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Contents

Thermo Scientific

EA IsoLink IRMS System for CNSOH Operating Manual

Installing Flash IRMS Elemental Analyzer. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51

Preliminary Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51

Making the Gas Supply Plumbing Connections . . . . . . . . . . . . . . . . . . . . . . . . 53

Building the Gas Lines. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53
Purging Gas Lines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53
Connecting the Gas Lines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54

Electrical Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54

Mounting Peripheral Devices. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
Power Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
Performing Electrical Connections. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55

Installing the Reactors into the Furnaces . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
Setting Pressure and Flow Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63

NCS Determination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63
H-O Determinations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63

Installing Autosampler. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64
Isodat Software Suite . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64

Chapter 4

Installing MAS Plus Autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65

MAS Plus Autosampler Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
MAS Plus Autosampler Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67

Chapter 5

Installing AI 1310/AS 1310 Autosampler. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71

Preliminary Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71

Who Performs the Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71
Electrical Requirement. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71
Lift and Carry the Sampling Unit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72

Installing the Direct Injection Device for Flash IRMS Elemental Analyzer . . . . 72
Installing the Sampler Support on the Flash IRMS Elemental Analyzer . . . . . . . 73
Installing the AI 1310/AS 1310 on the Flash IRMS Elemental Analyzer . . . . . . 76

Installation of the Sampling Unit. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77
Installing the Syringe . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 79
Electrical Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81
Starting-up. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82

Chapter 6

Using EA IsoLink IRMS System for CNSOH . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83
Dual Measurement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84

Procedure. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84

Performing a Jump Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
Creating an Isodat Method for N+C Measurement (Dual Measurement)  . . . . . 88
Creating an EA Method for N+C Measurement  . . . . . . . . . . . . . . . . . . . . . . . . 92
Creating an Isodat Method for Single Mode S Measurements . . . . . . . . . . . . . . 93
High-Temperature Conversion – Analysis of H and O Isotopes  . . . . . . . . . . . . 94

Bottom Field Connector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94

Summary of Contents for EA IsoLink IRMS System

Page 1: ...EA IsoLink IRMS System for CNSOH Including the Flash IRMS Elemental Analyzer Operating Manual 31707010 Revision B December 2016 ...

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Page 3: ...31707010 Revision B December 2016 EA IsoLink IRMS System for CNSOH Including the Flash IRMS Elemental Analyzer Operating Manual ...

Page 4: ...without notice All technical information in this document is for reference purposes only System configurations and specifications in this document supersede all previous information received by the purchaser Thermo Fisher Scientific Inc makes no representations that this document is complete accurate or error free and assumes no responsibility and will not be liable for any errors omissions damage...

Page 5: ...___________________________________________________________ Address ___________________________________________________ __________________________________________________________________ City State _________________________________________Postal Code__________________________________________________________________ Country ___________________________________________________ _______________________...

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Page 7: ...ntific performs complete testing and evaluation of its products to ensure full compliance with applicable domestic and international regulations When the system is delivered to you it meets all pertinent electromagnetic compatibility EMC and safety standards Safety This device complies with the following safety standards according to Low Voltage Directive 2014 35 EU EN 61010 1 2010 3a ed IEC 61010...

Page 8: ...cified by Thermo Fisher Scientific could impair any protection provided by the instrument Notice on the Susceptibility to Electromagnetic Transmissions Do not use radio frequency transmitters such as mobile phones in close proximity to the instrument THIS DEVICE COMPLIES WITH PART 15 OF THE FCC RULES OPERATION IS SUBJECT TO THE FOLLOWING TWO CONDITIONS 1 THIS DEVICE MAY NOT CAUSE HARMFUL INTERFERE...

Page 9: ...e you purchased the product Number of product pieces and the estimated total weight and volume Pick up address and contact person include contact information Appropriate pick up time Declaration of decontamination stating that all hazardous fluids or material have been removed from the product For additional information about the Restriction on Hazardous Substances RoHS Directive for the European ...

Page 10: ...ecyclé par celle s ci Pour davantage d informations rendez vous sur la page www thermoscientific fr rohs WEEE Direktive 2012 19 EU Thermo Fisher Scientific hat Vereinbarungen mit Verwertungs Entsorgungsfirmen in allen EU Mitgliedsstaaten getroffen damit dieses Produkt durch diese Firmen wiederverwertet oder entsorgt werden kann Weitere Informationen finden Sie unter www thermoscientific de rohs ...

Page 11: ...s by the user are not covered Thermal Conductivity Detector Warranty The Thermal Conductivity Detector P N 419 07510 is assembled using the highest quality materials and operationally tested The operator must not touch the Thermal Conductivity Detector and in case of any suspected problems should contact a service engineer for diagnosis Only in the case that a qualified service engineer determines...

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Page 13: ...xiv Precaution for Hydrogen xxiv Precaution for Nitrogen xxiv Precaution for Sulfur Dioxide xxiv Precaution for Carbon Dioxide xxiv Precaution for Carbon Monoxide xxv Hazardous Substances Precautions xxv Venting Toxic Gases xxv Residual Risks xxv High Voltage xxv Hot Parts xxv Hazardous Chemical xxvi Maintenance Precaution xxvi Personal Protective Equipment xxvi Training xxvii Chapter 1 Getting Fa...

Page 14: ...e Area 21 Power Supply Area 22 Gases Supply Area 22 Transformers Compartment 23 Devices for the Furnaces Control 25 Devices Supplying the Furnaces 25 Status Panel 25 Autosamplers 26 MAS Plus Autosampler for Solid Samples 26 AI 1310 AS 1310 Autosampler for Liquid Samples 27 Ramped GC Oven 28 Chapter 2 Analytical Principles 31 About Your System 31 Pneumatic Circuit 32 Pressure Regulators 35 Electron...

Page 15: ...MAS Plus Autosampler Overview 65 MAS Plus Autosampler Installation 67 Chapter 5 Installing AI 1310 AS 1310 Autosampler 71 Preliminary Information 71 Who Performs the Installation 71 Electrical Requirement 71 Lift and Carry the Sampling Unit 72 Installing the Direct Injection Device for Flash IRMS Elemental Analyzer 72 Installing the Sampler Support on the Flash IRMS Elemental Analyzer 73 Installin...

Page 16: ...thod 115 Events During Acquisition 116 Chapter 7 Maintenance 119 Post Analysis Operations 120 Putting the Instrument in Standby Mode 120 Maintaining the Instrument 122 Current Maintenance Program 122 Replacing Reactors and Adsorption Filters 122 Replacing the Filling Materials 123 Ashes Removal and Crucible Cleaning 124 Maintaining the Reactor of the Pyrolysis Unit 125 Replacing the Gas Chromatogr...

Page 17: ...Contents Thermo Scientific EA IsoLink IRMS System for CNSOH Operating Manual xvii Using Isodat Software Suite and EagerSmart Data Handling Software at the Same Time 152 ...

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Page 19: ... IsoLink IRMS System for CNSOH providing high performance analytical capabilities for both research and routine applications More information about the use of this system can be found in related documentation sources and by using the provided contact information WARNING Thermo Scientific systems operate safely and reliably under carefully controlled environmental conditions If the equipment is use...

Page 20: ...ollowed by WARNING or CAUTION which indicates the degree of risk of personal injury instrument damage or both Cautions and warnings are followed by a descriptor such as BURN HAZARD A WARNING is intended to prevent improper actions that could cause personal injury A CAUTION is intended to prevent improper actions that might cause personal injury and or instrument damage You find the following safet...

Page 21: ...instrument or component might occur This damage might not be covered under the standard warranty LIFTING HAZARD Indicates that a physical injury could or might occur if two or more people do not lift an object READ MANUAL Alerts you to carefully read your instrument s documentation to ensure your safety and the instrument s operational ability Failing to carefully read the documentation could or m...

Page 22: ... Protective conductor terminal Frame or chassis terminal Equipotentiality On supply Off supply Equipment protected throughout by DOUBLE INSULATION or REINFORCED INSULATION Equivalent to Class II of IEC 536 Instruction manual symbol affixed to product Indicates that the user must refer to the manual for specific WARNING or CAUTION information to avoid personal injury or damage to the product Cautio...

Page 23: ...o supply the Flash IRMS Elemental Analyzer Maximum 250 300 kPa 2 5 3 bar for helium He Maximum 250 300 kPa 2 5 3 bar for oxygen O2 Safety Cut Off Device When an alarm condition is detected this device cuts off the power to the heating resistors of the oxidation reduction furnaces and to the GC Oven For more details see Safety Cut Off Device on page 5 WARNING The instrument must be used according t...

Page 24: ... air it can create an explosive mixture Precaution for Nitrogen Liquid nitrogen is a colorless and odorless gas It can cause rapid suffocation when concentrations are sufficient to reduce oxygen levels below 19 5 A Self Contained Breathing Apparatus SCBA may be required Oxygen concentrations must be monitored in the release area Precaution for Sulfur Dioxide Sulfur dioxide is a colorless gas with ...

Page 25: ...m your system Residual Risks Users of Flash IRMS Elemental Analyzer must pay attention to the following residual hazards High Voltage Hot Parts WARNING Before using hazardous substances toxic harmful and so on read the hazard indications and information reported in the applicable Material Safety Data Sheet MSDS Use personal protection according to the safety requirements WARNING DO NOT OPEN the el...

Page 26: ...g of a particular compound CAUTION Always use original Thermo Fisher Scientific materials and products The use of materials not meeting the technical specifications of our products does not ensure a good operation of the instrument and may even damage it WARNING When for technical reasons it is necessary to work on instrument parts which might involve an hazard moving parts components under voltag...

Page 27: ...compounds and filling materials for preparing and cleaning reactors and filters and for removing the ashes from the crucible when used Training Thermo Fisher Scientific offers worldwide training on instruments and software Experience has shown that maximum results can be obtained from a scientific instrument if the instrument operator receives an adequate training We recommend that the key operato...

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Page 29: ... EA IsoLink IRMS System includes the Flash IRMS Elemental Analyzer the Thermo Scientific ConFlo IV Universal Interface and a Thermo Scientific Isotope Ratio Mass Spectrometer Contents Technical Features Instrument Configurations Software Requirements Instrument Basics Labels Location on the Instrument Use of Gases Front Panel Back Panel Top Panel Furnaces Compartment Oven Compartment Detection Sys...

Page 30: ...ernal interface RS 232 serial line Instrument control Isodat Software Suite 3 0 EagerSmart Data Handling Software Power supply 230 Vac 10 50 60 Hz 2 Hz 1400 VA Dimensions cm Height 50 54 with fittings Width 59 Depth 58 Mass kg 65 Sound Pressure Level Less than 70 db A Table 2 EA IsoLink IRMS System for CNSOH Analytical Capabilities Configuration Description H Quantitative weight and stable isotope...

Page 31: ...ocated in a thermostatic chamber at controlled programmable temperature This chamber also accommodates the analytical column Chromatographic columns The chromatographic column performs the chromatographic separation of the reaction products generated during the combustion or high temperature conversion process The chromatographic column for high temperature conversion is placed in the thermostatic...

Page 32: ...min This avoids melting the copper within the reactor which will cause poor performance 3 Increase it to the operating temperature of 1020 C Protective Cap Figure 1 Protective Cap Note The EA IsoLink IRMS System for CNSOH comes standardized for a 18 mm OD reactor For 25 mm reactor tubes the MAS Plus and the top of the EA must be modified See the section Upgrading EA for 25 mm OD Macro Reactor on p...

Page 33: ...ard and display A synoptic on the instrument front allows you to monitor the instrument status Safety Information Safety Cut Off Device When an alarm condition is detected this device cuts off the power to the heating resistors of the furnaces and to the EA Oven CAUTION The instrument must be used according to the specifications of this guide Improper use can adversely affect the instrument protec...

Page 34: ...ocation on the Instrument The following illustrations show the location of the safety labels attached on the instrument Figure 2 EA IsoLink IRMS System for CNSOH Analyzer Model Serial Number and Electrical Data Figure 3 EA IsoLink IRMS System for CNSOH Alert Labels Analyzer Model Serial Number and Electrical Data Label Alert Label Alert Label Alert Label Hot Surface Labels ...

Page 35: ... Analyzer gas supplies is 700 kPa 7 bar Hot Surface Label CAUTION Before using gases carefully read the hazard indications and information reported in the Material Safety Data Sheet MSDS supplied by the manufacturer referring to the CAS Chemical Abstract Service number It is the your responsibility to see that all local safety regulations for the use of gases are obeyed Note ConFlo II III IV and I...

Page 36: ...ust Tube Connection Precaution for Sulfur Dioxide Note For the nominal pressure of the gases used by ConFlo II III IV and IRMS Delta models TF Bremen manufacturing refer to the relevant manuals Note The pressure must be adjusted to about 4 kPa through the reducing valves mounted at the cylinder ATTENTION Carbon Monoxide is toxic When working with this gas good ventilation is essential Otherwise th...

Page 37: ...xplosive mixture Use the following safety precautions when using hydrogen Ensure that the hydrogen cylinder complies with the safety requirements for proper use and storage Hydrogen cylinders and delivery systems must comply with local regulations Make sure the gas supply is turned completely off when connecting hydrogen lines Perform a bubble test to ensure that the hydrogen lines are leak tight ...

Page 38: ...reducing valve must be open 2 Open the main valve for two or three seconds to let the gas purge the whole valve system 3 Close the on off valve then close the main valve 4 Mark manometer positions of the on off valve and main valve and wait for 10 15 min 5 A leak may be present if the manometer positions have changed 6 To detect a leak use soap solution on all valves and connections Check for bubb...

Page 39: ...ge 25 Oven compartment including the pressure regulators pressure gauges adsorption filters isothermal GC oven housing the TCD detector the gas chromatographic column and the HeM module See the section Oven Compartment on page 16 Note On the internal wall of the front door you will find holders designed for a paper copy of the Consumables and Spare Parts Catalog and tools for maintenance See Figur...

Page 40: ...erface gas inlets and electrical connections See the section Connections Panel on page 21 Transformers compartment Access to the transformer compartment is obtained by removing the back panel cover See the section Transformers Compartment on page 23 Place holders for the ramped GC Oven for EA IsoLink CNSOH See Figure 10 and the section Ramped GC Oven on page 28 Figure 10 Instrument Back Panel with...

Page 41: ...ConFlo Universial Interface connection Furnaces Compartment The furnaces compartment can be accessed from the instrument front by removing lifting the cover See Figure 12 Figure 12 Furnace Compartment with Protection Plate Gas Connections Fittings for Reactors Autosamplers Furnace compartment protection plate Furnace Compartment Cover WARNING Do not open the furnace compartment during operation du...

Page 42: ...are limited to the following maximum temperatures to avoid reduced lifetime and damage LEFT Furnace 1450 C RIGHT Furnace 1100 C The furnace temperature is monitored by a thermocouple located inside the furnace The furnaces are cooled when required by the operator or if there is a safety cut off The cooling time depends on the operating temperature and the room temperature Protection Plate Left Fur...

Page 43: ...eral hours e g overnight or periods lasting several days or longer the furnaces should be placed into Stand By Mode as defined by the Standy By Mode which can be activated automatically at the end of a sample sequence a If the instrument is not used for a long period of time e g several weeks it is recommended to switch off the furnaces The furnaces should be cooled down using the furnace Cool Dow...

Page 44: ...ontaining the thermal conductivity detector TCD and the gas chromatographic column located behind the protecting plate See To access to the thermostatic chamber on page 17 The adsorption filters are housed in this compartment and are attached to the protecting plate using securing clips Note Two adsorption filters are required as shown in Figure 15 One filter is required for the High Temperature C...

Page 45: ...ng screws on the protecting plate See Figure 16 Figure 16 Access to Thermostatic Chamber Figure 17 shows the detector compartment the heating block surrounding the thermal conductivity detector TCD and the gas chromatographic column Figure 17 Thermostatic Chamber Internal View Note One chromatographic columns is installed for OH analysis with the high temperature furnace A second chromatographic c...

Page 46: ...en pure carrier gas flows through both the reference and the analytical channels a constant temperature gradient is established between the elements and the detector walls and the Wheatstone bridge is balanced namely there is no output signal As a component is eluted a change in heat transfer occurs with consequent variation of the filaments temperature Since electrical resistance is a function of...

Page 47: ...12 Mother board It provides interlocking between low voltage boards and with the rest of the instrument This board can be connected to a NiCd 3 6 V 280 mA h rechargeable battery located nearby The rechargeable battery replacement must be performed by specialized technical personnel CPU 1112 This board has full control of the instrument operation It controls the communication between operator and m...

Page 48: ...the mains power and supplies it to the following devices Cooling fan Furnaces transformers Heater of the detector thermostatic chamber Six fuses are provided on the board See Table 6 AC 1112 Furnaces Power Supply Supplies 48 Vac power to the furnaces It contains the SSR relays for the furnaces control Also see the section Devices for the Furnaces Control on page 25 Two fuses are provided on the bo...

Page 49: ...e autosamplers and the helium management device and the automatic switching valve See Figure 20 Figure 20 Interface Area A 9 pin connector marked RS 232 to dialog with the computer via serial line A 25 pin connector marked Aux Connector for the remote start of the instrument A 2 pin connector marked Autosampler HO for the MAS Plus autosampler installed on the left channel for HO determinations A 2...

Page 50: ...Gases Supply Area The gas supply area comprises the gas inlet ports See Figure 22 Figure 22 Gases Supply Area The helium and oxygen gas inlet ports marked He and O2 are directly connected to the pressure regulators Table 7 details the pressure value to be set for each gas inlet port Gas pressures must be set and controlled through the pressure regulators and the pressure gauges of the instrument T...

Page 51: ...of the instrument the compartment of the transformer is accessible firstly by removing the back panel of the instrument then by removing the relevant protection plate See Figure 23 Figure 23 Accessing the Transformer Compartment Table 8 Pressure Units Conversion To convert Into Multiply By kPa bar 0 01 psi 0 145 bar kPa 100 psi 14 51 psig kPa 6 89476 bar 0 0689476 Back Panel Transformer Compartmen...

Page 52: ...ering the furnaces and controlling their temperature Figure 24 shows the devices contained in the compartment Figure 24 Transformer Compartment Internal View WARNING DO NOT OPEN the transformers compartment there are no user serviceable parts inside Any operation inside the compartment must be carried out only by authorized and trained Thermo Fisher Scientific personnel LTA 1 HT LTA 2 Transformers...

Page 53: ...unction LTA 1 LEFT LTA 1 RIGHT They read the values of the thermocouple present in the relevant furnace and send the signals to the TCR 1112 board SSR LEFT SSR RIGHT Solid State Relays SSR contained in the AC 1112 board Each SSR is coupled with a proper safety sensor which detects any malfunction The SSR control the power supply to the relevant furnace and cut off power to the heating resistor whe...

Page 54: ...the proper reactor tube See Figure 26 Figure 26 MAS Plus Autosampler for Solid Samples Table 11 Status LED Description LED Meaning Power On When lit the instrument is powered on Ready When lit the instrument is ready to run analyses Run When lit an analysis is in progress Standby When lit the instrument is in standby condition During this condition helium gas flows are decreased to 10 mL min and t...

Page 55: ...lash IRMS EA by means of the appropriate support See Figure 27 Figure 27 AI 1310 and AS 1310 Autosamplers for Liquid Samples The autosampler consists of A sampling unit An 8 position AI 1310 or 105 position AS 1310 sample tray Table 12 Sample Tray Numbering Sample Tray Locating Mark Numbering 1 Seat marked 1 one from 1 to 32 2 Seat marked 0 zero from 33 to 63 3 Seat marked 0 zero from 64 to 94 4 S...

Page 56: ...c Ramped GC Oven The Ramped GC Module for the temperature control of the chromatographic column Figure 28 shows the Ramped GC Oven installed on the back of the Flash IRMS EA Figure 28 Ramped GC Oven MAS Plus on the Right Channel for NCS Determinations MAS Plus on the Left Channel for OH Determinations Ramped GC Oven Right Side View Left Side View ...

Page 57: ...ts See the numbering in the images in Figure 29 1 AC Input Connector 2 Power Switch to power the Ramped GC Oven On Off Position I instrument On Position O instrument Off 3 9 pin connector for the control of the GC 4 Compartment for the Thermo Scientific smartEA option 5 Jumo controller for the manual temperature program setting 2 3 4 5 6 1 7 ATTENTION The start and the stop of the temperature prog...

Page 58: ...d GC Oven 30 EA IsoLink IRMS System for CNSOH Operating Manual Thermo Scientific 6 Gas inlet outlet ports for the connection of the carrier gas 7 Cooling fan CAUTION For installing connecting and operating the Ramped GC Oven refer to the Ramped GC Oven Operating Manual ...

Page 59: ...minimized water adsorption and reduced nitrogen background The NCS separation column is operated in a ramped GC oven attached to the back panel of the Flash IRMS EA The molecular sieve for high temperature conversion analysis is installed in the isothermal GC oven of the EA Two autosamplers on top and full software control automate the analysis of five isotopes with two sample drops The additional...

Page 60: ...8 Installing an additional CO2 trap for N isotope analysis in single mode reduces the analytical time S isotope analysis in single mode If no separation of N2 and CO2 is needed a dedicated single reactor for triple NCS analysis and an optimized separation column and temperature program can be used This reduces the analytical time See Creating an Isodat Method for Single Mode S Measurements on page...

Page 61: ...V4 2 1 7 6 4 5 EFC T 3 2 1 EVP1 3 2 1 2 1 2 1 2 1 2 1 EV1 2 1 7 6 4 5 Purge NCS 8 9 3 HO NCS MS Purge HO 2 1 7 6 4 5 8 9 3 2 1 EV2 2 1 EV3 2 1 EV4 AUTOMATIC SWITCHING BLOCK COMBUSTION NCS AUTOMATIC SWITCHING BLOCK 3 3 3 3 3 2 Column Right Furnace 0 1100 C Left Furnace 0 1450 C ConFlo TCD 1 2 R1 R2 1 4 AS 1 2 H O CO TRAP 2 AS Carrier Gas Purge Gas HO NCS MS Purge HO Purge NCS 2 1 EV3 OUT IN BFC NV1...

Page 62: ...5 EFC T 3 2 1 EVP1 3 2 1 2 1 2 1 2 1 2 1 EV1 2 1 7 6 4 5 8 9 3 2 1 EV2 2 1 EV3 2 1 EV4 AUTOMATIC SWITCHING BLOCK 3 3 3 3 2 1 7 6 4 5 Purge NCS 8 9 AUTOMATIC SWITCHING BLOCK 3 HO NCS MS Purge HO HIGH TEMPERATURE MODE PYROLYSIS O H 3 2 Column Right Furnace 0 1100 C Left Furnace 0 1450 C ConFlo TCD 1 2 R1 R2 1 4 AS 1 2 Cap AS Carrier Gas Purge Gas HO NCS MS Purge HO Purge NCS 2 1 EV3 OUT IN BFC NV1 2...

Page 63: ...components See Table 13 NCS Configuration uses the right channel Note The reference flow enters the pyrolysis reactor from the bottom before it ends as purge in the Autosampler NCS OH Configuration uses the left channel Note The carrier gas flow is not shown here It enters the pyrolysis reactor from the bottom The reference flow enters the system at the combustion reactor and ends as purge for the...

Page 64: ...let port O2 Oxygen inlet port F Stainless steel filter EV1 Two way solenoid valve to control oxygen inlet EV2 Three way solenoid valve to control helium inlet and to allow switching between helium and oxygen EV3 Two way solenoid valve normally open to control the inlet of helium flowing back from the TCD detector analytical channel The valve is closed during the leak test EV4 Two way solenoid valv...

Page 65: ...e EVP2 electronic controller proportional valve EVP1 Electronic flow controller for helium as carrier gas and oxygen to control the flow rates of gases according to the flow values set EVP2 Electronic flow controller for helium as reference gas to control the flow rate according to the required flow value Table 14 Parts of the EFC t Module Sheet 2 of 2 Component Description and function 2 1 EV1 2 ...

Page 66: ...arrier gas flow to the ConFlow In pyrolysis O H analysis controls the reference gas flow to the ConFlow EV4 In combustion NCS analysis controls the purge gas flow to the right autosampler In pyrolysis O H analysis controls the purge gas flow to the left autosampler Carrier Gas Reference Gas He O2 PI1 PI2 PRV2 PRV1 He O2 F F EV1 6 5 mL min 300 kPa 3 2 1 2 1 S1 EVP1 EV2 2 3 1 2 1 EVP2 S2 F F 1 EV3 2...

Page 67: ...s from a single sample Large volumes like the reactors require high flows of 80mL min Since peak broadening starts in the reactors higher flows are favorable to enhance peak shape HeM module allows high reactor flows of 180 mL min This increase in carrier flow is compensated by recirculating up to 2 3 of the He flow back into the system for purging HeM module works through a valve block which is i...

Page 68: ...Flo the reactor flow carrier gas is stabilized When the sample drops or is injected by liquids autosampler the carrier gas flow is maintained for a fixed period until all analyte gases produced upon conversion of the sample in the reactor are certainly on the chromatographic column analysis mode Split valve 2 EV2 is open at that time In general the flow through the chromatographic column is 50 mL ...

Page 69: ...e on the chromatographic column in the combustion system the reference flow 50 150 mL min is split using EV3 and reunited after the chromatographic column Thus V3 is also open all the time Setting Different Flows and Switching Times It is possible to change the default settings for switching the He Save Mode Click on the button and choose the tab HeM Here you can define when the He Save Mode is sw...

Page 70: ... Figure 38 Figure 38 Needle Valves In general there is no need to adjust the splits It may become necessary if the restrictions after the valve block i e water trap GC column change or if the flow conditions i e carrier gas flows are modified This chapter is about the procedure to change the settings Note Any changes may have influence on the system performance and should be done only when necessa...

Page 71: ... Set carrier flow to 180 mL min and the reference flow to 70 mL min 4 Disconnect the purge line of your autosampler see measuring point TP1 in Figure 39 and measure the flow It should read 200 mL min 2 mL min If the flow is higher use a screwdriver to gently close needle valve V2 turning it counter clockwise If the flow is lower use a screwdriver to open the needle valve turning it clockwise 5 Now...

Page 72: ...romium Oxide Reduced Copper Silvered Cobaltous Cobaltic Oxide F2 Absorption Filter Material Plexiglas Quartz Wool Magnesium Perchlorate Anhydrone CC2 Gas chromatographic Column Material Stainless Steel Note In some cases it can be advantageous to use copper oxide instead of chromium oxide Reactors filled with copper oxide must be operated at 900 C 920 C Check your calibration with appropriate stan...

Page 73: ... leaks 2 Increase the temperature from room 400 C to 900 C in steps of 100 C and hold at 900 C for at least 15 min This avoids melting the copper within the reactor which will cause poor performance 3 Increase it to the operating temperature of 1020 C Note The EA IsoLink IRMS System for CN OH comes standardized for a 18 mm OD quartz glass reactor For 25 mm reactor tubes the MAS Plus and the top of...

Page 74: ...a proper preparation of the filling layers refer to the filling diagram of the concerned instrument configuration as described in the section Preparation of Reactors and Adsorption Filter on page 44 When using macro reactors 25 mm D then use the same packing instruction 17 mm 60 mm 355 mm 15 mm 5 mm 5 mm 100 mm 15 mm 17 mm 60 mm 355 mm 15 mm 5 mm 5 mm 130 mm 15 mm 30 mm 270 mm 270 mm A B Reactor f...

Page 75: ...he mouth of the reactor conical end Gently press the quartz wool using the rod provided as shown in Figure 44 Note The conical end of the quartz glass tube must be at the bottom WARNING Before using the filling materials required for this operation please read the hazard warnings and information reported in the Material Safety Data Sheets MSDS provided referring to the relevant CAS Chemical Abstra...

Page 76: ...onto the workbench 4 Pour sequentially the required filling materials into the reactor as shown in Figure 45 ensuring that each layer has the indicated size At each step gently press the quartz wool using the rod provided 5 The last step of the sequence consists in introducing a sufficient quantity of quartz wool to form the last required layer as shown in Figure 46 Figure 46 Introduction of Quart...

Page 77: ... wool to form the required layer as shown in Figure 47 Figure 47 Introduction of Quartz Wool into the Tube 2 While plugging the tube mouth with your hand press gently the quartz wool using the rod provided 3 Screw the nut complete with its seal onto the threaded mouth as shown in Figure 48 WARNING Before using the filling materials required for this operation please read the hazard warnings and in...

Page 78: ... Figure 49 Figure 49 Preparation of the Adsorption Filter The Ramped GC Oven The Ramped GC Oven is controlled by a JUMO controller The controller is pre programmed and locked It allows to switch between two setpoints SP1 and SP2 SP1 is the start temperature of 70 C SP2 is the end temperature of 240 C When receiving the GC start signal GC On from Isodat the Ramped GC Oven increases automatically th...

Page 79: ... If for any reason your system is not installed by a Thermo Fisher Scientific FSE you should ensure that the following operations are performed Standard Outfit Use the standard outfit checklist accompanying the instrument to verify that all items have been received Verify Site Preparation Before installing the EA IsoLink IRMS System for CNSOH your laboratory must be in compliance with the guidelin...

Page 80: ...quipment to the dealer or the factory without prior Thermo Fisher Scientific authorization Placing the Instrument Place the EA IsoLink IRMS System for CNSOH on the workbench allowing free access to electrical connections and gas lines You should already have prepared your laboratory according to the space requirements specified in the Preinstallation Requirements Guide The gas and power supplies s...

Page 81: ...tanks To regulate and connect tubing 1 Make sure the initial supply valves are turned off 2 Connect the regulator to the gas supply tank Use an open ended wrench or adjustable wrench to tighten the regulator connection 3 Determine the length of tubing you need Use only enough tubing to connect the instrument to the gas cylinders but allow enough slack in case the instrument should be moved at leas...

Page 82: ...of the EA IsoLink IRMS System for CNSOH and helps you install and configure peripheral devices and EagerSmart Data Handling Software Mounting Peripheral Devices Unpack them and follow instructions included with them Follow the instructions in the paragraphs below to connect your peripheral devices to the EA IsoLink IRMS System for CNSOH CAUTION The maximum pressures of the gases to supply the Flas...

Page 83: ...232 serial line connection is required 2 Connect the RS 232 cable supplied in the standard outfit between the COM1 or COM2 ports of your computer and the 9 pin connector marked RS 232 on the instrument connection panel If your computer is equipped with USB ports a Serial to USB adapter is required for properly connecting the cable 3 Plug in the instrument and computer power cables WARNING This ins...

Page 84: ...e 2 Open the furnaces compartment by lifting the cover and removing the protection plate See Figure 50 Figure 50 Access to the Furnace Compartment 3 If present remove the protection cap from the coupling union of each channel a By using a 32 mm wrench unscrew the reactor retaining nut Remove the protection cap the washer and the conical O ring as shown in Figure 51 Note In the following figures th...

Page 85: ...n Cap Reactor Retaining Nut Washer Conical O ring Coupling Union Right Channel Combustion Left Channel Pyrolysis Protection Cap Reactor Retaining Nut Washer Conical O ring Coupling Union Bottom Feed Connector ATTENTION Do not dispose of the protection cap but keep it in your lab for future use The protection cap should be reinstalled on the coupling union in case the instrument is not used for a l...

Page 86: ...t with washer and o ring on the BFC Insert the ceramic tube from top Fix it in this position using the upper o ring See Figure 53 Figure 53 Introduction of the Reactor with a Bottom Feed Connector 1 2 Insert the bottle brush in the glassy carbon tube and introduce it in the ceramic tube from top Use your other hand to carefully slip it over the o rings of the BFC while keeping the ceramic tube up ...

Page 87: ...rew the nut and slip it with washer and o ring over the ceramic tube at the bottom Fix it using the steel rod and a 32 mm wrench See Figure 56 Figure 56 Introduction of the Reactor with a Bottom Feed Connector 4 4 Slowly insert the granules into the glassy carbon tube from top Make sure no granule blocks the tube Check the height with the mark on the graphite crucible remover tool by placing the c...

Page 88: ...on tube 6 To complete the operation manually screw the fixing nut of the autosampler See Figure 63 Figure 57 Reinstall MAS Plus Autosampler 7 Close the furnace compartment with the protecting plate and the front cover To Install the combustion reactor into the right furnace 1 Carefully introduce and guide the reactor into the furnace until the conical O ring on the top of the reactor touches the f...

Page 89: ...tom of the furnaces slide first the reactor retaining nut then the washer and finally the conical O ring paying attention that the conical section of the O ring must be turned downwards See Figure 59 and Figure 60 Figure 59 Conical O ring Figure 60 Introduction of the Combustion Reactor Into the Right Furnace 2 3 Insert the reactor end into the coupling union located on the base of the furnace com...

Page 90: ...nd the 32 mm wrench to tighten the retaining nut See Figure 62 Figure 62 Introduction of the Combustion Reactor Into the Right Furnace 4 6 To complete the operation manually screw the fixing nut of the autosampler See Figure 63 Figure 63 Reinstall MAS Plus Autosampler 7 Close the furnace compartment with the protecting plate and the front cover Retaining Nut Coupling Union 32 mm Wrench Coupling Un...

Page 91: ... kPa Helium as reference gas 70 mL min for pressure 280 300 kPa Oxygen 250 mL min for pressure 250 kPa Table 19 O H Determination Pressure and Flow Parameters Setting Parameters Flow adjustment control through software by EFC t control Flow to set through EagerSmart Data Handling Software sodat Software Suite Helium as carrier gas 100 mL min for pressure 280 300 kPa Helium as reference gas 100 mL ...

Page 92: ...at Software Suite The instrument comes with installed Isodat Software Suite and appropriate configuration The software includes all necessary tools to operate the Flash IRMS and the mass spectrometer simultaneously If for any reason Isodat Software Suite is not installed install Isodat Software Suite as described in the Isodat Software Suite manual IMPORTANT A Flash IRMS can also be run as a stand...

Page 93: ...ure 64 MAS Plus Autosampler It consists of An anodized aluminum block sampler body provided on the left side with fittings for carrier gas and reference gas lines connection A 32 position sample holding tray numbered 1 to 32 It is provided with a reference pin to be introduced into the seat marked 1 one which has a locating mark See Figure 65 Contents MAS Plus Autosampler Overview MAS Plus Autosam...

Page 94: ...are not interchangeable See Figure 66 Figure 66 Additional Sample Trays The sample numbering is detailed in Table 20 Any sample has to place in the locating mark position The correct alignment of the locating mark is important for the installation of the sample tray on the MAS Plus autosampler See Figure 67 Table 20 Sample Tray Numbering Sample Tray Locating Mark Numbering 1 Seat marked 1 one from...

Page 95: ...o install a MAS Plus autosampler Tip The viewer on the sampler body allows observation of the Flash combustion Locating Mark Sample Tray Drum 4 Sample Tray Drum 3 Sample Tray Drum 2 Sample Tray Drum 1 Flash Combustion Before Sampling WARNING Before starting make sure that the EA IsoLink IRMS System for CNSOH is powered off and that the reactors required for your analyses are installed in their cor...

Page 96: ...t the autosampler on top of the left furnace is connected to the connector marked HO and the autosampler on top of the combustion furnace is connected to the connector marked NCS See Figure 20 on page 21 5 Install the samples tray a Manually rotate the toothed wheel clockwise until the guide located on its rim is perfectly aligned with the metal pin of the autosampler body b Check that the sample ...

Page 97: ...relevant seats marked 0 zero and placing the samples properly IMPORTANT Before installing an additional sample tray make sure that the samples to analyze are placed in all the seats of the previous tray installed CAUTION Before starting samples analyses make sure that the protection cover is positioned over the sample tray A complete deaeration of the area where samples are housed is only possible...

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Page 99: ...rect operation For more details please contact Thermo Fisher Scientific local representatives Should the instrument not be installed by Thermo Fisher Scientific personnel strictly adhere to the instructions reported in this section Electrical Requirement The instrument has the following power supply rating 24 Vdc through a portable external power supply level VI efficiency input 100 240 Vac 50 60 ...

Page 100: ...evice for Flash IRMS Elemental Analyzer This device is installed in replacement of the MAS Plus autosampler when present See Figure 69 Figure 69 Direct Injection Device CAUTION The power line and the connections between the instruments must maintain good electrical grounding Poor grounding represents a danger for you and might seriously affect the instrument performance Do not connect the AI 1310 ...

Page 101: ... Figure 70 Figure 70 Direct Injection Device Installation a Mount the septum by using the septum holder provided in the standard outfit b Connect the gas line to the direct injection device Installing the Sampler Support on the Flash IRMS Elemental Analyzer The AI 1310 AS 1310 sampling system is installed on the Flash IRMS Elemental Analyzer by using the appropriate support provided See Figure 71 ...

Page 102: ...racket on the top panel of the Flash IRMS Elemental Analyzer To install the sampler support on the Flash IRMS Elemental Analyzer 1 Mount the support bracket a From the top panel of the Flash IRMS Elemental Analyzer remove the four plastic caps covering the corresponding fixing holes See Figure 72 Figure 72 Plastic Caps Removal b Mount and fix the support bracket on the top panel of the Flash IRMS ...

Page 103: ...Mounting Sampler Support a Insert the provided fixing screw into each slot present on the support b Insert each screw into the relevant spacer paying attention to keep its largest surface turned toward the support base c Hold the spacers in position with their flat side toward the inside then place the sampler support on the support bracket d Guide the two fixing screws located on the external spa...

Page 104: ...support pin into the dedicated hole on the top plate See Figure 75 Figure 75 Mounting Support Pin Installing the AI 1310 AS 1310 on the Flash IRMS Elemental Analyzer This section provides the instruction for installing the AI 1310 AS 1310 on the Flash IRMS Elemental Analyzer See Figure 76 Figure 76 AI 1310 AS 1310 Installation Note The support pin is NOT required if you must install an AI 1310 Sup...

Page 105: ...Syringe Electrical Connections Starting up Installation of the Sampling Unit To install the sampling unit 1 Lift the sampling unit and insert it into the guide pivot located on the sampling system support Introduce the guide pivot into the hole provided on the bottom of the base See Figure 77 Figure 77 Installation of the Sampling Unit 2 Open the safety door and remove the protection of the inject...

Page 106: ...ting Manual Thermo Scientific Figure 78 Remove Protection 3 Insert the centering plate into its seat located in the right side section of the sampling unit base paying attention that the guide hole present on the arm of the centering plate correctly fits the injector nut See Figure 79 Figure 79 Centering Plate Protection Injection Nut Centering Plate ...

Page 107: ...dicated support plate into its appropriate housing of the sampling unit base Place the 105 position sample tray on the hub located on the support The system will automatically recognize the sample tray at the instrument power on See Figure 81 Figure 81 105 position Sample Tray Installing the Syringe The installation of the syringe is a simple operation However it must be performed with caution to ...

Page 108: ... for CNSOH Operating Manual Thermo Scientific To install the syringe 1 Open the safety door of the turret 2 Insert the syringe needle into the vial capture device See Figure 82 Figure 82 Syringe Installation 1 Vial Capture Device Syringe Body Seat Plunger Head Plunger Head Guide Syringe Needle Syringe Body Plunger Flange Flange Guide ...

Page 109: ...e 83 Syringe Installation 2 5 Close the safety door of the rotating turret Electrical Connections To perform electrical connections 1 By using the cable provided connect the 9 pin female connector marked RS232 located on the sampling unit back side to a 9 pin serial port connector COM of the PC 2 Plug in the tampered connector provided into the 6 pin female connector marked GC located on the sampl...

Page 110: ... 24 Vdc located on the sampling unit back side 2 Connect the power cord of the external power supply to the mains outlet The AI 1310 AS 1310 sampling system will automatically run the self testing routine during which the following automatic checks and settings are carried out Alignment between AI 1310 AS 1310 sampling system and injector Check of the turret travel Acknowledgment of the installed ...

Page 111: ...ne element per sample two elements per sample or three elements per sample The ASV allows to switch unattended between pyrolysis and combustion so that five elements of a sample can be analyzed from two sample drops This chapter covers the setup of dual measurements Single measurement can be derived from it Triple measurements are only recommended with the ramped GC Oven These measurements are cov...

Page 112: ...g up of the reactor avoids temperature overshooting and hence melting of the reduced copper contained in the reactor Alternatively use HeatUpFlash from the Context Menu with a right click on the Flash IRMS peripheral visualization See Figure 85 HeatUpFlash It is possible to perform dual measurements of hydrogen and oxygen as well as carbon and nitrogen from a single sample with the system This ana...

Page 113: ...hing to another Gas Configuration is necessary In contrast to a single element measurement in which the magnetic field runs the gamut from high to low and after that to the pre calculated magnetic field there is not sufficient time in dual measurement to perform this procedure for the next gas configuration For this reason a so called Jump Calibration from the first gas configuration to the next g...

Page 114: ... 6 Start Jump Calibration Procedure a Jump to CO along hysteresis curve b Perform a peak center for CO in order to get the signal height c Jump to H2 along hysteresis curve H is origin d Jump to CO not along hysteresis curve e Perform a peak center for CO in order to catch the peak f Repeat until magnet field setting is within the magnet window defined Note If no Jump Calibration is available in t...

Page 115: ...6 Using EA IsoLink IRMS System for CNSOH Performing a Jump Calibration Thermo Scientific EA IsoLink IRMS System for CNSOH Operating Manual 87 ...

Page 116: ... gas configuration denotes the starting gas configuration for an analysis When analyzing only one element e g CO2 the starting gas configuration must be changed accordingly The dilution for the second gas configuration appears only after defining a Switch Gas in the Time Event List see below The settings are examples and must be adjusted to your sample type Dynamic dilution is only available with ...

Page 117: ... you enter a waiting time of 10 seconds the software will delay the peak jump as specified in the time event list by a maximum of 10 seconds If the N2 peak has already reached background until the time specified in the time events list then the peak jump will occur straight away at that specified time If the N2 peak hasn t reached background until the specified time in the time events list and the...

Page 118: ... Creating an Isodat Method for N C Measurement Dual Measurement 90 EA IsoLink IRMS System for CNSOH Operating Manual Thermo Scientific Figure 91 NC Method Evaluation N2 Figure 92 NC Method Peak Detection N2 Figure 93 NC Method Printout N2Tab ...

Page 119: ...ing an Isodat Method for N C Measurement Dual Measurement Thermo Scientific EA IsoLink IRMS System for CNSOH Operating Manual 91 Figure 94 NC Method Evaluation CO2 Tab Figure 95 NC Method Peak Detection CO2 Tab Figure 96 NC Method Printout CO2 Tab ...

Page 120: ...to remove CO2 The analysis time has to be reduced even further In this case the entry Switch Gas CO2 can be deleted in the Time Event List of the Isodat Method Note The temperature of the high temperature conversion furnace left furnace may be different depending on the intended use of it Note Sampling delay and oxygen injection end vary depending on the sample nature O2 injection can be crucial i...

Page 121: ...on and Evaluation Parameters Figure 101 TCD Control Parameters Creating an Isodat Method for Single Mode S Measurements This Isodat method must be used with reactor packing as for the triple NCS measurements The elution time of the SO2 peak can be decreased if the GC oven temperature is ramped earlier For setting up an Isodat method for single mode S analysis only please refer to the Ramped GC Ove...

Page 122: ...mperatures of the reactor minimizing the bake out intervals The filling of the trap is given in Figure 102 using quartz wool at top and end and to separate the filling material Figure 102 Trap Pyrolysis Bottom Field Connector The EA IsoLink IRMS System for CNSOH is equipped with a bottom feed connector for high temperature conversion analysis also referred to as pyrolysis It allows high sample thr...

Page 123: ...ble on the crucible remover and inserting it into the glassy carbon tube The distance from the top of the crucible to the rim of the ceramic must be 270 mm Here is the hottest zone of the furnace 5 Drop the crucible into the reactor and introduce the insert on top of the glassy carbon tube Removing the Reactor from the Bottom Feed Connector BFC To remove the reactor from the bottom feed connector ...

Page 124: ... ConFloIV and IRMS in less than 7min offering fast sample throughput and high productivity The technique is suitable for both solid and liquid samples Different autosamplers are used to measure different sample types see Table 21 For the analysis of two isotopic species hydrogen and oxygen from a single sample a method that comprises both must be defined As soon as the hydrogen peak 3 in Figure 10...

Page 125: ...page 85 If a jump is already defined make sure the jump is re calibrated regularly It is recommended to perform a re calibration on a daily basis Preparing the Hardware To prepare the hardware components 1 Set the reactor temperature to 1450 C 2 Set the GC column temperature to 90 C Set it to 70 C if you are running N containing samples 3 Set the helium flow to 100mL min 4 Set the reference flow t...

Page 126: ...thod 5 Set the Instrument parameters for your new dual measurement method as shown in Figure 105 6 Click the tab Time Events see Figure 106 Figure 106 Time Events Page of the Dual Measurement Method 7 Set the Time Events parameters for your new dual measurement method as shown in Figure 106 8 Double click on CO in the column Switch Gas The Event Time is active since for example 130s ...

Page 127: ...tch is to be performed for example Isodat Eval PeakFound The switch is performed when the peak is found 11 For Waiting Time enter for example after 30 s If a peak is found the jump takes place If no peak is found the waiting time elapses before the jump takes place immediately 12 Click OK 13 Click the tab Evaluation H2 See Figure 108 Figure 108 Evaluation H2 Page of the Dual Measurement Method Not...

Page 128: ...Advanced Parameter to open the advanced parameter settings see Figure 110 Figure 110 Peak Detection H2 Page Advanced Parameters of the Dual Measurement Method 18 Set the Advanced Parameters parameters for your dual measurement method as shown in Figure 110 19 Select the Printout H2 tab of your new dual measurement method see Figure 111 Figure 111 Printout H2 of the Dual Measurement Method Note The...

Page 129: ...he Evaluation CO parameters for your new dual measurement method as shown in Figure 112 22 3 Click the tab Peak Detection CO see Figure 113 Figure 113 Peak Detection CO Page of the Dual Measurement Method Note Usually the printout of results is not performed until the complete measurement has been finished Therefore it is recommended to choose No Printout irw on the Printout H2 page Printout optio...

Page 130: ...ates 26 Click Save Save as to save this method with the file ending met 30 27 Enter a name for your method and click Save Creating an EA Method for H O Measurement The following figures show how an EA method for a dual analysis H O may be set up Figure 115 HO EA Method Instrument Temperature Note The Start Detection time must be adjusted so that the spikes on the mass traces from the magnet jump a...

Page 131: ... has to be reduced even further In this case the entry Switch Gas CO2 can be deleted in the Time Event List of the Isodat Method Note Sampling delay and oxygen injection end vary depending on the sample nature O2 injection can be crucial in a single reactor if it exceeds the required amount The reference flow is used for the autosampler purge This flow can be set to values between 20 mL min and 70...

Page 132: ...ual Thermo Scientific Creating a Sequence for Dual Measurement To create a new sequence for dual measurement 1 Place a sample for example 0 281 mg of benzoic acid in the solids autosampler 2 Open Acquisition 3 Click the New button to create a new sequence The File New dialog box opens see Figure 117 Figure 117 Creating a New Sequence ...

Page 133: ...e 119 Figure 119 Creating a Sequence for Dual Measurement 7 For each row enter the Amount of the individual sample for example 0 260 8 Enable to perform a Peak Center prior to measurement see Figure 119 9 Select an EA Method for example Py_iHeM eam 10 Edit text in Identifier 1 to identify the sample for example benzoic acid 11 Select Method for example Py_iHeM 12 Save the sequence with a name of y...

Page 134: ...ivated after 20 seconds for 20 seconds The H2 reference gas pulse is activated after 60 seconds for 20 seconds The sample is dropped into the reactor The H2 sample peak appears approximately 15 seconds after reaction start See Figure 121 The CO sample peak appears approximately 100 seconds after reaction start See Figure 121 The CO reference gas pulse is activated after 340 seconds for20 seconds T...

Page 135: ...e CO related peaks See Peaks Nr 4 5 and 6 in Figure 123 Figure 123 Dual Measurement CO Result Grid H3 Factor Determination Protonation reactions in the ion source result in H3 ion production The H3 portion of the m z ion beam is determined as the H3 factor The H3 factor is used to correct the H3 contribution to the m z3 signal A low and stable H3 factor is needed for a good DH H2 determination H3 ...

Page 136: ...Ω Procedure Sulfur measurements are performed using a specially equipped Elemental Analyzer Combustion and reduction are carried out in a single reactor filled with tungsten oxide WO3 and copper Cu as reducing agent The technique used for sulfur determination is based on the quantitative Dynamic Flash Combustion method The samples sometimes together with vanadium pentoxide V2O5 are wrapped in tin ...

Page 137: ...at enough reduced copper Cu is present in the combustion tube If this is not assured sulfur trioxide SO3 will only be reduced partially and isotope fractionation will occur Light isotopes 32 SO3 are reduced more easily than heavy isotopes 34 SO3 Therefore sulfur dioxide SO2 gas is depleted in 34 S compared to the original sample and the δ value becomes more negative Table 22 Parts of Sulfur Measur...

Page 138: ...e packing should be as shown in Figure 124 Figure 124 Packing of the Reactor About 150 to 200 analyses can be performed using the reactor type described above Before Starting a Sulfur Measurement We assume that the user already has working experience with the isotope ratio mass spectrometer Before starting a sulfur measurement make sure that 1 The Elemental Analyzer is set up that is The SO2 react...

Page 139: ...perature increase to 1020 C Increase column temperature to 100 C 14 It is recommended to keep the reactor over night at end temperature to stabilize the conditions Create a Gas Configuration for a Sulfur Measurement A Gas Configuration determines a combination of masses which are collected in the cups for evaluation of ratios and eventually δ values The Gas Configuration is specific for the partic...

Page 140: ...as follows To create a gas configuration for sulfur measurement 15 Open the Acquisition module 16 Open theGas Configuration Editor It is only available if no acquisition is running Per default the Gas Configuration CO2 is being created as the first one If the Gas Configuration SO2 has already beencreated it occurs in the list above If the Gas Configuration SO2 has not been created yet it does not ...

Page 141: ...w below a Mark SO2 b If Ratio Groups other than SO2are marked clear them all 19 Confirm by OK 20 The new Gas Configuration SO2 appears in the list as a row of its own Figure 125 Creating a New Gas Configuration 21 In the Calibration column select your current calibration file Note Figure 125 shows a common cup configuration as used in most Delta mass spectrometers i e universal triple collector If...

Page 142: ...on by a click on its row the number of cups required for measurement is displayed together with the assigned masses 23 Select a Calibration which is valid for the selected cups 24 Press the Save Close button Starting a Sulfur Measurement EA IsoLink Setting See Table 24 Note A value of 1 denotes unlimited Table 24 Setting for EA IsoLink Carrier 180 mL min Oxygen 25 mL min Reference 20 mL min Cycle ...

Page 143: ... Sulfur Measurement Thermo Scientific EA IsoLink IRMS System for CNSOH Operating Manual 115 Defining an Isodat Method Instrument Figure 126 Starting a Sulfur Measurement Instrument Tab Time Events Figure 127 Starting a Sulfur Measurement Time Events Tab ...

Page 144: ...Thermo Scientific Evaluation Figure 128 Starting a Sulfur Measurement Evaluation Tab Peak Detection Figure 129 Starting a Sulfur Measurement Peak Detection Tab Printout Figure 130 Starting a Sulfur Measurement Printout Tab Events During Acquisition See Figure 127 on page 115 and Figure 130 on page 116 1 Peak center procedure ...

Page 145: ...nce Gas pulse activated at 90 s duration 20 s It is assigned as Standard pulse for δ value calculation See Time column in Figure 127 on page 115 4 EA starts at 105 s At this time the oxygen is injected into the reactor 5 Autosampler activated by EA after a sampling delay defined in the EA method e g 10 s after oxygen injection 6 Sample peak appears approximately 100 s after Autosampler activation ...

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Page 147: ...suggesting to refer to the documentation accompanying the instrument When a maintenance operation is performed the operator must have received proper training to carry out specific actions WARNING When the instrument is switched off consider that its does not cool down immediately but heat tends to concentration in the upper part of the furnaces area It should be made clear that it is better to co...

Page 148: ...tly and will reduce operating costs The standby conditions can be defined by the operator There are these options Reduce the flow only This option reduces the carrier and reference flow to 10 mL min and the oxygen to 0 mL min Define an EA method This option allows to define settings in an EA method which are uploaded to the EA The Standby function can be activated immediately or automatically at t...

Page 149: ...the standby function after sequence end In the Sequence Options of an Isodat Software Suite Software Suite sequence there are two boxes See Figure 132 Sequence Standby Options ConFlo IV Standby after Sequence Reduces the helium flow in the ConFlo IV to a minimum required to protect the ion source from ingress of air through the Open Split The following action are taken The ConFlo is set into LF Mo...

Page 150: ...he column lifetime in EA IsoLink IRMS System for CNSOH instrument is evaluated in years Replacement of the seals of the reactors coupling unions placed on the furnace compartment base Current Maintenance Program Each reactor each filter and relevant fillings need to be replaced according to the analytical configuration used Please refer to the CookBook for the best analytical setup for your sample...

Page 151: ...To replace the filling material in adsorption filters on page 124 To replace the filling material in quartz reactors Remove the quartz reactor from the furnace then do the following 1 Introduce the cleaning tool into the reactor as shown in Figure 134 Figure 134 Removing the Filling Material from a Quartz Reactor 2 Rotate the tool exerting a slight pressure to scrape off the filling material 3 Col...

Page 152: ... the filter nut and remove the filling material 2 Restore the sequence of the layers of filling materials introducing the new ones into the filter Ashes Removal and Crucible Cleaning To remove the ashes and clean the crucible Remove the crucible from the reactor If the crucible is made of quartz remove the ashes by using a spatula If the crucible is made of steel then do the following 1 Introduce ...

Page 153: ...granules in a separate bowl 3 Clean the inside of the glassy carbon tube with the bottle brush 4 Insert new quartz wool and silver wool 5 Clean the granules with a tissue or a sieve until they are shiny again 6 Remove all granules that are not shiny anymore or show a porous surface 7 Clean the outside of the crucible with a tissue and remove the molten silver inside or use a new one To clean repla...

Page 154: ...tweezers see A of Figure 137 and place it on a clean cloth 6 Insert the crucible remover inside the graphite crucible See B in Figure 137 7 Pull the graphite crucible out of the reactor See C in Figure 137 8 Drop a new graphite crucible into the reactor or remove the deposits outside and inside of the graphite crucible and use it again 9 Remount the parts proceeding in the reverse order Maintenanc...

Page 155: ...described in the To clean replace the graphite crucible operating sequence After cleaning the crucible may be used again See also reactor maintenance Replacing the Gas Chromatographic Column The instrument rarely requires the gas chromatographic column replacement however in case operate according to the following operating sequence To replace the gas chromatographic column in the GC oven of the E...

Page 156: ...and the gas chromatographic column Figure 139 Compartment Housing the Chromatographic Column 3 Unscrew the fittings from the column ends and remove the column from the compartment 4 Introduce the new column and connect its ends to the fittings 5 Re mount the protection panel and the adsorption filters Note According to the instrument configuration there can be one or two analytical columns Securin...

Page 157: ...agerSmart Data Handling Software Main Menu Edit Edit Elemental Analyzer parameters or just click the icon The Analyzer Parameter window is visualized 3 Click Send and wait 2 3 minutes to discharge the gas out the circuit 4 Remove the frontal cover of the MAS Plusautosampler as shown in Figure 140 Figure 140 Removal of the MAS Plus Autosampler Cover 5 From Main Menu select the menu View View Elemen...

Page 158: ...mpler 10 Re introduce the shaft into the autosampler until in place keeping its rack turned downward as shown in Figure 143 Figure 143 Reinstalling the Shaft 1 11 Slightly pushing the shaft with one finger of your hand as shown in Figure 144 click Step Sampler tray position again The autosampler mechanism first tries to eject the shaft then on the motor reversal the mechanism will hook the shaft a...

Page 159: ...o their relevant seats 1 Remove the three from the shaft body by using tweezers or a spatula paying attention to not scratch the shaft 2 Take the new green O rings package and the removal tool 3 Insert the first O ring into the internal seat of the shaft a Place one of the three O ring with the lip turned inwards on the conical section of the tool Materials Required Tweezers or spatula Green O rin...

Page 160: ...ace the second O ring with the lip turned inwards on the conical section of the tool b Move the O ring along the tool up to reach the border c Move the tool on the shaft body up to reach the middle seat d Move and inset the O ring into the middle seat then remove the tool 5 Insert the third O ring into the external cavity of the shaft The use of the tool is not necessary a Manually place the last ...

Page 161: ...the introduction sample fitting with the nut for the 18 mm OD reactor P N 35008417 from the MAS Plus paying attention to do not damage the internal gasket 3 Screw manually the introduction sample fitting with the nut for the 25 mm OD macro reactor P N 35008418 provided in the MAS Plus standard outfit into the MAS Plus Tighten the fitting by using the 23 33 mm open ended wrench 4 Access the furnace...

Page 162: ... with the proper Allen wrench Place and fix the upper connector for 25 mm OD macro reactor 6 On the top of left right furnace remove the adaptor for 18 mm OD reactor and its sealing adapter 7 Reinstall the protecting plate and the cover of the furnace compartment 8 Install the macro reactor tube into the furnace and reinstall the MAS Plus Upper Connector for 18 mm OD Reactor Upper Connector for 25...

Page 163: ...own the instrument and call an authorized customer support engineer for proper actions The service engineer must be fully informed on the nature of the concerned substance WARNING Cleaning must be performed with the instrument off the furnaces at room temperature and the power cord disconnected WARNING It is your responsibility to avoid that dangerous liquids and or materials seeping inside the EA...

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Page 165: ...oblem Diagnosis Remedy High nitrogen blank Presence of leak Check that helium and oxygen lines are sealed and in case eliminate possible leak Oxygen line or cylinder contaminated Purge for 10 20 minutes Replace the contaminated cylinder Autosampler not purged Check that the helium flow is correct High constant nitrogen blank in several sequential analyses Oxygen cylinder contaminated Replace the o...

Page 166: ...quate purity Exclude autosampler and check the oxygen blank Inadequate oxygen dosage Increase oxygen injection time High carbon blank Tin containers contaminated Check the tin container box tweezers work bench are clean Memory effect due to bad combustion of previously run analyses Remove ash and analyze lower amounts of sample Decreasing nitrogen blank values Oxygen line contaminated Wait 10 20 m...

Page 167: ...able 26 to find out the error status and have mode information Figure 146 Special function window The following Table 26 reports the error messages and the explanation of the relevant correlated problem Table 26 Error Messages Sheet 1 of 2 Message Description What to do Under voltage protection Safety Cut Off message Voltages supplied to the electrical circuits are too low or out of tolerance Chec...

Page 168: ...a the flow of oxygen does not reach the set point Verify that the pressure at the manometer is at second stage higher or equal to 350 kPa Table 26 Error Messages Sheet 2 of 2 Message Description What to do CAUTION The error message is generally due to the specific cause indicated Sometimes it may generated by different electric factors or caused by failures not depending on the system In this case...

Page 169: ...a Handling Software Manual To install EagerSmart Data Handling Software Contents EagerSmart Software Installation Configuring the Analyzer Performing a Leak Test Adjusting the Detector Signal Level View Sample Being Acquired Configuring EagerSmart Data Handling Software Using Isodat Software Suite and EagerSmart Data Handling Software at the Same Time ATTENTION If you want to operate with the EA I...

Page 170: ...rol Panel Add Remove Programs b In the dialog window visualized select the precedent Eager version to remove c Click Add Remove 2 Install the new version of EagerSmart Data Handling Software When the USB stick is introduced in a free USB port of the computer the following installation window is visualized See Figure 147 Figure 147 EagerSmart Data Handling Software Installation Menu 3 Start install...

Page 171: ... the operation reboot the computer Start EagerSmart Data Handling Software again selecting Start Programs EagerSmart 8 Follow the prompted indications At the end of the installation the Main Menu is visualized EagerSmart Main Menu The Main Menu of EagerSmart Data Handling Software shown in Figure 149 is the starting point to enter all menus and relevant functions Figure 149 EagerSmart Data Handlin...

Page 172: ... d Click OK The system ask to exit and reboot EagerSmart e At the reboot of EagerSmart the simplified Main Menu for IRMS is visualized See Figure 151 Figure 151 Main Menu for IRMS Menus and buttons of the Main Menu for IRMS are described in the following Table 28 and Table 29 respectively Table 28 Main Menu for IRMS Description of Menus Menu Description Sub menus and Options File Monitors the anal...

Page 173: ...ings Polarity Positive i In the field Sampler Setting select the type of autosampler installed on the instrument In the case of autosampler for liquid samples also specify the serial port of the computer to which the autosampler is connected and the number of vials Click Ok to go back to the window of Figure 152 then click Ok to return to Main Menu for IRMS 2 In Main Menu for IRMS click the icon T...

Page 174: ...out 50 minutes the furnaces reach the temperature settings and the LED Ready on the status panel lights up The instrument is now ready to run analyses However before starting an analytical cycle a leak test must be carried out for checking the Carrier and Reference pneumatic circuits are free of leaks Note The leak test must be performed also any time a component of the pneumatic circuit is replac...

Page 175: ...w the operating sequence To check the leaks on page 147 To check the leaks 1 In Main Menu for IRMS click the icon The following dialog window is visualized See Figure 154 Figure 154 Analyzer Status Page 2 Select Special Functions tabbed page See Figure 155 Figure 155 Special Function Tab 3 In the field Command click Leak Test The window of Figure 156 is visualized indicating the status of the leak...

Page 176: ...d Reference Flow must be within 0 and 3 mL min Higher values indicate that the system is not leak free c Click Stop and Done for ending the leak test and restoring the flow operating values Adjusting the Detector Signal Level To adjust the level of the TCD detector s signal follow the instructions reported in the operating sequence To adjust the level of the detector signal on page 148 To adjust t...

Page 177: ...uisition of the instrument currently in use The system after a confirmation stops the acquisition saving the chromatogram data up to the moment of the stop command and a report is generated if required Exit Monitor Detector Exits from detector monitoring The program returns to the Main Menu but the acquisition continues in the background View Menu Gives access to the following functions Fit to Hig...

Page 178: ...lly re draws the entire chromatogram with the new required scale This modification has effect only on the real time display but it does not affect the integration and the chromatogram printout Set Manual Scale Sets manually the values for the beginning and the full scale You can enter the signal on the window display or you can display the signal with a desired attenuation This modification has ef...

Page 179: ...our EA IsoLink IRMS System for CNSOH for opening the relevant contents For example Temp 1 Analyzer 1 Double click on the Eager ini file for opening the file See Figure 159 Figure 159 Eager ini File 1 6 Search Pyrolysis 0 line Indicates the configuration of EagerSmart Data Handling Software to control a standard EA IsoLink IRMS System for CNSOH For controlling a EA IsoLink IRMS System for CNSOH mod...

Page 180: ...ite 1 Before using either software make sure the other software is completely closed 2 Open Acquisition The OCX is automatically registered for Isodat Software Suite if EagerSmart Data Handling Software is completely closed down first If problems occur a Safety Cut Off message is visualized Go to the Isodat Software Suite Configurator and Re Register OCX then wait 10 seconds 3 Close Configurator a...

Page 181: ... IRMS as Stand alone Instrument Using Isodat Software Suite and EagerSmart Data Handling Software at the Same Time Thermo Scientific EA IsoLink IRMS System for CNSOH Operating Manual 153 EAGER For FLASH Active X Vers_1_x ...

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Page 183: ...mer Service Engineer Ctrl control key of the keyboard d depth DAC digital to analog converter dc direct current DS data system EMC electromagnetic compatibility ESD electrostatic discharge ºF Fahrenheit FSE Field Service Engineer ft foot g gram GND electrical ground h height h hour H hydrogen harmonic distortion A high frequency disturbance that appears as distortion of the fundamental sine wave H...

Page 184: ...ry RS 232 industry standard for serial communication s second slow average A gradual long term change in average RMS voltage level with typical duration greater than 2 s surge A sudden change in average RMS voltage level with typical duration between 50 μs and 2 s S sulfur TCD Thermal Conductivity Detector transient A brief voltage surge of up to several thousand volts with a duration of less than...

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