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Frontier EGA/PY-3030D, Operation Manual

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Frontier EGA/PY-3030D Operation Manual Download Page 7

A - 7  

Ver.1.36 

TABLE OF CONTENTS

 

BEFORE USING THIS PYROLYZER

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A-2

 

PRODUCT WARRANTY

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A-2 

ABOUT PRODUCT SUPPORT PERIOD

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A-2 

FOR YOUR SAFETY

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A-3

 

CONTENTS

 

IN THE PACKAGE

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A-5

 

TABLE OF CONTENTS

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A-7 

 

CHAPTER 1  ABOUT MULTI-SHOT PYROLYZER

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1-1

 

1.1  BACKGROUND OF DEVELOPMENT ···················································································· 1-1 

1.2  FEATURES OF EGA/PY-3030D ··························································································· 1-3 

1.3  PERIPHEREAL DEVICES ··································································································· 1-4 

1.4  SCHEMATIC OF MULTI-SHOT PYROLYZER FURNACE ·························································· 1-5 

 

CHAPTER 2  SPECIFICATIONS

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2-1

 

About cooling time of pyrolyzer furnace ························································································· 2-3 

 

CHAPTER 3  INSTALLATION

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3-1

 

3.1  PREPARING INSTALLATION ······························································································ 3-1 

3.1.1  Before installation ······································································································ 3-1 

3.1.2  Pumping down MS (for saving installation time) ······························································· 3-2 

3.2  REPIPING CARRIER GAS LINE ··························································································· 3-2 

3.3  SETTING UP GC INJECTION PORT ····················································································· 3-3 

3.3.1  Replacing septum nut of GC injection port ······································································ 3-3 

3.3.2  Replacing septum ······································································································ 3-3 

3.3.3  About injection port liner······························································································ 3-3 

3.4  SETTING UP PYROLYZER FURNACE ·················································································· 3-3 

3.4.1 

Installing quartz pyrolysis tube to pyrolyzer ····································································· 3-3 

3.4.2 

Attaching interface union and needle ············································································· 3-3 

3.4.3 

Mounting pyrolyzer on GC ··························································································· 3-3 

3.5  CONNECTING TEMPERATURE CONTROLLER ····································································· 3-4 

3.5.1 

Connecting power cable to outlet ·················································································· 3-4 

3.5.2 

Connecting to control PC ···························································································· 3-4 

3.5.3 

Hooking up remote signal cable ···················································································· 3-4 

3.6  CONNECTING COOLING GAS LINE ···················································································· 3-4 

3.6.1 

About cooling gas ······································································································ 3-4 

3.6.2 

Connecting temperature controller and pyrolyzer······························································ 3-4 

3.7  CONNECTING FURNACE PURGE GAS TUBE ······································································· 3-5 

3.7.1 

When He or N2 is used as a carrier gas ········································································· 3-5 

3.8  INSTALLING PERIPHERAL DEVICES ··················································································· 3-6 

Summary of Contents for EGA/PY-3030D

Page 1: ...Ver 1 36 MULTI SHOT PYROLYZER MODEL EGA PY 3030D OPERATION MANUAL www frontier lab com ...

Page 2: ...arts can be purchased from your local sales representative office Physical appearance and specifications are subject to modifications without notice 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...

Page 3: ... 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 Other important handling information is placed in a frame like this It indicates that incorrect handling may cause severe personal burn CAUTION HOT Thi...

Page 4: ...er code plug or the cable connectors clean them thoroughly Be sure to unplug the power code Do not use water or organic solvent Use a dry cloth or brush There is a risk of fire if dusty connectors are used WARNING This product uses compressed air or nitrogen for cooling the pyrolyzer furnace Ensure that you have a good ventilation if nitrogen gas is used There is a risk of suffocation if it is use...

Page 5: ...A 5 Ver 1 36 CONTENTS IN THE PACKAGE ...

Page 6: ...A 6 Ver 1 36 ...

Page 7: ...time 3 2 3 2 REPIPING CARRIER GAS LINE 3 2 3 3 SETTING UP GC INJECTION PORT 3 3 3 3 1 Replacing septum nut of GC injection port 3 3 3 3 2 Replacing septum 3 3 3 3 3 About injection port liner 3 3 3 4 SETTING UP PYROLYZER FURNACE 3 3 3 4 1 Installing quartz pyrolysis tube to pyrolyzer 3 3 3 4 2 Attaching interface union and needle 3 3 3 4 3 Mounting pyrolyzer on GC 3 3 3 5 CONNECTING TEMPERATURE CO...

Page 8: ...ation procedure 4 7 4 3 2 Set up for Double Shot analysis and operation procedure 4 9 4 3 3 Set up for Direct EGAt analysis and operation procedure 4 12 4 3 4 Set up for Heart Cut EGA analysis and operation procedure 4 14 4 4 OTHER FUNCTIONS 4 17 4 4 1 Saving loading analysis set ups 4 17 4 4 2 Temperature calibration of pyrolyzer furnace and other set ups 4 17 4 4 3 Printing set ups 4 20 4 4 4 Se...

Page 9: ...cement parts 6 11 6 2 6 Periodic maintenance and inspection 6 11 CHAPTER 7 TROUBLESHOOTING 7 1 7 1 PYROLYZER FURNACE 7 1 7 2 TEMPERATURE CONTROLLER 7 3 7 3 TYPICAL TROUBLESHOOTING PROCEDURE 7 4 7 4 LIST OF ERROR CODES FROM COTROL SOFTWARE 7 6 CHAPTER 8 GUARANTEE OF BASIC PERFORMANCE REPRODUCIBILITY 8 1 CONSUMABLE PARTS LIST Appendix 1 PYROLYZER MAJOR CONSUMABLE PARTS Appendix 3 LIST OF OPTIONAL PR...

Page 10: ...ble Shot pyrolyzer features a temperature programmable furnace which can be used to perform Evolved Gas Analysis EGA With this technique volatiles and pyrolyzate gasses from a polymeric sample evolve continuously as the sample is heated A plot of sample temperature vs detector response is termed as an EGA thermogram EGA is similar to thermal gravimetric analysis TGA EGA is currently used in many r...

Page 11: ...ed on a proprietary high temperature resistant ceramic heater with very low heat capacity The ceramic heater along with a re engineering of the sampler base and the injection port interface has yielded a sophisticated GC inlet that has the versatility to analyze virtually any sample produces amazing precision and increases laboratory productivity by over 60 The EGA PY 3030D appears to offer the an...

Page 12: ...igned adapter This ensures thermo homogeneity and greatly improves the analysis of high boiling compounds 6 Various types of sample analysis four analytical methods and five samplers Choose an analytical method and a sampler based on your analytical purposes and sample matrix The standard operating software is used for Single Shot GC Double Shot GC Evolved gas analysis EGA MS Heart Cut EGA GC MS F...

Page 13: ...hods and peripheral devices available with the EGA PY 3030D Peripheral devices Auto shot sampler Micro UV irradiator F Search 1 Carrier gas selector Selective sampler MicroJet Cryo Trap Analytical methods Evolved gas analysis EGA MS a d Single Shot analysis b c d Double Shot analysis b c d req Heart Cut EGA analysis b c d Req Req Other analytical methods Thermal desorption analysis d Analysis in a...

Page 14: ... of Multi Shot Pyrolyzer Quartz pyrolysis tube Carrier gas Cooling gas ITF heater block Double O ring Screw Purge valve GC Heat sink adapter GC injection port Separation column Ceramic heater Cooling fan Sampler Sample cup standby position Sample cup dropped position ITF needle ...

Page 15: ...ated by gradient multi layer treatment Sampler Double Shot sampler For Double Shot and Single Shot analyses Liquid sampler For introduction of liquid samples regular 10 µL micro syringe can be used Sample cup Eco cup SF small Maximum capacity 50 µL deactivated stainless steel Eco cup LF large Maximum capacity 80 µL deactivated stainless steel 3 Temperature controller PC control PC not included Fun...

Page 16: ...kg or 120 W x 310 D x 310 H mm 7 6kg Recommended GC and GC MS Agilent Agilent 7890 GC Agilent 5975 GC MS Jeol JMS Q1000GC Mk II Perkin Elmer Clarus GC GC MS Shimadzu GCMS QP2010 GC 2010 Thermo Fisher Trace GC Trace ISQ SCION Bruker SCION GC Others Contact us for details 6 Options Peripheral device AS 1020E Auto sampler for Multi Shot pyrolyzer automated analysis of max 48 samples CGS 1050Ex Carrie...

Page 17: ...with 3P socket 4 Control PC A PC running Windows 10 8 1 8 7 Vista or XP operating system with a USB port If the recommended GC or GC MS is used the PC can be shared with GC MS control software programs Fig 2 1 Relationship between pyrolyzer furnace temperature and cooling time when varying cooling air pressure ambient temperature 20 C Pyrolyzer Resistive pipe PY1 7801 P 500 700kPa Air compressor 0...

Page 18: ...te and air pressure is shown in Fig 2 2 Air flow rate L min P Air pressure KPa 2 4 6 8 10 12 14 16 0 50 100 150 200 Air flow rate L min P Air pressure KPa 2 4 6 8 10 12 14 16 0 50 100 150 200 Fig 2 2 Relationship between air flow rate and air pressure ...

Page 19: ...m from the temperature controller Alternatively 1 8 in or 3 mm pipe can be used for connection with supplied nylon tube having flow restrictor 5 Vent free GC MS adapter2 Part No MS402180 MS402190 MS402195 Depends on GC MS model Optional Permits switching of separation columns while maintaining vacuum of MS 6 Installation space Space for temperature controller Width 20 cm Depth 35 cm or more The le...

Page 20: ...separation column for the pyrolyzer operational verification Ultra ALLOY 5 diphenyl 95 di methylpolysiloxane L 30 m id 0 25 mm df 0 25 µm is supplied with the pyrolyzer as standard 3 2 REPIPING CARRIER GAS LINE The installation of the pyrolyzer onto a GC requires redirecting the carrier gas line Fig 3 1 shows the carrier gas flow paths before and after the installation of pyrolyzer Refer to this f...

Page 21: ...iency and the associated discrimination that occurs in conventional split injection ports 3 4 SETTING UP PYROLYZER FURNACE 3 4 1 Installing quartz pyrolysis tube to pyrolyzer Be sure to use the supplied quartz pyrolysis tube part No PY1 3018A The tubes PY1 2018A used for the preceding models such as PY 2020iD iS cannot be used for this pyrolyzer because they are different lengths 3 4 2 Attaching i...

Page 22: ...his cable the temperature controller receives Ready signal from the GC and sends GC START signal back to the GC 3 6 CONNECTING COOLING GAS LINE 3 6 1 About cooling gas Nitrogen or compressed air is normally used as a cooling gas Since the gas passes through high temperature surfaces it should not contain oil or moisture The purity of the gas does not directly influence analytical results 3 6 2 Con...

Page 23: ...When the furnace temperature is 700ºC or lower there is no need to connect the tube 3 7 1 Connecting N2 gas tube A inert gas line such as N2 and connect it to the furnace purge gas tube via the purge gas restrictor B supplied in the package In the case where the supply pressure is 500 kPa there is approximately 100mL min of gas flow If air is used there is no effect of preventing oxidative degrada...

Page 24: ... AS 1020E to the RS 232C port located at the rear of the temperature controller Do not directly connect it to your PC The Auto shot sampler is indirectly connected to PC via the temperature controller 3 8 2 Connecting other peripheral devices Selective sampler SS 1010E MicroJet Cryo Trap MJT 1030Ex MJT 1035E and Carrier gas selector CGS 1050Ex can be also controlled through the temperature control...

Page 25: ...d New Hardware window when the temperature controller is turned ON 2 Place the CD ROM EGA PY 3030D control software in the CD drive in the example below CD drive is assigned to D drive 3 A dialog box asks whether you want to start a setup program Do not proceed and just cancel and terminate the dialog 4 Now as shown in Fig 3 4 specify a folder and install the USB serial driver Fig 3 4 Installing U...

Page 26: ...elect System Move to the Hardware tab and select the Device manager button Open Port COM and LPT as shown in Fig 3 6 to obtain the COM port number used for the USB serial port 2 Select the COM port number in the dialog box shown in Fig 3 5 Select the OK button will start the control software 3 If the port assigned is not in the range between 1 and 8 the port number needs to be reassigned Right cli...

Page 27: ...3 9 Ver 1 36 Fig 3 7 Resetting COM port number ...

Page 28: ...wn in Fig 3 8 Fig 3 8 Views from different angles of pyrolyzer ITF cover ITF needle ITF union N Cooling fan Carrier gas tube Cooling gas Inlet port Cable connectors Exhaust of cooling gas Liquid Sampler Sampler base Sampler base fixing screws O ring P 6W O ring P 12 Side view Rear view Front view Furnace purge gas tube ...

Page 29: ...S 232C port For AS 1020E only External device control ports Main breaker Power for peripheral devices 100VAC 100W total Main power in 100 115V 400W Connect remote signal cable Connect to pyrolyzer Breakers for heaters Control valves for cooling gas and peripheral devices Cooling gas out Connect to pyrolyzer Cooling gas in Connect cooling gas line Ground terminal for pyrolyzer Connect ground cable ...

Page 30: ... 1 Starting program From the Start menu select Programs EGA PY 3030D Control The start up screen shown in Fig 4 1 is displayed followed by the set up screen shown in Fig 4 2 Fig 4 1 Start up screen for the EGA PY 3030D Control software Fig 4 2 Set up screen for Single Shot analysis ...

Page 31: ...Shows analysis mode currently selected E Pyrolyzer set ups Set parameters for pyrolyzer This area depends on analysis mode selected E 1 Turns ON OFF the pyrolyzer furnace heater Checking the box turns the heater ON E 2 Turns ON OFF the interface heater Checking the box turns the heater ON E 3 Sets interface temperature Fig 4 3 Double shot screenshot A Title bar B Menu bar C Toolbar H Status bar D ...

Page 32: ...e accessories to be used G Comments Comments can be added for each analysis mode H Status bar Displays the progress of the program I Start Stop button Starts or stops the program J Monitoring area Shows operating condition of each device connected J 1 Shows the current temperature of the pyrolyzer furnace J 2 Shows the set temperature of pyrolyzer furnace or final temperature set in the program J ...

Page 33: ... 2 1 System Configuration 4 2 1 1 Selecting a device or devices 1 Click on Settings button F in Fig 4 3 will display the screen shown in Fig 4 4 2 Check the small checkbox to indicate that the device will be used 3 If air is used as an atmosphere gas refer to section 4 2 1 3 of this manual 4 Click OK to end 4 2 1 2 Abbreviations for accessory devices CGS Carrier Gas Selector SS Selective Sampler M...

Page 34: ...s shown in Fig 4 5 b 3 He Purge Time C in Fig 4 5 a is the time it takes for the Carrier Gas Selector to completely purge the helium in the Pyrolyzer with air Normally the default value 1 0 min is used 4 He Purge Time in Column D is the time it takes to completely replace the helium in the column with air Normally 2 0 min is used 5 Air Purge Time in GC MS E is the time it takes to completely purge...

Page 35: ...he pyrolyzer furnace temperature the interface temperature set in E 3 is the upper limit temperature For example the relationship between the Pyrolyzer furnace and interface temperatures is shown in Fig 4 6 In this example the Auto mode is selected using E 4 and the upper temperature is set to 300 C using E 3 the Pyrolyzer furnace is heated from 50 C to 500 C The interface initial temperature is a...

Page 36: ...lable 4 3 1 Set up for Single Shot Analysis and operation procedure From the menu bar select Tool Analytical Modes Single Shot Analysis or click on the Single Shot Analysis icon A on the toolbar The set up screen shown in Fig 4 7 will be displayed Fig 4 7 Set up screen for Single Shot Analysis B C Pyrolysis temperature 40 1050 C A D Hold time at pyrolysis temperature E ...

Page 37: ...es for the needed devices 5 Place sample in a sample cup and attach the sample cup to the sampler Then attach the sampler to the Pyrolyzer Wait 2 minutes in order to purge the dead space at the sampler furnace coupling A Double Shot sampler can be used as a Single Shot sampler Just slide down the sampler head and secure it at Single Shot position 6 Press START button 7 The dialog box shown in Fig ...

Page 38: ... is to be done enter 0 in the second row in the Rate column 3 If pyrolysis is to be done following the thermal desorption check the checkbox in D and enter parameters for thermal desorption in J through K 4 If auto sampling is to be done using the Selective Sampler and or if auto cryo trapping is to be done using the MicroJet Cryo Trap check the checkbox for each step desired in L Fig 4 9 Set up s...

Page 39: ...mmediately click on the Start button of the dialog box or hit ENTER key on the PC keyboard This will start the thermal desorption sequence 9 When the thermal desorption program is complete the dialog box shown in Fig 4 11 will be displayed Pull up the Double Shot sampler this positions the sample cup above the furnace at near ambient temperature When the column inlet pressure has stabilized click ...

Page 40: ...nce program in Double Shot Analysis 1st TD Initial min 1st TD Final min PY 1st TD Initial C 1st TD Final C Pyrolysis C 1st TD Rate C min 1st TD PY Initial min START END A dialog box Prepare for pyrolysis is displayed If pyrolysis is to be done pull up the Double Shot sampler all the way then click Yes button This will start GC analysis When GC is ready a dialog box Ready for pyrolysis is displayed...

Page 41: ... checkboxes for Furnace and Interface B to turn on the heaters 2 Enter parameters for Step 1 in D through H 3 Type in parameters for Step 2 Entering 0 for Rate C min in subsequent rows will stop executions of the steps beyond Fig 4 15 illustrates a schematic diagram for a 4 step heating sequence In direct EGA analysis a one step sequence step 1 only is normally used 4 When the sequence is automate...

Page 42: ...interface and Selective Sampler are all READY the dialog box shown in Fig 4 16 will be displayed Immediately drop the sample cup into the furnace click the Start button in the dialog box or hit ENTER key on the PC keyboard Fig 4 16 Dialog box showing start of Direct EGA Analysis Fig 4 15 EGA Multi step heating program STEP 1 1 T1 1 T2 2 T2 2 R1 1 C min min T2 2 STEP 2 2 STEP 3 3 STEP 4 4 t2 2 t2 2...

Page 43: ...rmogram obtained by Direct EGA Analysis The temperature zone elution time range to be analyzed is based upon the EGA thermogram Each EGA thermal zone is automatically introduced into the GC column utilizing a Selective Sampler For example six EGA thermal zones are observed in the EGA thermogram 100 to 600 C 20 C min of a ceramic composite material see Fig 4 17 Fig 4 17 EGA thermogram of a ceramic ...

Page 44: ...0 0 min fixed Temperatures of the Initial C and Final C are automatically calculated and displayed 4 The Selective Sampler and MicroJet Cryo Trap are automatically controlled by the software Click on the Settings button E to display the accessory devices set up screen Then check the checkboxes for desired devices 5 Whether a zone is analyzed or vented and whether or not auto cryo trapping is used ...

Page 45: ...GA Analysis In this example Zones A through D are sampled but Zone B is not analyzed Initial min Zone A Initial C Zone A Final C Zone A START END Dialog box Ready for injection is displayed As soon as the sample cup is dropped to the pyrolyzer furnace click the START button At this point GC analysis is not started Zone B Final C Zone B GC analysis Zone D Final C Zone C Final C GC analysis GC analy...

Page 46: ...t analysis if the filename is specified as Test mtd the actual filename saved will be Test_SS mtd To overwrite a file with the current file select File Save Analytical mode Suffix added to filename Single Shot SS Double Shot DS Direct EGA EG Heart Cut EGA HC 4 4 2 Temperature calibration of the pyrolyzer furnace and other set ups From the menu bar choose Tools Maintenance A dialog box shown in Fig...

Page 47: ...the Single Shot analysis mode 1 Enter the actual temperature measured in A2 using a reliable thermometer of your choice 2 Click the Save button to finish the temperature calibration 3 Make sure that the temperature displayed matches the actual temperature measured as Fig 4 23 If not repeat the operations 1 through 3 described above 4 The interface temperature calibration can be done in a similar m...

Page 48: ...septum liner needle etc is finished click on the Clear button F2 4 4 2 3 Checking valves operations Valves which are controlled by the pyrolyzer EM valves for Pyrolyzer cooling air Selective Sampler MicroJet Cryo Trap and Carrier Gas Selector can be functionally tested i e opened and closed This is done by checking the checkboxes in Manual valve check I Closing the Maintenance screen will bring al...

Page 49: ... pyrolyzer furnace Enter desired date and time pyrolyzer furnace temperature and interface temperature and click the Run button to activate the timer In the example shown in Fig 4 24 at 21 00 on March 10 2011 the pyrolyzer furnace temperature will be set to 700 C and the interface temperature will be 300 C At 0 00 on March 11 2011 the pyrolyzer furnace temperature will be set to 100 C and the inte...

Page 50: ... to the analytical column and a portion exiting via the split vent A typical instrument configuration for a Py GC MS system is shown in Fig 5 1 An example of a Single Shot analysis using the polystyrene solution is described below The test sample vial contains 2 5 mg of polystyrene and approx 5 wt wt of methyl stearate Adding 0 5 mL of dichloromethane benzene or toluene makes a test solution 5 µg ...

Page 51: ...e furnace Fig 5 2B Immediately click the Start button GC analysis will start The pyrogram in Fig 5 3 has peaks for the polystyrene pyrolyzates monomer dimmer trimer and methyl stearate Fig 5 3 Fig 5 3 Pyrogram of polystyrene obtained by Single Shot analysis Single Shot analysis Pyrolysis temp 550 C ITF temp 300 C Injection port temp 300 C Oven temp 70 C 20 C min 320 C 1 min hold Column Ultra ALLOY...

Page 52: ...ases arising from the decomposition of the polymer sample are released and detected as shown in Fig 5 6 The standard polystyrene solution is used to demonstrate EGA This sample is a dichloromethane solution of polystyrene 5 µg µl with methyl stearate added An analysis example is described below From the EGA thermogram obtained the thermal desorption and pyrolysis conditions can be determined STEP1...

Page 53: ...between 50 C and 200 C 2 The polymer decomposition starts about 350 C and ends at 500 C Therefore the EGA results indicate that the volatiles can be thermally desorbed between 50 C to 200 C while the pyrolysis temperature for the polymer is 550 C Our experiences indicate that optimal pyrolysis temperature should be set 50 C higher than the end of the EGA signal This helps ensure good reproducibili...

Page 54: ... sample cup and fix it to the sampler Fig 5 7A Pull the slider of the sampler to the up position and attach the sampler to the pyrolyzer Fig 5 7B Loosen the air purge nut located on the side of the sampler and leave it open for 2 min Tighten the air purge nut before proceeding STEP4 Click the START button when the temperatures and pressures are stabilized When the Ready for injection dialog box is...

Page 55: ...gram contains peaks of both A 1 and A 1 combined A 1 Thermal desorption TD TD temp 100 C 30 C min 200 C 3 min hold ITF temp 300 C Injection port temp 300 C Oven temp 70 C 20 C min 320 C 1 min hold Column Ultra ALLOY 5 30m 0 25φ 0 25 μm He 1 mL min split ratio 1 50 Sample Polystyrene solution 5 µl 25 µg MS scan range 50 350 MS scan speed 3 scans second or greaterMS scan speed 3 scans second or grea...

Page 56: ... MicroJet Cryo Trap a maximum of eight temperature zones can be automatically analyzed by GC MS Here ceramic composite material is analyzed Based on its EGA thermogram Fig 5 10 four temperature zones are determined and the evolved gases from each temperature zone are analyzed by GC MS 10 20 min 40 200 400 ºC 600 100 300 500 A B C D ZONE 0 28 15 5 8 18 10 20 min 40 200 400 ºC 600 100 300 500 A B C ...

Page 57: ...peratures and pressures are stabilized When Ready for injection dialog is displayed slide down the sampler slider to introduce the sample cup into the furnace then click Start button The controlled heating program will start When the program for each temperature zone is completed GC analysis will start The chromatograms of evolved gases from each temperature zone obtained by GC MS are shown in Fig...

Page 58: ...or less Thermal desorption and EGA analysis may require more depending on target compounds Granular or chunk polymer samples are not uniform in sample shapes and have low thermal conductivities resulting in a poor reproducibility of pyrograms If this is the case you may need to use a small amount of sample or to make a thin film or powder There are four methods to make a film or powder out of soli...

Page 59: ...stic materials use either method A1 or A4 A3 Using a cutter knife Using a sharp knife or surgical knife a chunk of sample material is sliced into thin flakes It is difficult to obtain good uniform slices thus giving a poor reproducibility A4 Freeze grinding using liquid nitrogen and metal ball This method involves pulverization of a liquid nitrogen frozen material using a metal crushing ball Note ...

Page 60: ...is is useful for samples with relatively large volumes Regular S Eco cup SF PY1 EC50F 100 pcs 50 No For all applications except for Micro UV Irradiator UV Py GC MS This cup provides slightly better pyrogram reproducibility in flash pyrolysis GC mode than Eco cup LF Flow through Eco cup LHF PY1 EC80HF 20 pcs 80 No This cup provides better peak shape resolution of volatile compounds C3 10 than regul...

Page 61: ...y remain in the cup If this is the case physically remove all the residues using a cotton swab and the like then clean it using volatile solvents such as acetone and dichloromethane and dry it 3 Tests conducted by Frontier Laboratories with polyethylene and polystyrene show that reproducible pyrograms n 5 are obtained when the cups are cleaned as described above 4 The decrease of deactivation of t...

Page 62: ...b If a pair of tweezers is used do not to scratch the inner surface of the sample cup 2 Place sample cups to be cleaned in a beaker containing a solvent This is to dissolve or swell residual polymer Verify that the solvent used will dissolve or swell the polymer sample 3 Apply ultrasonication for one minute 4 Remove the solvent from the sample cups and clean the inner wall of the cup with a cotton...

Page 63: ...ytical precision The instruction for replacing the contaminated pyrolysis tube with a new one is provided below 1 Loosen the three securing screws of the sampler base The O rings do not usually require replacement but look for contamination or cuts 2 Remove the ITF cover of the pyrolyzer furnace 3 Remove the heat sink adapter ITF protection cover Securing screws Securing screws 2 pcs Securing scre...

Page 64: ... the pyrolyzer 6 Attach a new graphite Vespel ferrule to the bottom of the pyrolysis tube which is sticking out from the pyrolyzer at the bottom Make sure that the large outer diameter end goes in first Finger tighten the ITF union 7 Gently insert the supplied hexagonal screw driver from the top of the pyrolyzer and push the pyrolysis tube down until the end of the quartz tube hits the ITF union F...

Page 65: ...e carrier gas The column inlet pressure goes up and should be the same as the carrier gas supply pressure if there is no leakage If leaking refer to Chapter 7 3 Typical troubleshooting procedure When joining the quartz pyrolysis tube and ITF union graphite the Vespel ferrule must be firmly tightened particularly when using a new graphite Vespel ferrule with which a leakage can occur when cooled do...

Page 66: ...h For your safety this operation must be done in a designated place Because the very hot quartz pyrolysis tube needs to be handled heat resistant gloves and safety goggles must be worn while working 1 As shown in Fig 6 3 red heat the quartz pyrolysis tube This can be done most effectively while flowing air through the tube 2 Cool down the heated pyrolysis tube in a secured place Allow 15 min to co...

Page 67: ...h to burn out the debris This is most effective when an inert gas is flowing through the needle 2 Plug the sharp end of the needle with a septum and pressurize the needle using an inert gas Remove the septum the sudden depressurization may push the debris to the opening If so remove the debris using a pair of tweezers 6 1 3 3 Connecting union ITF union N Metal ferrule is attached to the ITF needle...

Page 68: ...rature is low such compounds tend to deposit on the interface needle and on the glass insert liner If this occurs set the injector temperature to 350 C and allow it to bake for two to three hours with the carrier gas on remove the column during this bake out Inspect the injection port inner wall every one to two weeks 6 1 4 3 Column Column degradation depends primarily on the analytical conditions...

Page 69: ... unexpected troubles 3 Double Shot sampler a Make sure that the slider moves smoothly If there is difficulty slide it up and down several times until it moves smoothly if this fails to smooth out the movement it may be necessary to disassemble it prior to cleaning After cleaning a lubricant must be applied Contact us if you prefer it to be re conditioned at Frontier Labs charged b Check the O ring...

Page 70: ...y a torch while running an inert gas through it The pipe needs to be checked every three to four months of use 6 2 3 Temperature controller 1 Make sure that connectors for heater power of pyrolyzer temperature sensor and temperature controller have good electrical contact 2 Make sure the temperature controller is properly grounded 6 2 4 When not in use for a long period of time If the pyrolyzer is...

Page 71: ...with septum debris ITF union N PY1 3513 1 year Standard accessory for EGA PY 3030D ITF union ASN PY1 3533 1 year Used when Auto Shot sampler is used O ring P 6W PY1 2017 As needed For sealing pyrolysis tube M30 2 pcs used Eco pickup PY1 EP55F 1 year Replacement not needed when Auto Shot Sampler is used all the time Septa for liquid sampler 20 pcs PY1 2025 1 year Inspection may only be needed if li...

Page 72: ...ak tailing Degraded column Replace column Abnormal diffusion from pyrolyzer furnace up to column inlet Increase split vent flow Pyrolysis temperature too low Increase pyrolysis temperature by 100ºC Low recovery of high boiling compounds Peak tailing of high boiling compounds ITF and injector temperature too low Increase temperature Eg from 200ºC to 300ºC Do not set GC injector temperature over 350...

Page 73: ...needed No cooling gas Cooling gas not supplied Check cooling gas supply valve and pressure Malfunctioning of EM valve in the rear of controller Repair needed Cooling in the range of 800 to 1050 ºC If furnace temperature is 800ºC or higher the cooling gas does not flow the furnace is allowed to cool itself Once the furnace is below 800 ºC the cooling gas is turned ON Cooling gas tube is plugged Con...

Page 74: ... configuration software Breaker is off Re set the main breaker on the rear panel of the controller Beep sound Sensor cable is not connected or contact failure Ensure cable from pyrolyzer is properly connected to connector labeled POWER SENSOR at rear of controller Sensor failure Repair needed Cooling fan not running It is blocked by a foreign object Make sure it is not blocked by foreign object or...

Page 75: ...on the column head pressure increases and should be the same as the supply pressure If not there is a leakage Use a He leak detector to locate the problem The causes of gas leakage originating from the pyrolyzer are provided here along with the solutions O ring Fig 7 1a that seals the upper end of pyrolysis tube has become loose Further tighten the three hexagonal screws or replace the O ring P 6W...

Page 76: ...le opening may be clogged with septum or sample residues If this is the case the symptoms shown below will be observed After addressing the needle clogging loosen the septum cap nut a bit and then repeat the leak check When the sampler is removed the injector pressure drops very slowly or does not drop It should drop to zero in 1 to 2 seconds The carrier gas total flow is unstable and eventually g...

Page 77: ...ling fan failure Sample cup stand by position Contact your nearest sales office 4 COM Port USB cable contact failure Re seat the USB cable at the PC 11 Connection Connection failure to Auto Shot Sampler 1 Ensure that the cable from Auto Shot Sampler is properly connected to RS 232C connector on the rear of the controller 2 Make sure the Auto Shot Sampler is powered on 12 Cup chute Cup chute not at...

Page 78: ...atories guarantees that the reproducibility of the apex of the polystyrene peak is 0 3 RSD Pyrolysis Frontier Laboratories guarantees that the reproducibility of the peak area ratio between methyl stearate added as internal standard and the styrene trimer SSS is 2 RSD The analytical conditions and typical chromatograms are shown in Figures 8 1 and 8 2 There is a risk of burn injury Since the pyrol...

Page 79: ... 300 Fig 8 2 Test conditions and a typical check out sample pyrogram Analytical conditions Separation column Ultra ALLOY 5 5 phenyl 95 dimehtylpolysiloxane L 30m id 0 25mm df 0 25 µm Column flow 1 0ml min Split ratio 1 100 Oven temp 70 320 C 20 C min 1 min hold Injector temp 300 C Py furnace temp 550 C Py GC ITF temp 300 C Sample Polystyrene contains 5 wt methyl stearate Sample wt 25 µg 5µl of 5µg...

Page 80: ...5 1 set Includes ITF union N 1ea ITF needle 2ea and Needle nut 1ea 1 set M ITF union ASN PY1 3533 1 pcs For Auto Shot Sampler and EGA PY 3030D Deactivated Heat sink adapter kit 3030SA PY1 3551 1 set For EGA PY 3030D Used for Agilent7890 6890 and Shimadzu GC 2010 17A includes 2 securing screws Heat sink adapter kit 3030PE PY1 3552 1 set For EGA PY 3030D For PE Auto system Clarus GC includes 2 secur...

Page 81: ...pcs Magic Chemisorber protection tube PY1 MCP01 1 set Protection tube for Magic Chemisorber L contains 2 pcs 7 Harris Micro Puncher tool used to easily punch out discs from a thin sheet of sample Micro puncher 050S FMP 0 50S 1 set Disc size 0 50 mmΦ contains 3 pcs cutting mat L 1pc Micro puncher 075S FMP 0 75S 1 set Disc size 0 75 mmΦ contains 3 pcs cutting mat L 1pc Micro puncher 125S FMP 1 25S 1...

Page 82: ... pcs Used for Shimadzu P N PY1 7304 5 pcs O ring P 6W P N PY1 2017 20 pcs ITF union N P N PY1 3513 1 pc Graphite Vespel ferrule P N PY1 7911 5 pcs Quartz pyrolysis tube A30 P N PY1 3018A 1 pc O ring P 12 P N PY1 7811 10 pcs Fig A 1 PYROLYZER MAJOR CONSUMABLE PARTS GC Heat Sink Adapter Used for Agilent and Shimadzu P N PY1 3551 1set Used for Thermo Fisher P N PY1 3555 1set Used for PerkinElmer P N ...

Page 83: ...udes two polymer libraries containing data for 700 polymers library containing data for pyrolyzates of 165 polymers and library containing data for 494 additives and their pyrolyzates PY 1111E 161 F Search Library Search software Ver 3 5 Library search software program required for library search PY 1112E 141 EGA MS 14B Library Evolved gas MS library contains thermograms and average MS spectra of ...

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