section ( ) Schematic display of TD-100 status A simple schematic illustrating the status of TD-100 can be displayed on the screen at all times during system operation. This is accessed using the status icon ( ) or by selecting View and then Status Show. The schematic display of TD-100 status is linked directly to operation of the instrument. The display is thus not just cosmetic, but is a representation of the actual status of the instrument Controlling method One method is identified by TD-100 as that controlling the system i.e. the method dictating the set parameters. This method is called the Controlling Method and cannot be deleted or closed until another method is loaded as the controlling method. To load another method use either the Load icon or select File and then Load from the menu. The loaded method will not automatically become the controlling method. The controlling method is always identified as such in the bar at the top of its window, whether active or not. To make a loaded method the controlling method, select it (to make it the active method) then click the icon. Once set TD-100 immediately starts to set the new parameters. The instrument status changes accordingly. Only one method is identified as the controlling method at any one time. Note: An active method is not necessarily the controlling method. The active method is simply that last modified or accessed by the operator The Trap Heat Function The trap heat function allows the cold trap to be heated without running a full thermal desorption analysis. All steps that usually occur before trap desorption e.g. prepurge, tube desorption etc. are not performed. The trap QUI-1069 TD-100 Operators Manual 22

28 heat can be used for cold trap conditioning or for assessing sample carryover specifically caused by the cold trap. TD-100 can use two sets of parameters when undertaking Trap Heat. Either those used in the existing Controlling Method or a special set of parameters identified as the Trap Heat Method. The choice between these two is made under Options, see section The selected option will then appear as the default Trap Heat conditions whenever this function is accessed. To view and edit the Trap Heat method click View > Trap Heat Method. The required parameters are entered in the boxes. Checking the relevant boxes will activate the split on during trap heat / standby. Trap Heat is selected either by selecting Instrument and then selecting Trap Heat, or by selecting the Trap Heat icon ( ) on the toolbar. The following dialogue box then appears. Once Trap Heat has been selected, TD-100 will ask you to confirm that the default method is that which you wish to use. For example, if the default method was set to Use Controlling Method Parameters then the box message will read Heat Trap with the Controlling Method Parameters? Select Yes, No, or Cancel. If Yes is selected, TD-100 proceeds with trap heat. If No is selected the instrument software immediately takes you to the relevant section under Options to change your selection. Also, a Wait for GC Ready, before Heating? option is made available. Depending on the response to this option, TD-100 will either wait for an External Ready signal from the GC equipment before proceeding, or continue the trap heat regardless of the GC status. Caution: Ensure that the dedicated Trap Heat Method or the Controlling Method, if being used, is compatible with the maximum temperature of the least stable sorbent in the cold trap. Caution: For newly installed traps containing carbon molecular sieves the Trap Heat Method must not be used until the trap has been extensively purged with helium immediately prior to Trap Heat. Refer to the cold trap certificate supplied with your trap for further information The Reset TD-100 icon This icon ( ) is again only accessible from the active environment screen. Once pressed, it brings up the dialogue box shown below. QUI-1069 TD-100 Operators Manual 23

29 If the user decides to proceed, the TD-100 will unload any tubes or tray in the instrument and return to its default mechanical positions Operating environment The software operates in two environments: Active is available while the system is in Standby. It allows editing (and reviewing) of all method and sequence files. Edit is available while the system is running by clicking on the Edit icon as shown below, or by selecting View and then Run/Edit View. It allows editing (and reviewing) of any non-controlling method or sequences. Edit environment is not available while the instrument is in standby mode. Once in the Edit Environment, select the normal Open File icon (or select File followed by Open ). Then select the desorption method or sequence file you wish to edit. Note: The system does not allow you to edit the current controlling method or sequence files. Methods and sequences may be modified, generated and stored using the edit environment without impacting the sequence that is currently in progress The Sequence Window This details the order of analyses that will be undertaken when the system is started. A sequence may be stored and recalled from memory, but only one sequence can be designated as the active (controlling) sequence at any one time. To activate a sequence highlight the sequence window and click the controlling method icon ( ). The Active Sequence section comprises three windows arranged in tabs. Sequence Builder Sequence Viewer Sequence Reporter Builds an automated sequence Presents a visual representation of the sequence and its real time progress Presents a complete history of a sequence of analyses including any deviations that occurred QUI-1069 TD-100 Operators Manual 24

30 Sequence Builder The sequence builder is used to build/generate an automated sequence of analyses to be run by TD-100. It is accessed by clicking on the relevant tab of the sequence window (in either active or edit environment). Definitions: A set set is a series of tubes which initially are all assigned the same desorption method. A sequence sequence is constructed of a number of sets sets Creation of sequences and sets Sequences and sets are created or amended using a drop down list which is displayed by right clicking anywhere on the Sequence Builder window. The options listed are as follows: New Sequence Open Sequence Add Sequence Add set of tubes Add tube Delete item Opens a completely new Sequence window Opens the common dialogue box from which you can select the sequence file you wish to open. An existing sequence may be modified to create a new one. Opens the common dialogue box from which you can select the sequence file you wish to append to the end of the current sequence Adds a number of tubes to comprise a set Adds another tube to the currently selected set Deletes the selected/highlighted line from the Sequence or Set Adding a TD-100 set A set is added to the opened sequence by selecting Add set of tubes from the dropdown menu list above. This opens a dialogue box from which you should select the desorption method you wish to use for this set of samples. After selection of the desorption method, the Add New Set dialogue box is opened. QUI-1069 TD-100 Operators Manual 25

31 The following parameters may now be entered: Set name Method 1st tube Last tube No of Injection Sample (base) Name Enter name used to distinguish this particular set of samples. The stored desorption method to be used to analyse this set of samples (this was selected from the common dialogue box (see above) earlier. However, double clicking on the method name here will allow you to change this method choice if required. The first tube to be analysed in this set. The last tube to be analysed in this set. The number of desorptions required per tube. An identifier for this set of samples (for example if the base name is Room 1_ and there are seven tubes in this set, they will be named Room 1_1, Room 1_2 etc. Any number of sets of tubes can be added to a single sequence by repeating the Add TD-100 Set operation. The same tubes can be included in multiple different sets; for example, if the user wishes to desorb a set of tubes at several different temperatures or re-run the tubes in conditioning mode after the series of analytical desorptions has completed Viewing & changing parameters for tubes within a set A tube-by-tube listing of any set can be viewed by clicking on the + alongside a set name. This expands the set and shows a dropdown list of all the tubes in the set. The set is minimised by clicking on the -. See representation below. QUI-1069 TD-100 Operators Manual 26

32 Each individual tube has the following parameters associated with it: Set Type Method Tube Injection A unique name (e.g. the ID No.) can be entered May be designated as sample, blank or calibrant Specifies the desorption method applied The position of the tube in the tray stack The number of replicate desorptions required Each of the individual tube parameters (except the Set Set column) may be edited by highlighting the field of interest and modifying it as required. If Method Method is highlighted, double clicking on it takes you to the stored method files. This flexibility means that the Set function provides a quick and easy way of generating a long sequence of tubes, but does not restrict selection of separate desorption methods for individual tubes, or groups of tubes within a set, if required. The Method Method may be modified for one or all of the tubes in a set. If more than one desorption method is selected within a set, the method column header will display 'Various Various' Adding new samples to an existing set First expand (by clicking on the + sign) to display all the samples already listed. Highlight a single sample and right click. A dropdown list will be displayed, identical to that in Section above, but with additional 'Add Tube' function. The same menu (dropdown) may be accessed by clicking on Automation Automation in the menu toolbar. Select 'Add tube' and a common dialogue box will appear asking you to Select Method to be used with Set or Sample. Once the method is selected, click OK and the Add Sample to Set window will appear. This allows QUI-1069 TD-100 Operators Manual 27

33 you to define other parameters for the new sample such as the tube number, number of injections and Sample Name. Select 'OK' to close the window after the appropriate parameters have been entered Deleting an item To delete a whole set or a single sample from an expanded set listing, open the drop down item list. Select Delete item or press the delete on the keyboard and the highlighted item will be deleted Storing and re-calling sequences Having completed the sequence table using the Sequence Builder, use the Save or Save As functions on the toolbar. Stored sequences can be recalled using the Open File icon, by selecting File and then Open (toolbar) or by right clicking on the Sequence Builder window and selecting 'Open Sequence' from the list Sequence recycling A sequence may be recycled by ticking the Recycle Recycle box at the top of the Sequence Builder window. This opens two additional check boxes, Stop after and Recycle. If the Stop after box is ticked then this will activate the Recycle box - enter the number of cycles that the sequence should go through before stopping. If the 'Stop after' check box is not ticked, the sequence will continue recycling indefinitely until the Stop icon is pressed or Instrument then Stop is selected from the dropdown menu bar Sequence Viewer This gives a graphical overview of the sequence that has been built. It is accessed by clicking on the relevant tab of the sequence window. A grid is displayed which graphically indicates the position of all the tubes in the sequence. QUI-1069 TD-100 Operators Manual 28

34 Tubes are designated as follows: Empty Sample Sample+ Calibration Blank Active No tube in this position A sample to be analysed A sample tube which is called up by more than one set in the sequence A calibration tube A tube designated as a blank The tube currently being analysed by TD-100 Tube designations are distinguished by colour. Colour choice (for all options except Empty Empty ) may be selected using assignment boxes. (Simply right click on the assignment box and select the colour from the options displayed). Information on any tube can be viewed by clicking on the respective box in the grid. As a sequence progresses, the Sequence Viewer is continually updated to display current system status Sequence reporter (run log) The Sequence Reporter presents a complete history of a sequence of analyses including any deviations that occurred up to that point, and is created at the end of every sequence. Examples of deviations that may occur include leak test failure, missing tube or TD-100 door open. Any tubes present on the system, but unassigned in the sequence, will be ignored by the system and will not be reported. To access Sequence Reporter, select the tab in the Active Sequence section. The number and assignment of columns in the Sequence Reporter table can be modified to display additional information such as the time and date of each specific tube and trap desorption. To re-assign existing table columns or create and assign parameters to new columns, select the Options function under 'View' on the main software control toolbar, click to select 'Reporting' from the list and then tick the desired parameters from the list. Click OK OK. QUI-1069 TD-100 Operators Manual 29

35 All sequence reports are stored in the install directory. To view or export these files using standard Excel spreadsheet software go to: C:\Program Files\TD100 D100\Reports where you will find the.csv files stored under the name of the sequence and the date there are two files generated for each sequence: e.g. test_f1jan2010_ csv This full file contains all available reporting information. test_p1jan2010_ csv This partial file contains only the reporting options selected in the Options Reporting tab. Open the required file into Excel as usual Tube pressure ratio (PR) Calculated ratio (P1/P2) of pressure measured before (P2) and after (P1) sample tube when sealed into the flow path during the leak test. A value of 1.00 indicates an unimpeded tube while a value of 0.00 would indicate a completely blocked tube System Operation Loading a sequence Open the stored sequence file by selecting File and Open from the dropdown menu or by clicking the usual open file windows icon. Designate the file as the controlling sequence by selecting File and Load from the dropdown menu or by clicking the Load icon in the windows toolbar. Only one sequence can be designated as the controlling sequence at any one time. QUI-1069 TD-100 Operators Manual 30

36 Initiating a sequence To start a sequence, press the Run icon on the main toolbar. The method associated with the first tube of the sequence is recalled. TD-100 then selects and loads the first tube designated in the sequence and begins the series of runs. Desorption steps and analysis sequence of each tube are described in Section 2.2. Note: If a method has been modified but not stored, then when the run is started the original non-modified method will be recalled and used. Ensure you save any changes to your operating method Unloading the tube After completion of the primary desorption the tube oven starts to cool. Once it has cooled to the unload Temperature the desorbed tube is unsealed and unloaded back into the tray. The unload temperature is set under Options and is recommended to be set at 100 C. Click on View, Options and open the Configurations tab Loading the next tube The next tube in the sequence will be lifted and sealed into position as soon as the previous tube is replaced in the tray, provided that the TD-100 desorption oven is at or below its load temperature (section 2.2.2). This ensures that the tube does not get warm prematurely, causing loss of volatiles during leak test and pre-purge. Under default conditions, with a GC cycle time of 0, the system will proceed with leak test and purge of the next tube, but will not begin primary (tube) desorption until the GC reaches Ready status. However, if a GC cycle time has been entered (to optimise sample throughput), TD-100 will calculate when to start the primary (tube) desorption so that the GC will become Ready just prior to the end of the desorption time. This means that after the first tube, cycle times for subsequent samples are determined just by the GC (/MS) analysis cycle time, see section Stopping a sequence A Sequence may be stopped at any time using the Stop icon on the main toolbar. Clicking the icon brings up the Stop Link dialogue box. This instructs TD-100 to stop the sequence and return to standby. A number of options are available. Continue Running will allow you to continue uninterrupted if you have unintentionally clicked Stop Stop. QUI-1069 TD-100 Operators Manual 31

37 Stop after next injection of this sample will stop the sequence after it has finished sampling and injected the sample (row) that is currently running. Stop after all injections of this sample will stop the sequence after it has finished all of the sampling steps and injections defined in the current sample (row). Stop at the end of this set will stop when the current set has completed. Stop at the end of this cycle will complete all the sets in a sequence and then stop (this is useful for interrupting a sequence when Cycle Indefinitely has been chosen) Stop immediate will stop the TD-100 immediately even if it is halfway through a sampling step. Selecting this option could mean that the cold trap is loaded with sample when you come to start the next sequence Extending a progressing sequence To add additional samples to a sequence that is already in progress, first stop the sequence (section 3.6.5), then generate a new or modified sequence (section 3.5.2). This sequence should contain those samples from the old sequence that were not yet analysed plus the new set(s) of tubes you wish to add. The sequence must be saved (section 3.5.7) and loaded (section 3.5) to make it the controlling sequence. The new tubes should be added to empty or unfilled trays in the stack, (this is best completed while the sequence is stopped). Restart the system with the new/modified sequence (section 3.6.2). Note: Remember that if the thermal desorption sequence is altered and restarted as described, the GC(/MS)/data processing sequence will almost certainly need changing to reflect this. Caution: It is not advisable to add tubes or trays to TD-100 mid-sequence. However, if this is necessary, under no circumstance must the active tray be moved even if it has not yet begun to be withdrawn into the machine. Caution: Take care if opening the TD-100 door mid-sequence (section( 2.3.2) 3.7. TD-100 Options The Options page is accessed in the TD-100 software via View > Options Configuration This is accessed by selecting View > Options > Configuration. The configuration page contains the current TD- 100 hardware configuration settings and several sequence options. QUI-1069 TD-100 Operators Manual 32

38 Instrument Configuration TD-100 has two basic instrument configurations; one without automated re-collection capability (TD-100 Standard) and one with automated re-collection capability (TD-100 Advanced). Communications Port The communications port section determines the serial port number (e.g. Com1) that is used for communicating with the Trap Module and the Autosampler. Sequence Options Tube Load Temperature The tube load temperature determines the temperature below which the autosampler tube oven must be before a tube will be loaded into place. Sequence Options Tube UnLoad Temperature The tube unload temperature determines the temperature below which the autosampler tube oven must be before a tube will be unloaded. Sequence Options Post Tube Desorb Pressure Release Time Pressure can be released from a sample tube prior to completion of desorption. This reduces the potential loss of adsorbent from a pressurised tube, particularly if the tube has no gauze fitted to restrain the adsorbent, as it is unsealed from the TD-100 flow path. The Post Tube Desorb Pressure Release 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. Internal Standard TD-100 can be configured with an Internal Standard Accessory. When fitted this option must be enabled in order to gain acces to the additional method parameters required for Internal Standard introduction. QUI-1069 TD-100 Operators Manual 33

39 GC Interface Used to set the GC Interface logic. The GC Interface logic is set to reflect whether the GC sense is Open or Closed for both GC Start (Out) and GC Ready (In) i.e. for the particular GC being used is the contact Open or Closed to reflect a Start signal, and Open or Closed to reflect a Ready signal. This information is usually provided in the GC Users Manual Gas & Flow This page contains all settings for the carrier gas and mass flow controllers. If an MFC has been installed on TD-100 it is configured under the Flow Control section of this page. For further information please refer to the TD-100 installation manual. QUI-1069 TD-100 Operators Manual 34

40 The Carrier Gas being used can be set using the drop down box. Note: Carrier type only needs to be set when using MFCs. The carrier gas pressure as measured by the pressure transducer, within the TD-100, can be displayed in either psi or kpa depending upon preference, and is selected here Methods This is accessed by selecting View > Options > Methods. There are two method functions which can be changed. QUI-1069 TD-100 Operators Manual 35

41 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. Paths Show Method Path If selected then the active window bar will show the text entered in the Method Name section of the properties dialogue box. Paths Show Method Name If selected then the active window bar will show the file name of the method in use, with or without the full path depending on whether Show Full Path is selected. Trap Heat Method UNITY 2 can use one of two sets of parameters when undertaking Trap Heat. Either those used in the existing Controlling Method or a special set of parameters identified as the Dedicated Trap Heat Method. The choice between these two is made here. See section for further details. User Details Details of the Author and Company which will automatically appear in the properties dialogue of each saved method Reporting option This option influences the information recorded in the sequence reporter page of method linking, see Section Recording parameters are selected by clicking on the appropriate box(es). QUI-1069 TD-100 Operators Manual 36

42 Sample Name Displays the name of the sample as entered in the sequence builder. Sample Tube Displays the sample tube number analysed. Method Name Displays the name of the method used. Desorb Start Time Displays the time at which tube desorption started. Desorb End Time Displays the time at which tube desorption was completed. Peak Desorb Temp Displays the maximum temperature the tube oven reached during the analysis. Trap Fire Time Displays the time at which the cold trap desorption started (and therefore the time at which a GC connected to the TD-100 would have been triggered to start). Trap Module Deviation Displays any error messages, associated with the trap module, encountered during operation. Autosampler Deviation Displays any error messages, associated with the autosampler, encountered during operation (e.g. Tube Leaked) QUI-1069 TD-100 Operators Manual 37

43 Injection Count Displays the number of times a given sample has been analysed. Cycle Count Displays the number of sequence cycles that have been completed. Tag Displays the information relating to TubeTAG when in use. See section TD-100 method options Split on or off in standby When TD-100 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). However if TD-100 is being operated with a mass spectrometer (MS) or an electron capture detector (ECD) on the gas chromatograph, it is strongly recommended that the split be left on in standby [if there is no positive gas flow passing through the split vent for long periods of time, air will enter the system through the split vent and cause an undesirable increase in background signal. This is common to all split capillary injectors]. The split flow may be reduced to 10 ml/min to minimise carrier gas consumption if required. Checking the box on the top line of the method page selects Split On in Standby. An unchecked box will turn the Split Off in Standby Determining the prepurge time The flow through the sample tube during the ambient temperature purge is controlled as follows: Trap in line, split off Trap off line, split on Trap in line, split on purge flow controlled via the needle valve on the desorb flow vent purge flow controlled via the needle valve on the split vent total purge flow = flow through cold trap (controlled via the needle valve on the desorb flow vent) + flow through split vent (controlled by the needle valve on the split vent) The Prepurge time should be set such that, with the given purge flow, the necessary purge volume is passed through the sample tube before the end of ambient purge and the beginning of tube heat. Typical prepurge times are 1-3 minutes for normal sorbents and materials samples and 10 minutes for molecular sieves and carbonised molecular sieves Desorption modes Two modes are available: Standard 2(3) Stage Desorption Tube Conditioning Select between the modes by using the up and down arrows or left clicking the desired option. QUI-1069 TD-100 Operators Manual 38

44 Tube conditioning mode This mode is used to condition sorbent tubes prior to sampling. Freshly packed sorbent tubes, including the Tenax tube shipped with TD-100, will require conditioning prior to use. There are several points to note when conditioning sample tubes using TD-100 as opposed to an external Tube Conditioning/Dry-Purge Rig (e.g. a TC20). Always use the dedicated Tube Conditioning Mode so that contaminants from the tube are vented to the charcoal filter and are not passed onto the cold trap. Set the split flow to at least 50 ml/min (preferably 100 ml/min) to assist efficient conditioning. Carefully double-check the maximum isothermal temperature for the sorbent in use. We advise restricting the conditioning temperature to at least 10 C below this sorbent maximum. Set the flow path temp to at least 190 C while conditioning tubes. This prevents contaminants from condensing inside the TD-100 flow path and helps to condition the system. In tube conditioning mode, the cold trap is off line all the time so that desorbed materials cannot contaminate this or the GC analytical column. Method parameters may either be entered by clicking on each box in turn, typing in the parameter and then pressing Enter or by entering in the first parameter and then using the tab key to automatically enter the parameter and move the cursor to the next active box. The last parameter change should always be completed by pressing Enter. Only a few of the usual thermal desorption parameters are relevant in a Tube Conditioning Method: Mode Split on in Standby Prepurge Set to Tube Conditioning. Click on the box to enter a check if Split On in Standby is required. Set Prepurge time by clicking in box and typing the required time. 1 minute at 30 ml/min is enough to purge oxygen from most sorbent tubes. However, this should be extended to 5 or 10 mins at 30 ml/min for molecular sieve and carbonised molecular sieve type sorbents. Note: The cold trap is, by default, off line during ambient purge in tube conditioning mode. The split flow is therefore switched on by default. Tube Desorb The desorb time - Time 1 - and desorption temperature - Temp 1 - are set by clicking in the relevant boxes and typing in the required values. The split flow is automatically switched on during tube desorption in this mode. The gas flow through the sample tube is controlled by the needle valve on the split flow vent. Flow Path Temp Min Carrier Pressure It is recommended that a split flow of at least 50 ml/min be used during tube conditioning. Set the temperature required for the sample flow path by clicking in the box and typing in the required value. High temperatures (180 to 200 C) are recommended during tube conditioning. Set a minimum carrier gas pressure just below that at which you normally operate TD-100 and the GC analytical column. If the carrier gas pressure drops below this minimum pressure, TD-100 status will change to Low Carrier Pressure and TD- 100 will become Not Ready. This prevents tubes being heated with a low carrier gas supply which could damage the sorbents in the tube. QUI-1069 TD-100 Operators Manual 39

45 Standard 2(3) stage desorption Standard 2(3) stage desorption is the mode used for most routine thermal desorption work. Mode Split on in Standby Prepurge Set to Standard 2(3) stage desorption. Click on the box to enter a check if Split On in Standby is required. Set the ambient Prepurge Time by clicking in the relevant box and typing the required time (see section for advice on prepurge times). If required, select Trap In Line during the prepurge by clicking on the box to enter a check. Similarly, click on the Split On box to enter a check if a split is required during the prepurge. Remember one or other or both of these flows must be selected during the prepurge. QUI-1069 TD-100 Operators Manual 40

46 Tube Desorb Set the Time 1 - desorption time - and the Temp 1 - desorption purge temperature - by clicking in the relevant boxes and typing in the required values. Tube desorption may be carried out split or splitless i.e. all the sample from the sample tube can be transferred to the trap or part of it sent to the split vent. If a split is required during tube desorption (a so-called inlet split, see section 2.2.5) check the relevant box. If the split is selected to be off during tube desorption, all the analytes will be transferred from the tube to the cold trap. If an elevated temperature purge is required, see section 3.9.4, then Time 1 and Temp 1 should be set to reflect the required elevated Prepurge time and temperature. In this case, Time 2 and Temp 2 become the actual analytical tube desorption time and temperature and time values should be entered appropriately. Typical elevated temperature purge settings are 5-15 minutes at C. QUI-1069 TD-100 Operators Manual 41

47 Trap Desorb Set the Trap Low temperature by clicking in the box and typing in the required value. Flow Path Temp Most applications work well with a Trap Low of -10 C. Obvious exceptions to this include the analysis of samples containing high levels of water or standards containing unwanted solvent. In these cases it may be useful to maintain a Trap Low temperature at or near ambient (25-30 C). This allows water and volatile solvents such as methanol and methylene chloride to breakthrough the trap (depending on which sorbents are in the trap) and be eliminated from the system before trap desorption and the beginning of the chromatographic analysis. Set the Trap High temperature as appropriate for the trap sorbent and target analytes. The correct Trap Hold time should ensure all analytes are desorbed from the trap and that the trap is again clean and ready to use for the next sample. This is typically set to 3 minutes. Trap desorption can be carried out split or splitless i.e. if a split is required during trap desorption (a so-called outlet split, see section 2.2.7), check the relevant box. If the split is selected to be off during trap desorption, all the analytes will be transferred from the trap to the GC analytical column during desorption. The flow through the trap while firing = GC column flow + split flow vent, if any. Set the temperature required for the heated valve and sample flow path by clicking in the box and typing in the required value. The following general guidelines may be applied: All analytes, volatile enough to be present in the air in the vapour phase at ambient temperature, will pass comfortably through the system with the flow path between 120 C and 150 C. For ease of use, extended system lifetime and trace level operation a lower QUI-1069 TD-100 Operators Manual 42

48 temperature (e.g. system default temperature of 140 C) is often preferred. Whenever analysing labile compounds use a low (<100 C) flow path temperature and, where possible, increase gas flow rates (linear gas velocities) inside the system. Use the highest possible flow path temperature ( C) for analysing semi volatile organics. Min Carrier Pressure GC Cycle Time Split Ratios split flow calculator Set a minimum carrier gas pressure below that at which TD-100 is normally operated. If the carrier gas pressure drops below this minimum pressure, TD-100 status will change to Low Carrier Pressure and TD-100 status will read Not Ready. If the carrier gas pressure drops below the minimum pressure during a run, TD- 100 will enter Low Carrier Gas status and the tube oven (if heating) and trap heater (if heating) will start to cool down. The GC Cycle Time = GC Run Time + GC Cool Down Time + Equilibration (if appropriate). If a GC Cycle Time is entered, TD-100 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. To enter a GC Cycle Time click in the relevant box and type in the required value (in minutes). Note: This tool only calculates the split flows it does not set them. The inlet, outlet and total split ratios can be viewed, when applicable, in the box at the bottom right hand corner of the method page once the measured flows have been entered into the method. Flows may be entered by clicking on the Confirm/Enter Flows button to bring up the relevant dialogue box. Once the values have been entered and confirmed by pressing OK, the split ratios are automatically calculated and displayed. For measurement of gas flows see section QUI-1069 TD-100 Operators Manual 43

49 Sample tube prepurge With normal porous polymer or graphitised carbon sorbents, a volume of carrier gas, ~ 10 times the capacity of the sample tube, is required to completely eliminate air. This equates to 20 ml purge volume for glass tubes (capacity ~2 ml) and 30 ml purge volume for stainless steel tubes (capacity ~ 3 ml). A more stringent purge (~50 times the tube volume) is required to completely eliminate air from tubes packed with conventional or carbonised molecular sieve-type sorbents. Control of the carrier gas flows during ambient purge The ambient purge carrier gas flow can either pass through the cold trap to the 'desorb flow' vent or through the split filter to the 'split flow' vent or both as it comes out of the sample tube. Trap in or out of line The cold trap is user selectable to be in or out of line during the ambient temperature purge. It is generally recommended for the cold trap to be off line at this stage, to ensure that any water purged from the tube is not re-trapped on the cold trap. Applications involving the direct desorption of volatile components from materials such as pharmaceuticals, plastics etc. are an exception to this rule. In these cases, and especially if the material contains ultra volatile target analytes such as acetaldehyde, it is advisable to have the trap in line. Split on or off If the trap is selected to be off line during tube purge (the most usual configuration), by default the split flow is always turned on to give a flow through the tube. If the trap is selected to be in line the user has a choice of whether the split vent is on or off. The split should be selected to be the same as during the tube desorb process and is therefore determined by the sensitivity of the analysis. Further information on selecting and setting split flows is given in section Sample tube prepurge at elevated temperature The elevated purge option is used for selectively eliminating water and/or high levels of unwanted volatile components. The trap is, by definition, almost always out of line during elevated temperature purge, which means that the split flow must be on. The elevated temperature purge immediately follows, and does not replace, the ambient temperature purge. Example applications are: Eliminating high levels of water collected on sorbent tubes when monitoring humid atmospheres. Eliminating high levels of ethanol from a sample of the flavour profile of potable spirits when the components of interest are higher boiling esters and ketones. Eliminating high levels of volatile solvent from higher boiling (e.g. aromatic) standards introduced onto sorbent tubes as droplets of liquid solution. It is the entry of the second tube desorb time (Time 2) 2 in the appropriate box, which indicates to the system that an elevated temperature purge is required. When a value is entered for Time 2 an extra Trap In Line check box appears in the line referring to stage 1 of tube desorb. As stage 1 of tube desorb is now, effectively, an elevated temperature purge, it becomes appropriate, as in ambient temperature purge, to deselect the cold trap. The cold trap is invariably selected off-line and the split flow on during elevated temperature purge because the purpose of elevated temperature purge is generally to eliminate volatiles from the tube and system before analysis of higher boiling target analytes. Gas flows during elevated temperature purge are controlled as for the ambient temperature purge. QUI-1069 TD-100 Operators Manual 44

50 When using 2 stages of tube desorption, remember to place a check in the second split on box if an inlet split is required for the analysis. The gas flow through the hot tube during its analytical desorption = the flow through the cold trap (the so-called desorb flow - controlled via needle valve) + the inlet split flow i.e. the flow through the split vent (also controlled via needle valve), if any SecureTD-Q - Re-collection for repeat analysis TD-100 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. Manual re-collection available on all TD-100 systems Automated re-collection available as on advanced system and as an upgrade option, see section 7. To re-collect the split effluent, the normal charcoal-packed split filter tube (P/N SERUTD-5065) supplied with TD-100 must be replaced with a conditioned sorbent tube - the SecureTD-Q tube. Note: this procedure should only be carried out with the system in standby mode. In order to access the tube on the split side (charcoal or SecureTD-Q), the exchange split tube icon ( ) must be selected. This will isolate the split tube from the carrier gas supply without disrupting the flow to the analytical column allowing chromatography to continue uninterrupted as the SecureTD-Q and charcoal tubes are exchanged. Once exchange split tube has been selected, lift the right-hand levered tube cover to release the charcoal split tube from one of its seals. Use your fingers or the tube extractor tool to gently pull the tube free from the other seal. Once the charcoal tube has been removed, the clean (SecureTD-Q) sorbent tube should be inserted with its sampling (grooved) end pointing to the rear of the instrument. Lower the right-hand levered tube cover to seal it into position then press the stop icon ( standby status. ) to return the carrier gas flow path to normal If the sample is being re-collected during an analysis, re-activate the exchange split tube icon as soon as the desorber returns to standby mode after trap desorption. Remove the re-collected sample using the above procedure and cap it immediately. Insert another clean (SecureTD-Q) sorbent tube or the charcoal split tube as required, and press the stop icon ( Note: ) to return to normal standby mode. SecureTD-Q will not work for methods that are operated entirely splitless. Either an inlet or outlet split or both are required. As well as repeat analysis, SecureTD simplifies method development, provides a convenient method validation tool and allows critical samples to be archived when required. For further information on split re-collection for repeat analysis see TDTS Cold Trap conditioning The cold trap must be cleaned/conditioned prior to its first use. If the cold trap contains no molecular sieve or carbonised molecular sieve type sorbents, trap conditioning is most easily achieved using the Trap Heat function on TD-100 (see section 3.4.3). 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. In addition, use a split flow of at least 50 ml/min to ensure efficient conditioning of the trap and to reduce the mass of contamination allowed to reach the analytical column. QUI-1069 TD-100 Operators Manual 45

51 For cold traps containing molecular sieve sorbents refer to the relevant cold trap certificate and purge the trap with sufficient quantity of helium (by using the set gas flow option, see section 3.13) prior to operating the Trap Heat Method TD-100 parameter specifications Parameter Mode Split on in standby Range Standard 2(3) Stage Thermal Desorption Tube Conditioning 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 Trap in-line during tube purge Elevated temperature purge or stage 1 of primary (tube) desorption (optional) Yes/No Yes/No 35.0 to C (settable in 1 increments) for 0 to minutes (settable in 0.1 minute increments) Trap in-line during elevated tube purge Split on during elevated tube purge Primary tube desorption (stage 2 if optional elevated temp. purge employed) Split on during primary (tube) desorption Cold trap focusing temperature Cold trap (secondary) desorption temperature minutes Cold trap heating rate Split on during secondary (trap) desorption Yes/No Yes/No 50 to 400 C (settable in 1 increments) for 0 to 999 minutes (settable in 0.1 minute increments) Yes/No -30 to +50 C (settable in 1 increments) -30 to 400 C (settable in 1 increments) for 0 to 99.9 minutes (settable in 1 minute increments) Max (rapid heating reaching 100 C/sec during first critical stages of trap heat) or options between 1 and 40 C/sec Yes/No Flow Path Temperature 50 to 200 C GC Cycle Time Minimum Carrier Gas Pressure 0 to minutes 0.0 to 99.0 psi Tube not found If TD-100 moves to a tube location included in the sequence, but finds no tube present, a record of the 'tube not found' error is stored in the Sequence Reporter (section ). The desorber automatically triggers the GC system start to keep the GC (/MS) sequence in step with the desorber. TD-100 then looks for the next tube QUI-1069 TD-100 Operators Manual 46

52 in the sequence and if it cannot find that tube either, the same functions are carried out by the instrument as described above. TD-100 will continue to look for tubes in the order determined by the sequence and will continue to log an error message and trigger the GC start for all tubes that aren't found until a tube from the sequence is successfully found Tray not found If TD-100 moves to a tray location specified in the sequence, but finds no tray present, a record of the 'tray not found' error is stored in the Sequence Reporter (section ). In this case, the desorber does not trigger GC start, but awaits operator intervention in standby mode while displaying the error 'Tray not found' on the main system status bar Manual Leak Test This function is only accessible from the active environment screen (see Section 3.4.5). Clicking the Leak Test icon ( ) opens the dialogue box shown below. Select the tube number required for the leak test and press Load. TD-100 proceeds to load the tube selected (during this time the buttons in the dialogue box becomes grayed out). Click on the Pressurise button to pressurise the flow path - this button now changes to Test Leak. After allowing some time for the flow path to pressurise, click on the Test Leak button, which shuts off carrier to the flow path. Note the pressure reading on the status bar at the bottom of the main TD-100 screen. If the flow path is leak tight then the pressure reading will remain constant. The tube is returned to the tray on clicking on the Unload button The Set Gas Flow function The Set Gas Flow function is accessed by selecting Instrument and then Set Gas Flow from the dropdown menu, or alternatively by clicking on the toolbar Set Gas Flows icon ( ). A dialogue box is then displayed. QUI-1069 TD-100 Operators Manual 47

53 If the analysis method is to include a split (single or double) then click Yes Yes. The TD-100 flow path will then alter to allow both the desorb flow and the split flow to be adjusted and measured at the split and desorb flow vents. If the analysis method is completely splitless, or if only the desorb flow needs to be set, select No No. The TD- 100 flow path will then alter so that there is only the desorb flow (no split flow) to be adjusted and measured. The lower section of the dialogue box (highlighted) is only relevant to the TD-100 advanced model or if the recollection accessory is installed on the TD-100 basic model see section Measuring and adjusting flows during Set Gas Flow A flow meter is used to measure the gas flows on TD-100 (non Electronic Carrier Control, ECC). A simple bubble flow meter will suffice. However, a digital one is more convenient and is available from Markes International Ltd (C-FLMTR). Note: When TD-100 is set up with ECC, the flow can be read from the GC. However it can be useful to confirm the flow readings with a flow meter. Most applications will require a flow meter with a minimum working range of between 1 and 100 ml/min. If a manual bubble flow meter is being used, then a stopwatch will also be required. It only makes sense to adjust and measure flows for the current controlling method. To measure the flow, push the flow meter tubing over the relevant copper outlet pipe. Flows are adjusted by turning the adjustment knob clockwise to close the needle valve and reduce the flow and anticlockwise to open and increase the flow. Note: The flows measured using Set Gas Flows are approximate. Approximate flows and split ratios are sufficient for most methods, as there will be minimal run to run flow/split ratio variability. If it is necessary to know absolute flow rates for some reason, re-measure the actual flows by desorbing a blank tube before the start of sample analysis. Measure the desorb and split flow (if applicable) during tube desorption and the split flow again (if applicable) during trap desorption. The split flow may be slightly lower during trap desorption than during tube desorption because of the relatively higher impedance of the narrow cold trap tube. The column flow should be measured at the detector end using procedures recommended for the GC in question. Once adjusted and measured as required, all the flows can be entered into the Confirm/Enter Flows dialog box on the controlling method, see section TD-100 systems configured with Electronic Mass Flow Control Mass Flow Control Accessories are available and offer automatic adjustment and closed loop control of the flows during the thermal desorption cycle. For example, this means that different split flows can be set for QUI-1069 TD-100 Operators Manual 48

54 each of these different phases of operation. The accessories also offer electronic flow readout during manual adjustment of the desorb flow. For further information see section To exit the Set Gas Flow function After the measurement of gas flows is complete, the user must click on the Stop sequence icon ( the Set Gas Flows function and return TD-100 to Standby status. ) to exit Gas flow constraints - minimum & maximum settings The system must be set up with at least 10 ml/min flow through the tube - and at least 2 ml/min desorb flow through the cold trap during tube desorption to provide efficient desorption of the tube and efficient transfer of analytes to the cold trap. Use much faster flows through the hot tube (>50 ml/min) and at least 10 ml/min through the cold trap when analysing high boilers (>n-c20). At least 2 ml/min must be used when desorbing the trap. The total flow can be directed to the GC analytical column or to a combination of column and split vent. The flow through the cold trap should not normally be allowed to exceed 100 ml/min during either tube desorption or trap heat. Some variation in flow will be observed through a needle valve if used at less than 2 ml/min. Flow through tube during tube desorption = desorb flow + split flow (if selected) Flow through trap during tube desorption = desorb flow Flow through trap during trap heat = column flow + split flow (if selected) QUI-1069 TD-100 Operators Manual 49

55 4. TubeTAG All models of TD-100 are fitted with TubeTAG read/write technology Introduction Associating sample and usage data with thermal desorption (TD) tubes, has historically relied on manually recording tube serial numbers. Barcode technology has proved difficult to apply to TD tubes because the high temperatures required limit the lifetime and readability of labels. In addition, barcodes cannot be programmed to record tube history or sample specific information (e.g. sampling time and date, etc.). TubeTAG represents a revolutionary advance in sorbent tube informatics. The product comprises an RFID tag and clip that can be attached to individual sorbent tubes. A TAGScribe or a TD-100 can then be used to automatically read and write tube and sample specific data to these tagged-tubes. TubeTAGs are generally used in two ways: Sample specific mode here a given tag is attached to a conditioned sample tube in the laboratory prior to field deployment. That tag then stays with and tracks that sample tube whilst sampling in the field, where further sampling information can be logged to it, until its return to the laboratory. On return to the laboratory the information is read back off the tag prior to sample analysis. The tag is then removed and the tube analysed. The information on the tag is then cleared and it is then ready to go out with another tube to track another sample. Tube specific mode In this case a specific tag is associated with a specific tube throughout its life time so that it logs both sample specific data and tube history information number of thermal cycles, back pressure during sampling, when the tube needs repacking, etc. Both modes of operation offer a significant step forward and a new range of benefits to the busy air monitoring lab. Tags themselves can be re-used almost indefinitely Placing TAG tubes in sample trays When placing TAG tubes in the sample tray they should be oriented as shown below Manual tag read / write QUI-1069 TD-100 Operators Manual 50

56 To manually access the information on the TAG click the Re Read / Write tag icon in the toolbar. When the toolbar tag icon is clicked the Manual tag Read Write window is displayed. This window allows you to manually read from and write to tags while the system is in standby. To read a tag from a specific tube it must first be loaded by selecting the tube number from the drop down menu and clicking Load Load. While the tube is being loaded, read from or written to all the function buttons are grayed out. Once loaded the tag information is automatically read. (Note: when using the manual read/write function the data read from the tag is not stored to file). QUI-1069 TD-100 Operators Manual 51

57 Once a tag has been read all the stored information is displayed in the relevant boxes. For information on the fields available see section If you wish to alter any of the tube or sample information use the text boxes or drop down menus. Note: The alphanumeric fields have a limited number of characters, place the mouse over the field and a text box will appear stating the maximum field length. If the correct Tube Type, TD Method or Adsorbent Packing is not shown refer to section 4.6 for instructions on altering the available options. QUI-1069 TD-100 Operators Manual 52

58 To write the updated information to the tag click Write Tube & Sample Info To prevent accidental loss of information a password is required to write data. The user name is left blank and the password is: Mona Lisa Note: Once the password has been entered you will not be asked for it again until the software is restarted. If you wish to clear all the information on a tag (e.g. if you were moving the tag to a different tube) click Clear Tube Info. Once again to prevent accidental loss of information a password is required to clear the data. The user name is left blank and the password is: Mona Lisa Note: Once the password has been entered you will not be asked for it again until the software is restarted. A final window then appears asking you to confirm clearing the tag data. QUI-1069 TD-100 Operators Manual 53

59 If you wish to clear the sample info fields when you write to the tag tick the Clear Sample Info on Write. To unload the tube click Unload, the tube and cap heater / bobbin will then cool to the unload temperature, see section If loading a second tube simply repeat the tube load procedure, the system will cool then unload the first tube before loading another. Note: If several tubes are to be loaded for manual read / write lowering the flow path temperature to the unload temperature will speed up the procedure Tube information field descriptions Tube Letter/Number These two fields are designed to take the tube serial number (and letter) to which the tag is attached they are limited to one letter and six digits (note: numbers beginning with zero(s) will be truncated i.e will be truncated to when read back from the tag). QUI-1069 TD-100 Operators Manual 54

60 TAG ID Read-only field containing the factory set unique identifier for a given tag Tube type By default this field is designed to take the tube type i.e. ¼ stainless steel, ¼ Silcosteel etc. The options available in this drop down list are completely customisable and could be used for example to designate Environmental Tubes for Diffusive Sampling or General Purpose Screening Tubes etc. For information on editing the available options in these drop down menus see section 4.6 Adsorbent Packing Packing date Thermal cycles TD Method Pressure ratio Tube status Designates the nature of the sorbent packing inside the sample tube by default the list contains a selection of some of the most common packings. The options available in this drop down list are customizable see section 4.6 If entered this designates the date on which the sample tube was packed and allows the user to track the age of the sorbent packing. Tracks the number of times the sorbent in the tube has been heated (conditioned or analysed). This value is incremented automatically when run on TD-100. Alternatively a value may be typed in directly. Allows the user to designate the recommended TD analytical method for analysis of this sample tube. The options in this list box are customizable information on editing the contents is given in section 4.6 Displays the most recent pressure ratio measurement large changes here could denote a tube that is becoming blocked or has lost its sorbent packing. Valid values are between and where would denote completely blocked and would denote completely free flowing. Note the value is reported in the sequence reporter and automatically updated with the most recent value. This field should be used to denote the current status of the sample tube to which the tag is attached. The default options include conditioned, sampled and desorbed. The options for this list box are customizable information on editing the contents is given in section 4.6 NOTE: there is the special tube status of re-collected which gives you the option to note the number of the tube from which a sample originated when using the automated Secure-TDQ option of TD-100, see section Sample Information field descriptions Sample Ref Free text field limited to eight alphanumeric characters that will allow the user to uniquely identify this sample QUI-1069 TD-100 Operators Manual 55

61 Pump Reference Sampling mode Sample start time Free text field limited to three alphanumeric characters that will allow the user to identify the pump used to take this sample Drop down menu allowing the user to define whether this is a pumped/active sample or a diffusive/passive sample Allows user to define sampling start date and time to a two-second resolution Start flow rate Sample end time End flow rate Allows the user to log the pumped sampling flow rate at the start of sampling Allows user to define sampling end date and time to a two-second resolution Allows the user to log the pumped sampling flow rate at the end of sampling QUI-1069 TD-100 Operators Manual 56

62 4.4. Sequence reports with TAG tubes When a tube with a tag fitted is loaded into TD-100 the tag information is read and displayed in the sequence reporter. In the sequence reporter tab any columns containing data read from a tag are highlighted in blue. To select which columns are displayed in the sequence reporter go to View Options then the Reporting Reporting tab. You can now select / deselect the columns as required. (Note it is necessary to close and re-open the control software for these changes to the sequence reporter to be taken into account) 4.5. Tag information/error messages The new tag deviations column in the sequence reporter is used to report information/errors pertaining to the tag read/write process: Read/Write OK Multiple tag failure: Sample read + sample write + collect read + collect write Sample R/W OK Collect: failed read + failed write Successful read write Read/write error on the sample tube or the re-collection tube due to no tag being present or a corrupt tag. Sample tag read / write ok, re-collection tube tag read / write failed (either the selected re-collection tube has no tag or the re-collection tube tag is corrupt) QUI-1069 TD-100 Operators Manual 57

63 Errors written to the Tube Status field on the tag (and to the report file): Leak test failure: tube not desorbed Tube failed leak test, sample retained Instrument failure: sample retained An error on the instrument occurred before primary desorption Instrument failure: sample lost An error on the instrument occurred during or after primary desorption of tube 4.6. Altering the TubeTAG drop down menus If you wish to add additional options in the Tube Type, TD Method or Adsorbent Packing drop down menus you must first browse to your TD-100 program directory. (Default location: C: C:\Program Files\TD100 TD100 ) Using Notepad you can open the following files: tagadsorbents.txt tagmethods.txt tagtubetypes.txt (tagstatus.txt) (We recommend that you only add to the files and do not remove or change any of the default states in these files, this could cause your tag to be written with the incorrect information). To add additional options (in the example shown Special Packing has been added) take the next avaliable number in the list (e.g. 11), then a comma (no spaces between) and the description (e.g. Special Packing) followed by another comma (no spaces between) and N. Index no. text to be displayed QUI-1069 TD-100 Operators Manual 58

64 Once the changes have been made save the text file with the original file name e.g. tagadsorbents.txt and restart the software. (Note: Do not use commas in names as they are used to separate the different sections of information.) You can use the manual tag read / write window to confirm the changes were successful. Note:Text files will need to be copied to all relevant PCs if the same data is to be recalled from the tags.on multiple TD-100s. QUI-1069 TD-100 Operators Manual 59

65 5. Internal Standard Addition/Dry Purge Accessory (ISDP) The internal standard / dry purge (ISDP) accessory for TD-100 is used to load a gas phase internal standard onto sorbent tubes loaded into the autosampler flowpath. It is also used to dry purge humid samples. Standard and/or purge gases are introduced onto the tube from the sampling end - i.e. gas flows onto the tube in the same direction as that used to collect sample. The tube and flow path are leak tested before purge and/or standard gases are introduced. If a leak is detected the tube is immediately returned intact to the tube tray (without purging or standard addition) Internal standard calibration gas: The ISDP accessory requires a pressurised cylinder containing an appropriate calibration gas. The cylinder must be equipped with appropriate (inert) step-down gas pressure regulation fitted with a length of 1/-8-inch or 1/16-inch clean, stainless steel connection tubing. (Note that the length and volume of pressure regulation equipment and connecting tubing should be kept as small as possible.) The pressure of internal standard gas required to be delivered to TD-100 is typically in the range (10-20) psig. A suitable internal standard would contain one or more gas-phase organic components that behave in a similar way to the target analytes of interest, but are not found in the sample e.g. deuterated toluene for BTX analysis on single-bed sorbent tubes. The volume of calibration gas introduced onto the tube is determined by a sampling loop on a gas sample valve incorporated into the ISDP. The standard loop supplied with the ISDP is 1 ml volume. This means that the concentration of internal standard gas in the pressurised cylinder should be such that a 1 ml volume of internal standard gas introduces a similar mass of internal standard compound as the mass of target analytes collected during a typical monitoring exercise. For example, if the ISDP is to be used for calibration of 10 L volumes of real air containing compounds at ~1 ppb concentration, the concentration of internal standard should be approximately 10 ppm Gas connections The ISDP module requires a separate supply of carrier (purge) gas along with the internal standard gas to function correctly. When setting the pressures the order should be: Carrier (purge) gas > 2 psi > Carrier gas > 2 psi > Internal standard gas e.g. 20 psi e.g. 18 psi e.g. 16 psi QUI-1069 TD-100 Operators Manual 60

66 Carrier (purge) gas g input Internal standard Internal standard Internal standard flow needle valve 5.3. ISDP flow path / sequence of operation Operation is as shown in section 2.2 with additional steps shown. (1) Standby, (2) Load tube, (3) Leak test (4) Filling F standard Internal Standard IS HV To GC P P1 Key Pressure and flow Pressure no flow IS flow Re-collection vent Trap / desorb vent Split vent During filling standard mode the 1 ml sampling loop is swept with IS gas. On first operation the flow should be measured and adjusted during a dummy run using the needle valve and vent as shown in section 5.2. Note: This is the only stage where the IS gas is vented to atmosphere QUI-1069 TD-100 Operators Manual 61

67 (5) Inject I standard / Dry purge Internal Standard Carrier HV To GC P P1 Key Pressure and flow Pressure no flow Carrier + IS flow Re-collection vent Trap / desorb vent Split vent During Inject standard mode the 1 ml loop is swept with carrier gas onto the sampling end of the sorbent tube. During this stage the internal standard is added to the tube and dry purging takes place. The flow is determined by the re-collection needle valve located on the front of the instrument. On first operation the flow should be measured and adjusted during a dummy run using the needle valve and vent as shown in section 5.2. (6) Pre purge, (7) Primary desorption, (8) Pre-trap fire purge, (9) Trap fire QUI-1069 TD-100 Operators Manual 62

68 5.4. Dry purge without internal standard addition If only dry purging of samples is required then the internal standard gas must be disconnected from the rear of the ISDP, see section ISDP method options When the ISDP is configured in the software, see TD-100 installation manual for further information, the additional options become available in the TD method Dry Purge Dry purge enables sample tubes to be purged with carrier gas at ambient temperature in the direction of sampling, to eliminate water from the tube prior to analysis Inject standard The inject standard option will introduced the gaseous internal standard onto the sampling tube prior to analysis. Two parameters are associated with the inject standard option. The Inject Standard time is the amount of time for which carrier gas is purged through the sample loop to transfer IS to the sample tube. Loop Fill Time is the time for which the internal standard gas is swept through the sample loop prior to loading onto the tube. A minimum of ten times the volume of the loop should be used to ensure the loop is filled correctly. QUI-1069 TD-100 Operators Manual 63

69 6. TD-100 systems and Electronic Mass Flow Control The Mass Flow Control accessory module(s) offer automatic adjustment and closed loop control of gas flow during TD-100 operation, this means different split and/or trap flows can be set for the different phases of operation Information on setup can be found in the TD-100 installation manual. Once installed all MFC controlled flows will have a flow set point box as shown. Once the TD method is saved the flows set are retained with the method. This means different methods with different flows can be run in the same automated sequence. Note: If the MFC fitted has a maximum flow of 100 ml/min then the permitted range that can be entered is ml/min If the MFC fitted has a maximum flow of 200 ml/min then the permitted range that can be entered is ml/min 6.1. Ensuring split flow stability during trap fire with MFCs When an MFC changes from one set point to another it can take several seconds for the flow to equilibrate. There is one step in the TD operation where this equilibration can cause an issue trap fire. To ensure the MFC is calibrated prior to trap fire the pre-trap fire purge split flow should be set the same as the outlet split, as highlighted below. QUI-1069 TD-100 Operators Manual 64

70 7. Automated SecureTD-Q re-collection operation Automated re-collection is available on the TD-100 advanced model and as a separate upgrade to the basic TD-100. The SecureTD-Q process may be automated to allow quantitative and automated re-collection of the outlet split flow from up to 50 sorbent tubes into 50 re-collection tubes. (Alternatively up to 100 TD samples can be automatically re-collected back onto the original sorbent tube if required). Note: Automated re-collection only collects the outlet (trap) split. If re-collecting then ensure the TD method used has the outlet (trap) split ticked Adding re-collection to a sequence Add a set as described in section In the dialogue box there is the re-collection drop down box available. Re-collection None - do not re-collect any samples in this set Same - re-collect the sample back onto the same (sample) tube Next tube t - if this option is selected the system will re-collect the sample onto a particular tube number. The tube number is selected by using the drop down menu 1st to indicate the tube number from which the re-collection should start. The re-collection will then proceed numerically. i.e. if tube 63 is selected, a five tube re-collection set will be made onto tubes 63, 64, 65, 66, 67. In the sequence builder the set can be expanded and the re-collection field can be edited, if required, by double clicking in the field. QUI-1069 TD-100 Operators Manual 65

71 7.2. Sequence of operation with automated Secure TD-Q Operation is as shown in section 2.2 with additional steps shown. (1) Standby, (2) Load tube, (3) Leak test, (6) Pre purge, (7) Primary desorption (8) Unloading sample tube HV To GC P2 4 Key P1 Pressure and flow Pressure no flow Re-collection vent Trap / desorb vent Split vent After completion of the primary desorption the tube oven starts to cool. Once it has cooled to the UnLoad Temperature the desorbed tube is unsealed. If the sample is to be re-collected onto the same sorbent tube, the tube is then re-sealed. QUI-1069 TD-100 Operators Manual 66

72 (9) Loading re-collection tube To GC HV P2 4 Key P1 Pressure and flow Pressure no flow Re-collection vent Trap / desorb vent Split vent If the sample is to be re-collected onto a different sorbent tube, the TD-100 then moves the tray containing the re-collection tube to the active position and, assuming the desorption oven is not above its Load temperature will load the re-collection tube into position. QUI-1069 TD-100 Operators Manual 67

73 (10) Leak testing re-collection tube To GC HV P2 4 Key P1 Pressure and flow Pressure no flow Re-collection vent Trap / desorb vent Split vent The re-collection tube (whether the same or different to the sample tube) is then leak tested as described in section If the tube passes the leak test then the sequence of operation continues. If the tube fails the leak test twice, then the sequence of operation is as follows: Re-collection on a different sorbent tube If the re-collection tube fails the leak test twice then TD-100 will unload the tube to the tray. The original sample tube will then be re-loaded and leak tested. If this sample tube passes the leak test then the sequence of operation will continue and the split portion of the sample will be re-collected back onto the original sample tube. This will be reported in the sequence reporter. If however the original sample tube fails the leak test twice then the sequence of operation will continue however the split portion of the sample will be passed through the TD-100 split tube and vent and not be recollected. The system will then report an error and stop awaiting operator intervention. Re-collection on the same sorbent tube QUI-1069 TD-100 Operators Manual 68

74 If the original sorbent tube now fails the leak test twice prior to re-collection then the sequence of operation will continue however the split portion of the sample will be passed through the TD-100 split tube and vent and not re-collected. The system will then report an error and stop awaiting operator intervention. (11) Pre-trap fire purge (12) Trap fire (with re-collection) HV To GC P2 4 Key P1 Pressure and flow Pressure no flow Re-collection vent Trap / desorb vent Split vent Just prior to trap fire the heated valve switches to allow gas flow from the cold trap to the re-collection tube as well as the GC column. Note: The flow rate to the re-collection tube is controlled by the re-collection needle valve, see section 7.3. QUI-1069 TD-100 Operators Manual 69

75 7.3. Setting re-collection split / dry purge flow If using the TD-100 advanced model or if the ISDP or re-collection accessories have been installed on the TD- 100 basic model the re-collection / dry purge flow can also be checked / adjusted. To do this a tube must be loaded into the flow path. Use the drop down box to select a tube and click Load Blank Tube Once loaded click Set re-collection split / dry purge flow Measure and adjust flow from the re-collection needle valve in the same manner as section Once finished Unload Blank Tube before closing the dialogue box To exit the Set Gas Flow function After the measurement of gas flows is complete, the user must click on the Stop sequence icon ( the Set Gas Flows function and return TD-100 to Standby status. ) to exit QUI-1069 TD-100 Operators Manual 70

76 8. Routine maintenance 8.1. Autosampler O-ring replacement The nozzle o-rings to check / replace, size 007 U-COV0 COV07 7 (pk( 10), are highlighted opposite. Cold end nozzle o-ring o To access these follow the below instructions. Hot end nozzle o-ring o Remove the white plastic thumb nuts highlighted located on the rear of the autosampler. Remove the rear sloping cover. QUI-1069 TD-100 Operators Manual 71

77 Remove the rear left top side panel by pulling the back (narrow) edge of the panel sideways (away from the instrument) and then by pushing the panel backwards and sliding out. Loosen the white thumbscrew highlighted then tilt the fan backwards. Loosen the two securing screws holding the oven retaining bracket in place and slide the bracket temporarily upwards in the frame to release the oven. QUI-1069 TD-100 Operators Manual 72

78 Rotate the oven assembly around its hinge point towards the back of the instrument. To remove the o-rings use the o-ring removal tool (supplied). The o-rings can be replaced by hand. Caution: ensure the hot end nozzle is cool before touching it Split tube O-ring / PTFE filter replacement The o-rings to be checked / replaced are size 010 (U-COV10 (pk 10), U-COV100 (pk 100)) In the software click the exchange split tube QUI-1069 TD-100 Operators Manual 73

79 icon to divert carrier gas pressure. Remove the split tube. If they are required to be changed they should be hooked out with the O-Ring extraction tool (SERZ SERZ ) from the shipping kit. Use the same pointed implement to hook out the PTFE filter disks. The clean filters (U-DISK1 DISK1) should be pushed in with the O-Ring insertion tool (SERZ SERZ ) or with any clean, flat-ended metal rod of suitable diameter. New O-rings should also be pushed into position using the O-Ring insertion tool supplied in the shipping kit. Also use the O-Ring insertion tool to smooth around the inner diameter of the O-Ring as it is being pushed into place to avoid distortion Replacing a cold trap Ensure the power to TD-100 is switched OFF. Remove the front top cover from TD-100. QUI-1069 TD-100 Operators Manual 74

80 1) Disconnect the 2 solenoid connections. 2) Hold the desorb pneumatric assembly to prevent it twisting and damaging the cold trap, while loosening the securing screw 3) Gently pull the desorb pneumatic assembly towards the front of the instrument, being careful not to damage the end of the cold trap, and lift off. Once clear of the screw, pull the pneumatics forward and rotate to the right Care do not damage trap The cold trap can now be removed by gently pulling it. DO NOT APPLY ANY SIDEWAYS FORCE OR THE COLD TRAP MAY SNAP If the operator hasn t replaced a cold trap before it can be useful to practice using the trap alignment tool (supplied in TD-100 shipping kit). QUI-1069 TD-100 Operators Manual 75

81 This is a metal rod of identical diameter to a quartz cold trap and provides a means of determining the feel of inserting a trap without any risk of damaging a real cold trap. 1. Place the trap alignment tool into the cold trap box. 2. The tool should pass smoothly up to the o- ring in the heated valve before further gentle pressure moves the tool another 1-2 mm. 3. Remove the trap alignment tool NEVER SWITCH TD-100 ON WITH THE TRAP ALIGNMENT TOOL INSTALLED 1-2 mm past o-ring Holding onto the trap as close as possible to the cold trap box, gently push the trap into the cold trap box. DO NOT APPLY EXCESSIVE FORCE TO THE QUARTZ COLD TRAP. Push the trap in until it passes the o-ring. QUI-1069 TD-100 Operators Manual 76

82 Bring the pneumatic assembly back and relocate the screw in the slot. Push the assembly gently back in the horizontal plane guided by the screw, taking care to align the trap and stainless steel connector. MISALIGNMENT CAN CAUSE THE END OF THE QUARTZ TRAP TO SNAP Apply gentle steady pressure to push the trap into the sealing O-ring located inside the steel trap connector. Ensure good alignment here when re-installing the pneumatics Keep hold of the pneumatics while Retightening the screw firmly. Reattach the two solenoid connections. Refit the front cover 8.4. Cold trap O-ring replacement The user may change the cold trap O-ring seal on the pneumatic assembly if the cold trap has been broken and damaged the seal. QUI-1069 TD-100 Operators Manual 77

83 To change the seal remove the pneumatic assembly taking care not to damage the cold trap (see section 8.3) Loosen the thread on the steel connector and remove the cap Replace the O-ring (U-COV06 COV06). QUI-1069 TD-100 Operators Manual 78