MicroJet Cryo-Trap MODEL MJT-1030Ex OPERATION MANUAL

Transcription

1 MicroJet Cryo-Trap MODEL MJT-1030Ex OPERATION MANUAL

2 BEFORE USING THIS DEVICE Thank you for purchasing our MicroJet Cryo-Trap (MJT-1030Ex). We advise you to read this operation manual carefully before attempting to use this device in order to fully exploit the capabilities of this device. This manual contains descriptions on installation, operation, performance tests, and troubleshooting. We recommend that you make handy the operation manuals of your gas chromatograph, Pyrolyzer and/or Micro Reactor, when using this device. PRODUCT WARRANTY Frontier Laboratories Ltd. warrants this product against defects or failures in accordance with the warranty terms and conditions stipulated in a separate sheet. The product warranty can also be downloaded from our website. ABOUT PRODUCT SUPPORT PERIOD We will stock consumable and maintenance parts and will accept inspection and repair orders seven years from the date of product sales termination. However, in the event where electronic parts supplied from parts manufacturers are discontinued; thus our stock level becomes too low, we may not be able to provide support even within seven years from the date of product sales termination,. FOR YOUR SAFETY To use this product safely and properly, be sure to read the safety precautions and warnings before attempting to operate. If this product is used in a manner not instructed in this manual, the protective functions of this product may not be activated. Frontier Laboratories Ltd. will not be responsible for losses incurred due to the neglect of these precautions and warnings.! WARNING This hazard signs indicates that incorrect handling may cause hazardous conditions, resulting in death or severe personal injury.! CAUTION This sign indicates that incorrect handling may cause hazardous conditions resulting in minor or moderate personal injury and physical damage.! Note Other important handling information is placed in a frame like this. A-2

3 CONTENTS IN THE PACKAGE MJT-1030Ex Packing contents check list This product is including following items. We recommend that you first examine the contents of the package you have received. If the contents differ from the package list below, or some items are missing, contact your dealer immediately. A) Liquid N 2 Feed Tube F) Others E) Others C) Operation Manual H) Stand Base D) Flow Controller G) Liquid N2 Container 2L H) Stand Base A) contents: A1) MJ View from top (top layer) (middle layer) (bottom layer) Liquid Nitrogen Feed Tube Ex(1ea) B) contents: C) contents: D) contents: C1) PY D1) B1) MJ MS Trap Tube (1ea) B2) MJ Operation manual CD Installation guide Inspection report H) contents: H1) MJ Flow Controller (1unit) G) contents: G1) MJ Stand Pole (KD pole with a washer and a screw, 1set) * a part of Liquid Nitrogen Container Kit Stand Base (1ea) * a part of Liquid Nitrogen Container Kit Liquid N2 Container 2L (1ea) *a part of Liquid Nitrogen Container Kit E) contents: E1) E2) MJ E3) MJ E4) MJ AC Power Cable (1ea) 100V (Re-order: PY1-7001, 1ea) MJT Control Cable (1ea) MJT Signal Cable (1ea) Clamp (1ea) * a part of Liquid Nitrogen Container Kit E5) MJ E6) E7) MJ Indicator (1ea) * a part of Liquid Nitrogen Container Kit MicroJet Tube (2ea) (Re-order : MJ1-1111, 1ea) LN2 Saver (2ea) A-3

4 F) contents: Installation Kit [one of these kit(f1)] F1) MJ1-K580: MJT-1030E/Ex Installation Kit for HP5890 (1set) MJ MJ F1) MJ1-K680: MJT-1030E/Ex Installation Kit for Agilent6890/7890 (1set) MJ MJ Support Plate [with sems screw (M4 x 8) 4ea, MJT O-ring ( P-5) 4ea, 1set] Tube Hanger (1set) Support Plate [with sems screw (M4 x 8) 4ea, MJT O-ring ( P-5) 4ea, 1set] Tube Hanger (1set) F1) MJ1-K201: MJT-1030E/Ex Installation Kit for Shimadzu GC-17A/2010 (1set) MJ MJ F1) MJ1-K380 MJT-1030E/Ex Installation kit for Varian CP3800GC (1set) MJ MJ Support Plate [with sems screw (M4 x 12) 4ea, MJT O-ring ( P-5) 4ea, 1set] Tube Hanger (1set) Support Plate [with sems screw (M4 x 8) 4ea, MJT O-ring ( P-5) 4ea, 1set] Tube Hanger (1set) F1) MJ1-K801: MJT-1030E/Ex Installation Kit for PerkinElmer Clarus GC (1set) MJ MJ F1) MJ1-K901: MJT-1030E /Ex Installation kit for TRACE GC (1set) MJ MJ Support Plate [with sems screw (M4 x 8)4ea, MJT O-ring ( P-5) 4ea, 1set] Tube Hanger (1set) Support Plate [with sems screw (M4 x 8)4ea, MJT O-ring ( P-5) 4ea, 1set] Tube Hanger (1set) F1) MJ1-K903: MJT-1030E/Ex Installation Kit for Thermo TRACE 1300/1310GC (1set) MJ Support Plate [with sems screw (M4 x 8) 2ea, MJT O-ring ( P-5) 4ea, 1set] F2) MJ F3) MJ F4) MJ F5) MJ1-K300 MicroJet Tube Securing Kit (1set) Short Plug (1ea) Container Cap 2L (1ea) Thermal Exchange Coil 2L (1ea) MicroJet Tube Union Set (with a hexagon cap nut and a fixing nut, 1set) (Re-order : MJ1-3101) Graphite Ferrule (2pcs/pk) (Re-order: MJ1-7941, 5pcs/pk, 1set) A-4

5 MJT-1030Ex & PY-1030Ex-CHG (Change Option of Liq. N2 Container) Packing contents list MJT-1030Ex & PY-1030Ex-CHG (Change Option of Liq. N2 Container) Packing contents check list This product is including following items. We recommend that you first examine the contents of the package you have received. If the contents differ from the package list below, or some items are missing, contact your dealer immediately. A) Liquid N 2 Feed Tube F) Others E) Others B) Operation Manual C) Flow Controller View from top (top layer) (second layer) (third layer) (bottom layer) A) contents: B) contents: C) contents: A1) MJ B1) PY C1) Liquid Nitrogen Feed Tube (1ea) Operation manual CD Installation guide Inspection report Flow Controller (1unit) D) contents: D1) MJ MS Trap Tube (1ea) E1) E) contents: E2) MJ G) contents: G1) MJ Thermal Exchange Coil for 30L (1ea) *a part of Thermal Exchange Coil Set for 30L AC Power Cable (1ea) 100V (Re-order: PY1-7001, 1ea) MJT Control Cable (1ea) E3) MJ E4) E5) MJ MJT Signal Cable (1ea) MicroJet Tube (2ea) (Re-order : MJ1-1111, 1ea) LN2 Saver (2ea) A-5

6 F) contents: Installation Kit [one of these kit(f1)] MJ F1) MJ1-K680: MJT-1030E/Ex Installation Kit for Agilent6890/7890 (1set) MJ MJ Support Plate [with sems screw (M4 x 8) 4ea, MJT O-ring ( P-5) 4ea, 1set] F1) MJ1-K201: MJT-1030E/Ex Installation Kit for Shimadzu GC-17A/2010 (1set) MJ MJ Tube Hanger (1set) F1) MJ1-K380 MJT-1030E/Ex Installation kit for Varian CP3800GC (1set) MJ Tube Hanger (1set) Tube Hanger (1set) F1) MJ1-K801: MJT-1030E/Ex Installation Kit for PerkinElmer Clarus GC (1set) MJ MJ Tube Hanger (1set) F2) MJ F3) MJ1-K300 MicroJet Tube Securing Kit (1set) F4 )MJ Short Plug (1ea) MicroJet Tube Union Set (with a hexagon cap nut and a fixing nut, 1set) (Re-order : MJ1-3101) Graphite Ferrule (2pcs/pk) (Re-order: MJ1-7941, 5pcs/pk, 1set) Container Cap for 30 liters Container (1ea) *a part of Thermal Exchange Coil Set for 30L A-6

7 TABLE OF CONTENTS BEFORE USING THIS DEVICE A-2 PRODUCT WARRANTY TERMS AND CONDITIONS A-2 ABOUT PRODUCT SUPPORT PERIOD A-2 FOR YOUR SAFETY A-2 CONTENTS IN THE PACKAGE A-3 TABLE OF CONTENTS A-7 CHAPTER 1 ABOUT MICROJET CRYO-TRAP Overview of Product Principle Front and Rear Panels of Flow Controller 1-4 CHAPTER 2 SPECIFICATIONS 2-1 CHAPTER 3 INSTALLATION Getting Prepared for Installing MicroJet Cryo-Trap Attaching Liquid Nitrogen Feed Tube Securing Plate Installing Flow Controller Installing Liquid Nitrogen Feed Tube Attaching MicroJet Tube Connecting Tubes and Cables Checking and Calibrating Temperature Display Installing Stand Installing Column Inserting Thermal Exchange Coil to Liquid Nitrogen Container Un-plugging the liquid N2 feed tube from MJT control cable 3-20 CHAPTER 4 OPERATION Handling Thermal Exchange Coil Setting Nitrogen Pressure Manual Mode Operation Control from Temperature Controller of Pyrolyzer 4-2 CHAPTER 5 PERFORMANCE TESTS Testing Flow Rate Testing Cooling Temperature Testing Trapping Performance 5-1 CHAPTER 6 TROUBLESHOOTING 6-1 CHAPTER 7 REPLACEMENT PARTS 7-1 A-7

8 CHAPTER 1 ABOUT MICROJET CRYO-TRAP 1.1 Overview In capillary chromatography, when dilute gases such as gases produced from a heated polymer sample are introduced into a separation column for analysis, the gases are introduced into the capillary column as an extremely broad band, resulting in poor resolution of peaks. To avoid this problem, gases must be trapped at the front of the column to narrow the band width to increase the peak separation. To date several methods have been devised for this purpose; however, they have all experienced problems such as requirement of a large amount of coolant, inadequate cooling performance, and difficulties evolved in automated operation. Frontier Lab has addressed these issues and developed the MicroJet Cryo-Trap, based on an innovative technique not found in the past. Our MicroJet Cryo-Trap allows trapping of low boiling species such as butane (n-c 4 ) by cooling the front portion of a capillary column down to near -196ºC. Combining this with our Pyrolyzers or Micro Reactors, it allows various automated analysis. MicroJet Cryo-Trap: United States Patent Principle Fig shows the flow diagram of the MicroJet Cryo-Trap. Flow controlled dry nitrogen (by Flow Controller) is liquefied by passing through a thermal exchange coil immersed in liquid nitrogen. The liquefied dry nitrogen is allowed to blow against the front of the column in the GC oven to cool only the front portion of the column. Gases introduced into the column are captured at the trap. The flow diagram of the Flow Controller is shown in Fig Nitrogen gas flowed into the Flow Controller passes through the stopcock and its flow rate is then controlled by restrictor and mass flow controllers. Restrictor supplies 10mL/min of nitrogen gas all times, regardless of the state of the solenoid valve in order to prevent the liquid nitrogen feed tube from icing. The solenoid valve performs OPEN/CLOSE control of nitrogen from mass flow controller. With the valve OPEN, the column in the oven is chilled by the liquid nitrogen passing through the thermal exchanger. The mass controller controls the nitrogen flow rate to obtain a required cooling temperature. A safety valve located at the exit of the Flow Controller prevents sudden rise of pressure in the vent of clogged liquid nitrogen feed tube. Drawings in Fig illustrate how the trap works when the column is cooled and when trapped species are thermally desorbed. Employing our newly designed MicroJet tube and LN2 saver configuration prevents the inside of the tube from contacting moisture in the air while cooling with liquid nitrogen jet. Therefore, it can be used even in moist atmosphere without icing of the column (Fig A). Once the solenoid valve is closed, heated air (e.g. 40ºC) in the oven passes through the trap, as shown in Fig B, to rapidly heat the trap tube at a rate of ca. 10ºC/sec to desorb the trapped species. 1-1

9 Liq. N 2 Feed Tube Pyrolyzer or other attachment MS Trap Flow Controller MicroJet Tube N2 Cylinder Thermal Exchange Coil Liq. N 2 Container Column Holder Column Fig Flow Scheme of MJT-1030EX Stopcock N 2 GAS IN Restrictor (10ml/min) Mass Flow Controller (7L/min) Pressure Gauge Solenoid Valve Safety Valve GAS OUT 1 Fig Flow Scheme inside Flow Controller 1-2

10 A. Trapping Temperature Sensor MicroJet Liq N 2 Flow H 2O in Air N 2 Column Holder N 2 LN2 Saver Column B. Desorbing Heated Air N 2 OFF Fig Trapping by Liquid N 2 and Thermal Desorption by Heated Air 1-3

11 1.3 Front and Rear Panels of Flow Controller Power Lamp Pressure Gauge Cooling Lamp Stopcock Control Mode Switch N2 Flow Adjust Knob Fig Front Panel of Flow Controller Power Switch N 2 Gas Inlet N 2 Gas Outlet Control Cable connector Circuit Breaker AC Power Code Socket Fig Rear Panel of Flow Controller 1-4

12 CHAPTER 2 SPECIFICATIONS * Cooling Temperature Safety Device Required Pyrolyzers Temperature Display Column Size : -180ºC (with 7L/min N2 gas flow and 40 C of GC oven temperature) : Excessive pressure protection valve (Max 600kPa) : EGA/PY-3030D, PY-3030S, PY-2020iD, PY-2020iS : Available through EGA/PY-3030D or PY-2020iD : id 0.25mm or less for metal capillary columns or id 0.5mm or less for fused silica capillary columns Power Requirement : AC 100V/110V, 0.5A Operating Environment : Less than 30 C recommended Required GC System : Agilent 7890, 6890 Shimadzu GC-17A, 2010 Thermo TRACE 1300/1310, TRACE GC Ultra Perkin Elmer Clarus GC No additional attachments must be installed on and over GC oven. * Subject to modifications for improvement. 2-1

13 CHAPTER 3 INSTALLATION 3.1 Getting Prepared for Installing MicroJet Cryo-Trap 1) Nitrogen - When this device is being operated, 7L of nitrogen is consumed every minute. If a nitrogen cylinder is used, a dedicated nitrogen cylinder should be used. Sharing nitrogen cylinder with other instrument may end up with pressure fluctuations. Nitrogen used must contain no greater than 5ppm of oxygen, with dew point of less than -65ºC. 2) Pressure Regulator - If nitrogen cylinder is used, the maximum use pressure of the secondary pressure should be greater than 1MPa, and the maximum flow rate should be greater than 20L/min when the pressure difference is 400KPa. Inadequate flow rate will result in poor cooling performance. 3) Power Source - 3-pin AC 100V/110V (max 0.5A) power source with a grounding wire. The length of the supplied power code is 2 m. 4) Butane gas - Butane gas of a cigarette lighter. Used for performance inspection.! WARNING Suffocation hazard - This device uses a large amount of nitrogen gas. Be sure to install this device in a well-ventilated area.! WARNING Suffocation hazard - If sufficient liquid nitrogen is vaporized so as to develop low oxygen atmospheres, you are at risk of oxygen deprivation. Exposure to low oxygen atmospheres can quickly bring about unconsciousness without warning. Use this product in a well-ventilated area and avoid spilling liquid nitrogen.! CAUTION When immersing the thermal exchange coil in liq. N 2, allow nitrogen gas to flow through the coil for at least one minute to purge moisture in the liq. N 2 feed tube, then while streaming nitrogen gas through it, lower it slowly down into the liq. N 2.! CAUTION While immersing the thermal exchange coil in liq. N 2, leave the nitrogen gas cylinder valve and the stopcock of the Flow Controller (MJT-1030Ex) open (See Fig ). 3-1

14 3.2 Attaching Liquid Nitrogen Feed Tube Securing Plate Installing onto Agilent 7890, 6890GC 1. Remove aluminum sheet located on the top of the GC oven by cutting off parts of the sheet shown in Fig using nippers. Cut off at these points Fig Aluminum Sheet on GC Oven (Agilent Technologies 6890) 2. Push a screw driver or a similar object into the thermal insulator at the opening of the upper wall inside the GC oven, and force it to make a through hole with 1cm in diameter (see picture below). The picture shows the top wall of GC oven with SS adaptor of our Selective Sampler installed. Make a hole of 1cm in diameter. Make a hole over here. Fig Making a Through Hole at the Top Wall of GC Oven 3-2

15 3. Push down the tube guide of the liquid nitrogen feed tube securing plate into the hole made in step 2 so that the plate is seated on the GC oven (Fig ). 4. Secure the plate with two screws supplied (M4 x 8mm) as shown below. 5. Attach two guide posts on the plate as shown in Fig Secure the plate on top of GC oven using screws. The screw holes may differ by version. Two screws are used to secure the plate Tube guide Fig Attaching Liquid Nitrogen Feed Tube Securing Plate Install guide posts at threaded holes. Attach two O-rings (P5) to each guide posts Fig Attaching Guide Posts 3-3

16 3.2.2 Installing onto Shimadzu GC-17A/ GC The installation position differs depending on the GC models. In reference to the descriptions below, make a hole at the proper position. [GC-17A] Drive a screwdriver or a similar object all the way into the thermal insulator at the top cover of GC oven shown in Fig (a) and make a through hole with a diameter of 1 cm. Also, remove the cover supporting rod (Fig (a)). [GC-2010] The MicroJet Cryo-Trap is installed at the location where a detector is installed. Make a through hole with a diameter of 1 cm from inside the GC oven (Fig.3.2.5(b)). Ensure the opening of the column holder faces the right direction. See section 3.4 for details. Make a hole in thermal insulator Installation position a. Installing on to GC-17A b. Installing onto GC-2010 Fig Making a through hole on the top of GC oven 2. Insert the tube guide, located at the bottom of the liquid nitrogen feed tube securing plate, into the hole made in step 1 and secure the plate on the top of GC oven with two screws (M4x8) (Figs and 3.2.6). Guide Post Screw Hole of Securing Plate Tube Guide (In GC Oven) Attach O-rings to the guide posts. (Two O-rings (P5) for each) Fig Liquid Nitrogen Feed Tube Securing Plate 3-4

17 3.2.3 Installing onto Perkin Elmer Clarus GC 1. At the position indicated in Fig drive a screwdriver or a similar object all the way into the GC oven through the thermal insulator and make a through hole with 1 cm in diameter. Position to make a hole Fig Making a through hole at the top of GC oven (Clarus GC) 2. Insert the tube guide of the liquid nitrogen feed tube securing plate into the hole made previously (section 1) and secure the plate to the top of the GC oven with supplied screws. Guide posts Tube guide (Inserted into GC oven) Attach two O-rings (P-5) to each of guide posts Fig Liquid nitrogen feed tube securing plate 3-5

18 3.2.4 Installing onto Thermo TRACE 1300/1310GC 1. At the position indicated in Fig take out the detector module and install a thermal insulator at the detector position. Thermal insulator Fig Installing a thermal insulator at the detector position of GC oven 2. Insert the tube guide of the liquid nitrogen feed tube securing plate into the hole made previously (section 1) and secure the plate to the top of the GC oven with supplied screws. Guide posts Tube guide (Inserted into GC oven) Attach two O-rings (P-5) to each of guide posts Fig Liquid nitrogen feed tube securing plate Fix the plate using two screws. Fig Attaching liquid nitrogen feed tube securing plate. 3-6

19 3.3 Installing Flow Controller Set Flow Controller and liquid nitrogen container in secured place. An example is shown in Fig An optional 10 L nitrogen container or your own container of 20 L or more should be placed on the floor right in front of your GC. The length of the liquid nitrogen feed tube is fixed. Liquid nitrogen container Flow controller PY temperature controller Fig Setting Flow Controller and Liquid Nitrogen Container! CAUTION Liquid nitrogen feed tube can be damaged, if the moving parts of sample introduction device hit the feed tube. Provide extra care for the tube not being damaged. 3-7

20 3.4 Installing Liquid Nitrogen Feed Tube 1. Carefully insert the end of liquid nitrogen feed tube into the hole of the liquid nitrogen feed tube securing plate, and secure the tube holder by inserting tube guide posts into guide post holes (see Figs and 3.4.2).! CAUTION Utmost care must be exercised in handling liquid nitrogen feed tube to avoid damaging the column holder (made of pure gold). Column holder Tube holder The opening of the column holder is parallel to that of the MicroJet tube. This can be misaligned when in use. If this is the case, loosen the tube holder fixing screw and rotate the tube holder to adjust alignment. Guide post holes Tube holder securing screws Fig End of Liquid Nitrogen Feed Tube Insert the end of the liquid nitrogen feed tube to the hole (tube guide) of the For Shimadzu GC-2010, orient the liquid nitrogen feed tube so that the opening of the column holder is parallel to the GC oven door (Fig (b)). For other GC models, orient the tube so that the opening of the column holder is perpendicular to the GC oven door. Tube guide Column holder opening Insert guide posts into guide post Fig (a) Installing Liquid Nitrogen Feed Tube Fig (b) Column Holder Opening Facing GC Oven Door (for GC-2010) 3-8

21 2. When the liquid nitrogen feed tube has been fixed, affix the supplied arrow seal to the front of the tube to indicate the direction of column holder opening. (See Fig.3.4.3) Fig Arrow indication of the liquid nitrogen feed tube insertion direction. 3. Pass the thermal exchange coil pipes through the liquid nitrogen container lid, and connect the liquid nitrogen feed tube with thermal exchange coil (Fig ). Join two sets of pipes together by hand-tightening the cap nuts. Next, gently tighten them using a wrench (1/4 turn or less) 4. Pass the liquid level indicator through the small hole of the liquid nitrogen container lid, and attach a stopper at the end (Fig ). Temperature sensor connector Liquid nitrogen connector Liquid level indicator stopper Liquid level indicator Connect these pipes Thermal exchange coil Fig Connecting thermal exchange coil and attaching liquid level indicator. 3-9

22 3.5 Attaching MicroJet Tube 1. MicroJet tube securing kit is attached to the quartz MicroJet tube. First, insert a cap nut and graphite ferrule into the MicroJet tube and join it with MicroJet tube union. Hand-tighten the cap nut, followed by turning 1/3 turn more with a wrench. See Fig Be careful not to tighten it too hard or the MicroJet tube may be broken. Hand tightening, followed by turning 1/3 turn more with a wrench. MicroJet tube union A Graphite ferrule MicroJet tube nut Fig Attaching MicroJet Tube Securing Kit 2. Attach freeze protection jigs to the MicroJet tube (Fig.3.5.2) Hand-tighten plus 1/3 turn more Micro Jet tube union A LN2 Saver Fig Attaching freeze protection jigs to MicroJet tube 3-10

23 3. First, screw the nut of MicroJet tube securing kit into the tube guide of the liquid nitrogen feed tube securing plate. This is followed by attaching the MicroJet tube with a union previously attached (Fig ). Guide post Tube holder Liquid nitrogen feed tube securing plate GC oven top panel Column holder Tube guide Nut MicroJet tube Fig Connecting tube guide to MicroJet tube 4. By turning the MicroJet tube, adjust the position of the column holder, so that it is positioned at the center of the horizontal tube of the MicroJet tube. Then securely fix the MicroJet tube by tightening the nut (Fig ). Fix the position of the MicroJet tube with this nut. Position the column holder at the center of the MicroJet tube. Fig Positioning and fixing MicroJet tube 3-11

24 3.6 Connecting Tubes and Cables 1. Using MJT control cable, connect the Flow Controller and liquid nitrogen feed tube (see Fig ), making sure to match the color of the cables. Liquid nitrogen feed tube Connect these together MJT control cable Fig Connecting Flow Controller and Liquid Nitrogen Feed Tube 2. Using PY signal cable, the Flow Controller and Temperature Controller of Pyrolyzer are connected. Plug the valve connector of the PY signal cable into socket labeled PY at the rear panel of the flow controller (see Fig.3.6.2), and connect the sensor connector to MJT control cable. 3. Referring to Fig , connect cables to VALVE and SENSOR sockets at the rear panel of the pyrolyzer temperature controller.! WARNING Before connecting any cables, turn off power of all devices and unplug the power codes. 3-12

25 Fig Signal Cable Connection to Flow Controller 3 rd and 4 th from top (non-polarized) VALVE E VALVE E Sensor Cable SENSOR R 1 st from top: red 2 nd from top: white SENSER R Valve Cable B. Connection to Multi-Shot Pyrolyzer (EGA/PY-3030D) A. Connection to Double-Shot Pyrolyzer (PY-2020iD) Fig Signal Cable Connection to Pyrolyzers 3-13

26 4. Connect outlet labeled OUT of the MS trap tube to port labeled N 2 GAS IN at the back of the Flow Controller. Then connect inlet labeled IN of the MS trap tube to a nitrogen cylinder. OUT N2 IN MS trap tube Fig Connecting MS Trap Tube 5. Fig is the overall picture showing how nitrogen tube, valve control cable and sensor cable are connected. Make sure that these are properly connected. MS trap tube Liquid nitrogen feed tube N2 MJT signal cable Gas Signal MJT-1030Ex Controller GC MJT control cable Fig MicroJet Cryo-Trap Connection Scheme 3-14

27 3.7 Checking and Calibrating Temperature Display Depending on the combination of the liquid nitrogen feed tube and the temperature controller of Pyrolyzer, liquid nitrogen temperature (-196ºC) may not be correctly displayed. Follow the procedure described below to check and calibrate temperature readings. 1) [EGA/PY-3030D] After starting the pyrolyzer control Software program, and click Settings, then click on the checkbox for MicroJet Cryo-Trap(MJT) (Fig.3.7.1(1),A). The current temperature of MicroJet Cryo-Trap will be displayed at he lower right corner of the window (Fig (1),B). [PY-2020iD] After starting the pyrolyzer control Software program, go under Tools menu, under Instrument Set up, and click on the checkbox for MicroJet Cryo-Trap (Fig.3.7.1(2),A). The current temperature of MicroJet Cryo-Trap will be displayed at he lower right corner of the window (Fig (2),B) A. Click on the checkbox.. B. Temperature reading for MicroJet Cryo-Trap Fig (1) Cooling temperature display (EGA / PY-3030D) A. Click on the checkbox. B. Temperature reading for MicroJet Cryo-Trap Fig (2) Cooling temperature display (PY-2020iD) 3-15

28 2) Pull the liquid nitrogen feed tube out from the top of the GC, and immerse the tip of the tube in the liquid nitrogen. Liquid nitrogen feed tube Liquid nitrogen Fig Immersing Temperature Sensor in Liquid Nitrogen 3) Check to see if the temperature reading for cryo-trap in Fig is -196±1 C. If the temperature does not fall into this range, proceed to 4 for temperature calibration. 4) Go under Tools menu, and select Maintenance. Then type the pass word of each instrument to display a screen shown in Fig ) While the temperature sensor is immersed in the liquid nitrogen, enter the temperature reading (step C), then click Save (step D). Check to see if the temperature reading now is -196±1ºC. C. Enter current Cryo-Trap temperature reading B, then click Save B. Current temperature reading for MicroJet Cryo-Trap Fig (1) Calibrating temperature display (EGA/PY-3030D) 3-16

29 B. Current temperature reading for MicroJet Cryo-Trap -170 C. Enter current Cryo-Trap temperature reading B, then click Save -170 Fig (2) Calibrating temperature display (PY-2020iD) 3.8 Installing Stand Attach the stand support rod on the stand base then attach the clamp to the rod (Fig ). Clamp with holder Stand support rod Stand base Fig Installing Stand 3-17

30 3.9 Installing Column 1. Place a column on the column hanger inside GC oven. 2. Put the front of the column through the column holder, then connect the end to the GC injection port (see Fig ). Run column through column holder (gold tube) Column LN 2 Saver MicroJet tube Column Fig Putting Column through Column Holder Column connected to injection port Column connected to detector Fig An Example of Column and MicroJet Cryo-Trap Installed 3-18

31 3.10 Inserting thermal exchange coil to liquid nitrogen container 1. Open the main valve of nitrogen cylinder, followed by opening its stopcock. Then turn control mode switch of Flow Controller to ON. While allowing nitrogen to flow through the thermal exchange coil, immerse thermal exchange coil into a liquid nitrogen container (Fig ). Fig Inserting Thermal Exchange Coil into Liq. N2 Container! WARNING When handling liquid nitrogen, be sure to wear cryogenic gloves such as leather gloves for protection against liquid nitrogen splashes. Never use gloves made of cloth.! WARNING When immersing the thermal exchange coil into liquid nitrogen, exercise extra care to work slowly and carefully to avoid liquid nitrogen splashes.! CAUTION Be sure to immerse the thermal exchange coil into liquid nitrogen, while streaming nitrogen gas through the coil. Otherwise, moisture in air becomes frozen and clogs the coil.! CAUTION Even while no cooling is performed, a small amount of liquid nitrogen is consumed. Therefore, remove the thermal exchange coil from the liquid nitrogen container when not in use for a long period of time. 3-19

32 2. Secure liquid N 2 feed tube by the cramp as shown in Fig Liq. N2 feed tube Clamp with holder Stand support rod Fig Fixing liquid nitrogen feed tube! WARNING The liquid N 2 feed tube must be secured by stand to prevent falling down the liquid N 2 container Unplugging the liquid N 2 feed tube from MJT control cable When the liquid N2 feed tube is disconnected from MJT control cable, the sensor connector of the MJT control cable should be shorted with the supplied short plug as shown in Fig With this connector is open, actual temperature of Pyrolyzer (PY and ITF) may shift from their target temperature. MJT control cable Connect these Short plug Fig Connection of the short plug 3-20

33 CHAPTER 4 OPERATION 4.1 Handling Thermal Exchange Coil 1. When adding liquid nitrogen to the liquid nitrogen container, be sure to remove the thermal exchange coil from the liquid nitrogen container. 2. Allow dry nitrogen to flow through the thermal exchange coil for at least 1 min to purge the coil to remove any residual moisture prior to inserting it into the liquid nitrogen container (see Fig ). It should be immersed as slowly as possible. 3. While the thermal exchange coil remains immersed in the liquid nitrogen container, a small amount of liquid nitrogen is consumed, even if it is not actually used. If it is not used for a long period of time, remove it out of the liquid nitrogen container.! WARNING When the thermal exchange coil is being immersed in the liquid nitrogen container, make sure that the stopcocks of nitrogen cylinder and MJT-1030Ex Flow Controller be open (Fig ) to allow nitrogen to flow through the system, otherwise, the liquid nitrogen feed tube may be clogged with frozen moisture. 4.2 Setting Nitrogen Pressure Set the nitrogen pressure to 600kPa. The Flow Controller has been so configured at the time of shipping that, with this setting, it can provide adequate flow rate to the system. Inadequate pressure will deteriorate the cooling performance. 4-1

34 4.3 Manual Mode Operation (Manually turning ON/OFF of COOLING) 1. Open the stopcock of the nitrogen cylinder, then open the stopcock of the Flow Controller. 2. Flip the POWER switch located at the back of the Flow Controller (Fig ) to ON position, and make sure that the POWER lamp in the front panel comes on. 3. Setting the control mode switch to ON position will light the COOLING lamp and initiate cooling. Cooling can be stopped by flipping the switch to OFF. The cooling temperature is displayed on the PY-2020iD control screen. 4. The head of the separation column is cooled down to near liquid nitrogen temperature in 2 min as shown in Fig When desired temperature is reached, inject a sample into the system. 5. When sample has been injected, turn the control mode switch to OFF and start your GC. ºC 40 0 N2 gas flow L/min L/min L/min 4 min Cooling start Fig Cooling Temperature Profile GC oven: 40 ºC 4.4 When operating with Pyrolyzer or µ-reactor When this device is used in conjunction with Pyrolyzer or µ-reactor, set Control mode switch on the front panel of temperature controller to AUTO. Analytical conditions are set through their each control software. Refer to their each operation manual for the operation of the software. 4-2

35 CHAPTER 5 PERFORMANCE TESTS 5.1 Testing Flow Rate 1. Set the secondary pressure of nitrogen cylinder connected to the Flow Controller to 600kPa. 2. Turn on POWER switch located at the rear panel of the Flow Controller (Fig.1.3.2). 3. Open the stopcock on the front panel (Fig ). 4. While keeping the thermal exchange coil at room temperature, turn ON the control mode switch of the Flow Controller. At this point, make sure that the pressure gauge of the Flow Controller reads 340kPa. Within this pressure range, required flow of nitrogen stream can be obtained. 5.2 Testing Cooling Temperature 1. While allowing nitrogen to flow through the thermal exchange coil, slowly insert it into the liquid nitrogen container. 2. Make sure that the temperature drops to -180 C or below in less than 3 min.! WARNING Prior to inserting the thermal exchange coil into the liquid nitrogen container, purge the liquid nitrogen feed tube for at least 1 min by flowing nitrogen through it, then slowly immerse the coil into liquid nitrogen. 5.3 Testing Trapping Performance 1. Turn the control mode switch to COOLING OFF. 2. Install a column into a GC, and set the GC oven temperature to 40 C. Use normal GC settings for others such as injection port and detector temperatures, etc. 3. Inject 2µL of butane gas from a cigarette lighter into GC using a regular 10µL syringe. 4. Make sure that a peak due to butane is observed (see Fig A). 5. Turn ON the control mode switch of the Flow Controller to initiate cooling. 6. Once the temperature reaches -180 C (normally in 2~3min), inject 2µL of butane gas into GC as mentioned above. 7. Make sure that peak due to butane is not observed at the retention time for butane upon the operation described above (section 3). 8. After 3 min, turn OFF the control mode switch to terminate cooling. Then make sure that butane trapped is again observed on the GC chart (see Fig B). 5-1

36 A) Trap disabled n-c 4 iso-c 4 C 3 B) Trapped for 3 min No butane observed Cooling stopped after 3 min iso-c 4 n-c 4 C min Fig Testing Trapping Performance Using Butane Column: Ultra ALLOY-5 + (5% diphenylpolysiloxane, 30m, 0.25mm i.d., 0.25µm film) GC oven temp.: 40 C, Injector temp: 250 C, Detector: FID or MS Column gas flow rate: 1mL/min, Split ratio: 1/50~100 This concludes all the performance tests. If there are any problems, refer to CHAPTER 6 TROUBLESHOOTING. 5-2

37 CHAPTER 6 TROUBLESHOOTING Symptom, causes, and solutions are summarized below. SYMPTOM CAUSE SOLUTION 1. System completely dead. Power code not plugged. Plug power code in power outlet. 2. Trap not cooled to -180 C 3. Pressure reading of Flow Controller too high (over 500kPa) Not controllable from pyrolyzer. 5. Peaks too broad or peaks split. Inadequate N 2 flow rate. Inadequate N 2 flow rate. N 2 leaking. Liquid N 2 too low. Oven temp too high. Room temperature too high. Thermal exchange coil or liquid nitrogen feed tube clogged. Pyrolyzer signal cable not connected. Control mode switch of Flow Controller not set to AUTO Cryo Trap setting of pyrolyzer temp controller not set to auto control. Inadequate cooling. Turn POWER switch to ON, and make sure power lamp comes on. If it does not come on, check circuit breaker. Press reset button, if circuit breaker has been activated. a. In normal operation at cooling, the N 2 pressure reading should be 250~300kPa. If thermal exchange coil is left immersed in liq. N 2, it is clogged with ice from air moisture, and pressure gauge of Flow Controller may read over 500kPa. Remove the thermal exchange coil from the liq. N 2 and allow N2 to flow through it for 5min. b. Pressure regulator of N 2 cylinder not capable to provide 10L/min of flow may cause this problem. If this is the case, replace the pressure regulator. Make sure all connections are made securely. For best performance, at least bottom 5cm (2 in) of thermal exchange coil must be submerged in liq. N 2. Standard 2L container requires at least 300mL of liq. N 2. Add more liq. N 2, if needed. Set the initial oven temperature to below 70 C. This device operates 30 C or below. Refer to 2a above. Connect pyrolyzer signal cable. See section 3.6 of this manual for details. Turn control mode switch to AUTO position. Enter 1 in Cryo Trap field of FUNCTION screen. See section 4.3 of this manual for details. Increase flow rate of N 2 or add more liq. N 2. See 2. above. 6. Butane not trapped. Column in trap covered with ice. Inadequate cooling. Increase flow rate of N 2. See 2. above. If trapping temperature is above -180 C, resolve the problem according to 2. above. 6-1

38 CHAPTER 7 REPLACEMENT PARTS See your dealer to place an order for replacement parts listed in table below. PART NAME PART No. QTY DESCRIPTION Liquid nitrogen feed tube securing plate (for Agilent6890/7890, with screws) Liquid nitrogen feed tube securing plate (for HP5890, with screws) Liquid nitrogen feed tube securing plate (for Shimadzu GC-17A/2010, with screws) Liquid nitrogen feed tube securing plate (for Thermo TRACE GC Ultra, with screws) Liquid nitrogen feed tube securing plate (for Thermo TRACE 1300/1310 GC, with screws) Liquid nitrogen feed tube securing plate (for Varian CP3800 GC, with screws) Liquid nitrogen feed tube securing plate (for PerkinElmer Clarus GC, with screws) MJ Used for Agilent6890/7890 MJ Used for HP5890. MJ Used for Shimadzu GC-17A/2010 MJ Used for Thermo TRACE GC Ultra MJ Used for Thermo TRACE 1300/1310 GC MJ Used for Varian CP3800 GC MJ Used for PerkinElmer Clarus GC Liquid nitrogen feed tube Ex MJ Column holder attached Guide post MJ A set of 2 posts required Thermal Exchange Coil 2L MJ Thermal exchange coil for 2 liters container (see Fig.3.4.4) Thermal Exchange Coil 10L MJ Thermal exchange coil for 10 liters container Thermal Exchange Coil 30L MJ Thermal exchange coil for 30 liters container MicroJet tube MJ Tube made of quartz (see Fig ). LN2 Saver MJ Used with MicroJet tube. (see Fig ). MicroJet tube securing kit MJ1-K300 1 Used to install MicroJet tube on GC (see Fig ). MJT control cable MJ Cable for N2 and sensor signal. MJT signal cable (for PY-2020D) MJ Used for valve control. Tube Hanger for HP5890, Shimadzu GC-17A/2010, TRACE GC, CP3800 MJ Liquid nitrogen feed tube hanger (for HP5890, Shimadzu GC-17A/2010, TRACE GC and Varian CP3800) Tube Hanger for Agilent6890 MJ Liquid nitrogen feed tube hanger (for Agilent6890) 7-1