GAS CHROMATOGRAPHY TURBOMATRIX SERIES THERMAL DESORBERS User’s Guide
TurboMatrix Series Thermal Desorbers User’s Guide
Release History Part Number Release Publication Date M041-3331 E January 2007 User Assistance PerkinElmer, Inc. 710 Bridgeport Avenue Shelton CT 06484-4794 email: info@perkinelmer.com Notices The information contained in this document is subject to change without notice. PerkinElmer makes no warranty of any kind with regard to the material, including, but not limited to, the implied warranties of merchantability and fitness for a particular purpose.
Contents Introduction ....................................................11 Introduction...................................................................13 Available Optional Accessories .............................15 About this Manual ........................................................16 Other Manuals and Reference Material ........................17 Unpacking the Instrument.............................................17 Symbols Used on the Instrument ..................................
Contents Installing the Heated Transfer Line.............................. 51 Capillary Analytical Column Directly connected to the TD..................................... 51 Installation Through the GC Rear Panel................ 53 Installation Through the GC Injector..................... 55 Installation at the ATD/TD.................................... 57 Leak Test ..................................................... 58 Installing the Transfer Line through the Rear Panel of the GC.....................
Contents Temperature Tab ....................................................97 Timing Tab.............................................................99 The Options Tab...................................................103 Operating Modes ..................................................107 Pneumatics Tab ....................................................109 The Log Tab .........................................................110 Tools ...................................................................
Contents Run Tab ............................................................... 162 Config Tab ........................................................... 163 PPC Config. ............................................... 164 Setup Tab ............................................................. 168 Connect Tab......................................................... 172 Loading Tubes ..................................................... 173 Loading the ATD Carousel..................................
Contents Determination of Adsorbent Strength ..................222 Sandwiched Packings for Wide Boiling Range Samples ................................................................225 Selecting Packing Material for the Cold Trap ..............................................................227 Setting Sample Split Ratios ........................................228 Determining a Suitable Overall Split Ratio .........229 Zero Split (Splitless) Operation ...........................
Contents Ambient Pressure Calibration .................................... 259 Checking the Pneumatics for the TurboMatrix Series PPC Units................................... 260 Tube and Trap Impedance Calibration for the TurboMatrix 650 ATD ......................................... 262 Removing and Replacing the Cold Trap .................... 269 Removing the Cold Trap ..................................... 270 Replacing the Cold Trap...................................... 275 Cold Trap Maintenance .......
Contents Environmental Monitoring...................................316 Extraction of Organic Volatiles from Liquids and Solids .............................................................316 Limitations of Thermal Desorption Techniques ..317 Sampling Techniques ..................................319 Theory of Diffusive Monitoring .................................321 Uptake Rates on PerkinElmer Tubes ..........................325 Diffusion Monitoring Applications......................
Contents Nitrogen Flow Rates ............................................ 392 Index .............................................................
Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Figure 10 Figure 11 Figure 12 Figure 13 Figure 14 Figure 15 Figure 16 Figure 17 Figure 18 Figure 19 Figure 20 Figure 21 Figure 22 Figure 23 Figure 24 Figure 25 Figure 26 Figure 27 Figure 28 Figure 29 The ATD/TD Input/Output (I/O) Port .....................43 Connecting the Fail Output Signal in Parallel with the Start Signal ..................................................
Figures Figure 30 Figure 31 Figure 32 Figure 33 Figure 34 Figure 35 Figure 36 Figure 37 Figure 38 Figure 39 Figure 40 Figure 41 Figure 42 Figure 43 Figure 44 Figure 45 Figure 46 Figure 47 Figure 48 Figure 49 Figure 50 Figure 51 Figure 52 Figure 53 Figure 54 Figure 55 Figure 56 Figure 57 Figure 58 Figure 59 Figure 60 Figure 61 Figure 62 Figure 63 Figure 64 x Setup Tab ............................................................... 121 Password .............................................................
Figures Figure 65 Glass or Stainless Steel Sample Tubes Containing Adsorbents of Increasing Strength Linked Together in Series .......................................................................226 Figure 66 Packing a Single Sample Tube with Adsorbents of Increasing Strength ..................................................226 Figure 67 Double Split Operation...........................................235 Figure 68 Direct Introduction of Liquid Standards onto a Sample Tube ............................
Figures Figure 101 Open Loop Purging Apparatus with Removable Adsorbent Tube....................................................... 334 Figure 102 Soil Probe ............................................................... 335 Figure 103 Sampling Liquids and Emulsions .......................... 337 Figure 104 Sampling Resins and Ointments ............................ 338 Figure 105 Sampling Solids .....................................................
Table 1 Table 2 Table 3 Table 4 Table 5 Table 6 Table 7 Table 8 Table 9 Table 10 Table 11 Table 12 Table 13 Table 14 Table 15 Table 16 Table 17 Table 18 Table 19 Table 20 Table 21 Table 22 Table 23 Table 24 Table 25 Table 26 Table 27 Table 28 Table 29 Table 30 Table 31 Table 32 Table 33 ATD/TD Shipping Kit ...............................................19 Electrical Protection ..................................................21 AC Line Cord Connections .......................................
Tables Table 34 Table 35 Table 36 Table 37 Table 38 Table 39 Table 40 Table 41 Table 42 Table 43 xiv Column (0.32 mm) Flow Rates with Helium Carrier Gas ................................................. 389 Column (0.53 mm) Flow Rates with Helium Carrier Gas ................................................. 390 Column (0.22 mm) Flow Rates with Hydrogen Carrier Gas ............................................. 390 Column (0.25 mm) Flow Rates with Hydrogen Carrier Gas ......................................
Introduction 1
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Introduction Introduction IMPORTANT: Throughout this manual. TD refers to the manual single-tube Thermal Desorber instrument. ATD refers to the automated 50 tube Thermal Desorber Instrument. Thermal desorption is a technique that extracts volatiles from a nonvolatile matrix by heating the matrix/sample in a stream of inert gas. The extracted volatiles are subsequently refocused onto a cold trap from which they are transferred in a narrow band to a gas chromatographic column for analysis.
Introduction TurboMatrix 100 TD: Single-tube, manual-pneumatics model, can be upgraded to the automated version. Also includes a separate trapclean-and-test function, which saves time and protects the GC column and detector. Can be upgraded to the TurboMatrix 150 ATD. TurboMatrix 150 ATD: Automated sampling of up to 50 tubes with manual pneumatics. Overlaps tube desorption with GC analysis for optimum productivity.
Introduction See the following table for model descriptions.
Introduction About this Manual This manual is an integral part of your thermal desorber. It begins with unpacking and general safety information in Chapter 1. Installation and setup are described in Chapter 2. Operation of the instrument is covered in Chapter 3. Optional accessories are described in Chapter 4 and method development is offered in Chapter 5. A routine maintenance schedule and the related procedures are discussed in Chapter 6. The principles of thermal desorption are covered in Chapter 7.
Introduction NOTE: The term Note indicates any significant information that can help you avoid false analytical results or deterioration in instrument performance. All eight-digit part numbers listed in this manual are PerkinElmer part numbers unless stated otherwise. Other Manuals and Reference Material Before you install or use your thermal desorber, to get the best results, you should be familiar with all the instruments in the system and know how to operate them.
Introduction the side. WARNING Improper lifting can cause back injuries. The ATD weighs 34 kg (75 lbs.) and requires two people to safely lift it. The TD weighs 25 kg (55 lbs). 3. Lift out the instrument using the two lifting straps. 4. Check that all ordered parts have been supplied undamaged. The following items should be included with your instrument.
Introduction Part Number Description Quantity M041-5320 Socket, 1/2" 1 N620-0116 CAP Assembly 4 N620-0117 Clamp Assembly Transfer Line 1 M041-7030 Terminal Block Plug 1 M041-3331 TD User’s Manual 1 M041-5339 Washer, #6 Ceramic, Insulating Trap to Heated Valve 1 M041-3535 Packed Trap Tanex TA 1 M041-0316 Valve Array Bushing 1 N930-1376 Ceramic Column Cutter 10 N101-1206 Cable Assy-Start/Ready 2 L100-3027 Vespel ferrule for 0.
Introduction Symbols Used on the Instrument Indicates the off position of the main power switch Indicates the on position of the main power switch Indicates the Protective Conductor Terminal Indicates Hot Surface Indicates Risk of Electric Shock Indicates an earth ground terminal Indicates that there is a risk of pinching that could cause a personal injury. Indicates a risk of danger. Documentation must be consulted to determine the nature of the potential hazard and any actions which have to be taken.
Introduction Possible hazards that could harm the user or result in damage to the instrument are clearly stated throughout this manual. Before using this instrument it is essential to read the manual carefully and to pay particular attention to any advice it contains concerning potential hazards that may arise from the use of the instrument.
Introduction . • This instrument must be grounded for maximum protection against electric shock. Intentional interruption or disconnection of the protective conductor (earth/ground) inside or outside the instrument is prohibited. • Hazardous voltages are present in the instrument. To prevent the risk of electrical shock, the line cord must be unplugged from the AC outlet before removing any instrument covers or panels requiring the use of a tool.
Introduction Terminal Cord Lead Colors International USA Live Brown Black Neutral Blue White Protective Conductor (earth/ground) Green/Yellow Green Table 3 AC Line Cord Connections Servicing of incoming AC power line components in your laboratory must be performed by a licensed electrician. Fuses—Use only fuses with the required current rating and of the specified type for replacement.
Introduction Mechanical Hazard When working with the instrument, please observe the following: • Keep your hands, clothing and other objects away from the moving parts of the instrument. • Do not operate the instrument without the safety covers. • Do not touch any moving parts. • Do not load or unload the magazine while it is in motion. Chemicals Some chemicals used with this instrument may be hazardous or may become hazardous after completion of an analysis.
Introduction The responsible body (e.g., the Laboratory Manager) must take the necessary precautions to ensure that the surrounding workplace is safe and that instrument operators WARNING are not exposed to hazardous levels of toxic substances (chemical or biological) as defined in the applicable Material Safety Data Sheets (MSDS) or OSHA, ACGIH, or COSHH documents. If you are working with volatile solvents, toxic substances, etc.
Introduction • Do not heat the cylinders or expose them to direct sunlight. The cylinders may rupture at high temperatures. • Do not mutilate cylinders. • Do not drag or roll cylinders. Large cylinders should only be moved on carts designed for compressed gas cylinders. Do not move cylinders without the valve protection cap in place. • Always secure cylinders before removing the cylinder valve protection cap.
Introduction • Do not move or detach the regulator when it is pressurized or when it is in use. • Before connection, ensure the cylinder valve and the regulator CGA connection are clean. You must also direct the exhaust vapors from the GC detector and split vent ports to a fumehood. Use flexible tubing to vent these ports to a fumehood or outdoors. The pressure set by the method will determine the outlet flow rates at these ports.
• Secure the Dewar vessel so that it cannot fall over. • Protect the Dewar vessel from any damage and from sources of heat. The Dewar vessel must be fitted with a pressure relief valve. • Cold, vaporized nitrogen is heavier than air and can collect in low lying parts of the laboratory, representing a suffocation risk. Waste Disposal If the materials being sampled are hazardous in any way, you must treat the collected samples, and the tubes that contained them, as hazardous waste.
Introduction • Do not use felt tip pens to mark sample tubes as they may introduce solvents into the tubes. Do not use adhesive labels as they will jam in the tube handling system. • Sample tubes recently unloaded from instrument to the carousel can be very hot. Once the sequence is complete, cool and vent the sample tubes before you reuse or store them. • Sample tubes, caps and nuts must be cleaned and conditioned before reuse.
Introduction A label with a crossed-out wheeled bin symbol and a rectangular bar indicates that the product is covered by the Waste Electrical and Electronic Equipment (WEEE) Directive and is not to be disposed of as unsorted municipal waste. Any products marked with this symbol must be collected separately, according to the regulatory guidelines in your area.
Installation and Setup 2
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Installation and Setup Introduction Before the instrument arrived, you may have received the pre-installation checklist given in this chapter to ensure that your lab is setup correctly. If you did not receive the checklist, refer to the pre-installation checklist in this section to ensure that you have enough space for the GC and all the related support equipment and that the electrical and gas supplies meet the requirements of the ATD/TD. Installation consists of the following 7 steps: 1.
Installation and Setup Operating Environment on page 35. 2. Read in Safety in the Introduction chapter and ensure that you have complied with the requirements for each section. 3. If you are using the PC software, you must have a computer capable of running the software. If you are running TotalChrom, the TD Control Software can be run from the same computer. 4. Obtain the required gas supplies. See Gas Supply Specifications on page 70. Ensure that you have the required carrier gas filters. 5.
Installation and Setup (Tenax TA recommended for most applications), gauze rings and glass wool if you pack tubes or traps yourself. 11. If you are using the LN2 accessory you need to obtain a supply of liquid nitrogen. 12. Ensure that you have all the required supplies for your GC and data handling system and that they are up and running correctly. 13. Review this manual and write down any questions that arise.
Installation and Setup Altitude (operating) Sea level (0 metres) to 2000 m (6,562 feet) Storage (nonoperating) You can store the instrument safely under the following conditions: • Ambient temperature –20 to 60 ºC (-4 to 140 °F) • Ambient relative humidity of 20% to 75%, (non-condensing) • Altitude in the range 0 m to 12000 m (39,370 feet) When you remove the instrument from storage, allow it to stand for at least a day under the approved operating conditions before putting it into operation.
Installation and Setup Space Requirements for the Instrument The space requirements for the instrument are shown in Table 6. You should leave sufficient room around the instruments to access all of the connections at the rear, and reach the electrical supply points. The TurboMatrix Series TD models are the 100 and 300. The TurboMatrix Series ATD models are the 150, 350 and 650.
Installation and Setup Allow at least 94 cm (3’) on either side of the TD/GC to accommodate additional equipment (for example, the computer). The laboratory bench should be sturdy enough to support the full weight of the GC, the TD as well as additional support equipment (i.e., computer and/or printer). Expect the total weight of the GC/ ATD and accessory equipment to be at least 136 kg (300 lbs). The TD may be positioned to the left or right of the GC.
Installation and Setup Electrical Connections AC Line Connections Power Consumption Approximately 1000 VA for the ATD/TD.
Installation and Setup It should be checked by a qualified electrician before you connect the instrument. To avoid interference caused by ground loops, always connect the ATD/TD and any accessory to the same phase of the line power supply and insure that they share a common earth ground. Observe outlet power limits. Refer to the individual accessory manuals for details of installing various accessories and their power requirements. Before you alter or make any new electrical connections: 1.
Installation and Setup Although the SMPSU incorporates thermistors, to limit the “inrush” current these are only effective when they are close to room temperature. During normal operation these components run at an elevated temperature and, as a result of their reduced electrical resistance, are unable to prevent the passage of high surge currents associated with brief interruptions of the external supply.
Installation and Setup injector or detector port at the top can be used. This may be the case if you have an older GC or a GC equipped with PPC. Another consideration is whether or not you have AutoSampler installed. If you have an AutoSampler and PPC installed on your GC, contact your PerkinElmer service engineer. The ATD/TD is controlled from a computer (PC) or from its own touch screen keypad.
Installation and Setup The ATD/TD Input/Output Port The Input/Output Port of the ATD/TD enables communication with other instrumentation, for example GCs and data handling systems. The communication consists of a number of relay contact signals provided by the ATD/TD, which can be read by the external device and a relay contact signal provided by the external device, which is read by the ATD/TD. Figure 1 shows the signal connections to the ATD/TD Input/Output Port.
Installation and Setup The contacts remain closed for 6 seconds. The Start signal is normally used to start a GC run, by connecting it to the GC Start terminals. See Figure 4. Fail Output Signal —The ATD/TD can be used with instrumentation that is unable to read the BCD sample tube number and therefore unable to report it with the chromatographic results. (Also useful even if BCD is present, to synchronize data handling sequence with ATD/TD sequence.
Installation and Setup Use of the Fail signal to start an external device and maintain synchronization depends on the device having completed its previous run and being in a state from which a blank run can be started.
Installation and Setup The Fail signal can be generated at a number of points in the sequence, including detection of an empty tube position or an error condition. Closure of the Fail contacts is always associated with an error message or a fatal error message. ATD/TD Input Signals Ready In—The ATD/TD can determine the status of external instrumentation using the Ready In signal.
Installation and Setup Timed Event Relays NOTE: Timed Event Relay is only available when options board is connected. If you will be controlling external devices through the relays on the options board and timed events, you must first connect the external devices to the ATD/TD and then program the events. The 4 relay contacts are rated to switch 10 W (maximum). Do not exceed 50V or 0.5A. External devices include external switching valves, audible alarms, very small motors, etc.
Installation and Setup Connect the opposite end to the GC EXT START pins 3 and 4. TURBOMATRIX 14 9 6 5 14 13 12 11 10 9 8 7 6 5 4 3 2 1 16 15 11 10 4 3 14 13 12 11 10 9 8 7 6 5 4 3 2 1 GROUND GROUND GROUND START IN STOP IN READY IN FAIL OUT NO START NO READY NO READY NC GC READY OUT EXT START Figure 3 Connecting the ATD/TD to the AutoSystem XL GC using the Ready/Start Cable Connecting the ATD/TD to Other GCs Except the HP 5890 and HP 6890 1.
Installation and Setup 14 13 12 11 10 9 8 7 6 5 4 3 2 Pin # 1 Ready +5 V 0V Ext Start GC TurboMatrix I/O Port Figure 4 Connect the ATD/TD to Another GC Using the Ready/Start Cable 2. The ATD/TD requires a contact closure, or equivalent, to be applied between pin 9 (Ready In) and Ground (pins 12, 13 or 14) to receive a GC ready signal. The ATD/TD provides a contact closure between pin 5 and pin 6 (Start Out) to start a GC run.
Installation and Setup 2. Locate the I/O port on the rear panel of the ATD/TD. 3. Connect the white wire of the cable assembly (P/N N610-0402) to the Start - Normally Open (Pin #5). 4. Connect one of the black wires to the Ground (Pin #12). 5. Connect the red wire to the Ready In (Pin #9). 6. Connect the remaining black wire to the Start Normally Open. (Pin #6) The HP 6890 GC cannot accept BCD signals from any external samplers including PerkinElmer samplers.
Installation and Setup Installing the Heated Transfer Line NOTE: For TurboMatrix Series the transfer line material maybe Silktec. All other parts of the procedure remain the same. The heated transfer line connects the ATD/TD to the gas chromatograph and consists of an insulated heater surrounding a stainless steel tube. A silicone foam tube forms the exterior insulation. The transfer line may be heated to between 50°C and 300°C.
Installation and Setup CAUTION The stationary phase of your column must be able to withstand the temperature extremes of the transfer line and the heated valve.
Installation and Setup Normally you will install the outer components of the transfer line at the GC and then at the TD. Lastly, you will run either the fused silica transfer line or the analytical column, through the transfer line, from the GC oven to the ATD/TD and make the required connections. Installation Through the GC Rear Panel Clarus 500 or AutoSystem XL—A cut out for the ATD/TD transfer line is located on the rear panel of the AutoSystem XL.
Installation and Setup back of the oven outer wall should be visible. See Figure 9. 6. Remove both of the PVC end caps from the oven entry insulation (comprising L427-1103, L427 1104, L4271144, 0497-3923). 7. Use a knife to cut a hole in the insulation between the oven liner and the outer wall of the oven. The diameter of the hole should be equal in size to the outer diameter to the transfer line assembly. Remove and discard the insulating material. 8.
Installation and Setup Rear Panel of the AutoSystem XL or Clarus 500 M/U Air or H2 2 Carr M/U Air Carr 2 or H2 Transfer Line Access Hole Transfer Line Figure 6 Location of the Access Hole on the AutoSystem XL and Clarus 500 GC Rear Panel Installation Through the GC Injector To install the heated transfer line, through the top of the GC: 1. Disconnect the GC from any electrical or gas supply. 2. Two right-angle bends with a radius of approximately 8 cm (3.
Installation and Setup 9 cm Straight Length ATD End 78 cm Between Center Lines GC End Fused Silica Transfer Line 50 cm Straight Length Add Stainless Steel Sleeve Aluminum sleeve Silicone Foam Rubber Tube Figure 7 Bend Dimensions for Connecting the ATD/TD Transfer Line to an AutoSystem GC or Clarus 500 GC 4. Remove the cap from the GC injector port. Refer to the GC manual for details. 5.
Installation and Setup Installation at the ATD/TD 1. Disconnect the ATD/TD from the electrical supply. Allow heated zones to cool. WARNING You must allow 20 to 30 minutes for the heated blocks to cool before handling any internal parts. Severe burns may result from touching the heated blocks before they have cooled. 2. If you are installing on a TD you can obtain the required access by opening the front door. 3.
Installation and Setup 9. From the GC end, pass the fused silica transfer line, or the front end of the GC column (as you prefer), through the installed transfer line until the end is visible in the ATD/TD. Take care not to nick or scratch the transfer line or column in the process or feeding it through the transfer line assembly. You will need to cut off excess transfer line, leaving approximately 20cm exposed to attach your column.
Installation and Setup If your GC has passed the leak test you have successfully installed the ATD/TD.
Installation and Setup Transfer Line Assembly Silicone Foam Rubber Tube Aluminum Sleeve Stainless Steel Sleeve Graphitzed Vespel Ferrule Electrical Connectors Heated Line Clamp Fused Silica Transfer Line or Fused Sulfinert Line Upper Heated Block Vespel Ferrule Fused Silica Line entering into the heated valve Valve Heated Block Cold Trap Valve Rotor Graphite Ferrule or Vespel if EDC or MS is used Heated Valve Figure 8 Connect the Transfer Line to the TD Instrument 60
Installation and Setup Installing the Transfer Line through the Rear Panel of the GC The hardware installed within the GC oven to allow installation of the transfer line depends upon the type of column (capillary or packed). If you are using a capillary column, it can be connected directly to the ATD/TD or connected to the fused silica tubing transfer line with a union. For packed columns, connection must always be via the fused silica tubing line.
Installation and Setup Oven Sensor Stainless Steel Sleeve Silica Transfer Line (P/N L116-1484) Union for Capillary (P/N 0497-2073) or Union for Wide Bore Column (P/N 0992-0145 Bracket (P/N N610-1462) Capillary Column Fan Guard Figure 9 Installation of the Transfer Line through the Rear Panel 2. Install a union (P/N 0497-2073 for capillary columns or P/N 0992-0145) into the bracket (P/N N610-1462) fir wide bore or packed columns using two hairpin cotters (P/N 0992-3058). 3.
Installation and Setup 6. In the GC oven, cut the fused silica line within reach of the union. Place the 1/16” stainless steel nut (P/N 04972824) on the fused silica line.Cut about 1 cm (3/8”) from the end of the fused silica using a wafer scribe (P/ N N930-1386) or other column cutting tool. Break off the tubing at the score mark making sure that the break is clean and square. Examine the cut with a magnifying glass and compare it to Figure 10.
Installation and Setup are not included in the kit. We recommend that you use the 0.53mm ID Retention Gap kit, Part No. 0497-8449. Installing the Transfer Line Through the Top of the GC You can put the heated transfer line through the top panel of the GC. You may need to do this if you have a PPC module installed on your GC. If you have an AutoSampler installed you will not be able to use the GC injector ports. If you have two injectors you can use the PreVent port or a detector cutout.
Installation and Setup union using either a graphitized Vespel ferrule (P/N 0497-2066) or the graphite ferrule supplied with the union (not for ECD or MS). After passing the column end through the ferrule, cut off a further 0.5cm of fused silica to avoid the possibility of a blockage. The silica line should end in the center of the union. It is essential that the fused silica line does not touch any part of the oven wall. NOTE: The ferrules are fitted with the tapered end away from the body of the union.
Installation and Setup (35 kPa), better carrier gas control can be achieved by inserting a length of narrow bore, fused silica tubing, between the column and the detector to increase the inlet pressure. For example, use for a tube that is 0.1-mm bore, 100 cm long, We recommend that you use the 0.53mm ID Retention Gap kit, Part No. 0497-8449. Connecting a Packed Column To connect a packed column to the TD: 1.
Installation and Setup 5. Place the 1/16” stainless steel nut (P/N 0497-2824) and a 0.5-mm graphitized, Vespel Ferrule (P/N 0497 2066) on the silica line at the ATD/TD end. After passing the column end through the ferrule cut off a further 0.5cm of fused silica to avoid the possibility of a blockage. Withdraw the silica line and stainless steel sleeve from the transfer line, so that the free end of the silica line can be pushed into the heated valve with 3.5 cm of silica line entering into the valve.
Installation and Setup 0497-2066) or the graphite ferrule supplied with the union (not for ECD or MS). After passing the column end through the ferrule cut off a further 0.5cm of fused silica to avoid the possibility of a blockage. The silica line should end in the center of the union. It is essential that the fused silica line does not touch any part of the oven wall. NOTE: The ferrules are fitted with the tapered end away from the body of the union. Tighten the nut just enough to avoid leakage. 8.
Installation and Setup 5. Do a Column Leak test the system. See the procedure, Column Leak Test later in this chapter. 6. Connect the column to the GC detector as described in the GC manual. Replace the cover plates. NOTE: For columns that require an inlet pressure of less than 35 kPa (5 psig), better carrier gas control can be achieved by inserting a length of narrow bore fused silica tubing, for example 0.1-mm bore, 100 cm long, between the column and the detector to increase the inlet pressure.
Installation and Setup should be installed at every gas line connection. The carrier gas connections require 1/8” tubing with 1/8” parallel compression fittings. WARNING Observe proper handling procedures for compressed gas cylinders. See Handling Compressed Gases on page 25. Check the gas lines and connections regularly for leaks. Oxygen filters (N930-1179), moisture filters (N930-1193) and charcoal filters (N930-1192) are recommended for carrier gas lines.
Installation and Setup Dry Air Dry air is used to drive the pneumatic systems and to purge the Peltier coolers on the cold trap. Use extra-dry air with a dew point less than 50°C. If extra-dry air is unavailable, then use a zero-air generator or bottled air with a dew point less than -50°C. Liquid Nitrogen If the ATD/TD is fitted with the LN2 accessory, it requires a supply of liquid nitrogen. The liquid nitrogen does not come into contact with the sample.
Installation and Setup Use only carrier gases with a purity of 99.995% or better. Only top quality gases are suitable; typical laboratory supplies are usually not pure enough for thermal desorption. Gas purity can be improved when filters are included in supply lines. Hydrocarbon, oxygen and moisture filters are recommended for carrier gas lines.
Installation and Setup See Handling Compressed Gases on page 25. 2. Connect a clean, high purity, two-stage regulator with a stainless steel diaphragm to the carrier gas tank. The regulator should also have a 1/8”, parallel, compression fitting with which to connect the regulator to the TD. The delivery pressure must be adjustable to 90 psig (620 kPa). NOTE: The regulator must be absolutely clean and free from any oil or other contamination. 3.
Installation and Setup compression fitting with which to connect the regulator to the TD. The delivery pressure must be adjustable to 90 psig (620 kPa). 2. The connections for the gas lines are located at the rear of the instrument. 3. Connect a moisture filter, as close as possible to the ATD/TD. 4. Connect the supply line to the Dry Air In port. The purge connection at the rear of the instrument is a 1/8” compression fitting.
Installation and Setup Supply Pressure 90 psi/620 kPa 1/8” Stainless Steel Compression Fitting Carrier In 1/8” Stainless Steel Compression Fitting Standard In 1/8” Brass Compression Fitting Dry Air In Clean Air Figure 14 ATD/TD Gas Connections 75
Installation and Setup Column Leak Test 1. To perform the column leak test, cap one end of the column and/or transfer line with a rubber septa. Connect carrier gas, and pressurize the system. 2. Go to the Tools drop down menu and select Maintenance and select Column Leak Test. The following screen will appear. Press OK to start the test. Check for leaks or pressure drop 3.
Installation and Setup the instruments cold trap. To install the dryer assembly use the instructions provided with this assembly (Part No. N6710048). Setting the Carrier Gas Flows When you set the carrier flow you are setting the flow for the desorption system which includes purging the sample tube, primary and secondary desorption, inlet and outlet split flows and the GC column flow rate. Relatively high flow rates (20 to 100 mL/min) are required for purging and desorption.
Connect the gas supply line to the carrier in port on the rear panel of the TD. 1. Ensure the transfer line has been connected correctly to the GC. See Installing the Heated Transfer Line on page 51. 2. Set the carrier gas delivery pressure to 90 psig (620 kPa). See Connect to the ATD/TD Gas Supply System on page 69. Do not set the delivery pressure higher than 100 psig (690 kPa). WARNING 3. Open the PNU tab and adjust the pressure regulator to obtain the required head pressure.
Installation and Setup may need to make minor adjustments. Use this interactive process until you obtain the desired flow rates. An Inlet Split flow of at least 25 mL/min should be established even if inlet split is disabled during analysis. After desorption and cooldown, and before being unloaded, sample tubes are depressurized using the inlet split function. The instructions below are for both the TD and ATD.
Installation and Setup 7. Allow a few minutes for the flow to stabilize before disconnecting the flow meter. 8. To set the desorb flow, connect a flow meter to the desorb vent. Adjust the Desorb needle valve to obtain the required flow. Typical desorb flow rates are in the order of 20 to 100 mL/min. If either helium or hydrogen is used for the carrier gas, the desorb flow rate should not be higher than 100 mL/ min.
Installation and Setup 2. Select Outlet Split. This opens the solenoid valve on the outlet split vent. 3. Connect a flow meter to the split vent and use the outlet split needle valve to adjust the flow rate. A minimum flow of 3 mL/min is recommended. NOTE: If a column carrier flow rate of less than the required minimum trap flow is used, then use the outlet split flow to make up the difference. 4.
Installation and Setup 82
Operation 3
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Operation Operation Operation of the instrument will be covered in this chapter. A brief description of the user interface is provided first in order to familiarize you with the basic operation of the instrument. Loading tubes and starting a run are at the end of this chapter. Detailed method development is covered later in Chapter 5. Chapter Organization The manual pneumatics models (TurboMatrix 100 TD and 150 ATD) will be the first section of this chapter.
Operation TurboMatrix 350 ATD: Automated sampling of up to 50 tubes, incorporating PPC. Supports pressure, flow and velocity control of the carrier gas through the GC column. Overlaps tube desorption with GC analysis for optimum productivity. Also incorporates loading of internal standard into clean tubes to provide sampleintegrity validation and to improve precision (repeatability) of the analysis.
Operation Safety Precautions for the all Models of the TurboMatrix Series To protect yourself from harm and to avoid damaging the instrument, please observe the following notes: • Before using this instrument, read and observe the safety information in Chapter 1. • Do not sample carbon disulfide or other solvents with a selfignition point of 100°C or less. • Always follow the correct safety procedures and the manufacturer’s recommendations when using any solvent.
Operation Attention: Before attempting to disconnect the TD/ATD from the GC or to shut off the carrier gas supply, ensure that: • The GC oven and detector are cool. • If an MS is used the GC-MS transfer line and the MS ION source are cool. The filament is off. • TD/ATD heated zone (trap, heated valve, transfer line) are turned off and cool. • If you disconnect the TD transfer line from the GC column, plug the transfer end and the GC column inlet to protect them from contamination and ambient air.
Operation 43 cm (17”) Pneumatic Adjustments Transfer Line Receptacle 34 cm (14”) Heated Valve and Cold Trap Compartment Tube Loading Area 48 cm (19”) Mobile Seal Door Latch Touch Screen Display Figure 15 Layout of the Thermal Desorber (example shown here is the TurboMatrix Series 100 TD) 89
Operation 43 cm (17”) Transfer Line Receptacle 56 cm (22”) Pneumatic Adjustments 48 cm (19”) Carousel Touch Screen Display Tube Loading Area Figure 16 Dimensions of the Automated Thermal Desorber (example shown here is the TurboMatrix Series 300 TD) To begin operation of the ATD or TD: 1. Connect the electrical and gas supply lines, set the required flow rates and check all gas connections. Refer to Chapter 2 for details. 2.
Operation 3. Ensure the GC and any related support equipment and software are installed and are displaying a ready status. i.e. the GC detectors, GC data acquisition systems, etc. 4. If you have any options installed, ensure they are turned on and allowed to warm-up as required. Refer to the documentation supplied with each installed accessory. 5. Press the On switch. The power switch is located on the rear panel of the ATD/TD. 6. The ATD/TD splash screen will be displayed. 7.
Operation • set and view current configuration parameters (Status tab) • run analyses using one or multiple methods (Run tab) • view instrument information (Log tab) The Status tab provides information on the current ATD/TD settings. You can also make changes to the ATD/TD parameters directly from the Status screen. Changes you make on the Status tab will take effect immediately unless an analysis is in progress. The ability to edit parameters will be disabled until the analysis is complete.
Operation Manual Pneumatics TurboMatrix Series 100 TD and 150 ATD The Run Tab Once you have created a method by which to run the samples, you will manually load a single tube or load the carousel and run the samples from the Run tab. See Chapter 5 for details on creating methods. You can run samples using a saved method or a sequence of saved methods. Figure 17 Run Tab The options on the Run tab are determined by selections that have been made on the Preferences tab.
Operation has been selected, then you only need to enter the tube range. The selected method will be displayed and you will not be able to access the drop down method list. 2. Beside the Tubes label radio button, you will enter the start and stop tubes. The tube range will default to 1 to 50. Press the first entry box to enable the option. If you are using a TD, the tube range is fixed at 1. 3. Press the plus or minus button to select the desired start tube. Then enter the desired end tube. 4.
Operation To run a series of tubes using different methods, you can set up a sequence. The sequence can be retained for routine use or it can be edited as required. NOTE: Multiple method operation must be enabled on the Preferences tab. See the Preferences/Run tab section later in this chapter. 1. Switch to the Run tab. 2. Select the Sequence button to enable the option. Press the start tube entry box. 3. Press the plus or minus button to select the desired start tube. Then enter the desired end tube. 4.
Operation method. The instrument status will be Standby until the instrument reaches all of the set points. If you are using a TD, you must now load the tube. Once the ATD has reached the set points, the first tube will be loaded and the analyses will continue as determined by the sequence. Editing a Sequence To delete an entry from the sequence, select the entry in the list and press the Delete button.
Operation Temperature Tab There are five temperature settings for the TD. The Tube oven temperature, the heated Valve, the Transfer line temperature and the cold trap secondary desorption temperatures (Low, High). You will also set the heating Rate for secondary trap desorption. Entering a value of zero for any temperature parameter, disables the related heater.
Operation The ATD/TD incorporates a packed cold trap to concentrate the volatiles before injection onto the GC column. It is cooled to temperatures between -30°C and +150°C. The cold trap can be cooled to -100°C with optional LN2 accessory. Heat Rate—Once the volatiles are transferred from the sample tube, the trap is heated. Set the heating rate to any value between 5, 20, 40 and 99°C/second (ballistic).
Operation new temperature. Allow a few minutes for the instrument to reach the new value. You can switch to actual to view the current instrument temperatures. The new value will be displayed in red until it reaches the new set point. 5. To save your settings as a new method or to update the existing method, press the Tools button and select Save As. 6. To save the method existing name press OK. To create a new method, enter a new name for the method by pressing the method name.
Operation Figure 19 Timing Tab The name of the method that is currently loaded on the Run tab is also displayed. The settings displayed here are from this method. You can change the settings and create a new method or update an existing method. Purge Time—When the leak tube test has been completed, air is purged from the tube prior to heating it for desorption. This is done to reduce the risk of adsorbent or analyte oxidation during desorption.
Operation Figure 20 Trap Timing Popup Standard Inject Time—If your ATD/TD is equipped with the Internal Standard Addition accessory, a gaseous internal standard can automatically be introduced onto every sample tube prior to desorption. The standard will be added after the tube purge. The Internal Standard (IS) valve is activated for the duration of the Standard Injection time to allow the introduction of a volume of standard onto the sample tube.
Operation Enter a Loop Load time. This will determine the time interval that ISV1 is open to load the sample loop in preparation to introducing the Internal Sample onto the sample tube. The length of time required is a function of the loop load flow rate and the volume of the loop. Typically, 10 loop volumes should be passed through the loop to ensure complete filling of the loop with the standard.
Operation NOTE: The GC Cycle Time enables the system to initiate desorption of the next tube while the current sample is being chromatographed. This setting is intended to ensure that the current run has finished in time for the trap desorption of the next sample. NOTE: Laboratory temperatures can strongly influence the GC oven cool-down time and can vary (for example, overnight). The GC cycle time setting should take into account the longest oven cool-down time expected during the analytical sequence.
Operation Figure 22 Options Tab for a TurboMatrix 150 ATD If you have the Standard Injection option installed, but do not need to use it, then de-select it here. You can enable heated sample tube purge, Inlet and Outlet sample Splitting and multiple injections from a single tube from this tab. You will also select the various ATD/TD operating modes from this tab.
Operation Standard Injection—If your ATD/TD is equipped with the optional Internal Standard Addition accessory (P/N M041-3657) you can enable or disable the option from this tab. A standard can automatically be introduced onto every sample tube prior to desorption. The standard is added after the tube is purged. If you have enabled this option, then you must enter a standard injection time on the Timing tab (see the Standard Inject Time in the Timing tab section above).
Operation is when the sample is purged of residual air at ambient temperature. If you enabled the heated purge option, then the tube will be heated as it is purged. The default setting is 50°C (1°C increments with a temperature range of 20°C to 100°C). See the following figure. NOTE: For the manual pneumatic models the Purge flow Rate is unavailable (only available in PPC models) and is grayed out).
Operation Operating Modes The ATD/TD can operate in any one of five modes. A basic overview of each mode is provided here. A detailed description of each, including flow diagrams are shown in Chapter 7. Two Stage Desorption—This is the mode used to perform most of the analyses. Primary Desorb takes place after the sample tube has been leak tested and purged of air.
Operation In this mode, only the cold trap is heated and the contents of the trap are desorbed and vented through the Input Split flow control to prevent contaminants from entering the GC column. Trap Test-In this mode, only the cold trap is heated, the contents of the trap are desorbed onto the GC column and a GC run is started to verify that the trap is clean before starting a sequence of analyses.
Operation Pneumatics Tab The Pneumatics tab (PNU) displays the pressure settings for your application. The TurboMatrix 100 TD and the TurboMatrix 150 ATD has a manual pressure control system. The following screen is the Status page, pneumatics tab for the TurboMatrix 100 TD and the TurboMatrix 150 ATD. Figure 24 Pneumatics Tab (TurboMatrix 100 TD and the TurboMatrix 150 ATD) Pressure values and split flows are adjusted manually.
Operation Column Pressure—In the TD/ATD, the Pressure Control system is a manual Pressure Regulator (not a programmable function). Setting a value here is only for notation. Therefore, the Column Pressure on the PNU tab is only a reading when you check the Show Actual check box. Manually adjust the Pressure Regulator while monitoring the pressure value in the Column Pressure box. See Setting the GC Column Head Pressure on page 77.
Operation Figure 25 Log Tab The information is overwritten when a new sequence is started. The Log Report is a log of all events. During a sequence, events can be logged after every injection, or only deviations may be logged. If every injection is to be logged, then the Log Report will contain the following information: • When the method and sequence were started. • When a successful sample injection from a tube is completed.
Operation Tools Pressing the Tools button opens a pop-up menu of tools that enable you to perform various functions such as creating and editing methods and configuring the options available on your instrument. Figure 26 Tools Menu Method Editor The Method Editor command opens the tab. This tab allows you to create and store methods for your application. You can store up to 9 methods. Once the methods have been saved, they can be recalled at any time for use in a sequence or can be recalled for editing.
Operation New Method—To create a new method, open the method by entering the desired method parameters and then save the method. (See Save/Save As command below.) Open Command—To revise an existing method, select the Open command from the File menu. Select the method that you want to edit and press OK. Save As—Use this command to save new methods or update existing ones. 1. Select the Method Editor tab and enter or update the desired method parameters. 2. Select Save if you are updating an exiting method.
Operation Del key to delete the characters. 5. Press OK to enter the new name for your method and then press OK to save the method. Press Done to complete the selection and return to the Run tab. Activate Command—This command makes the currently selected method active. The method is loaded from memory and the instrument is heated or cooled to the new settings. NOTE: Do not activate a method if the TD or ATD is performing an analysis.
Operation Preferences Selecting this option will take you directly to the Preferences tab. See the Preferences Tab section in this chapter for details. Calculator You can use the calculator in standard view to do simple calculations. To perform a simple calculation: 1. Enter the first number in the calculation. 2. Click + to add, - to subtract, * to multiply, or / to divide. 3. Enter the next number in the calculation. 4. Enter any remaining operators and numbers. 5. Click =. 6.
Operation Maintenance Tab You will use the Maintenance tab to set flows or perform routine maintenance on the instrument. The Maintenance tab contains the following commands. Inlet Split and Outlet Split-You must set the inlet split flow manually using the inlet split needle valve on the TD. You also need to set the outlet split flow separately using the outlet split needle valve.
Operation Preferences Tab You will use the Preference tab to set the configuration options for the TD. The selections you make here will enable or disable various options on the Status tab and in the Method Editor. The Preferences tab contains four tabs. The Run tab sets the options for running analyses. The Config tab contains the options related to the operation of the TD. The Setup tab contains settings for various parameters and options.
Operation Figure 28 Preferences Run Tab Single Method Operation—If you select single method operation you can also specify the method to be used. The options on the Run tab will allow you to enter a range of tubes to be analyzed and you will be allowed to select a method from a drop-down menu. Instructions are also provided on the tab. Single Method Operation with a Pre-selected Method—This option allows you to select the method to be used for the selected tube range.
Operation Config Tab The Config Tab provides the means to select the instrument configuration for the methods selected. NOTE: For the manual pneumatic models the PPC Config and Integrity Testing are unavailable (only available in PPC models) and are grayed out. See the Routine Maintenance chapter later in this guide for these procedures. See the following figure for a view of the popup screen.
Operation split on. See Setting the Outlet Split Flow on page 80 for details on setting the outlet split flow. Liquid N2 Option—Check this option to enable it on the Status tab. The option allows you to cool the cold trap down to –100°C. This option (L427-0009) must be installed on your instrument at the factory or by a service engineer. Number of Injections—Use the plus/minus buttons to set the number of injections you require.
Operation Figure 30 Setup Tab Password Protection—You can protect the instrument from unauthorized access to the Preference tab using the password protection. If you enable this option, users must enter a password to gain access to the Preferences tab.
To enable and use this option: 1. Select the Setup tab. 2. Press the Password Protection check box. A check mark will appear in the box to enable the option. 3. Press OK to close the Preferences tab. This confirms your selection. If you press Cancel, the TD will revert to the previous settings. 4. Press Tools and select Preferences. An alphabetic keypad is displayed. Enter the password “HSTD”. The password is not case sensitive. Once you have entered the correct password the, tab is displayed.
Operation 1. Select the Setup tab. 2. Press the Economy Mode check box. A check mark will appear in the box to enable the option. 3. Press the Config button to open the configuration dialog box. Figure 32 Economy Mode Dialog Box 4. The instrument will only go into Economy mode during a specified interval. Select the time during which the instrument is allowed to enter Economy mode. 5. The ATD/TD will only go into economy mode after a predetermined interval during which there is no activity.
Operation Connect Tab Key Clicks— If enabled, this option sounds a tone each time a button is pressed, to confirm that you have pressed a key. Baud Rate—Refer to the computer setup options to determine the baud rate, as this value will depend on the computer. The ATD/TD baud rate can be set from 300 to 57600 to match the computer’s setting. The default setting is 9600. NOTE: A baud rate of 9600 is required to allow use of the remote Control Software (option).
Operation Auxiliary RS-232—This port is available if you have the options board installed. This is for future development. Date/Time—Select the desired date format and then enter the correct date. Next, enter desired time format and then enter the correct time. Press OK to accept the new time. Loading Tubes Loading the ATD Carousel During primary desorption, the carrier gas will flow through the sample tube from the bottom to the top.
Operation groove, and prying them apart. Other techniques, such as twisting the pen-clip from the tube, can cause permanent damage to the pen-clip. Do not use pen-clips that have been permanently deformed (loose). Up to 50 capped sample tubes may be loaded onto the carousel. The sample tube should be loaded onto the carousel with the TurboMatrix brass analytical caps in place on both ends of the tube or the PTFE analysis caps.
Operation Ensure that sample tubes are cool before handling them. WARNING During primary desorption, the carrier gas will flow through the sample tube from the bottom to the top. It is therefore essential that sample tubes are loaded with their sampling ends (grooved end) upwards. This will ensure that the volatiles are desorbed from the collection end of the sample tube and do not pass through the whole length of the adsorbent bed. Sample tubes with pen clips may be loaded onto the TD.
Operation Single Method Operation on the TD Ensure that sample tubes are cool before handling them. WARNING Once you have set up the TD and entered a method for your application you are ready to begin analyzing your samples. Never try to access a tube on the TD while it is running. The oven heater may be activated and can cause a serious burn WARNING Single method operation is the simplest. Single Method Operation must be selected. See Preferences Tab on page 117. 1. Ensure that the GC is ready. 2.
Operation 8. Center the tube in the lower mobile seal and push down on the seal with the tube. Gently push the tube in and center the tube under the upper seal while it is seated and then release the tube. 9. The method can be stopped at any time by pressing the Stop button. A confirmation pop-up window will be displayed, press Yes to confirm that you want to stop the run. The analysis on the current tube is aborted and the tube will be unloaded.
Operation The method can be stopped at any time by pressing the Stop button. A confirmation pop-up window will display, press Yes to confirm that you want to stop the run. The analysis on the current tube is aborted and the tube will be unloaded and returned to the carousel. The method will be interrupted and the instrument will revert to Standby. Multiple Method (Sequence) Operation You can create a sequence of methods if you have varied applications.
Operation 7. Press the green Start button to run the sequence. The instrument will configure itself based on the first method. Once the instrument has reached the set points, the first tube will be loaded and the analyses will continue as determined by the method. Shutdown Normally you do not need to shut down the instrument. You can put the instrument into economy mode overnight and over the weekend. See Preferences Tab on page 117.
Operation NOTE: Before powering up the TD/ATD again, ensure that a) Carrier Gas supply and Dry Air to the TD are restored, b) Wait 20 to 30 minutes to ensure that both the cold trap and its environment are absolutely dry before power is applied to the TD. Programmable Pneumatics Control (PPC) TurboMatrix Series 300 TD, 350ATD and 650 ATD System Setup The PPC module is being configured and the initial pressure or flow setpoint is being established during the SYSTEM SETUP step.
Operation The Run Tab Once you have created a method by which to run the samples, you will manually load a single tube or load the carousel and run the samples from the Run tab. See Chapter 5 for details on creating methods. You can run samples using a saved method or a sequence of saved methods. Figure 34 Run Tab The options on the Run tab are determined by selections that have been made on the Preferences tab.
Operation and stop tubes. The tube range will default to 1 to 50. Press the first entry box to enable the option. If you are using a TD, the tube range is fixed at 1. 3. Press the plus or minus button to select the desired start tube. Then enter the desired end tube. 4. From the method drop-down box, select the method to be used for the selected range of tubes. 5. The Start button will be green, indicating that ATD/TD and the GC are ready. Press the Start button to begin the analysis.
Operation in this chapter. 1. Switch to the Run tab. 2. Select the Sequence button to enable the option. Press the start tube entry box. 3. Press the plus or minus button to select the desired start tube. Then enter the desired end tube. 4. From the method drop-down box, select the method to be used for the selected range of tubes. 5. Press the Add button to add the entry to the sequence. 6. Repeat these steps until you have created the desired sequence. 7.
Operation Editing a Sequence To delete an entry from the sequence, select the entry in the list and press the Del button. To change the tube range, you must add a new entry with the revised tube range and then delete the old entry. If you edit the methods called by your sequence, the sequence will use the revised methods. If you need to edit a method but do not want to affect your sequence, then save the revised method with a different name.
Operation temperature, the transfer line heater will be turned off and the transfer line will be at ambient temperature. Figure 35 Temperature Tab Tube Oven Temperature—The tube oven consists of a thermostatted block that slides into contact with the sample tube during primary desorption. The oven temperature can be set between 50°C and 400°C.
Operation Heat Rate—Once the volatiles are transferred from the sample tube, the trap is heated. Set the heating rate to any value between 5, 20, 40 and 99°C/second (ballistic). The faster heating rates ensures that volatile compounds are transferred to the GC column in a narrow band. Lower rates provide a slower heating for use in the analysis of analytes that are thermally labile. The trap is heated to the high temperature at the selected rate. This is the secondary desorption step.
Operation 5. To save your settings as a new method or to update the existing method, press the Tools button and select Save As. 6. To save the method existing name press OK. To create a new method, enter a new name for the method by pressing the method name. An alphabetic keypad is displayed. To enter numeric characters, press the Num key. Press Alpha to return to the alphabetic keypad. 7. Press OK to enter the new method name and then press OK save the method and return to the Status tab.
Operation Figure 36 Timing Tab The name of the method that is currently loaded on the Run tab is also displayed. The settings displayed here are from this method. You can change the settings and create a new method or update an existing method. Purge Time—When the leak test has been completed, air is purged from the tube prior to heating it for desorption. This is done to reduce the risk of adsorbent or analyte oxidation during desorption.
Operation Specifies the length of time, during which the trap is held at its high temperature for trap desorption. You can enter any value from 0.0 to 999.0 minutes. Typically, a value of 1 minute is adequate. See the following figure. Desorb Flow Time - Specifies the time that the pressure will be held at the lower level during trap desorb in the Pressure Pulse Injection Mode. See the Pressure Pulse Injection Mode section later in this chapter.
Operation being chromatographed. This setting is intended to ensure that the current run has finished in time for the trap desorption of the next sample. NOTE: Laboratory temperatures can strongly influence the GC oven cool-down time and can vary (for example, overnight). The GC cycle time setting should take into account the longest oven cool-down time expected during the analytical sequence. The ATD will use this value to calculate when to load the next tube.
Operation Figure 38 Internal Standard Popup You will need to enter a standard injection time by selecting the Preferences entry on the Tools tab and then selecting the Internal Standard button, from the Config tab. This calls up a dialog box that allows you to enter the Inject Time as well as the Loop Load and Loop Equil for the internal standard. Enter an injection time between 0.1 and 9.9 minutes. Enter a Loop Load time.
Operation Figure 39 Internal Standard Popup for the TurboMatrix 650 ATD The Options Tab The Options button at the bottom of the Status screen provides access to the ATD/TD method options. Select the options that you have installed or that are required to complete your method.
Operation Figure 40 Options Tab If you have the Standard Injection option installed, but do not need to use it, then de-select it here. You can enable heated sample tube purge, Inlet and Outlet sample Splitting and multiple injections from a single tube from this tab. You will also select the various ATD/TD operating modes from this tab. Standard Injection—If your ATD/TD is equipped with the optional Internal Standard Addition accessory (P/N M041-3657) you can enable or disable the option from this tab.
Operation Inlet Split and Outlet Split Options—Two split points are provided on the ATD/TD: one before and one after the cold trap. By using either one, or both together, it is possible to set split ratios ranging from zero to 200,000:1, enabling the ATD/TD to handle sample concentrations ranging from part-per-trillion (ppt) to high percentage levels. For models operating with the PPC carrier gas control, you will use these check boxes to enable the split flows.
Operation If you enabled the heated purge option, then the tube will be heated as it is purged. The default setting is 50°C (1°C increments with a temperature range of 20°C to 100°C). See the following figure. Figure 41 Dry Purge Popup NOTE: For TurboMatrix 650 ATD model the Purge Flow Rate is available and can be set.
Operation Operating Modes NOTE: The screen above shows operating modes for a TurboMatrix 650 ATD. The ATD/TD can operate in any one of five modes. A basic overview of each mode is provided here. A detailed description of each, including flow diagrams are shown in Chapter 8 Troubleshooting. Two Stage Desorption—This is the mode used to perform most of the analyses. Primary Desorb takes place after the sample tube has been leak tested and purged of air.
Operation The following two modes are only available on the TurboMatrix 650 ATD Two Stage Desorption and Recollect Sample onto Same Tube During Secondary Desorption, the sample is split between the GC column and the tube the sample was originally collected on. Up to 50 tubes can be used in this mode. Two Stage Desorption and Recollect Sample onto New Tube During Secondary Desorption, the sample is split between the GC column and a new tube that has been loaded from the carousel.
Operation Load Internal Standard (ISTD) on Tube If the instrument has been equipped with the Internal Standard option, a metered volume of an analytical standard can be loaded onto a sample tube. This can be done prior to the sample being collected onto the tube or prior to the desorption of the collected sample onto the cold trap. Continuous Online Monitoring— ‘On-line’ is a continuous sampling mode in which sample is drawn through the ATD/TD and sampled at regular intervals.
Operation Pneumatics Tab The Pneumatics tab (PNU) displays the pressure settings for your application. Figure 42 Pneumatics Tab (TurboMatrix 300 TD, TurboMatrix 350 ATD and TurboMatrix 650 ATD) PPC (Programmed Pneumatic Control) is a feature available in the TurboMatrix 300 TD, TurboMatrix 350 ATD and TurboMatrix 650 ATD). Desorb Flow Rate-The desorb flow rate is maintained during the desorb time when the tube is switched into the carrier gas stream. Sample is carried from the tube onto the cold trap.
Operation Inlet Split- Set the Inlet Split flow rate by accessing the entry field and incrementing or decremented the displayed value with the plus/ minus buttons. This option must be enabled via the check box on the Options tab. Tube-The current tube number and the number of injections from this tube are also displayed. Column Pressure-In the TD/ATD, the Column Pressure is maintained with a Programmable Pressure Control system (PPC).
Operation Column dropdown allows you to change modes from Pressure to Flow. In Pressure mode, the Pressure is maintained to the commanded value by the control system. In the Flow mode, the pressure is varied by the control system to maintain the commanded Flow value. See the following figure NOTE: To run the TD in the Flow mode, column dimensions must be entered in the Tools > Preferences > PPC Config dialog box.
Operation Pressure or the Trap Desorb Flow Time is set to zero, the system will default to the Isobaric Pressure Injection Mode. To set the Trap Desorb pressure, press the Trap button on the PNU tab. A Trap Desorb dialog box will be displayed. Set the Trap Desorb pressure to a lower value than the Column Pressure displayed on the PNU tab. To set the Trap Desorb Flow Time, press the Trap button on the Timing tab. A Trap Timing dialog box will be displayed.
Operation status of the run. If the sequence has been completed then the time at which it was completed is also displayed. Figure 44 Log Tab The information is overwritten when a new sequence is started. The Log Report is a log of all events. During a sequence, events can be logged after every injection, or only deviations may be logged. If every injection is to be logged, then the Log Report will contain the following information: • When the method and sequence were started.
Operation also contain the date and time the sequence was started and when the sequence was completed. Tools Pressing the Tools button opens a pop-up menu of tools that enable you to perform various functions such as creating and editing methods and configuring the options available on your instrument. Figure 45 Tools Menu The Method Editor command opens the tab. This tab allows you to create and store methods for your application. You can store up to 9 methods.
Operation Open Command—To revise an existing method, select the Open command from the File menu. Select the method that you wan to edit and press OK. Save/Save As Command—Use these commands to save new methods or update existing ones. 1. Select the Method Editor tab and enter or update the desired method parameters. 2. Select Save if you are updating an exiting method. It will be saved with the same name. 3. Select Save As if you are creating a new method.
Operation complete the selection and return to the Run tab. Activate Command—This command makes the currently selected method active. The method is loaded from memory and the instrument is heated or cooled to the new settings. NOTE: Do not activate a method if the TD or ATD is performing an analysis. The newly activated method will overwrite the current method Delete Command—Use this command to remove an existing method from memory. You can store up to 9 methods.
Operation 4. Enter any remaining operators and numbers. 5. Click =. 6. Sqrt calculates the root of the displayed number. X^2 calculates the square of the displayed number. 7. Press the close button (x) on upper right corner of the title bar of the window to close the calculator. Reset-Use the Reset command to reset the instrument in the event of a fatal error or software problem.
Operation Maintenance Tab You will use the Maintenance tab to set flows or perform routine maintenance on the instrument. The Maintenance tab contains the following commands. Maintenance—Select this command in order to preform certain maintenance procedures. Check Pnu-The functioning of the PPC Flow Controllers can be monitored by this dialog box. To change the set point for a controller, enable the check box for the controller to be tested. The other controller inputs will be grayed out.
Operation NOTE: The controller set point is in mass flow units. There will be a discrepancy with the measured value if a volumetric flow meter is used. Please refer to Chapter 7 “Theory of Thermal Desorption” for an explanation of the difference. IS Loop Load and IS Tube Load - You must set the flow rates manually for the Internal Standard accessory.
Operation Preferences Tab You will use the Preference tab to set the configuration options for the TD. The selections you make here will enable or disable various options on the Status tab and in the Method Editor. The Preferences tab contains four tabs. The Run tab sets the options for running analyses. The Config tab contains the options related to the operation of the TD. The Setup tab contains settings for various parameters and options.
Operation Single Method Operation—If you select single method operation you can also specify the method to be used. The options on the Run tab will allow you to enter a range of tubes to be analyzed and you will be allowed to select a method from a drop-down menu. Instructions are also provided on the tab. Single Method Operation with a Pre-selected Method—This option allows you to select the method to be used for the selected tube range.
Operation Figure 48 Config Tab NOTE: Integrity Testing button is grayed out for all models except the TurboMatrix 650 ATD. See the section on Integrity Testing below for operation with a TurboMatrix 650 ATD PPC Config. Carrier Gas-Select the type of carrier gas being used. The correct selection must be made to ensure the proper control of the pneumatic components. NOTE: When a change is made to the carrier gas selection, the power to the instrument must be cycled.
Operation ID - input the ID of the transfer line. This information is required to run the instrument in the Flow Control mode. Direct Connection-Selection of the check box indicates a direct connection of the GC column to the instrument, without a transfer line. Selection of this configuration disables the input box for the Transfer Line ID.
Operation Liquid N2 Option-Check this option to enable it on the Status tab. The option allows you to cool the cold trap down to -100°C. This option (L427-0009) must be installed on your instrument at the factory or by a service engineer. Number of Injections-This will record the total number of injections since the last RESET. Maintenance Alarm-Use this option to set the number of samples to be performed until a warning message is displayed.
Operation Old Trap New Trap Figure 50 Old and New Trap See the Routine Maintenance, chapter 6 later in this guide for these procedures. See the following figure for a view of the Integrity Testing popup screen. Figure 51 Config Tab PPC Integrity Testing Popup (only available in the TurboMatrix 650ATD) Monitor Tube Impedance-Selection of the check box enables the input boxes for Lower and Upper Limits.
Operation Monitor Trap Impedance-Selection of the check box enables the input boxes for Lower and Upper Limits. The measured pressure will be reported in the Log file at the beginning of the sequence and will be compared against the entered values. Stop on Failure-Selection of the check box causes the instrument to stop the sequence when the measured values fall outside the entered Limit values.
Operation Figure 52 Setup Tab Password Protection—You can protect the instrument from unauthorized access to the Preference tab using the password protection. If you enable this option, users must enter a password to gain access to the Preferences tab. Figure 53 Password To enable and use this option: 1. Select the Setup tab. 2. Press the Password Protection check box. A check mark will appear in the box to enable the option. 3.
Operation Protection” and the pop-up Password box will appear in the figure above. If you wish to create a new password, touch each box and the alpha keypad will appear. The original (old) password is “hstd”, or another entry mode after installation. 4. Once you have entered the correct password press OK. 5. Press OK to close the Preferences tab. This saves your selection. If you press Cancel, the TD will revert to the previous settings.
Operation 3. Press the Config button to open the configuration dialog box. Figure 54 Economy Mode Dialog Box 4. The instrument will only go into Economy mode during a specified interval. Select the time during which the instrument is allowed to enter Economy mode. 5. The ATD/TD will only go into economy mode after a predetermined interval during which there is no activity. You can select this time.
Operation Connect Tab Key Clicks— If enabled, this option sounds a tone each time a button is pressed, to confirm that you have pressed a key. Baud Rate—Refer to the computer setup options to determine the baud rate, as this value will depend on the computer. The ATD/TD baud rate can be set from 300 to 57600 to match the computer’s setting. The default setting is 9600. NOTE: A baud rate of 9600 is required to allow use of the remote Control Software (option).
Operation Auxiliary RS-232—This port is available if you have the options board installed. This is for future development. Date/Time—Select the desired date format and then enter the correct date. Next, enter desired time format and then enter the correct time. Press OK to accept the new time. Loading Tubes Loading the ATD Carousel During primary desorption, the carrier gas will flow through the sample tube from the bottom to the top.
Operation The pen-clip can be removed from a sample tube by inserting a wide-bladed screwdriver between the clip and the tube, close to the groove, and prying them apart. Other techniques, such as twisting the pen-clip from the tube, can cause permanent damage to the pen-clip. Do not use pen-clips that have been permanently deformed (loose). Up to 50 capped sample tubes may be loaded onto the carousel.
Operation Sample tubes with pen clips may be loaded onto the TD. The tube must be placed into the TD with the pen clip facing back, toward the back of the instrument. To load the tube: 1. Remove both caps from the tube. Ensure that the instrument is Ready. 2. Place the tube into the tube compartment with the sampling end (grooved end) upwards. 3. Center the tube in the lower, mobile seal and push down on the seal with the tube.
Operation tab. 3. If you are running with a pre-selected method you only need to load the tube. 4. If the method has not been selected, select it now from the drop-down box. NOTE: These options can be preselected on the Preferences Tab. See Preferences Tab on page 117. 5. Remove both caps from the tube. Ensure that the instrument is Ready. 6. Place the tube into the tube compartment with the sampling end (grooved end) upwards. 7.
Operation operation, instructions will be displayed on the tab. 3. If you are running a single method and the method has been pre-selected then you only need to enter the start and stop tubes. 4. Press the start tube entry box and then press the plus or minus button to select the desired start tube. 5. Enter the desired end tube. 6. If the method has not been pre-selected, select the method from the drop-down box. NOTE: These options can be selected on the Preferences Tab. See Preferences Tab on page 117.
Operation 3. Enter the desired end tube. 4. From the method drop-down box, select the method to be used for the selected range of tubes. 5. Press the Add button to add the entry to the sequence. 6. Repeat these steps until you have created the desired sequence. To delete an entry from the sequence, select the entry in the list and press the Del button. To change the tube range, you must add a new entry with the revised tube range and then delete the old entry.
Operation CAUTION Before attempting to disconnect the TD/ATD from the GC, read and strictly follow the next set of instructions to protect the GC column and specific detectors. The TD/ATD is the sole supplier of carrier gas to the GC! a) Ensure that both the GC oven/detectors are cool. b) If an MS is used, the GC-MS transfer line (if used) and the Ion Source are cool. Filament is OFF. c) All TD/ATD zones (trap, heated valve, transfer line) are cool. To shut down the ATD or TD: 1.
Operation 180
Accessories 4
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Accessories Options Board An options board is available for the instrument. This board provides 4 programmable, time-dependent switch relays, the BCD interface, one RS-S232C port and support for the ATD automation module, and support for the LN2 option. The BCD option and the LN2 both require the option board to be installed and enabled. Timed Events The optional timed event connector has terminals for 4 programmable relays. External devices may be operated by these relays.
Accessories window. 8. If you are using the Method Editor, save your method. If you are using the Status tab, you must enter all of the other method parameters and then save the new method. 9. Run an analysis to test that your devices are connected properly and your events are programmed correctly. Example: To turn relay #1 on for 30 seconds, 2 minutes after the current analysis has started, you would enter: an event time of 120 seconds, Relay Number 1 and Action would be On.
Accessories RS-232C Communication Interface One serial RS-232C port is located on the rear of the instrument. Configuration of the port is available below. 1. From the Tools menu, select Preferences. 2. Select the Connect tab. BCD Interface The Binary Coded Decimals (BCD) interface is provided on the options board. The BCD interface is used to transfer the sample tube numbers to an external instrument such as an integrator. The BCD data channels (contacts 1 to 13) are set to negative logic.
Accessories Tubes and Caps The ATD/TD uses industry standard, patented stainless steel tubes. The stainless steel tubes are compatible with pumped and diffusive air monitoring and can be ordered prepacked. Glass and glass-lined tubes are also available for pumped monitoring. All tube types are suitable for direct sampling of solids and liquids. PerkinElmer tubes are manufactured to the tightest specifications to ensure trouble-free operation and high-quality analysis results.
Accessories further tighten the nut onto the cap. Again be careful not to overtighten the nut. If the cap fits the tube too tightly, then the ATD may not be able to decap the tubes correctly. NOTE: Never use tools to tighten the brass caps. Overtightening the fitting will result in damage to the PFA ferrules and possible damage to the tubes. The brass caps can be used for single use samples as well as long term sample storage.
Accessories Capped Sample Tubes (with PTFE Analysis Caps) Stainless Steel Glass Glass Lined Stainless Steel Qty M041-3595 M041-3598 M041-3597 10 M041-3596 N/A N/A 50 Sample Tubes Without Caps Stainless Steel Glass Glass Lined Stainless Steel Qty L427-0128 L407-1594 N/A 10 L427-0129 N/A N/A 100 Prepacked Sample Tubes Stainless Steel Glass Sorbent Qty N930-7001 N930-7008 Air Toxics Tube 10 N930-7002 N930-7009 Carbopack B 60/80 10 N930-7003 N930-7010 Carbosieve SIII 60/80
Accessories Accessories PTFE Analytical Caps N620-0119 20 Brass Caps with ferrules M041-3624 20 Ferrules (replacement ferrules for M0413624) M041-3625 20 Brass Long Term Storage Caps (requires teflon ferrule 0496-4467) 0990-8851 20 Teflon Ferrule (required for 0990-8851 0496-4467 1 Pen Clips L407-1029 1 Diffusion Caps L407-0207 10 Diffusion Caps with Membrane Ll407-0208 10 Unsilanized glasswool 0009-7993 100g Table 11 Replacement Sample Tubes and Caps Liquid Nitrogen Accessory (
Accessories (140 to180 kPa). A pressure relief valve set to 50 psig (350 kPa), should be installed in the tubing between the Dewar flask and the liquid nitrogen accessory. This will prevent build up of pressure WARNING in the tube should the liquid nitrogen accessory and the Dewar flask be turned off while liquid nitrogen is still present in the tubing. To conserve liquid nitrogen, the accessory will be turned off automatically under the following conditions: • when the ATD/TD is in Standby.
Accessories Internal Standard Accessory The Internal Standard (IS) Addition Accessory (P/N M041-3555) is an 8-port valve equipped with a 0.5-mL sampling loop. The valve is installed into the flow path as shown in Figure 58 for manual pneumatics. Figure 59 shows the PPC flow path (with the TurboMatrix 350 ATD flow chart given as an example of PPC). It is used to add an aliquot of a known standard onto each tube before primary desorption. The Internal Standard option is installed in the factory.
Accessories Figure 59 Flow Diagram of the TurboMatrix 350 ATD (PPC) with Internal Standard Accessory The standard addition accessory is kept at ambient temperature and is consequently restricted to relatively volatile internal standards Additionally, if you have the IS accessory installed, the Reverse Dry Purge option is available (Preferences/Config tab. Reverse dry purge may be used to prevent water from being transferred to the cold trap during primary desorption.
Accessories Principle of Operation The reference gas pre-fills the 0.5-mL loop during the loop load time. This has been set to 30 seconds, at the factory. The 30 seconds is the default setting which you can change. After a tube has been loaded into the desorption position and following the leak test and tube purge, the internal standard gas valve is switched so that the loop is in series with the sample tube. Carrier gas transfers the loop contents to the back of the tube.
Accessories 4. 4. In the same dialog box you can set the Inject Time (in minutes) to the amount of time you want helium to go through the loop onto the tube. This time will be based on the method used for your analysis. Enter an injection time between 0.1 and 9.9 minutes. 5. Set up the rest of your method parameters or if these parameters are already setup, run your samples.
Accessories standard easy to distinguish in a chromatogram run on a GC-MS system. Toluene-D8 does not exist in nature and so there is no interference with naturally occurring compounds. Description Part No. 0.5 mL Sample Loop P/N 0332-4902 1.0 mL Sample Loop P/N 0332-4903 5.0 mL Sample Loop P/N 0332-4904 NOTE: If you are using an internal standard at a concentration that exceeds the TLV limits, you must direct the Tube Load and Loop Load vents to a fumehood or another suitable location.
Accessories upon and set. This function is available by selecting the Preferences entry on the Tools menu and then selecting the Config tab and the Internal Standards button. A dialog box will appear with the Loop Load entry box. After connecting the IS canister to the TD unit, you will manually adjust the loop fill flow of the internal standard with the Loop Load needle valve, while monitoring the flow with a suitable flowmeter at the Loop Load vent (a flow of 20 mL is recommended).
Accessories number into the Loop Equil box. NOTE: For all the information and operating instructions, see the Internal Standard Addition Accessory Users Guide (Part No. 0993-4549). IS Tube Load— See the Status/Options tab, to check the Standard Inject box.This will enable the Internal Standard Addition accessory. A minimum gas volume of 15 to 20 times the loop volume is required for total transfer of the loop contents to the sample tube. If the loop volume is 0.
NOTE: Use a clean sample tube that does not contain a sample for the set-up procedure. The sample tube should contain the type of packing material that will typically be used for your applications. 2. When the TD is in Ready mode, open the Tools menu and select Maintenance. 3. Select IS Tube Load. 4. The ATD will load the tube from position #1 into the sampling position to complete the carrier gas path.
Accessories TD Control Software The TD Control Software is designed to run under Microsoft Windows. The software provides the means to operate the instrument through a PC. You can also create methods, and sequences and log information about the status of the TD. The Control Software runs in combination with TotalChrom, although TotalChrom is not required to run the control software.
Accessories Figure 61 Sequential Tube Sampler with monitoring pump. Contact PerkinElmer for further details about this accessory. Online Sampling Accessory Semi-continuous, online air sampling and GC analysis is a proven technique with applications ranging from urban air quality testing to occupational hygiene. In online air sampling a volume of air is pumped directly into the cold trap using a mass flow controller. Air is usually sampled for the greatest possible percentage of the cycle time.
Accessories Vacuum Turbomatrix TD Pump with Online Sampling Accessory AutoSystem XL or Clarus 500 GC XL AutoSystem with Heartcut Device, Dual FIDs and Internal LINK TotalChrom and TurboMatrix Remote Control Software Figure 62 GC System Refer to the user’s manual of the Online Air Sampler accessory for details of installation and operation.
Accessories 202
Method Development 5
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Method Development Method Development When you are creating a new method, you optimize the method by performing analyses at various settings until reliable results are obtained. You use the Status tab to enter the desired parameters and options and then run a few samples to evaluate the method. You then adjust parameters accordingly and run more samples until you obtain the desired results. Once your method is complete, use the Save As command in the Tools menu to save the new method.
Method Development The process of developing thermal desorption methods can be greatly simplified by keeping the principles given below in mind when parameters are initially selected. Optimizing Primary (Tube) Desorption To optimize the primary (tube) desorption, the analysis parameters should be set following these general guidelines: • The sample tube temperature needs to be set as high as possible.
Method Development Optimizing Secondary (Trap) Desorption To optimize the secondary (trap) desorption, the analysis parameters should be set following these general guidelines: • To elute all components retained by the cold trap and transfer them to the analytical column in as narrow a band of vapor as possible you must set the secondary desorb temperature as high as possible.
Method Development Setting System Parameters Temperature Tab There are five temperature settings for the TD: tube oven temperature, the transfer line temperature, the cold trap temperature and secondary trap desorption temperature. You will also set the temperature of the heated valve. Temperatures for tube desorption, cold trapping and trap desorption are selected to be as high as possible, as low as possible and as high as possible respectively, as described above.
Method Development they burn. Residual solvents are often locked (occluded) inside the crystal structure of the solid drug. You must ensure that molten pharmaceuticals do not move out of the sample tube and contaminate the system flow path. • Do not heat samples containing mercaptans above 200°C. Trap Low Temperature—The cold trap is cooled with a Peltier cooler to temperatures between -30°C and +150°C.
Method Development time but may be required for the analysis of thermally labile analytes. Trap High Temperature—The trap is heated to the high temperature at the selected rate. This is the secondary desorption temperature. Set the trap high temperature so that even the heaviest compounds will be moved from the trap onto the GC column. During the heating and high temperature hold time, you need rapid sample transfer without sample or sorbent degradation.
Method Development nature of chromatography it is often possible to extend the tube desorb time, since the GC run tends to be lengthy, without affecting productivity. During the analysis of labile or unknown materials, it is preferable to lower the temperatures used and extend the desorption times. Purge Time—When the leak test has been completed, air is purged from the tube prior to heating it for desorption. This is done to reduce the risk of adsorbent or analyte oxidation during desorption.
Method Development overlapping tube desorptions and analyses to maximize throughout. For example, if the CYCLE TIME is 42 minutes after the previous injection (trap heat).This means that the GC is expected to be ready to run at that moment (in order for no delays to occur). So the interval (in this example 42 minutes) must be sufficiently long to allow a full GC run to occur and for the GC to cool down and become ready again. Time 0 ATD heats trap to start the injection. GC starts run.
Method Development The Options Tab The Options tab provides further method options for your application. Number of Injections—This parameter specifies the number of desorptions per sample tube. For example, If you enter 99 the first selected tube will be loaded and will continue to go through desorption cycle until you press Stop. NOTE: However, if a value of 99 is entered for any of the methods in a sequence, the sequence will stop after that method is run and 99 injections have occurred.
Method Development If you have enabled this option, then you must enter a Standard Inject time on the Timing tab. The standard addition valve is activated for the duration of the standard injection time to allow introduction of a volume of standard onto the sampling/desorption end of the tube. After the end of the standard injection time, the valve is closed and the ATD/TD will proceed with desorption of the tube.
Method Development tube, but not so high that the sample starts to come off the tube. If sample starts to be desorbed it will be lost to vent during tube purge. If you enable this option, you must also enter a suitable purge temperature to the appropriate field on the Preferences tab. The default setting is 50°C. Heated purge takes place during dry purging. The minimum temperature is 50°C.
Method Development degrade rapidly and leak. You may also want to install high temperature o-rings into the fixed seal assembly. The high temperature o-rings (P/N 0920-0092 and 0920-0093) are intended for operation up to 300°C. The ferrule in the mobile seal assembly may also be adversely affected if you are regularly operating at temperatures above 225°C. It may be necessary to replace the ferrule every 2-3 months if you are operating at high temperatures.
Method Development required split ratio and then set the inlet split and outlet split flows rates accordingly. Carrier gas flow rates may be increased to enhance the process of desorption from the tube and trap, and to facilitate transfer to the cold trap during tube desorption. The option of using higher flow rates to speed desorption is particularly useful during the analysis of labile components when high temperatures cannot be used.
Method Development Upon completion of each flow adjustment an entry of its value can be made in the respective field of the Status/Pnu tab. These settings have no automatic function. They serve only notation purposes. For the Pressure and Flow adjustments see Setting the Carrier Gas Flows on page 77. NOTE: For the Loop Load Flow Rate and the Tube Load Flow Rate adjustments and operation instructions, see the Internal Standard Addition Accessory User's Guide P/N 0993-4549.
Method Development Adsorbent Weak Strong Sample Tube Vapor No Breakthrough Stainless Steel Gauze Vapor Breakthrough Figure 63 Sample Breakthrough PerkinElmer sample tubes for thermal desorption are compatible with both pumped and diffusive air monitoring, and are also used to trap volatiles purged from water, sediment and other sample matrices. A general guide to adsorbent selection is presented in Table 13.
Method Development (n-C4) n-C5 to nC14 400 100 Wide range of VOCs including ketones, alcohols and aldehydes (bp>75°C), and all polar compounds within the volatility range specified. Plus perfluorocarbon tracer gases. Chromosorb ™ 102 bp 50 °C to 200 °C 250 350 Suits a wide range of VOCs including oxygenated compounds and haloforms less volatile than methylene chloride Chromosorb ™ 106 bp 50°C to 200°C 250 750 Suits a wide range of VOCs including hydrocarbons from n-C5 to n-C12.
Method Development Molecular Sieve** -60°C to + 80°C 350 Charcoal* -80°C to + 50°C 400 Used specifically for 1, 3butadiene and nitrous oxide. >1000 Rarely used for thermal desorption because metal content may catalyze to analyte degradation. Use, with care, for ultravolatile C2, C3, C4 hydrocarbons. * These sorbents exhibit some water retention. Safe sampling volumes should be reduced by a factor of 10 if sampling at high (> 90%) relative humidity. ** Significantly hydrophilic.
Method Development temperatures, up to 300°C and more, for efficient thermal desorption.1 As a general policy it is a good idea to use similar sorbents in a tube so that conditioning the combined packings is facilitated. For example, if you use both Tenax (polymer, max temp 350°C) and Carbotrap (carbon, max temp 400°C) in the same tube, you can only recondition the tube to the lower temperature. If both packings were carbon you could obviously condition the tube to 400°C without ill effects.
Method Development 1000 Retention Volume - Extrapolated for 20°C Retention Volume (liters per gram) 100 200 liters per gram 10 200°C 150°C 1 10-1 10-2 10-3 103 X 1.4 1.8 2.2 2.6 3.0 1 °K T 3.
Method Development Compound Boiling Point (°C) Retention Volume at 20 °C (l/g) Heptane 98 170 Octane 125 780 *Benzene 80 62 Toluene 111 360 Xylenes 138-144 1500 Cumene 152 4800 Trimethyl benzene(s) 165-176 17800 Styrene 145 3000 Methylstyrene 167 12000 1, 1, 2-Trichloroethane 114 340 1, 1, 1, 2-Tetrachloroethane 130 780 1, 1, 2, 2-Tetrachloroethane 146 1700 Tetrachloroethene 121 480 Chlorobenzene 131 260 Propyl acetate 102 184 *Isopropylacetate 90 62 Butyl
Method Development Amines *Pyridine 116 78 Aniline 184 2200 * Indicates that a stronger adsorbent than Tenax should be selected if possible. Table 14 Compounds Suitable for Diffusive Sampling on Tenax GR Compound Boiling Point (°C) Retention Volume at 20 °C (l/g) Acetone 65 5.4 Dichloromethane 40 3.0 Ethanol 78 1.
Method Development Brass Swagelok Coupling with One Piece PTFE Ferrules Weak Adsorbent Sampling Air Flow Tenax Medium Adsorbent Chromosorb 102 Strong Adsorbent Spherocarb Figure 65 Glass or Stainless Steel Sample Tubes Containing Adsorbents of Increasing Strength Linked Together in Series In this case the light compounds break through the weaker sorbent and are retained on the stronger one.
Method Development The separate tube technique is also useful if sorbents of totally different substrates are used, since each tube can be conditioned individually under optimum conditions.
Method Development All forms of Tenax are susceptible to decomposition since they are polymer based, so there is always some background (artifacts) associated with its use. This can be exacerbated if the material is not properly conditioned. If you are working at higher levels, where hydrophobicity is perhaps a concern, and desorb temperatures to 350 °C max are acceptable, Tenax is suitable for compounds with volatility higher than that of C6.
Method Development secondary desorption. (i.e. while the trap is hot.) • The maximum gas flow rates that can be controlled using the multiple splitter needle valves at conventional GC column carrier gas pressures are between 150 and 200 mL/min. • The Peltier cooler will be unable to maintain a cold trap low temperature of -30 °C if gas flow rates exceeding 120 mL/min through the trap are employed when using helium or hydrogen as carrier gas.
Method Development your trap loading and column capacity and flow, figure out how much sample you need on the trap and therefore what the outlet split must be. Then figure out how much you need to split the tube sample in order to put the required amount on the trap. The overall split is the product of the two. Zero Split (Splitless) Operation One type of trap is offered for the TurboMatrix desorber, the “lowflow” type which has a built in capillary to reduce dead volume.
Method Development NOTE: Superior performance is always obtained, even at the expense of a small outlet split ratio, by increasing the velocity of the carrier gas through the trap during secondary desorption. During primary desorption: Flow Through the Tube = Flow Through the Cold Trap Equation 1 During secondary desorption: Flow Through the Heated Trap = Outlet Split Flow + Column Flow Equation 2 NOTE: The column flow must be measured at the column outlet during secondary desorption.
Method Development Outlet Split = 8 mL/min In the above example, the trap desorption flow of 10/mL/min is barely sufficient when using a standard trap tube; a narrow-bore trap would be better suited for this application. Example: In this example we want 2% of the tube sample to reach the GC detector. The column flow rate is 1 mL/min (measured during secondary desorption). Trap desorb flow is 50 mL/min and there is no inlet split flow.
Method Development during primary desorption in order to enhance component retention on the trap. 3. To establish a reasonably high flow through the heated cold trap during secondary desorption in order to enhance component elution from the trap. Double-split operation is enabled by selecting both the inlet split and outlet split options on the Option tab.
Method Development The percentage of components from the sampling tube which reach the analytical column is: Column Flow x Desorb Flow x 100 (Outet Split Flow +Column Flow) x (Desorb Flow + Inlet Split Fow) Equation 10 Example: In this example 10% of the tube sample must reach the GC detector. The column flow rate is 2 mL/min.
Method Development 1.5 mL/min and the outlet split flow is 150 mL/min Inlet Split = 150 mL/min Inlet Split Flow 150 mL/min Sample Tube Cold Trap Desorb Flow 1.5 mL/min 4.3 mg of Sample Inlet Split Ratio 100 : 1 Outlet Split Flow 150 mL/min 160 ng of Sample Reaches the Detector A split ratio of 27 000 : 1 Trap Column Flow 0.
Method Development Four major techniques are commonly used to introduce standards into desorption tubes. Vaporizing a Liquid Standard In the first method, standards are introduced in the vapor phase into a sample tube in the following way: A liquid sample is placed in a packed-column GC injector. The liquid sample is then vaporized in the injector and the vapor is swept onto the tube packing in the flow of carrier gas.
Method Development Injecting a Liquid Sample Directly onto the Sample Tube The second method involves injecting the liquid sample directly into the sample tube. The sample must be placed behind the adsorbent bed so that the compounds of interest pass through the adsorbent bed during the primary desorption. This imitates the desorption of real samples as closely as possible.
Method Development Internal Standard Addition Accessory The Internal Standard Addition accessory is required for the third method. A gaseous calibration standard from a pressurized tank is transferred directly onto the sample tube. See Internal Standard Accessory on page 191 for details of operation. Pumping a Calibrated Standard Gas Atmosphere The last method involves pumping a calibrated standard gas atmosphere, at a known flow rate, onto a sorbent tube.
Method Development Sample Integrity Testing The TurboMatrix 650 ATD offers the Sample Integrity Testing feature. This test will allow you to get information on whether the tube or trap have physically deteriorated. 1. load a know standard into a tube before it is sent out for sampling. 2. Go to the Status page Options tab. At the Mode drop down menu select Load ISTD on Tube. this mode of operation will inject an internal standard onto the selected tubes. 3.
Method Development Desorb-Rec-Same: This method will inject a sample but instead of loosing the sample to outlet split the split flow is directed to the original sample tube and recollected. Desorb-Rec-New: This method injects a sample into a new tube. positions 1-25 are for the original sample tubes with recollection on new tubes in position 25 to 50 (for example, sample tube 1 goes to position 25, sample tube 2 goes to position 27 etc.).
Routine Maintenance 6
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Routine Maintenance Routine Maintenance This chapter describes the maintenance procedures that can be performed by the user. WARNING Do not attempt to make adjustments, replacements or repairs to this instrument except as described in the following sections. The ATD/TD does require some regular maintenance to keep it operating efficiently. Replacement of some items will vary with usage.
Routine Maintenance Item/Operation Frequency Replace oxygen, moisture and charcoal filters on the carrier gas lines. As required Replace o-rings in the seals As required Leak test the system As required Replace the o-rings and filter disk in the mobile seal. As required Replace the cold trap As required Replace the trap filter disks Whenever the cold trap is replaced or repacked.
Routine Maintenance General Laboratory Cleanliness Thermal desorption is a very sensitive technique and the adsorbents used are very efficient trapping agents. If proper precautions are not taken, the surrounding environment will contaminate your system. NOTE: All users must be made aware of the circumstances that can lead to contamination of the system. The degree to which precautions are necessary depends on the sensitivity required for your application.
Routine Maintenance Sample Tubes and Storage Caps When samples have been collected, the tubes should be analyzed as soon as possible. If the tubes cannot be analyzed soon after sampling, you should cap them with Swagelok caps (P/N 04969332) and PTFE ferrules (P/N 0496-4467). Avoid storing tubes that contain sample in places where there are high levels of organic vapors, such as refrigerators and car trunks. Tubes in such places must be capped with Swagelok caps.
Routine Maintenance for the PTFE ferrules (P/N L427-5110) as graphite ferrules are permeable to air. Removing and Replacing the Front Covers of the ATD You may need to remove the front covers of the ATD in order to install the transfer line, and perform a number of routine maintenance tasks. The front covers consist of the arm housing and the transfer line cover. 1. Make certain that the ATD is in Standby. Turn off the instrument and disconnect it from the AC line power. 2.
Routine Maintenance Loosen Screw (Do not remove the screw) Door Latch Remove Screw Figure 69 ATD Arm Housing To gain access to the top of the heated valve, you must further remove the transfer line cover. 8. Remove the two screws at the rear of the transfer line enclosure (the upper, curved molding). 9. Slide the cover panel outward. To replace the covers: 10. Replace the transfer line cover first. Secure the screws at the rear of the enclosure. 11. Slide the arm housing back into place on the chassis.
Routine Maintenance Changing the O-Rings in the Fixed and Mobile Seals The sample tube is sealed into the carrier gas circuit by compressing it between two o-rings. These seals are located within the carrier block at the inlet end and within the nozzle at the outlet end of the tube. After several months of operation, leak test failures may begin to occur. When operating near the maximum valve and tube desorption temperatures, o-ring life expectancy could be approximately 100 analyses.
Routine Maintenance and 0920-0093) are intended for operation up to 300 °C. See High Temperature Operation on page 215 for further details. We recommend replacing the grip-seal o-ring whenever the tubeseal o-ring is replaced. To replace the sealing o-rings: 1. Make certain that the TD is in Standby. Turn off the TD and disconnect it from the AC line power. 2. If necessary, allow the instrument to cool. The heated valve, the tube oven, and the trap enclosure may be very hot.
Routine Maintenance Heated Valve O-ring Fixed Seal Assembly Filter O-ring O-ring Filter Mobile Seal Assembly O-ring Figure 70 Location of TD Sample Tube Seals 5. Use the ½” socket supplied in the shipping kit to loosen and remove the nut on the fixed seal. 6. Use tweezers or forceps to carefully remove the o-rings and the filter disk. NOTE: Tweezers or forceps with sharp points may scratch the inner sealing surface of the nut and cause leaks. 7.
Routine Maintenance NOTE: Do not over tighten the seal. O-Ring Viton High Temperature Size 009 L1003006 Pk/5 0920-0092, ea Size 010 0497-0343 Size 011 L1003008 Pk/5 0920-0093, ea Table 18 Fixed and Mobile Seal Replacement O-Rings Changing the O-Rings and Filter Disk in the TD Mobile Seal Change the tube-seal o-rings (P/N 0497-0434 and L1003006) whenever there is evidence of repeated tube leaks.
Routine Maintenance 3. Use tweezers or forceps to remove the o-rings and the filter disk. 4. It is possible that residue from the o-ring material will remain on the nut. Clean out any residue in the nut. 5. Using tweezers or forceps, place the smaller o-ring into the nut. Place the filter disk on top and then lastly place the larger o-ring into the nut. NOTE: Do not touch the o-rings or the filter disk with your fingers. 6. Again use the 1/2 inch socket to place the nut onto the fixed seal assembly.
Routine Maintenance 4. Remove the carousel and bottom cover. Cap Insert Figure 71 Automated Mobile Seal 5. Turn the mobile seal cap counterclockwise to remove it. At the same you are turning the mobile seal cap hold down the mobile seal body. 6. Using tweezers or forceps, remove the o-ring and filter disk from the mobile seal cap and insert body.
Routine Maintenance careful not to pull the insert body too far since this may damage the brazed tubes. 7. Install new o-rings and/or filter disk using tweezers or forceps. NOTE: Do not touch the filter disk with your fingers. 8. Reassemble the mobile seal and retighten the mobile seal cap. Do not overtighten the mobile seal. tighten only finger tight. Carefully insert the brazed tubes on the insert body and do not bend them. 9. Reinstall the carousel. 10. Turn on the dry air gas supply.
Routine Maintenance inserting the end of the column into a silicone septum. 1/8” packed columns may be capped using a 1/8” Swagelok® cap (P/N 0496-7810). 2. With the ATD/TD in Standby, set the carrier gas pressure to the maximum 30 or 60 psi (200 or 400 kPa) using the pressure regulator on the TD. Wait for the gas pressure to stabilize throughout the system, and then note the actual pressure on the display, or on the TD Control Software status. 3.
Routine Maintenance Standard Leak Test To perform a standard leak test go to the Tools drop down menu and select Maintenance and select Leak Test. Once you select Leak Test the following screen will appear. Press OK to begin the Leak Test. If your GC has passed the leak test then proceed to the Column Leak Test. Impedance Calibration See the section Tube and Trap Impedance Test for the TurboMatrix 650, later in this chapter for detailed information on this feature.
Routine Maintenance select Maintenance and select Column Leak Test. The following screen will appear. Press OK to start the test. If your GC fails this column leak check all connections and ferrules. GC Temp Calib This feature allows you to calibrate the GC oven temperature to a sensor that is used to control the PPC flow. To access this calibration go to the Tools drop down menu and select Maintenance and select GC Temp Calib. The following screen will appear.
Routine Maintenance Ambient Pressure Calibration The Ambient Pressure Calibration feature measures the pressure in the room. You can calibrate the PPC ambient pressure to an independent barometer.To access this calibration go to the Tools drop down menu and select Maintenance and select Amp Press Calib. The following screen will appear.
Routine Maintenance Checking the Pneumatics for the TurboMatrix Series PPC Units You may need to check the pneumatics on the three available units with PPC (the TurboMatrix 300 TD, 350 ATD and 650 ATD). 1. To perform this check go to the Tools drop down menu and select Maintenance and then select Check Pnu. 2. The screen now displayed will offer you four options: Inlet Split, Outlet Split, Desorb and Recollect.
Routine Maintenance 3. Attach a bubble flow meter to the vent. 4. Press the Set button on the screen to measure the flow at that point. 5. In the Actual box you will see the actual flow reading. At this point you will be able to tell how accurate your setpoint value is from your actual value. See following Note. 6. Press OK when completed. NOTE: Most mass flow controllers are calibrated in sccm (standard cubic centimeters per minute). This is the same as mL/min at 0 °C and 760mg Hg.
Routine Maintenance Where: Fa is the measured flow rate under ambient conditions (mL/min). Fs is the flow rate entered/displayed on the TurboMatrix system (sccm). Ps is the calibration pressure (760 mm Hg). Pa is atmospheric absolute pressure (mm Hg). Ta is the ambient absolute temperature (°K) Ts is the calibration temperature (273.15 °K) Tube and Trap Impedance Calibration for the TurboMatrix 650 ATD The TurboMatrix 650 ATD offers a unique feature to test for tube or trap impedance.
Routine Maintenance Figure 73 Filter in Place 3. Run the tube and trap leak tests and check the system and ensure that the system is completely free of leaks.
Routine Maintenance 4. Set the Valve temperature to the value required for the analysis. NOTE: For the best accuracy, the calibration procedure should be repeated if the valve temperature is changed. 5. To perform this check, go to the Tools drop down menu and select Maintenance and then select Impedance Calib..
Routine Maintenance 265
Routine Maintenance 6. Place a clean and empty glass or stainless steel tube into Position 1 (see the following figure) of the carousel and press the OK button. The empty tube will now be uncapped and loaded into the desorption position. Carrier gas at 50mL/min will be passed through the tube but no flow will be passed through the trap.
Routine Maintenance 7. Allow the Actual readings for the Tube and the Trap to stabilize. NOTE: Because of the very low pressure differences being monitored, some minor instability in the displayed values may be apparent.
Routine Maintenance 8. Manually transpose the average Actual values into the corresponding Offset fields.
Routine Maintenance 9. Press the OK button to accept the new calibration or press the Cancel button to keep the previous values. The carrier gas inside the tube will be vented for 1 minute; “Cooling Tube” will be displayed. The tube will be unloaded, recapped and returned to the carousel. The pressure transducers used for the impedance testing will now be calibrated and ready for use.
Routine Maintenance Removing the Cold Trap NOTE: Always have one or two spare traps on hand in case of breakage before proceeding. To remove the cold trap: 1. Disconnect the ATD/TD from the AC line power. Allow the system to cool. After the instrument has cooled, turn off the purge gas supply. 2. On the TD, open the front door. If you have an ATD, you need to remove the arm housing. See Removing and Replacing the Front Covers of the ATD on page 247. 3.
Routine Maintenance Metal Plate Figure 75 Location of Metal Plate 5. If the valve array bushing is installed, lift it off of the trap. It is not secured to the trap. 6. At the inlet of the trap, unscrew the nut holding the trap to the inlet fitting. 7. Remove the knurled nut and the knurled nut fittings from the trap. See the following figure.
Routine Maintenance Trap Nuts Knurled Nut Figure 76 Cold Trap Before shutting off both the air and carrier gas ensure that the GC oven and detector are cool. If the MS is used make sure that the GC-MS transfer line and the Ion Source are cool and the filament is off. CAUTION The heated valve, the tube oven, and the trap enclosure may be very hot. Allow 20 -30 minutes for these parts to cool. WARNING 8. Remove the Desorb line and slide it to the back. See the following figure.
Routine Maintenance Figure 77 Desorb Line 9. Remove the nuts from the left side of the trap using a 1/2 inch wrench. See the following figure.
Routine Maintenance 10. Carefully remove the o-ring from the trap by removing the nut and removing the brass ring. See the following figure. Brass Ring O-Ring Nut Figure 79 Trap O-Ring, Brass Ring and Nut 11. With the nut, brass ring and o-ring removed you can now carefully remove it. Slowly slide the cold trap out through the right side of the trap enclosure. The trap will slide past the opening toward the electrical connections.
Routine Maintenance CAUTION This tube is made from glass. The trap could fracture if it is bent or stressed. NOTE: If there is any sign of ice or water at the bottom of the trap enclosure, there is a problem with the dry air supply, which is used to purge the cold trap box of water. See Gas Supply Specifications on page 70 for dry air specifications. Replacing the Cold Trap Installing the cold trap is slightly more difficult than removing it.
Routine Maintenance 2. Also on the left side of the trap, reattach the brass nut and tighten. Brass Ring O-Ring Nut Figure 81 Trap O-Ring, Brass Ring and Nut 3. Put the Desorb line back into its proper position. Slide the Desorb tube into the trap. See the following figure. 4. Replace the knurled nut at the right end of the trap. Tighten by hand until snug. 5. Reattach the magazine and front panel to the instrument. 6.
Routine Maintenance Cold Trap Maintenance Conditioning the Trap NOTE: See Tube Conditioning and Figure 87, in the chapter Theory of Thermal Desorption of this User’s Guide. You may need to condition the trap if you have just installed a new trap or if you are encountering carry-over problems. In trap condition mode, a tube is not desorbed. The trap is heated to the trap high temperature for the duration of the trap hold time specified in the method.
Routine Maintenance When specifying a Trap Clean method in a sequence, the method must have a tube assigned to it. An empty tube is best suited for this method. To perform multiple Trap Clean steps at the beginning of a sequence, the Trap Heat method must be listed for a range of tubes. De-Icing the Cold Trap The dew point of the dry-air supply to the ATD/TD must be less than –50°C. If it isn’t, severe damage may occur to the trap or the Peltier cooler.
Routine Maintenance Repacking the Cold Trap NOTE: We highly recommend that you buy pre-packed traps unless you have experience in packing traps. There are 2 types of prepacked cold traps tubes. They are listed in the following table. Tube Type P/N Application Packed Cold Trap, Tenax MO41-3535 L427-5108 Air Monitoring Trap MO41-3628 Low-flow cold trap suitable for ozone precursor and air toxics monitoring.
Routine Maintenance 2. Using the cold trap packing tool (P/N L427-1203), remove the old packing. Insert the tool into the cold trap and gently push out the packing and glass wool. 3. To pack a narrow bore, low-flow cold trap tube, first place a glass filter disk into the empty trap tube. The low flow trap is standard on the TD and ATD.
Routine Maintenance glass filter disk (P/N L427-1290) can be used to separate the layers. It may be possible to separate the two adsorbents with a plug of glass wool, but this will reduce the volume of adsorbent that can be used. 7. It is normal not to use more than two adsorbents in the cold trap, but if more are required, continue packing as described above while making sure that added adsorbent is stronger than the previous one. 8. Insert another 5-mm plug of glass wool in the open end of the trap.
Routine Maintenance Under normal operating conditions, the filter disks do not require changing. However, they must be changed if the packing of the cold trap has been overheated or has moved, or if chromatographic problems have been observed (such as tailing peaks, sample loss or sample carryover). You must always replace filter disks when repacking the trap. To change the trap filter disks: CAUTION Always have a replacement trap available in case of breakage.
Routine Maintenance 5. At the inlet of the trap, disconnect the inlet fitting from the heated valve. 6. You should be able to remove the filter disk from the inlet fitting without removing the fitting from the heated valve. Use tweezers or forceps to remove the filter and replace it with a new one (L1003030,pk/10). Ensure that the filter disk is properly seated NOTE: Do not touch the filter disks with your fingers. They should only be removed from the bag when they are to be placed into the fittings.
Routine Maintenance 13. Connect the supply of purge air and carrier gas and begin purging the cold trap enclosure. Wait for 30 minutes before powering up the instrument. 14. You should run a trap conditioning cycle to remove any volatile impurities from the filter disks. Packing Sample Tubes There are three types of sample tubes. They are listed in the following table.
Routine Maintenance Stainless Steel Tubes In stainless steel sample tubes, the adsorbent bed is usually retained using stainless steel gauze disks. New stainless steel sample tubes already contain the initial retaining gauze disk at the front (grooved) end of the tube. Older tubes, which are being repacked, usually need to have this initial gauze disk placed in the correct position. To do this, we strongly recommend that you use the gauze-loading rig. See Gauze-Loading Accessory on page 286.
Routine Maintenance When tubes are packed with more than one adsorbent in series, the different beds of packing are usually separated with glass wool. Non-silanized glass wool is preferred. Gauze-Loading Accessory The gauze-loading accessory (P/N L407-0023) is a tool for inserting the retaining gauze disks into stainless steel sample tubes. Figure 83 shows a tube being positioned with downward pressure applied to the tube to depress the spring-loaded ball in the base.
Routine Maintenance 1. Slide a single disk into the mouth at the base of the barrel section of the tool until it drops into the tapered hole. NOTE: You must make certain that only a single gauze disk is inserted. Attempting to insert two disks stuck together will usually damage the plastic plunger. When viewed against a bright surface, two or more disks together will appear much darker than a single disk. 2. Press the plunger down slowly until the gauze reaches the required position, i.e.
Routine Maintenance conditioning stages until it is finally close to, or at, the maximum temperature limit for the packing material. Where possible, condition each freshly packed tube for approximately 1 hour before use, and ensure that the adsorbent has been taken to a higher temperature than that required for the analysis at least 25 degrees C. Use fast desorb flow rates, of at least 100 mL/min, during the tube conditioning process to speed up the removal of volatile contaminants.
Routine Maintenance 7. All other settings will be not be used while the ATD/TD is conditioning the tubes mode. 8. Save the tube conditioning method. Open the Tools menu and select Save As. Press the filename field to open the alphanumeric entry tab. Enter a name for the method and press OK. 9. Press OK to save the new method. Create a method for each set of conditioning parameters that you required. See Table 21. 10. Allow the ATD/TD to reach its temperature set points and then load a tube and press Start.
Routine Maintenance Once the packed tubes have been thoroughly conditioned in this way, subsequent conditioning runs (for example, after storage) would only require one 10-15 minute desorption at the maximum temperature of the packing. CAUTION When conditioning tubes that are packed with more than one adsorbent, do not exceed the maximum temperature of the least thermally stable material present. Storage and Lifetime of Packed Tubes Keep tubes capped and stored in a clean environment at all times.
Routine Maintenance once-a-week basis. Tubes packed with more stable materials, such as Chromosorb 102, Chromosorb 106, Tena and Spherocarb, should offer longer lifetimes. Cleaning the ATD Sample Tray If dirt is allowed to build up on the tray, the sample tubes may stick in the flutes and will not be loaded into the sampling position correctly. To prevent a build-up of contamination, only load clean sample tubes. Never use adhesive tape or any other type of adhesive materials on the tubes.
Routine Maintenance To replace fuses: 1. Ensure that the power cord is disconnected from the power entry module on the rear left side of the instrument. The fuse drawer is located in the top portion of this module. Refer to Figure 84. 2. Carefully pry the fuse door open with a flathead screwdriver. 3. Use the flathead screwdriver to slide out the fuse drawer. 4. Remove the blown fuse and replace it with a new one of the correct type and rating. Consult the fuse chart. Both fuses must have the same rating.
Routine Maintenance Fuses Fuse Drawer Power Switch Fuse Door AC Connector Line Cord Connector Figure 84 Replacing the Fuse 293
Routine Maintenance 294
Theory of Thermal Desorption 7
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Theory of Thermal Desorption Introduction Manual Pneumatics Two models of TurboMatrix Series offer the standard manual pneumatics. The TurboMatrix 100 TD offers a single tube thermal desorber with manual pneumatics. The TurboMatrix 150 ATD is an automated Thermal Desorber with manual pneumatics.
Theory of Thermal Desorption or decrease the carrier-gas pressure during trap desorption to improve desorption efficiency and give better recoveries and peak shapes. • Method sequencing allows the use of different flows and pressures in methods to enable different analyses to be performed in the same run and also to simplify method development and optimization.
Theory of Thermal Desorption Modes of Operation The ATD/TD has eight modes of operation: • 2-Stage Desorb • Desorb +Rec-Same Tube • Desorb + Rec-New Tube • Desorb+Condition • TRAP Clean • Trap Test • Tube Condition • Load ISTD on Tube The sequence of events for each mode is described in the following sections.
Theory of Thermal Desorption Outlet Split Vent Transfer Line to GC Inlet Split/ Tube Condition Vent SV5 Inlet Split Desorb Flow Vent SV4 Outlet Split SV3 Desorb Vent Valve A 1 Trap 4 2 3 Position B Sample Tube SV2 Carrier Supply A Carrier Pressure Supply PR Pressure Regulator Leak Pressure SV1 Desorb Supply Figure 86 Standby Configuration NOTE: SV is a solenoid valve, and PR is a pressure regulator in this section.
Theory of Thermal Desorption Trap Clean Mode In Trap Heat mode, a tube is not desorbed. SV2 connects A to B to supply carrier gas to the Trap-Transfer Line GC column. Only the cold trap is heated and a GC run is started for conditioning. Trap Heat mode can be used to condition the trap. Ensure there is an adequate flow of carrier gas through the trap before beginning a trap heat cycle.
Theory of Thermal Desorption Start of the Tube Conditioning Sequence—When the tube conditioning sequence is started, the carrier gas pressure is tested, the carousel moves to the first tube position and the system waits until the system is ready. The first sample tube is then loaded into the desorption position. Leak Testing, Purging and Conditioning a Sample Tube—After being placed in the desorption position, the tube is leak tested.
Theory of Thermal Desorption Cooling and Unloading the Tube—When the desorb time has elapsed, the oven is removed from the tube and solenoid valves SV1, SV3 and SV5 are closed. The sample tube cools for 2 minutes and then SV1 and SV5 opens for 15 seconds to depressurize it.
Theory of Thermal Desorption Upon finishing the leak test, SV1 and SV3 open and the sample tube is purged with carrier gas for the duration of the purge time. During the purge time, air is purged from the tube to reduce the risk of adsorbent oxidation during desorption. See Carrier Gas Purge of the Sample Tube on page 310. After the purge time has elapsed, the tube oven is brought into contact with the sample tube and the primary desorption begins.
Theory of Thermal Desorption Inlet Split function in the ATD/TD method. See Setting Sample Split Ratios on page 228 for details of inlet split operation. At the end of the desorb time, SV2 is switched to B, SV3 and SV5 are closed and the heated valve is rotated to Position B. Cooling and Unloading the Tube After Desorption—After desorption, the sample tube is allowed to cool for 2 minutes. SV3 and SV5 are opened for 15 seconds to depressurize the sample tube, which is then returned to the carousel.
Theory of Thermal Desorption If SV4 is open, it will remain open for the three minutes and switch with SV2. SV2 and SV4 (if selected) will switch three minutes after the last tube heat. If there are further desorptions, SV1 and SV2 switch to prevent the carrier gas from entering the trap, but SV4 remains open, if outlet split is enabled in the method.
Theory of Thermal Desorption desorbing the subsequent tube at a period of time prior to the GC becoming ready for injection. This period of time is equal to the total time required for the tube to be loaded, leak tested and desorbed. When the GC becomes ready for the next injection, the ATD/TD is ready to desorb the cold trap and start the next GC analysis.
Theory of Thermal Desorption Outlet Split Vent Transfer Line to GC Inlet Split/ Tube Condition Vent SV5 Inlet Split Desorb Flow Vent SV4 Outlet Split SV3 Desorb Vent Valve A 1 Trap 4 2 3 Position B Sample Tube SV2 Carrier Supply A Carrier Pressure Supply PR Pressure Regulator Leak Pressure SV1 Desorb Supply Figure 90 Pressurize Sample Tube Primary and Secondary Leak Test of the Sample Tube If no large leaks are detected, SV1 is closed, sealing the tube part of the system.
Theory of Thermal Desorption Repeating the leak test enables the ATD/TD to distinguish between real and apparent leaks. Apparent leaks can be caused by: • a low gas flow setting for either the Desorb flow or the Inlet Split flow. The pressurization time of 5 seconds is insufficient to fully pressurize the entire system because of the flow restriction by the needle valves. During the leak test period, gas continues to flow through the needle valves, reducing the pressure in the sample tube.
Theory of Thermal Desorption The number of retries can be set to between zero and two (0-2); the default value is two (with two retries, a total of three tubes are leaktested). Carrier Gas Purge of the Sample Tube When the leak test has been completed, the ATD/TD again checks that all heated zones are at their set temperatures and that the GC is ready. SV1 and SV3 are then opened and air is purged from the sample tube prior to heating it for desorption.
Theory of Thermal Desorption Transfer Line To GC Inlet Split/ Tube Condition Vent SV5 Inlet Split Outlet Split Vent Desorb Flow Vent SV4 Outlet Split SV3 Desorb Vent 1 4 2 3 SV2 Carrier Supply Trap Valve A Position A Sample Tube A Carrier Pressure Pressure Regulator Leak Pressure SV1 Desorb Supply Supply Figure 91 Tube Purge When purging a tube prior to desorption under the tube or trap conditioning modes, the purge gas does not flow through the cold trap.
Theory of Thermal Desorption adsorbent to strong adsorbent. Any volatiles purged out of the weak adsorbent will land on the strong adsorbent (see the following figure for the addition of the ISV2 solution valve). For the strong adsorbent, in this analysis, a hydrophobic adsorbent should be chosen, which allows water to pass out to the desorb vent without losing the volatile compounds. Heated purge can be used to more efficiently perform the reverse dry purge.
Theory of Thermal Desorption Cold Trap Flow Configuration The ATD/TD is configured for backflush flow of the cold trap. During tube desorption, the sample analytes enter the cold trap from the left (flow from the heated valve to the desorb flow vent), as seen from the front of the instrument.
Theory of Thermal Desorption Single-Stage versus Two-Stage Desorption Single Stage (Non-PerkinElmer) If the volatiles extracted from the sample by thermal desorption are swept directly onto the analytical column of the GC, the process is known as single-stage desorption.
Theory of Thermal Desorption Two Stage Desorption (PerkinElmer ATD) Inlet Split (optional) Carrier Gas Inlet Outlet Split (optional) GC Detector Hot Sample Tube Capillary Cryofocusing Device GC Analytical Column Figure 94 Cryofocusing on Capillary Tubing Inlet Split (optional) Carrier Gas Inlet Outlet Split (optional) GC Detector Hot Sample Tube Cold Trap GC Analytical Column Figure 95 Trapping on a Packed Cold Trap (TD and ATD) Both of these procedures reduce the component bandwidths and impro
Theory of Thermal Desorption in the environmental field where samples frequently contain a significant amount of water. Packed cold traps can function with higher carrier gas flow rates than capillary cryofocusing devices. This facilitates the introduction of one or more split points into the sample flow path, which, in turn, allows independent control of the gas flows during primary desorption, secondary desorption and chromatographic analysis.
Theory of Thermal Desorption matrices that cannot be injected directly into a gas chromatograph. These include solids, emulsions and salt solutions, among others. Limitations of Thermal Desorption Techniques The ATD/TD has a highly inert flow path and covers a wide temperature range (-100°C to 400°C) and in doing so, can handle the widest possible range of thermal desorption applications. There are, however, some chemical compounds that are not suited for analysis by thermal desorption.
Theory of Thermal Desorption 318
Sampling Techniques 8
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Sampling Techniques Introduction Two general methods of sampling are used for ATD/TD analyses i.e. Trapping Volatiles from the Vapor Phase and Direct Sampling. With direct sampling methods you place a known quantity of the sample into the tube. Alternatively, you can trap volatiles on the tube. Various sampling methods are discussed in this chapter. For more detailed information you may want to obtain some of the listed reference material (see later in this chapter and in Appendix C).
Sampling Techniques Concentration of Vapors in Environment Surface Area controlled to ± 1% Exposed End of the Sample Tube Concentration Gradient Diffusion Distance Gauze Ring supporting the Adsorbent Zero Concentration of Vapors on Adsorbent Surface Adsorbent Sample Tube Figure 96 Principles of Diffusive Sampling Under these conditions, components will migrate to the adsorbent or reactive surface at a rate that is dependent upon: • the path length between the outer surface of the monitor and the a
Sampling Techniques Early badge-type diffusive sampler designs with relatively large cross-sectional areas (A) and shallow diffusion gaps (D) suffered from severe restrictions because of air speed effects at the surface of the badge. This meant that the stable conditions required for diffusion according to Fick’s law could never be established.
Sampling Techniques If the concentration is required in ppm, then the formula is modified to include the molecular weight of the compound of interest and the molar gas volume, as follows: UP = 60 x D1 x A x MW 24.45 x Z Equation 14 Where UP = Uptake rate in ng ppm-1 min-1 NOTE: 24.
Sampling Techniques If a 1 µL injection of standard solution is to be used, the concentration of the solution must be approximately 0.1% by volume. 1 µL of a 0.1% styrene solution contains 0.91 µg styrene. If 0.91 µg of styrene had been collected on a diffusive tube over 480 minutes, the atmospheric concentration would have been 0.948 ppm. Therefore, 0.948 (ppm) should be entered into the data handling system as the “calibration amount” and 480 (minutes) as the “sample amount”.
Sampling Techniques Alternatively, the uptake rate can be determined experimentally. One quick experiment that can be used either to determine approximate uptake rates or to confirm published data is as follows: 1. Monitor an atmosphere containing the component of interest, using at least 6 identical diffusion tubes. 2. Monitor the same atmosphere, in parallel, using an independent method, three pumped sample tubes, for example. 3.
Sampling Techniques Protocol for Assessing the Performance of a Diffusive Sampler A joint US National Institute of Occupational Safety and Health (NIOSH)/UK TDE protocol for evaluating diffusive monitors has been agreed upon by research workers in these two organizations and was presented at the American Industrial Hygiene Conference in May 1988.
Sampling Techniques placed over the front of the tube to reduce the ingress of particulate material if required. (P/N L407-0208) The flow rate range conventionally used for air sampling is between 10 and 200 mL/min, although 500 mL/min can be used for shortterm (10 minute) monitoring. Factors limiting flow rate selection include: • analyte diffusion occurs at a rate equivalent to an air flow of approximately 1 mL/min on PerkinElmer tubes.
Sampling Techniques following analysis parameters, you will be sampling for benzene: • Expected atmospheric concentration: 100 ppb • Typical sample volume of air collected is 12 liters • Molecular weight of benzene is 78 g/mole • 24 liters of benzene vapor at 20°C and standard atmospheric pressure weighs 78 g • 12 liters of air at 100 ppb concentration of benzene contain 3.
Sampling Techniques Molecular Height of the Component MW = 50 MW = 75 MW = 100 MW = 150 MW = 200 1000 ppm 20 mg 30 mg 40 mg 60 mg 80 mg 10 ppm 200 μg 300 μg 400 μg 600 μg 800 μg 1 ppm 20 μg 30 μg 40 μg 60 μg 80 μg 10 ppb 200 ng 300 ng 400 ng 600 ng 800 ng 1 ppb 20 ng 30 ng 40 ng 60 ng 80 ng 10 ppt 200 pg 300 pg 400 pg 600 pg 800 pg Atmospheric Concentration Table 25 Mass of Component Collected on a Sample Tube During Pumped Air Monitoring The data in Table 26
Sampling Techniques Atmospheric Concentration 1000 ppm Uptake Rate * ng ppm-1min-1* UP = 1.3 UP = 1.5 UP = 1.7 UP = 2.0 UP = 2.5 0.624 mg 0.72 mg 0.816 mg 0.96 mg 1.2 mg 10 ppm 6.24 μg 7.2 μg 8.16 μg 9.6 μg 12.0 μg 1 ppm 0.624 μg 0.72 μg 0.816 μg 0.96 μg 1.2 μg 100 ppb 62.4 ng 72.0 ng 81.6 ng 96.0 ng 120.0 ng 10 ppb 6.24 ng 7.2 ng 8.16 ng 9.6 ng 12.0 ng 1 ppb 0.624 ng 0.72 ng 0.816 ng 0.96 ng 1.2 ng * The uptake rate (UP) is specific to PerkinElmer tubes.
Sampling Techniques Probability of Result Occurring obtained from regular monitoring for individual analytes will vary considerably. 3.33 5.77 10 17.32 30 Air Concentration (log.) Figure 99 Probability of a Result Occurring versus Air Concentration Due to the wide spread of results expected, at least 10 results, preferably 20, are frequently required before a true average air concentration or exposure level can be established.
Sampling Techniques Probability of Result Occurring In fact, in many cases, the mean has to be around 1/3 of the limit before there is 95% confidence that the atmospheric concentration or personal exposure level taken on any day would not exceed the maximum. See insert cross-ref. In other words, at this mean concentration, 1 in 20 results is still likely to be higher than the limit level.
Sampling Techniques Purge and Trap One of the variations of vapor phase sampling is the purge and trap technique. In this method, an inert gas is used to sweep volatile components from solid or liquid matrices into the vapor phase. The components are then concentrated on the sampling tube or tubes.
Sampling Techniques Brass Cap Stainless Steel Sample Tube with Adsorbent Diffusion Cap Silicone Membrane Figure 102 Soil Probe GC Certified Standards on PerkinElmer Tubes Certified reference materials on PerkinElmer stainless steel sample tubes are available from the European Community Bureau of Reference (BCR). These standard tubes are produced for verifying thermal desorption calibration procedures.
Sampling Techniques Compound Analytical Result Calculated Result Benzene: (1.053 ± 0.014) 1.054 µg per tube Toluene: (1.125 ± 0.015) µg per tube 1.123 µg per tube m-Xylene: (1.043 ± 0.015) µg per tube 1.039 µg per tube Table 28 GC Certified Standards on PerkinElmer Tubes These analytical results were in agreement with the values calculated from the charging data, indicating that adsorption and desorption were quantitative. Standards are available from the BCR (CRM 112).
Sampling Techniques CAUTION Do not heat tubes containing PTFE inserts to temperatures greater than 225°C. These inserts are highly recommended for solid samples, such as drugs and foods such as spices, flour and coffee. In the case of solid, resinous or liquid samples, use a preliminary adsorbent bed in the tube when necessary. This will ensure that none of the matrix material or other high-boiling compounds migrate into the gas lines of the system.
Sampling Techniques CAUTION The use of a small adsorbent bed is highly desirable to prevent high-boiling components of the sample (e.g., resins) from getting into the ATD/TD plumbing. Contamination of the ATD/TD at high concentration levels can be very timeconsuming to remove.
Sampling Techniques NOTE: Complete recovery of analytes can be verified during method development by redesorbing the same sample to ensure that none of the components of interest remain. Calibration of the entire analytical system can be performed using a simple external standard procedure. Refer to Calibrating Thermal Desorption Systems on page 235 for the details.
Sampling Techniques If a 1 µL injection of standard solution is to be used, the concentration of the solution must be approximately 25% by volume. 1 µL of a 25% chloroform solution contains 375 µg chloroform. If 375 µg of chloroform had been desorbed from 20 mg of solid sample, the concentration in the sample would have been 1.875% by weight. Therefore, 1.875 (%) should be entered into the data handling system as the “calibration amount” and 20 (mg) as the “sample amount”.
Troubleshooting 9
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Troubleshooting Troubleshooting Instrument fault conditions and the necessary corrective action are listed in this chapter. In addition, basic troubleshooting procedures are provided for some problems that may occur during normal operation. If you have service related questions contact the PerkinElmer Service Department. When you call, you should be in front of your instrument. You should also have this manual at hand. Please have the following information ready: 1.
Troubleshooting Status Description Economy Mode The instrument is in the economy mode. The heaters have been switched off and the carrier gas flow has been reduced to the minimum. Fatal Error A fatal error is a malfunction from which the TD cannot recover without user intervention. See Fatal Errors on page 364 for details of the fatal error. In Split Adj Adjust the inlet split flow. SV1 and SV5 are open.
Troubleshooting Status Description Purging Tube The sample tube is being purged with carrier gas to remove any air from the tube. Ready The instrument is ready to begin an analysis. Returning Tube The sample tube is being returned to the carousel. Rev Dry Purge The TD or ATD is purging the sample tube in the reverse direction in which the tube was sampled. Fault A fault is occurring. Trap Cond Heat The instrument is in trap condition mode and the trap is being heated to the set point.
Troubleshooting Status Description ARM TO DECAPPER Contact your PerkinElmer Service Representative if you get this message. ARM TO DESORB Contact your PerkinElmer Service Representative if you get this message. ARM TO MAGAZINE Contact your PerkinElmer Service Representative if you get this message. ARM EXTEND Check the air pressure, check if there is a valve leak or failure, check for any mechanical obstructions.
Troubleshooting Status Description CLEAR TUBE Manually remove the tube. COULD NOT CAP TUBES Check that correct the caps are used and are not overtightened. COULD NOT CLOSE GRIPPER The pen clips are in the way, or the gripper air or Valve has failed. If you still get this message after doing these checks contact your PerkinElmer Service Representative. COULD NOT DECAP TUBES Check the Pen clip position, could also be overtightened caps, or the decapper alignment is off.
Troubleshooting Status Description DECAPPER CLOSE Check the air pressure, the valve could be leaking or failing, check for a mechanical obstruction. If you still get this message after doing these checks contact your PerkinElmer Service Representative. DECAPPER OPEN Check the air pressure, the valve could be leaking or failing, check for a mechanical obstruction. If you still get this message after doing these checks contact your PerkinElmer Service Representative.
Troubleshooting Status Description HEATER RATE FAIL ZONE 2 Contact your PerkinElmer Service Representative if you get this message. HEATER RATE FAIL ZONE 3 Contact your PerkinElmer Service Representative if you get this message. HEATER RATE FAIL ZONE 4 Contact your PerkinElmer Service Representative if you get this message. Contact your PerkinElmer Service Representative if you get this message. INITIALIZE FAILURE One of the elements cannot be initialized.
Troubleshooting Status Description OVEN FAIL AT IDLE POSITION Contact your PerkinElmer Service Representative if you get this message. OVEN FAIL AT TUBE POSTION Check if there is low air, check if there is a leaking valve, check if the pen clip is in the way, check that the oven sensor is in alignment. If you still get this message after doing these checks contact your PerkinElmer Service Representative. OVEN UNLOAD RECOVERY Contact your PerkinElmer Service Representative if you get this message.
Troubleshooting Status Description SEALER MID POSITION Contact your PerkinElmer Service Representative if you get this message. SEALER DOWN Contact your PerkinElmer Service Representative if you get this message. SEALER UP Contact your PerkinElmer Service Representative if you get this message. SHOP AIR The shop air pressure is too low (90psi), and the sensor failed. Adjust the pressure. SERVICE ACCESS Contact your PerkinElmer Service Representative if you get this message.
Troubleshooting Status Description TUBE UNLOAD FAILURE Check if “Power OFF” caused the tube to slip in the arm jaws, preventing recapping. If you still get this message after doing this check contact your PerkinElmer Service Representative. TUBES WILL OVERLAP! Check tube numbers in the Methods. USER MUST CLEAR CAPS Following the “power out” you must manually remove the dropped caps. USER MUST CLEAR TUBE/ CAPS! Following the “power out” you must manually remove the dropped Caps/Tube.
Troubleshooting before switching off the ATD. Tube deviations are cleared when the next run is started. CAUTION You must ensure that tubes and caps are removed from the current tube position before resetting the TD. Failure to do so may result in damage to the TD. Disconnect the power cord and then remove the tubes and caps. Use caution when removing tubes and caps. Fault: Pneumatic Psi Too Low Cause: The demand for dry air has exceeded the supply.
Troubleshooting Fault: Carousel Motor Stalled Cause: An obstruction has caused the carousel to halt rotation. Action: Turn the ATD off and disconnect the power cord from the AC mains. Remove the obstruction and reconnect the line cord. Turn on the ATD. The instrument will initialize the motors. It will then return a Ready status if all of its systems have been initialized correctly.
Troubleshooting Cause: The sensor, for the heated transfer line, in zone 3 has failed. Action: Turn the ATD/TD off and disconnect the power cord from the AC mains. Ensure the electrical connector from the transfer line is securely connected to the motherboard. See Installation at the ATD/TD on page 57. Turn on the TD or ATD to see if the fault has cleared. Action: Contact your PerkinElmer service engineer. Cause: The sensor, for the trap, in zone 4 has failed.
Troubleshooting the gripper arm has dropped a tube. Action: Turn the ATD off and disconnect the power cord from the AC mains. Remove the case as outlined in Removing and Replacing the Front Covers of the ATD on page 247 and locate the missing tube and caps. Turn on the ATD. Fault: No Tubes in First-Last Cause: The first and/or last tubes from the specified range have not been placed on the carousel. Action: Press Stop and rotate the carousel to gain access to the tube location and insert a sample tube.
Troubleshooting and clean the outside of the tube. Ensure there is no adhesive material or residual sample on the outside of the tube before inserting it into the carousel. Touch the Tools button, press Reset in the menu and answer Yes to the pop-up question. The instrument will reset itself and clear the fault. Press the Start button on the display to start the analyses. Action: Do not use tubes that are not specifically identified for use with an automated thermal desorber.
Troubleshooting Action: Ensure nothing is touching the carousel. Action: Ensure all of your tubes have been installed correctly. If pen clips are installed on sample tubes, the tube must be inserted into the carousel with the pen clip facing in, toward the center of the carousel. Cause: The carousel has not been installed correctly. Action: Contact your PerkinElmer service engineer. Fault: Arm Fail at Carousel Position, Decap Position, or Desorb Position Cause: Mechanical problem has occurred.
Troubleshooting details. Cause: The carousel has not been aligned correctly. Action: Contact your PerkinElmer service engineer. Fault: Could Not Retract Arm Cause: The tube cannot get free of the mobile seal. Action: Turn the ATD off and disconnect the power cord from the AC mains. Remove the front covers as outlined in Removing and Replacing the Front Covers of the ATD on page 247. Slide the tube out of the gripper. Remove the caps from the decapping mechanism.
Troubleshooting Re-orient the tube on the carousel. Touch the Tools button, press Reset in the menu and answer Yes to the pop-up question.The instrument will reset itself and clear the fault. Press the Start button on the display to start the analyses. Cause: If there has been a power failure, it is possible that the gripper arm is still holding a tube. Action: Turn the ATD off and disconnect the power cord from the AC mains. Slide the tube out of the gripper.
Troubleshooting Remove the case as outlined in Removing and Replacing the Front Covers of the ATD on page 247. Locate the caps and slide the tube out of the gripper. Replace the case and power up the ATD. Fault: Could Not Decap Tubes Cause: The storage caps could not be removed from the sample tube. Action: Replace brass ¼” Swagelok caps with press fit caps when you are using the ATD. The ATD cannot decap tubes containing the threaded Swagelok caps.
Troubleshooting must be inserted into the carousel with the pen clip facing in, toward the center of the carousel. Re-orient the tube on the carousel. Touch the Tools button, press Reset in the menu and answer Yes to the pop-up question. The instrument will reset itself and clear the fault. Press the Start button on the display to start the analyses. Fault: Oven Fail at Idle Position Cause: A mechanical problem has occurred. Action: Contact your PerkinElmer service engineer.
Troubleshooting Cause: There is a leak at Valco Valve A. Action: Contact your PerkinElmer service engineer. Fault: Trap Failed Leak Test!! Cause: The trap is cracked. Action: Replace the cold trap as outlined in Removing and Replacing the Cold Trap on page 269 or contact your PerkinElmer service engineer. Cause: The trap has not been installed correctly. Action: You must ensure that the trap is aligned correctly before tightening the end fittings.
Troubleshooting Fault: Valco-A, B, C or D Valve Failed Cause: A Valco valve cannot be initialized. Valco valve A is the heated valve used for normal operation. Valve D is the internal standard valve. Valves B and C are components of the online accessory. Action: Contact your PerkinElmer service engineer. Fatal Errors NOTE: Fatal errors and tube deviations are cleared when the ATD/TD is switched off. Record the details of the fatal error and tube deviations before switching off the TD.
Troubleshooting cannot be cleared by switching the ATD off and then on again, contact your PerkinElmer service engineer. If you have encountered a tube or trap leak and fault, the TD or ATD will attempt to test three tubes. If three consecutive tubes fail at either the tube or the trap, then a fatal error is generated. Refer to the troubleshooting instructions in Instrument Fault Conditions on page 352.
Troubleshooting should be replaced as described in Installing the Heated Transfer Line on page 51. Cause: A poor connection between the transfer line and the analytical column can also cause peak broadening. Action: Ensure that the connecting ends of the column and the transfer line are cut cleanly using a fused silica cutting tool. Action: The union or connector assembly should be an inert, zero dead-volume fitting recommended for butt connecting capillary, fused silica tubing.
Troubleshooting trap filter disk, leading to poor recovery and peak shapes as well as peak splitting. Action: Replace the filter disks. See Changing the Trap Filter Disks on page 281. The Cold Trap Does Not Cool Cause: The Peltier coolers have failed. Action: Switch off the ATD/TD and contact your PerkinElmer service engineer. Cause: This effect is more likely to occur when a high thermal conductivity carrier gas, such as helium or hydrogen is used.
Troubleshooting Cause: There is ice forming on the cold trap. Action: De-ice the trap as outlined in De-Icing the Cold Trap on page 278. Ensure that the dry air and the carrier gas have a dew point of -50°C or lower. Cause: There is insufficient air flow through the instrument. Action: Make certain that the fan at the rear of the instrument is not blocked and that there is sufficient space at the rear of the ATD/TD to allow for proper air circulation.
Troubleshooting pen clips are installed on your tubes, the tube must be inserted into the carousel with the pen clip facing in, toward the center of the carousel. Cause: The sample is blocking the flow of carrier gas through the sample tube. Action: When analyzing solid or resinous materials, ensure that the carrier gas flows can still pass through the sample tube and that the sample is not completely blocking the flow path. Cause: The sample tube is not packed properly.
Troubleshooting matrix is not escaping from the tube or trap and migrating into the rest of the system. Use glass wool plugs in the tubes and trap, ensure that the filter disks at both ends of the trap are installed correctly. The trap packing material must be packed sufficiently well so that it does not shift back and forth when the flow direction changes. Cause: Contaminated filters Action: This is probably the most frequent cause of “carryover”.
Troubleshooting this is the source of the problem, proceed as follows: 1. Desorb a clean blank tube for two minutes, then desorb the cold trap and monitor the resultant chromatogram. 2. Extend the primary desorption time to 5 minutes and repeat the experiment. 3. Continue to extend the desorption time in this manner to determine whether the contamination increases with the time that the trap is exposed to the gas flow. 4.
Troubleshooting diffuse back into the system if the filters become overloaded. Action: The inlet and outlet split and desorb charcoal filters must be replaced periodically, especially if large amounts of solvent are split from the sample. Contact your PerkinElmer service engineer. Cause: Contamination is coming from the cold trap. Action: If the contamination appears to be coming from the cold trap itself, i.e.
Troubleshooting or trap into the gas lines of the system. For sample tubes, this involves routinely ensuring that the retaining gauze disks for the packing are in place, and not using a mesh adsorbent that is too fine. Use 60-80 mesh minimum size. 80-100 mesh is too fine. In the case of solid, resinous or liquid samples, using a small adsorbent bed inside the tube is highly desirable to prevent highboiling components of the sample (e.g., resins) from getting into the ATD/TD plumbing.
Troubleshooting The following conditions are particularly important: • • • • • • at least 10 mL/min flow is passing through the tube during primary desorption at least 1.
Troubleshooting of adsorbent for your application. Lastly, the tube must be packed so that the sample is retained only where the tube oven contacts the tube. See Packing Sample Tubes on page 284 for details. Action: If you are working with solid or resinous materials, ensure that the sample is placed in the center of the sample tube, and not within 1.5 cm of either end of the tube. The tube oven only has contact with the central portion (~6 cm) of the tube.
Troubleshooting Discrimination of Compounds Over a Wide Boiling Range Cause: The packing material contained in the trap or in the sample tube is not suitable for the application. Action: Ensure that the trap packing selected will quantitatively retain and desorb all the components of interest. If no one adsorbent can cover the entire analyte volatility range, use a series of two or more adsorbents.
Troubleshooting Action: To test for this, re-desorb the tube and check for carryover. Cause: High-boiling compounds are condensing somewhere along the flow path. Action: Verify that the temperature of the flow path is sufficiently high to prevent condensation of high-boiling compounds. Use only deactivated, uncoated fused silica in the transfer line.
Troubleshooting 378
Appendices 10
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Appendices Appendix A Customer Service Contact PerkinElmer for columns, supplies, accessories, and replacement parts. PerkinElmer offers a full selection of high-quality chromatography data handling products and gas chromatography supplies and columns through the PerkinElmer Xpress Catalog. The PerkinElmer Virtual Store is an exciting addition to the analytical instruments suite of interactive resources. The Virtual Store is easy to use and provides an electronic catalog with detailed product descriptions.
Appendices Appendix B Warranty Exclusions and Limitations The following consumable items are excluded from your instrument warranty agreement: • Fused Silica Transfer Line • Cold Trap Quartz Tube • Ferrules • O-rings • Filter Disks • Fuses WARNING Any attempts to perform installation or maintenance operations that are not detailed in this manual are at the user’s own risk.
Appendices Appendix C References Thermal Desorption Application Notes The listed titles can be ordered from PerkinElmer. Please contact your local PerkinElmer representative or order directly from the PerkinElmer web site at http://www.Perkin- Elmer.com A Review of Some Studies in Sampling and Thermal Desorption Carried Out at the British Petroleum Research Center, Sunbury-onThames, ..........................................................................
Appendices A Method for the Determination of Personal Exposure to Atmospheric Nitrous Oxide .................................................TDA-17 Determination of Solvents in Drugs Using the ATD 50 ......TDA-18 The Determination of High Levels of THF in a Drug Precursor Using the Model ATD 50 ....................................TDA-19 The Determination of Residual Freon 11 in Dried Vegetable Matter Using the ATD 50 ....................................................
Appendices Flavor and Fragrance Profiling by Thermal Desorption/Gas Chromatography.................................................................. TDA-32 An Overview of Sampling Strategies for Organic Pollutants in Ambient Air......................................................................... TDA-33 Field Preparation and Stabilization of VOCs of Water Samples....... .............................................................................................
Appendices International Standard Methods Relating to VOC Air Monitoring using Thermal Desorption ............................... GCA-77 Bibliography of Published or Presented Papers................. GCA-74 Model TD Precision Data ......................................................TDD-5 Model TD Inertness Studies ..................................................TDD-6 Calibrating Thermal Desorption Systems..............................TDD-9 A Guide to Adsorbent Selection ................................
Appendices TD Installation Requirements - A pre-installation laboratory check list................................................................................L-1904 TD Control Software, Product Description.........................GCA-88 The Sequential Tube Sampler (Model STS 25) for Air Pollution Profiling .............................................................. L-1570B On-line Monitoring of Ozone Precursors in Ambient Air Leaflet ..................................................................
Appendices Appendix D Carrier Gas Pressures The flow rates listed below are approximations only. In order to accurately determine the column flow rate you must connect a flow meter to the column outlet and measure the flow during standby and during secondary desorption. Record these value for future calculations. Helium Flow Rates Helium Flow Rates (mL/min) Column Diameter: 0.22 mm Optimum Flow: 0.63 ml/min Inlet Pressure 2 psi 5 psi 10 psi 16 psi 20 psi 25 psi 30 psi 60 psi 100 psi 10 m 0.
Appendices Helium Flow Rates (mL/min) Column Diameter: 0.25 mm Optimum Flow: 0.72 ml/min Inlet Pressure 2 psi 5 psi 10 psi 16 psi 20 psi 25 psi 30 psi 60 psi 100 psi 10 m 0.43 1.19 2.73 4.61 6.84 9.41 12.33 37.12 89.54 12 m 0.36 0.99 2.27 3.84 5.70 7.84 10.27 30.93 74.62 15 m 0.29 0.79 1.82 3.07 4.56 6.27 8.22 24.74 59.69 25 m 0.17 0.48 1.09 1.94 2.73 3.76 4.93 14.85 35.82 50 m 0.09 0.24 0.55 0.92 1.37 1.88 2.47 7.42 17.91 100 m 0.04 0.12 0.
Appendices Helium Flow Rates (mL/min) Column Diameter: 0.53 mm Optimum Flow: 1.79 ml/min Inlet Pressure 2 psi 5 psi 10 psi 16 psi 20 psi 25 psi 30 psi 60 psi 100 psi 10 m 8.78 24.04 55.06 93.08 138.08 190.07 249.06 749.72 12 m 7.31 20.03 45.89 77.56 115.07 158.40 207.55 624.77 15 m 5.85 16.02 36.71 62.05 92.05 126.72 166.04 499.81 25 m 3.51 9.61 22.03 37.23 55.23 76.03 99.62 299.89 723.46 50 m 1.76 4.81 11.01 18.62 27.62 38.01 49.81 149.94 361.
Appendices Hydrogen Flow Rates (mL/min) Column Diameter: 0.25 mm Optimum Flow: 1.25 ml/min Inlet Pressure 2 psi 5 psi 10 psi 16 psi 20 psi 25 psi 30 psi 60 psi 100 psi 10 m 0.97 2.67 6.11 10.33 15.32 21.09 27.64 83.19 200.69 12 m 0.81 2.22 5.09 8.61 12.77 17.58 23.03 69.32 167.24 15 m 0.65 1.78 4.07 6.89 10.21 14.06 18.42 55.46 133.79 25 m 0.39 1.07 2.44 4.13 6.13 8.44 11.05 33.28 80.28 50 m 0.19 0.53 1.22 2.07 3.06 4.22 5.53 16.64 40.14 100 m 0.
Appendices Hydrogen Flow Rates (mL/min) Column Diameter: 0.53 mm Optimum Flow: 2.97 ml/min Inlet Pressure 2 psi 5 psi 10 psi 16 psi 20 psi 25 psi 30 psi 60 psi 100 psi 10 m 19.67 53.88 123.42 208.62 309.49 426.03 558.23 12 m 16.39 44.90 102.85 173.85 257.91 355.02 465.19 15 m 13.11 35.92 82.28 139.08 206.33 284.02 372.15 25 m 7.87 21.55 49.37 83.45 123.80 170.41 223.29 672.16 50 m 3.93 10.78 24.68 41.72 61.90 85.21 111.65 336.08 810.78 100 m 1.97 5.
Appendices Nitrogen Flow Rates (mL/min) Column Diameter: 0.25 mmOptimum Flow: 0.37 ml/min Inlet Pressure 2 psi 5 psi 10 psi 16 psi 20 psi 25 psi 30 psi 60 psi 100 psi 10 m 0.48 1.33 3.04 5.13 7.62 10.49 13.74 41-36 99.77 12 m 0.40 1.10 2.53 4.28 6.35 8.74 11.45 34.46 83.14 15 m 0.32 0.88 2.02 3.42 5.08 6.99 9.16 27.57 66.51 25 m 0.19 0.53 1.21 2.05 3.05 4.19 5.50 16.54 39.91 50 m 0.10 0.27 0.61 1.03 1.52 2.10 2.75 8.27 19.95 100 m 0.05 0.13 0.
Nitrogen Flow Rates (mL/min) Column Diameter: 0.53 mm Optimum Flow: 0.79 ml/min Inlet 2 psi 5 psi 10 psi 16 psi 20 psi 25 psi 30 psi 60 psi 10 m 9.78 26.78 61.36 103.71 153.86 211.80 277.52 835.40 12 m 8.15 22.32 51.13 86.43 128.22 176.50 231.27 696.17 15 m 6.52 17.86 40.90 69.14 102.57 141.20 185.01 556.93 25 m 3.91 10.71 24.54 41.49 61.54 84.72 111.01 334.16 806.14 50 m 1.96 5.36 12.27 20.74 30.77 42.36 55.50 167.08 403.07 100 m 0.98 2.68 6.
Index A AC Line Connections 40 Accessory 200 BCD Kit 186 Caps 186 Gauze-Loading 286 Internal Standard 104, 145, 191, 213 Liquid Nitrogen (LN2) 189 STS-25 199 Tubes 186 Accuracy, Improved 310 ACGIH 25 Activate Method 114, 158 Adjust Desorb Flow 78 Flows Command 160 In Split Command 78 Adsorbent Cold Trap 279 Determining Strength 222 for Solid Samples 338, 373 Handling 279 Particle Size 284 Selection For Vapor Phase Sampling 218 Storage 245 Strength 280 Tenax 227 Air Monitoring Workplace 316 Toxics Tube 289
Index 290 B Backflush Configuration 281 Baud Rate 124, 172 BCD Data Logic 185 Bend Dimensions of Transfer Line 56 Benzene, Sampling 328 Binary Coded Decimals (BCD) 185 Brass Regulator 73 Breakthrough 219, 328 Broadening, Peaks 365 Brochures, Leaflets and Specifications 386 Bushing Valve Array 216 358 Loading 125, 173 Motor Stalled Fault 354 Orientation of Pen Clips C Cable HP6890 Ready/Start 49 Ready/Start 47 Calculator 115, 158 Calibration Data Handling System 238 Injecting Sample Directly onto Tube 2
Index From Sample Tube 368 From the Trap 369 Other Sources 369 Charcoal Contamination of Filters 371 Sorbent 221 Checklist Installation 33 Pre-Installation 33 Chemical Analyte Mass 329 Diffusive Sampling 321 MSDS 24 Pumped Sampling 327 Safety Information 24 Chloroform, Sampling 339 Chromatography Broadening or Splitting 365 Chromosorb Chromosorb 102 220 Chromosorb 106 220 Conditioning 289 Cleanliness Laboratory 245 Mass Spectrometer 246 Cold Trap Advantages 315 Backflush Configuration 281, 313 Changing F
Index Compliance EMC Directives 23 FCC 23 Compounds Safety Information 24 Sampling Emulsions, Liquids 337 Sampling Resins, Ointments 338 Sampling Solids 338 Suitable for Tenax (Diffusive Sampling) 225 Wide Boiling Range 376 Compressed Gases 25 Conditioning Air Toxics Tube 289 Chromosorb 106 289 Cold Trap 277, 301 Sample Tube 149, 287, Column 61 Carrier Gas 71 Dry Air 71 Fused Silica 63 Constant Flow Injection Mode 154 Consumables 87 Contamination Carrier Gas 370 Charcoal Filters 371 Cold Trap 372 Filter
Index Flow for Secondary Desorption 207 Flow Rate Pneumatics Tab 109, 154 Setting Flow Rates 78 Time 100, 140, 206, 211 Desorb Flow Rate 151 Desorption Incomplete 373 Overlapping Tube 306 Two-Stage 150, 303 Dew Point, Dry Air 71, 278 Dewar Flask 28, 70 Diffusion Monitoring Adsorbents 326 Applications 326 Compounds for Tenax 225 Example, Styrene 325 Fick's First Law 322 Tube-Type Monitor 323 Uptake Rate 324 Uptake Rates 325 Diffusive Monitoring Sample Tube 326 Sampler Assessment 327 Theory 321, 327 Dimensi
Index No Tubes in First-Last 356 Oven Fail at Cool Position 362 Oven Fail at Idle Position 362 Oven Fail at Tube Position 361 Robot Arm 354 Sealer Fail at Mid Position 362 Sealer Failed to go Down 362 Sealer Failed to go Up 362 Sensor Failure 354 Trap Failed Leak Test 363 Tube Failed Leak Test 362 Tube Missing 355 User Must Clear Caps 363 User Must Clear Tubes 363 Valco Valve Failed 364 Vial Load Failure 356 Vial Unload Failure 357 FCC Notice 23 Ferrules ATD Mobile Seal 253 Graphite 216 High Temperatu
Index Setting Column Head Pressure 78 Gauze Loading Accessory 286 Retaining Disk 285 GC Cycle Time 102, 141 GC Temp Calib 258 Glass Fiber Filters 219 Lined Stainless Steel Tubes 186 Tubes 186 Wool Plugs 280 GLP Tracking 125, 173 Graphite Ferrules 216 Gripper Could Not Close Fault 359 Could Not Open Fault 360 Guard Plate 57 H Handshake Mode 124, 172 Heat Rate 98, 138, 209 Heated Purge 214, 311 Purge Temperature 120 Heated Valve Maximum Temperature 122, 170 Rotor 210 Temperature 98, 138, 210 High Backgrou
Index GC 47 TD/ATD to HP6890 GC 49 Transfer Line 51 Tubing Requirements 71 Instrument Contamination 370 Dimensions 37 Fault Conditions 352 Input Signals 46 Layout 88 Manual 16 Operation 85 Output Signals 43 Safety Information 20 Shutdown 131, 178 Standby Configuration 300 Status Messages 343 Storage 36 Symbols Used for Safety 20 Unpacking 17 Weight 37 Weight Specifications 37 Integrity Testing 166 Interface Ready/Start Cable 47 Touch Screen 91 Interference Earth Loops 40 Internal Standard Description 191 E
Index Log Out Command 158 Report 111, 155 Tab 110, 154 Log Out 115 Loss of Sample 373 Low Temperature For Cold Trap 209 Method Development 205 Analysis Parameters 205 Analytical Objectives 205 Cold Trap Packing 227 Optimizing Primary (Tube) Desorption 206 Optimizing Secondary (Trap) Desorption 207 M Maintenance Alarm 120 Changing O-Ring Seals 249 Cleaning the Carousel 291 Cold Trap 269, 277 Trap 277 Manual Introduction 16 Other Reference Material 17 Mass of Analyte 329 Maximum Trap Temperature 122, 170
Index In this Manual 16 Number of Injections 105, 146, 213 O Ointments, Sampling 338 Open Command 113, 157 Open Loop Purging 334 Operation 85 Double Split 232 Environment 35 Modes 107, 148, 215 Multiple Method 94, 118, 130, 134, 163, 177 Pre-selected Single Method 118, 163 Single Method 93, 118, 129, 133, 163, 176 Single Split 230 Starting ATD 128, 129, 175, 176 Warnings and Safety Practices 20 Optimizing Primary (Tube) Desorption 206 Secondary (Trap) Desorption 207 Options Board 183 Heated Purge 120,
Index Peaks 365 Peltier Coolers De-Icing 278 Have Failed 367 Heat Rate 209 Pen Clips ATD Orientation 125, 173 Marking 125, 174 Removing 125, 174 TD Orientation 127, 175 PerkinElmer Customer Service 381 Essentials Catalog 381 Virtual Store 381 Pneumatic Connections 71 Options 110 Standby Configuration 300 Tab 109, 151 Pneumatics checking 260 manual 297 Programmable Pneumatic Control (PPC) 297 Pollution Degree 36 Poor Recovery 373 Porapak 220 Port Auxiliary RS-232 125, 173 Carrier Gas Inlet 73 Dry Air In 74
Index Purge Time 100, 140 359 Fail Fault 358 Gripper Could Not Open R Rate, Heat 98, 138, 209 Ready In Signal 46 Out Signal 43 Ready/Start Cable Assembly 47 HP6890 Cable Assembly 49 Redesorbing 339 Reference Material 17 Brochures, Leaflets and Specifications 386 Data Sheets 385 Regulator Carrier Gas 73 Dry Air 73 Gas Connections 71 Inline Flame Arrestor (H2) 71 Safety Practices 26 Relays 103 Rating 47 Timed Event 47 Replacing Mobile Seal Ferrule 253 Replacing the Cold Trap 275 Report Log 111, 155 Requ
Index Sample Tube 206 Assembling 186 Blocked 374 Breakthrough 328 Cleanliness 246 Conditioning 287 Conditioning Mode 149, 301 Contamination 371 Diffusion Monitoring 326 Glass 285 Glass-Lined Stainless Steel 285 Incomplete Desorption 368 Inserting Gauze Disk 286 Leak Testing 308 Loading ATD 125, 173 Loading TD 127, 174 Marking 125, 173 Not Heated Uniformly 368, 374 Packing 284 Pen Clips 125, 173 Pressurization 307 Primary Desorption 304 PTFE Inserts 336 Purging 303, 310 Replacement 186 Safety Information
Index Contacting 381 Customer 381 Setting Analysis Options 103, 144 Analysis Temperatures 97, 136 Analysis Times 99, 139 Carrier Gas Flow Rates 77 Date 125, 173 Desorb Flow Rate 78 GC Column Head Pressure 78 Outlet Split Flow 80 Time 125, 173 Setup Tab 120, 168 Shutdown 131, 178 Signal Fail 44 Inject 43 Ready In 46 Ready Out 43 Start In 46 Stop In 46 Single Method Operation 93, 118, 129, 133, 163, 176 Single Method Operation 93, 133 ATD 129, 176 TD 128, 175 Single Tube 105, 146 Soil Probes 334 Solid, A
Index Instrument 20 System Parameters Carrier Gas Flow Rates 216 Temperature 208 Timing 210 System Setup 132, 136 T Tab Connect 124, 172 Log 110, 154 Options 103, 144 Oven 110, 154 Pneumatics 109, 151 Preferences 117, 162 Run 93, 133 Setup 120, 168 Status 96, 136 TD Layout 88 Loading Tubes 127, 174 Shutdown 131, 178 Temperature Actual Value 98, 138 Analysis 97, 136, 208 Cold Trap 97, 137, 209 Column 98, 138 Extreme 27 Heated Purge 120 Heated Valve 98, 138, 210 High For Cold Trap 210 Laboratory 35 Low For
Index Calculator 115, 158 Exit Method Editor 114, 158 Log Out 158 Reset Command 115 Tools Menu maintenance options 160 Touch Screen Brightness 124, 172 Interface 91 Language Options 124, 172 Options Tab 103, 144 Run Tab 93, 133 Status Tab 96, 136 Transfer Line Bend Dimensions 56 Connecting to Packed Columns 66 Direct Connection 51 Fused Silica 57 Installation 51 Installation at Rear of the GC 53 Installation at the TD or ATD 57 Installation at Top of GC 64 Installation Through GC Injector 55 Temperature 9
Index Oven Temperature 97, 137 Overlapping Desorption 306 Packing 284 Pen Clips 125, 173 Pneumatics Tab 110 Primary Desorption 304 PTFE Inserts 336 Purging 303, 310 Range 93, 94, 133, 134 Replacement 186, 188 Secondary Desorption 305 Stainless Steel 285 Storage/Lifetime 290 Uptake Rates 325 User Must Clear 363 Tube Alarm Option 122, 170 Tube and Trap Impedance Test TurboMatrix 650 262 Tube Calibration TurboMatrix 650 ATD 262 Tube Condition 149 Tube Sampler (STS 25) 199 TurboMatrix Series 85 Two Stage Deso
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