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Revision A - 122 4730

ConFlo IVOperating Manual


ConFlo IVOperating Manual


© 2007 Thermo Fisher Scientific All rights reserved.

“Swagelok” is a registered trademark of the Crawford Fitting Company. “Teflon” is a registered trademark of E. I. du Pont de Nemours & Co. “VICI” is a registered trademark of Valco Instruments Co. Inc. and VICI AG. “Valco” is a registered trademark of Valco Corporation.

All other trademarks are the property of Thermo Fisher Scientific and its subsidiaries.

Technical information contained in this publication is for reference purposes only and is subject to change without notice. Every effort has been made to supply complete and accurate information; however, Thermo Fisher Scientific assumes no responsibility and will not be liable for any errors, omissions, damage, or loss that might result from any use of this manual or the information contained therein (even if this information is properly followed and problems still arise).This publication is not part of the Agreement of Sale between Thermo Fisher Scientific and the purchaser of an Thermo Fisher Scientific system. In the event of any conflict between the provisions of this document and those contained in Thermo Fisher Scientific’s Terms and Conditions, the provisions of the Terms and Conditions shall govern.System Configurations and Specifications supersede all previous information and are subject to change without notice.

Printing History: Revision A printed in September 2007.

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About this Manual

Welcome to the Thermo Fisher Scientific, ConFlo IV system! The ConFlo IV is an interface for the Thermo Fisher Scientific family of advanced isotope ratio mass spectrometer (IRMS) detectors.

This ConFlo IV Operating Manual intends to be a user guide for working with the combined system of an Elemental Analyzer (EA) and an Isotope Ratio Mass Spectrometer (IRMS) extended by a ConFlo IV. As the Elemental Analyzer and the IRMS have manuals of their own, this manual will focus on information specific to the ConFlo IV system.

It is assumed that the user is familiar with clean operating procedures and sample preparation. The user should also have some working experience with IRMS and the software Isodat 2.5.

This manual includes the following chapters:

• Chapter 1: “Functional Description” gives basic information about working principle and features of the ConFlo IV. It also describes the hardware layout of the ConFlo IV.

The chapter outlines the open split principle (sample open split and reference open split) and sample/standard referencing. Afterwards, the setup of the ConFlo IV is discussed, that is how to connect low-flow peripherals and high-flow peripherals. Furthermore, it treats the working principle of the incremental helium flow controller.

• Chapter 2: “Isodat 2.5” first describes how to create a ConFlo IV configuration in Isodat 2.5. Then it outlines the installation of an autosampler. Afterwards, the ConFlo IV Interface window is explained. The chapter ends with a description of the sequence batcher.

• Chapter 3: “Reference Gas Measurements” deals with the zero enrichment test and the linearity test as two means to check the basic performance of the mass spectrometer prior to execute sample sequences. Furthermore, the H3 factor calibration is outlined as a special linearity test which corrects for the non-linearity caused by the formation of H3

+ ions.

• Chapter 4: “Operating ConFlo IV with EA” starts by explaining the SmartEA™ function. Afterwards, the tab pages of an Elemental Analyzer method are discussed.

Thermo Fisher Scientific ConFlo IV Operating Manual i

Preface

Then, it is outlined how to set the instrument to standby and how to use the Auto-Ready function. The chapter ends by describing a weight percent determination.

• Chapter 5: “Operating ConFlo IV with TC/EA” illustrates how ConFlo IV is operated in connection with a TC/EA. Especially, the signal transmission from the ConFlo IV to the MAS 200R is treated.

• Chapter 6: “Technical Information” lists spare parts and treats the ConFlo IV installation kit. Furthermore, it deals with the connections to the ConFlo IV and the incremental helium flow controller.

The chapter ends with a description of the ConFlo IV Extended window which is not recommended to be used for standard operation of the ConFlo IV. Instead, it is mainly used for diagnostic purposes or for direct access to a specific valve.

ii ConFlo IV Operating Manual Thermo Fisher Scientific

PrefaceChanges to the Manual

Changes to theManual

To suggest changes to this manual, please send your comments to:

Editors, Technical DocumentationThermo Fisher ScientificAdvanced Mass SpectrometryHanna-Kunath-Str. 11

28199 Bremen

Germany

[email protected]

You are encouraged to report errors or omissions in the text or index.Thank you.

Thermo Fisher Scientific ConFlo IV Operating Manual iii

PrefaceTypographical Conventions

TypographicalConventions

Typographical conventions have been established for Thermo Fisher Scientific manuals for the following:

• Data input

• Admonitions

• Topic headings

Data Input Throughout this manual, the following conventions indicate data input and output via the computer:

• Messages displayed on the screen are represented by capitalizing the initial letter of each word and by italicizing each word.

• Input that you enter by keyboard is identified by quotation marks: single quotes for single characters, double quotes for strings.

• For brevity, expressions such as “choose File > Directories” are used rather than “pull down the File menu and choose Directories.”

• Any command enclosed in angle brackets < > represents a single keystroke. For example, “press <F1>” means press the key labeled F1.

• Any command that requires pressing two or more keys simultaneously is shown with a plus sign connecting the keys. For example, “press <Shift> + <F1>” means press and hold the <Shift> key and then press the <F1> key.

• Any button that you click on the screen is represented in bold face letters. For example, “click on Close”.

iv ConFlo IV Operating Manual Thermo Fisher Scientific

PrefaceTypographical Conventions

Admonitions Admonitions contain information that is important, but not part of the main flow of text.

Admonitions can be of the following types:

• Note – information that can affect the quality of your data. In addition, notes often contain information that you might need if you are having trouble.

• Caution – information necessary to protect your instrument from damage.

• Warning – hazards to human beings. Each Warning is accompanied by a Warning symbol.

Topic Headings The following headings are used to show the organization of topics within a chapter:

Chapter Name

The following headings appear in the left column of each page:

Second Level Topics

Third Level Topics

Fourth Level Topics

Thermo Fisher Scientific ConFlo IV Operating Manual v

PrefaceSafety and EMC Information

Safety and EMCInformation

In accordance with our commitment to customer service and safety, these instruments have satisfied the requirements for the European CE Mark including the Low Voltage Directive.

Designed, manufactured and tested in an ISO9001 registered facility, this instrument has been shipped to you from our manufacturing facility in a safe condition.

Caution This instrument must be used as described in this manual. Any use of this instrument in a manner other than described here may result in instrument damage and/or operator injury.

Identifying SafetyInformation

The ConFlo IV Operating Manual contains precautionary statements that can prevent personal injury, instrument damage, and loss of data if properly followed. Warning symbols alert the user to check for hazardous conditions. These appear throughout the manual, where applicable, and are defined in Table i.

Table i. Warning Symbols

Symbol Description

General This general symbol indicates that a hazard is present, which if not avoided, could result in injuries.

The source of danger is described in the accompanying text.

Electric Shock High voltages capable of causing personal injury are used in the instrument. The instrument must be shut down and disconnected from line power before service or repair work is performed.

ExplosiveThis symbols points to possible danger because of explosive gases and gas mixtures.

Noxious This symbol alerts to hazards resulting from noxious fumes.

Hot Surface / Heat Allow heated components to cool down before servicing them!

Poisonous Gases This symbols points to possible danger because of poisonous gases and vapors.

vi ConFlo IV Operating Manual Thermo Fisher Scientific


Material Safety Data Sheets (MSDS) provide summarized information on the hazard and toxicity of specific chemical compounds. MSDSs also provide information on the proper handling of compounds, first aid for accidental exposure, and procedures for the remedy of spills or leaks. Producers and suppliers of chemical compounds are required by law to provide their customers with the most current health and safety information in the form of an MSDS. Read the material safety data sheets for each chemical you use.

Instrument-SpecificHazards

Every instrument has specific hazards, so be sure to read and comply with the following general warnings and safety precautions. They will help ensure the safe, long-term use of your system. More specific warnings and recommendations are given in the corresponding chapters of the ConFlo IV Operating Manual.

1. The system should be operated by trained personnel only. Read the manuals before starting the system and make sure that you are familiar to the warnings and safety precautions!

2. Accurate results can be obtained only, if the system is in good condition and properly calibrated.

3. Service by the customer should be performed by trained qualified personnel only and should be restricted to servicing mechanical parts!

4. Service on electronical parts should be performed by Thermo Fisher Scientific Service Engineers only!

5. Before plugging in any of the instrument modules or turning on the power, always make sure that the voltage and fuses are set appropriately for your local line voltage.

6. Only use fuses of the type and current rating specified. Do not use repaired fuses and do not short-circuit the fuse holder.

7. The supplied power cord must be inserted into a power outlet with a protective earth contact (ground). When using an extension cord, make sure that the cord also has an earth contact.

Thermo Fisher Scientific ConFlo IV Operating Manual vii


8. Do not change the external or internal grounding connections.Tampering with or disconnecting these connections could endanger you and/or damage the system.

Caution The instrument is properly grounded in accordance with regulations when shipped. You do not need to make any changes to the electrical connections or to the instrument’s chassis to ensure safe operation.

9. Never run the system without the housing on. Permanent damage can occur.

10. Do not turn the instrument on if you suspect that it has incurred any kind of electrical damage. Instead, disconnect the power cord and contact a Service Representative for a product evaluation. Do not attempt to use the instrument until it has been evaluated. (Electrical damage may have occurred if the system shows visible signs of damage, or has been transported under severe stress.)

11. Damage can also result if the instrument is stored for prolonged periods under unfavorable conditions (e.g., subjected to heat, water, etc.).

12. Always disconnect the power cord before attempting any type of maintenance.

13. Capacitors inside the instrument may still be charged even if the instrument is turned off.

14. Never try to repair or replace any component of the system that is not described in this manual without the assistance of your service representative.

15. When leaving the system, make sure, that all protective covers and doors are properly connected and closed, and that heated areas are separated and marked to protect for unqualified personnel!

Warning Keep the system away from heat, e.g. radiators, to avoid damage to the internal circuits and the external surface!

viii ConFlo IV Operating Manual Thermo Fisher Scientific


Warning Avoid using aerosol sprays near the system as this could cause sudden ignition of the spray!

Warning Do not clean ConFlo IV using paint thinner, alcohol or other organic solvents!

Warning Do not put any objects, especially liquids, upon ConFlo IV!

Thermo Fisher Scientific ConFlo IV Operating Manual ix

Contents

Chapter 1 Functional Description.............................................................1-1Introduction...................................................................... 1-2Open Split Principle ......................................................... 1-3Sample/Standard Referencing ........................................... 1-3Setup of ConFlo IV........................................................... 1-4

Connection to Low-Flow Peripherals ............................. 1-5Connection to High-Flow Peripherals............................ 1-5Incremental Helium Flow Controller............................. 1-8Helium Consumption.................................................... 1-9Incremental Helium Dilution in Sample Open Split.... 1-10

Sample Open Split .......................................................... 1-11Reference Open Split ...................................................... 1-12

Reference Gas Consumption........................................ 1-15

Chapter 2 Isodat 2.5.....................................................................................2-1Creating ConFlo IV Configurations.................................. 2-2

Creating a Configuration for Two Flashs ....................... 2-3Installing a Flash EA or Flash HT .................................. 2-4

Adjusting Properties of Flash EA or Flash HT............. 2-4Installing an Autosampler.................................................. 2-6ConFlo IV Interface Window ........................................... 2-8

Dynexternals Window ................................................. 2-10Linearity Tab ............................................................ 2-10References Tab.......................................................... 2-12LF Dil Tab................................................................ 2-13HF I Dil Tab and HF II Dil Tab .............................. 2-14

Sequence Batcher ............................................................ 2-18Principle....................................................................... 2-18Using Sequence Batcher ............................................... 2-18Prior to Sequence Batch Execution .............................. 2-20Sequence Batch Execution ........................................... 2-21

Chapter 3 Reference Gas Measurements ...............................................3-1Zero Enrichment Test....................................................... 3-2

Setting up a Zero Enrichment Method .......................... 3-2Sequence and Starting the Run ...................................... 3-6

Linearity Test.................................................................... 3-9General Remarks............................................................ 3-9Setting up a Linearity Method ....................................... 3-9Sequence and Starting the Run .................................... 3-12

H3 Factor Calibration ..................................................... 3-15

Thermo Fisher Scientific ConFlo IV Operating Manual xi

Contents

General Remarks.......................................................... 3-15Setting up a H3 Factor Calibration Method ................. 3-16Sequence and Starting the Run .................................... 3-19

Chapter 4 Operating ConFlo IV with EA.................................................. 4-1SmartEA™ Function .......................................................... 4-2

Dynamic Dilution.......................................................... 4-2Example ...................................................................... 4-4Calibrating the TCD-MS Signal Relation ................... 4-4

Fixed .............................................................................. 4-4None.............................................................................. 4-4

EA Method ....................................................................... 4-5Instrument Tab.............................................................. 4-5

Temperature ............................................................... 4-5Flow/Timing............................................................... 4-6Detector...................................................................... 4-8

Evaluation Tab............................................................... 4-8TCD Control Parameter Tab......................................... 4-9

Set Instrument to Standby and Auto-Ready Function..... 4-10Weight Percent Determination ....................................... 4-11

Chapter 5 Operating ConFlo IV with TC/EA............................................ 5-1

Chapter 6 Technical Information ............................................................. 6-1Installation Kit for ConFlo IV........................................... 6-2Connections to ConFlo IV................................................ 6-3

Front Panel .................................................................... 6-4Rear Panel...................................................................... 6-5

Rear Panel from Outside ............................................. 6-6Connecting Elemental Analyzer by EA Splitter ........... 6-7SmartEA Option......................................................... 6-9Remark on Trigger Outputs........................................ 6-9Rear Panel from Inside .............................................. 6-10

View Inside ConFlo IV ................................................ 6-10Inlet Module ............................................................. 6-10Open Split Module ................................................... 6-12

Adress List of ConFlo IV.............................................. 6-13Compressed Air Connections ....................................... 6-14Interconnections Scheme of ConFlo IV ....................... 6-14

Incremental Helium Flow Controller .............................. 6-16ConFlo IV Diagnosis Window........................................ 6-17

Glossary .................................................................................... G-1

Index ............................................................................................ I-1

xii ConFlo IV Operating Manual Thermo Fisher Scientific

Figures

Open split principle .............................................................................. 1-3Principle of ConFlo IV .......................................................................... 1-4Sample open split operation for low-flow applications ........................... 1-5Sample open split operation for high-flow applications ......................... 1-6Rear panel of ConFlo IV ....................................................................... 1-6Connecting Elemental Analyzer to ConFlo IV ...................................... 1-7Schematic incremental helium flow controller - sample OS ................... 1-8Schematic incremental helium flow controller - reference OS ............... 1-9Reference gas supply ............................................................................ 1-12Dynamic range of reference gas dilution steps ..................................... 1-14List of predefined Elemental Analyzer - ConFlo IV sets ......................... 2-2Properties of Flash EA or Flash HT ....................................................... 2-5Available devices .................................................................................... 2-7Selecting COM Port of autosampler ..................................................... 2-8ConFlo IV Interface window ................................................................. 2-9Status of the two reference gas batches ................................................ 2-10Dynexternals - linearity parameters ..................................................... 2-11Dilution predelay ................................................................................ 2-12Dynexternals - reference gas connections ............................................. 2-12Dynexternals - dilution parameters for low-flow (LF) peripheral ......... 2-13Dynexternals - Dilution parameters for high-flow (HF) peripheral ...... 2-15Reference dilution and reference gas intensities ................................... 2-17Drag&drop of sequences ..................................................................... 2-19Sequences available in sequence batcher .............................................. 2-19Commands for sequence batch execution ............................................ 2-20Creating a zero enrichment method ...................................................... 3-2Zero enrichment test for CO2 - Instrument tab .................................... 3-3Zero enrichment test for CO2 - Time events tab ................................... 3-4Zero enrichment test for CO2 - Evaluation tab ..................................... 3-4Zero enrichment test for CO2 - Peak detection tab ............................... 3-5Zero enrichment test for CO2 - Printout tab ......................................... 3-5Creating a new sequence ....................................................................... 3-6Selecting IRMS method within sequence grid ....................................... 3-6Zero enrichment test for CO2 - Chromatogram .................................... 3-7Zero enrichment test for CO2 - Result grid ........................................... 3-7Zero enrichment test for CO2 - Calculation of stability ........................ 3-8Zero enrichment test for CO2 - Calculated stability for δ13C/12C ......... 3-8Zero enrichment test for CO2 - Calculated stability for δ18O/16O ........ 3-8Creating a linearity method ................................................................. 3-10Linearity test for CO2 - Instrument tab ............................................... 3-10Linearity test for CO2 - Evaluation tab ................................................ 3-11Creating a new sequence ..................................................................... 3-12Selecting IRMS method within sequence grid ..................................... 3-12

Thermo Fisher Scientific ConFlo IV Operating Manual xiii

Figures

Linearity test for CO2 - Chromatogram .............................................. 3-13Linearity test for CO2 - Result grid ..................................................... 3-13Linearity test data for 13C/12C and 18O/16O measurements ............... 3-14Creating a H3 factor calibration method ............................................. 3-16H3 factor calibration method - Instrument tab .................................... 3-17H3 factor calibration method - Evaluation tab ..................................... 3-18H3 factor calibration method - Peak Detection tab ............................. 3-18Creating a new sequence ..................................................................... 3-19Selecting IRMS method within sequence grid ..................................... 3-19H3 factor calibration - Chromatogram ................................................ 3-20H3 factor calibration - Result grid ....................................................... 3-20Dynexternals - Dilution parameters for high-flow (HF) peripheral ........ 4-2Creating a new EA method ................................................................... 4-5Instrument tab - Temperature ............................................................... 4-6Instrument tab - Flow/Timing .............................................................. 4-7Instrument tab - Detector ..................................................................... 4-8Evaluation tab ....................................................................................... 4-9TCD control parameter tab .................................................................. 4-9Interface standby after sequence checkbox ........................................... 4-10Auto-Ready tab in Status window of Elemental Analyzer .................... 4-11EA Status window - Detector tab ........................................................ 4-12Signal transmission from ConFlo IV to MAS 200R .............................. 5-1Start Sampler column in time events list ............................................... 5-2Ref 1 batch and Ref 2 batch at front panel ............................................ 6-4Rear panel - viewed from outside .......................................................... 6-6EA splitter (Part No. 122 8540) ............................................................ 6-7Connecting Elemental Analyzer to ConFlo IV by EA splitter ................ 6-8Block diagram (output stage) ................................................................ 6-9Rear panel with valve groups - viewed from inside .............................. 6-10Inlet module (Part No. 122 4450) ...................................................... 6-10Open Split module (Part No. 122 4450) ............................................. 6-12Addresses for ConFlo IV ..................................................................... 6-13Connecting ConFlo IV to DELTA V .................................................. 6-13Compressed air connections ................................................................ 6-14Interconnections scheme of ConFlo IV ............................................... 6-15Capillary positions in OS Reference and OS Sample ........................... 6-16Incremental helium flow controller (Part No 122 2330) ..................... 6-16ConFlo IV Diagnosis window ............................................................. 6-17

xiv ConFlo IV Operating Manual Thermo Fisher Scientific

Tables

Capillary dimensions and flows through different valves of sample open split 1-10Sample gas dilution steps - Example for 80 mL/min flow from EA ..... 1-11Capillary dimensions and flows through valves of reference diluter ..... 1-13Reference gas dilution steps ................................................................. 1-14Linearity tab ........................................................................................ 2-11Dilution values at EA carrier flows from 80-140 mL/min ................... 2-15Dilution values at EA carrier flows from 80-140 mL/min ................... 2-16Commands for sequence batch execution ............................................ 2-21Printout tab ........................................................................................... 3-5Dilution values at EA carrier flows of 80-140 mL/min .......................... 4-3Dilution values at EA carrier flows of 80-140 mL/min (pre-split on) .... 4-3Selected parts of ConFlo IV installation kit (Part No. 122 2770) .......... 6-2Parts of basic module of ConFlo IV (Part No. 122 2760) ..................... 6-3Parts at front panel of ConFlo IV .......................................................... 6-4Ports, functions and connector types at rear panel ................................. 6-7Capillaries of EA splitter ........................................................................ 6-8Parameters for trigger outputs ............................................................... 6-9Parts of inlet module (Part No. 122 4450) .......................................... 6-11Parts of 5-fold valve cluster for reference gas (Part No. 122 2360) ....... 6-12Parts of incremental helium flow controller (Part No. 122 2330) ........ 6-16

Thermo Fisher Scientific ConFlo IV Operating Manual xv

Chapter 1 Functional Description

This chapter provides a functional description of the ConFlo IV. It contains the following topics:

• “Introduction” on page 1-2

• “Open Split Principle” on page 1-3

• “Sample/Standard Referencing” on page 1-3

• “Setup of ConFlo IV” on page 1-4

• “Sample Open Split” on page 1-11

• “Reference Open Split” on page 1-12

Thermo Fisher Scientific ConFlo IV Operating Manual 1-1

Functional DescriptionIntroduction

Introduction The ConFlo IV is the universal interface for all online continious flow peripherals to the gas isotope ratio mass spectrometer (GIRMS). It allows to connect two high-flow peripherals (Elemental Analyzer, that is EA, and the TC/EA) plus one low-flow peripheral like e.g. a GC-C/TC (GC-Combustion) or/and high temperature conversion, a GasBench II or an LC IsoLink.

Prior to the analysis in an isotope ratio mass spectrometer the complex samples (solids, liquids, gases) have to be converted into simple gases. Usually, this is accomplished by oxidation, reduction or high temperature conversion. The resulting gases H2, N2, CO, CO2 and SO2 can be let into the mass spectrometer for high precision isotope ratio measurements.

Since precision and accuracy of the measurement depend on the conditions in the ion source as well, it is very important to keep the pressure in the ion source constant all the time. For online continuous flow isotope ratio mass spectrometers this is achieved by the open split interface where a small capillary - the MS capillary - sniffs the sample gas directly from constant atmospheric pressure into the ion source. This ensures a very stable sample gas flow into the mass spectrometer.

Common to all high precision isotope ratio measurements is the sample/standard referencing method. This requires the inlet of calibrated reference gases into the mass spectrometer in alteration to the sample inlet. The ConFlo IV provides the connection of five different reference gases (H2, N2, CO, CO2 and SO2) at a time to allow referencing to the various sample gases.

Another particularity for high precision isotope ratio analysis is the linearity of the mass spectrometer. Most important for hydrogen measurements (H2/HD) is to control the H3

+ ion formation in the ion source which interferes with HD+ in mass. The H3

+ ion formation is a function of the H2 pressure in the ion source.

Ideally, the sample concentration is identical to the concentration of the reference gas. This is the principle of the classical dual inlet technique which still gives the ultimate precision for isotope ratio measurements.

The ConFlo IV allows automatic linearity determination as well as automatic signal matching of sample and standard measurements within a sequence of analysis. This allows to control linearity effects on precision and accuracy of the isotope ratio measurements.

1-2 ConFlo IV Operating Manual Thermo Fisher Scientific

Functional DescriptionOpen Split Principle

Open Split Principle Helium is used as a carrier gas in the peripherals, and finally it carries the sample into the open split of the ConFlo IV. For instance, the helium flow of the Elemental Analyzer is about 80 to 140 mL/min which is much too high to be guided directly into the ion source of the IRMS. The ion source of the mass spectrometer works with helium flows of about 0.2-0.3 mL/min.

Thus, the sample gas flow needs to be reduced or splitted to avoid entering of too much gas into the ion source. This sample gas splitting is one of the main purposes of the open split. Since the gas flow splitting occurs at constant atmospheric pressure, the flow into the ion source is constant as well, which ensures stable conditions in the ion source. The concentration of the sample gas can be further diluted by mixing additional helium into the open split volume.

The MS capillary "sniffs" the gas from the open split volume and guides it into the evacuated ion source of the mass spectrometer. The active volume of the open split is at constant atmospheric pressure ensuring a stable gas flow through the MS capillary into the ion source. A stable gas flow into the ion source is a major prerequisite for high precision isotope ratio measurements. Figure 1-1 shows the open split principle.

Sample/StandardReferencing

The IRMS technique is no absolute measurement principle. Measured isotope ratios need instead to be referenced to a calibrated standard. In order to minimize effects of instrumental drifts it is recommended to measure a calibrated standard gas just before and/or after the sample gas peak. Preferably the sample gas intensity is matched by the reference gas intensity in order to minimize linearity effects of the mass spectrometer and of the ion source in particular.

The reference gas inlet into the mass spectrometer requires a separate open split for the reference gases with a separate capillary connected to the IRMS. Rapid and stable switching between reference gas and sample gas is acomplished by the ConFlo IV.

Figure 1-1. Open split principle

Elemental Analyzer~ 80-100 mL/min

IRMS~ 0.3 mL/min

open split


Functional DescriptionSetup of ConFlo IV

Setup of ConFlo IV

The basic setup of the ConFlo IV consists of two open splits: the sample open split and the reference open split. In Figure 1-2 the sample open split is schematically shown on the left hand side, whereas the reference open split is shown on the right hand side. The ConFlo IV is the universal interface of the continuous flow peripherals to the IRMS. The sample open split is prepared to be connected to one low-flow peripheral (LF) and two high-flow peripherals (HF I and HF II) at a time.

The typical gas flow from the low-flow peripherals (that is GC-C/TC, LC IsoLink or GasBench) is in the range of 1-2 mL/min, whereas the gas flow from the high-flow peripherals (that is EA, TC/EA) is in the range of 80-140 mL/min. Outside the ConFlo IV the EA flow is split to about 1:10 such that about 8-14 mL/min of sample gas flows into the sample open split.

Because of these considerable flow differences the requirements for the open split are different for low-flow and high-flow peripherals. The sample open split of the ConFlo IV is prepared to work with both high-flow and low-flow peripherals.

Note Prior to connecting the EA to the ConFlo IV the EA flow must be splitted to 1:10. The dynamic range for sample gas dilution in the open split is optimized for a sample gas flow less than 14 mL/min.

Figure 1-2. Principle of ConFlo IV

to MSLF

HF I

HF II

H2

N2

SO2

CO

CO2He

Re

fere

nce

IIR

efe

ren

ce

I

LF He

split

incrementalhelium flowcontroller

referenceopen split

sampleopen split



Connection to Low-FlowPeripherals

The low-flow peripheral is connected to the sample open split through the capillary installed on top of the sample open split. See Figure 1-3. There is a gas-tight connection between the sample capillary and the open split volume. The inner diameter of the capillary from the low-flow peripheral is 0.32 mm, which is wide enough to allow the 0.27 mm outer diameter MS capillary to be moved safely into it. In this position, about 0.3-0.4 mL/min of the sample gas flow is splitted into the MS capillary which is connected to the ion source of the mass spectrometer. The waste flow flushes arround the MS capillary and protects the MS capillary input from the outside air.

Close to the connection of the low-flow peripheral to the open split, a small T-piece is installed. The straight flow direction of the T-piece connects the sample gas flow in a straight line to the open split.

Connection to High-FlowPeripherals

In order to disconnect the low-flow peripheral from the open split, the on/off valve of the T-piece is opened. In this case about 90 % of the sample gas flow is vented through the vent capillary whereas just a tiny flow of 10 % enters the open split through the low-flow capillary. The MS capillary is pulled out of the low-flow capillary by a pneumatic piston into the larger active volume of the sample open split. Now, the open split is ready to be operated with high-flow peripherals. The small residual flow through the low-flow capillary prevents any flow of gas from the active volume of the open split into the low-flow capillary.

Figure 1-3. Sample open split operation for low-flow applications*

*that is, GC-C/TC, GasBench, LC IsoLink

HF-peripheral

connectiondilution gas

MS

LF-peripheral

connection

MS capillary position

for low-flow mode

HF out



In case no low-flow capillary is connected, a residual flow of helium is connected to the low-flow capillary to prevent flow from the active volume of the open split into the low-flow capillary. This is achieved by connecting a capillary between the LF input connector and the auxiliary LF helium outlet at the rear panel of the ConFlo IV. See Figure 1-5 and LF He at the bottom part of Figure 1-2.

Figure 1-4. Sample open split operation for high-flow applications*

*that is, EA and TC/EA

Figure 1-5. Rear panel of ConFlo IV

MS

HF peripheral

connectiondilution gas

0.2 mL/min

He purge flow

MS capillary position

for high-flow mode

HF in

HF out

180

315

H2

HeLF

LF He

N2

COOut Air In

Bakeout

CO2

SO2

MS MS Ref HF 1 HF 2

Ext 1 Ext 2



Two high-flow peripherals, HF I and HF II, can be connected to the ConFlo IV. See Figure 1-5. In this mode, the MS capillary is moved out of the low-flow capillary, and a small residual flow through the low-flow capillary prevents that any sample gas from the high-flow peripheral flows or diffuses into the low-flow capillary. See Figure 1-4.

For instance, now two Elemental Analyzers (FlashEA and TC/EA) can be connected to the ConFlo IV. By means of the HF-I and HF-II valves (see Figure 1-2), the flows of the high-flow peripherals can be switched on or off. The flow of the disconnected HF peripheral is then vented through the vent capillary (see Figure 1-2) installed at the HF valves.

The gas flow of the Elemental Analyzer is typically within the range of 80-140 mL/min. Before the EA is connected to the ConFlo IV, the sample gas must be splitted 1:10 (pre-split) such that only 8-14 mL/min gas enter the ConFlo IV. Inside the ConFlo IV, another split valve can reduce the flow by another factor of ten (post split).

This split valve is under computer control and can be switched by Isodat 2.5. The pre-split and the switchable post-split are used to adjust the EA flow into the sample open split.

In case the concentration of the sample gas is low, the post-split valve inside the ConFlo IV is off, and the flow of 8-14 mL/min is guided directly into the sample open split. Now the undiluted gas flow is entering the ion source of the mass spectrometer.

For some applications, a dilution of the sample gas is required. This can be achieved by adding helium into the sample open split via the incremental helium flow controller. In case even greater dilution values are required, the sample gas flow can be splitted inside the ConFlo IV by the post-split valve with a split ratio of 1:10. This increases the dynamic range of the sample gas dilution by another factor of ten and finally allows diluting the sample gas up to 99 % (which equals 1:100) with helium in the sample open split.

Figure 1-6. Connecting Elemental Analyzer to ConFlo IV

80-140

mL/min

from EA 10

:1sp

lit

pre

-sp

lit

72-126

mL/min

(to waste)

to

open

split

ConFlo IV

connection

HF

valve

10

:1sp

lit

po

st-s

plit

split

va

lve

8-14

mL/min4-14 mL/min* or

0.4-1.4 mL/min**

wa

ste

* 4-14 mL/min (split valve closed)

** 0.4-1.4 mL/min (split valve open)



Incremental Helium FlowController

The concentration of the sample gas in the open split can be varied by adding variable auxilliary helium flows into the active volume of the open split. The variable helium flow is best realized by a new type of high-precision flow controller. The requirements for a helium flow controller for high precision isotope ratio measurements are fast switching and short settling times in order to establish a stable flow within a few seconds.

Standard mass flow controllers or pressure controllers do not meet the demanding stability requirements needed for high precision isotope ratio measurements. Therefore, for the ConFlo IV a new principle of an incremental flow controller with high stability was invented by Thermo Fisher Scientific.

The incremental helium flow controller consists of a block of several on/off valves, where all valves are connected to the same pressurized helium reservoir. At each valve outlet, there is a capillary with a specific restriction. The capillaries are led together into one multi-hole ferrule.

From there, one different capillary guides the unified flows of the various valves into the active open split volume. Different valve combinations yield particular helium flows into the open split.See Figure 1-7.

Three valves with different restriction capillaries feed the dilution capillary for the sample open split. Another five capillaries with different restrictions feed the dilution capillary of the reference open split.See Figure 1-8.

Figure 1-7. Schematic incremental helium flow controller - sample OS

He in

EA in

to MS

flow A

flow B

flow C

V1

V2

V3



For technical information about the incremental helium flow controller, refer to “Incremental Helium Flow Controller” on page 6-16.

Helium Consumption The incremental helium flow controller allows to switch on/off and to adjust the helium flow as it is needed for the experiment. This reduces helium consumption considerably. The helium flow varies between 2 mL/min and 80 mL/min.

Beside the helium flow coming from the incremental helium flow controller, a basic dilution helium flow of 2 mL/min always protects the reference open split from entering air. At the sample open split however, there is no basic dilution flow in order to be able to measure the pure EA flow (that is, without any dilution).

Note The helium pressure should never ever be less than 100 kPa (≈ 1 bar). Otherwise, fractionation processes in the open splits might occur leading to erroneous measurements.

Figure 1-8. Schematic incremental helium flow controller - reference OS

He in

Ref in

to MS

flow A

flow B

flow C

flow D

flow E

V2

V1

V3

V4

V5

basic dilution



Incremental HeliumDilution in Sample Open

Split

The additional helium flow into the sample open split can be controlled by a combination of three switchable restrictions which yield three different helium flows. The three restrictions are determined by capillaries with different inner diameters and lengths. The three different flows can be turned on and off by valves. Table 1-1 summarizes the capillary dimensions and flows through the different valves of the sample open split.

The time needed for stabilization of flow conditions in the open split is in the range of about ten seconds only. The corresponding capillary dimensions and basic flows for the reference open split are listed in Table 1-3.

Table 1-1. Capillary dimensions and flows through different valves of sample open split

Valve Capillary dimensions(inner diameter/length, both in mm)

Helium flow at 1 bar(in mL/min)*

*0.1 MPa = 100 kPa ≈ 1 bar

V1 0.1/230 5

V2 0.18/950 10

V3 0.18/130 35


Functional DescriptionSample Open Split

Sample Open Split The sample gas flow from the high-flow peripherals of 8 mL/min or 0.8 mL/min can be further diluted by a combination of the three different helium flows as listed in Table 1-1. This leads to a set of different dilutions for each sample summarized in Table 1-2. The latter reveals that the sample gas flow can be adjusted from 100 % through 61.5 % to 1.6 % relative intensity.

Note Changing the helium pressure as well as changing the EA flow causes variation of the dilution behavior. Dilution calibrations will be obsolete and have to be measured anew.

Table 1-2. Sample gas dilution steps - Example for 80 mL/min flow from EA

Dilution step Valve combination

Flow (mL/min)

Relativeintensity (%)

Dilution (%)

8 mL/min into open split from high-flow peripheral (post-split off )

1 all valves closed

0 100 0

2 V1 5 61.5 38.5

3 V2 10 44.4 55.6

4 V1 + V2 15 34.8 65.2

5 V3 35 18.6 81.4

6 V3 + V1 40 16.6 83.4

7 V3 + V2 45 15.1 84.9

8 V3 + V2 + V1 50 13.8 86.2

0.5 mL/min into open split from high-flow peripheral (post-split on)

9 V1 5 9.1 90.9

10 V2 10 4.8 95.2

11 V1 + V2 15 3.2 96.8

12 V3 35 3.2 96.8

13 V3 + V1 40 2.4 97.6

14 V3 + V2 45 2.0 98.0

15 V3 + V2 + V1 50 1.6 98.4

Dilution (%) 100 % relative Intensity (%)–=


Functional DescriptionReference Open Split

Reference Open Split Five different reference gases can be connected to the ConFlo IV: H2, N2, SO2, CO2 and CO. The flow of each reference gas can be adjusted indivdually by a pressure regulator. Typically, the reference gas flows into the reference open split are adjusted to about 0.2 mL/min at a pressure of about 100 kPa (≈ 1 bar).

Each reference gas can be switched on and off by a valve. All five reference gas flows are connected to one reference gas valve block with five valves in order to turn each individual reference gas on or off. See Figure 1-9 which shows the reference gas supply together with pressure regulators and reference gas valves.

The reference gases are grouped into two batches:

• Reference gas batch I: CO2, CO

• Reference gas batch II: H2, N2, SO2

Figure 1-9. Reference gas supply

CO

CO2

H2

N2

SO2

V1

V3V4

V5

V2

Ref-II

Ref-I

Reference-II-gasReference-II-gasReference-I-gasReference-I-gasReference-I-gas

to-reference-open-split

to-reference-open-split

Ref-II

Ref-I

purge

purge



The gases of each batch are bundled into a separate reference capillary I and a reference capillary II, respectively. Both reference capillaries can be moved in an out of the active volume of the open split by pneumatic pistons.

By the reference gas valve block, two different reference gases can be selected at a time, one from reference gas batch I and one from reference gas batch II. The flow of the reference gases is rather small (in the range of 0.1-0.2 mL/min). The software control avoids the selection of more than one reference gas from one batch at at time.

Switching between the two activated batches takes less than a second. Switching between two reference gases within one batch is fast, but it takes about 2-3 min before the flow is stable and all dead volumes and surfaces inside the valve block and the capillaries are flushed by the small reference gas flow to yield a stable isotope ratio measurement.

The helium dilution of the reference gas in the reference open split is controlled by the incremental helium flow controller shown in Figure 1-8. It consists of five valves with different restrictions and gas flows.

Table 1-3 summarizes the capillary dimensions and flows through the different valves of the reference open split.

The reference gas flow of about 0.2 mL/min can be further diluted by a combination of the five different helium flows listed in Table 1-3. This leads to the dilutions summarized in Table 1-4. Only the most significant dilution steps are listed.

Table 1-3. Capillary dimensions and flows through valves of reference diluter

Valve Capillary dimensions(inner diameter/length, both in mm)

Helium flow at 100 kPa(in mL/min)*

*0.1 MPa = 100 kPa ≈ 1 bar

basic dilution 0.1/550 2

V1 0.075/350 1

V2 0.1/550 2

V3 0.1/230 5

V4 0.18/550 16

V5 0.18/130 35



Thus, the signal intensities of the reference gases can be varied between 100 % and 3.6 %. If the reference gas intenstity is adjusted to 30 V at dilution step 1 in Table 1-4, the largest dilution step results in a signal intensity of about 1 V.

Table 1-4. Reference gas dilution steps

Dilution step Valvecombination

Flow(mL/min)

Relativeintensity (%)

Dilution (%)

1 all valves closed 2 100.0 0

2 V1 3 68.8 31.2

3 V2 4 52.4 47.6

4 V1 + V2 5 42.3 57.7

5 V3 7 30.6 69.4

6 V3 + V1 8 26.8 73.2

7 V3 + V2 9 23.9 76.1

8 V3 + V2 + V1 10 21.6 78.4

9 V4 18 12.1 87.9

10 V4 + V1 19 11.5 88.5

11 V4 + V2 20 10.9 89.1

12 V4 + V2 + V1 21 10.4 89.6

13 V4 + V3 23 9.5 90.5

14 V4 + V3 + V1 24 9.1 90.9

15 V4 + V1 + V2 + V3 26 8.4 91.6

16 V5 37 5.9 94.1

17 V5 + V4 + V3 + V2 + V1 61 3.6 96.4

Figure 1-10. Dynamic range of reference gas dilution steps

100.0%

68.8%

52.4%

42.3%

30.6%

26.8%23.9%

21.6%

12.1% 11.5% 10.9% 10.4% 9.5% 9.1% 8.4%5.9%

3.6%

0.0%

10.0%

20.0%

30.0%

40.0%

50.0%

60.0%

70.0%

80.0%

90.0%

100.0%

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17

Dilution step

Rela

tive

inte

nsit

y



Note Changing the helium pressure causes variations in dilution behavior of both sample and reference gases. Dilution calibrations will be obsolete and have to be measured anew.

Note Special care has to be taken for the measurement of hydrogen. Because of the high diffusion rate of hydrogen, the open split should not be operated at gas flows smaller than 3 mL/min. Otherwise, fractionation effects inside the open split may corrupt the results.

Therefore, for hydrogen measurements at least V1 of the incremental helium dilution valve block should be open. This functionality is hard-coded into Isodat 2.5. By default, at least V1 is open in case H2 is selected.

Reference GasConsumption

With ConFlo IV, reference gas flows can be switched on and off by the reference gas valves. In order to save the calibrated high purity reference gas, it is recommended to open the reference gas valves only when the reference gas is really needed.


Chapter 2 Isodat 2.5

This chapter outlines how to prepare and conduct a measurement in Isodat 2.5. It contains the following software-related topics:

• “Creating ConFlo IV Configurations” on page 2-2

• “Installing an Autosampler” on page 2-6

• “ConFlo IV Interface Window” on page 2-8

• “Sequence Batcher” on page 2-18


Isodat 2.5Creating ConFlo IV Configurations

Creating ConFlo IVConfigurations

Before operating, a configuration containing the ConFlo IV interface needs to be created in the Configurator.

Note Choose between the predefined sets as they cover the vast majority of applications.

1. Start the Configurator.

2. Add a new configuration.

3. Give it a significant name, e.g. ConFlo IV + TC/EA.

1. Fully expand the MS tree by clicking on the + sign.

Thereby, the Capillary symbol becomes visible.

2. In the right tab, click on the Elemental Analyzer Sets - ConFlo IV tab.

The list of predefined sets will appear. See Figure 2-1.

Figure 2-1. List of predefined Elemental Analyzer - ConFlo IV sets

list of predefined setsto be chosen from



Note In a configuration always occupy only one port (that is, either HF I or HF II or LF) and not several ones simultaneously.

An Elemental Analyzer belongs to the group of high-flow peripherals. Isodat 2.5 treats Flash EA and Flash HT as equivalents. In the predefined sets, they are attached to the HF I symbol by default.

On the contrary, in the predefined sets a TC/EA will be attached to the HF II symbol by default. Thus, in the frequent case of one TC/EA plus one Flash EA (or Flash HT), the TC/EA will be attached to the HF II symbol whereas the Flash EA (or Flash HT) is attached to the HF I symbol.

Creating a Configurationfor Two Flashs

The seldom case of two Flashs (e.g. one Flash EA and one Flash HT) is not covered by the predefined sets. Instead, you must assign one of them to the HF II symbol on your own as follows:

1. Create a new configuration for the second Flash. Give it a significant name. Expand the MS tree so that the Capillary symbol becomes visible.

2. Click on the ConFlo IV Sets tab. It contains only one entry, ConFlo IV Interface.

3. Drag&drop it to the Capillary symbol in the left pane.

4. Change to the Advanced mode, if not already done. Thereby, access to the Devices tab will be possible.

3. In order to connect the ConFlo IV interface to the capillary port, drag&drop the appropriate predefined set you chose to the capillary symbol in the left pane.

In this example, the predefined set ConFlo IV Interface + TC/EA (HF II) has been chosen.

The three inlet ports LF, HF I, HF II of the ConFlo IV will be displayed.



5. Click on the Devices tab.

6. Click on the second Flash, e.g. Flash HT and drag&drop it to the HF II symbol in the left pane.

Note In a configuration always occupy only one port (that is, either HF I or HF II or LF) and not several ones simultaneously.

Installing a Flash EA orFlash HT

Adjusting Properties of Flash EAor Flash HT

In case of using a Flash EA or a Flash HT, the COM Port settings are important as well.

In order to show and edit the properties of a Flash EA or Flash HT proceed as follows:

1. In the Configurator, change to the Advanced mode via Edit > Advanced mode....

2. You are informed that you are about to enter the Advanced Mode. Click on on OK to confirm your action.

3. Click on the Devices tab to display the pool of available devices (access to the Devices tab is only possible in Advanced mode).

4. Right-click on the Flash EA icon or the Flash HT icon.

In the shortcut menu, do one of the following:

• Select Properties, if you only want to check the COM Port your Flash EA or Flash HT is connected to. Figure 2-2 will appear.

• Select Edit... to edit the default communication parameters.



Figure 2-2. Properties of Flash EA or Flash HT

Note When using the TCD for oxygen and hydrogen measurements with high temperature conversion in a Flash HT, the Polarity shown at the TCD Settings in Figure 2-2 must be changed to Negative.


Isodat 2.5Installing an Autosampler

Installing anAutosampler

A200S and GC PAL autosampler require operating signals from the software via RS 232 cable (COM Port). When you select a ConFlo IV set with liquid autosampler in the Configurator (see “Creating ConFlo IV Configurations” on page 2-2.), special scripts for using these autosamplers together with Isodat 2.5 are automatically installed.

To view the COM Port settings for the autosampler, do the following:

Note The COM Port settings are essential for proper communication with the autosampler. Incorrect settings will lead to inactive liquid autosampler control.

1. In the Configurator, change to the Advanced mode via Edit > Advanced mode....

2. You are informed that you are about to enter the Advanced Mode. Click on on OK to confirm your action.

3. Click on the Devices tab to display the pool of available devices (access to the Devices tab is only possible in Advanced mode).See Figure 2-3.


Isodat 2.5Installing an Autosampler

Figure 2-3. Available devices

4. Right-click on your autosampler, e.g. A200S.

Note For GC PAL autosampler, also right-click on A200S.

In the shortcut menu, do one of the following:

• Select Properties, if you only want to check the COM Port your autosampler is connected to. Continue with step 5.

• Select Edit... to edit the default communication parameters.


Isodat 2.5ConFlo IV Interface Window

Note The Properties command is available also in Normal Mode. That is, you do not need to be in Advanced Mode to only check the COM Port your autosampler is connected to. The Edit... command, however, is available only in Advanced Mode.

5. In the A200S Properties box, select the COM Port your autosampler is connected to (e.g. COM 1, see Figure 2-4). Confirm by OK.

Note Do not change the properties of an autosampler.

ConFlo IV InterfaceWindow

Two different windows give access to the ConFlo IV functionality:

• The ConFlo IV Interface window described below allows user-friendly operation of the ConFlo IV.

• The ConFlo IV Diagnosis window described at allows switching of individual valves. It is mainly used for diagnostic purposes or for direct access to a specific valve. It is not recommended to use this window for standard operation of the ConFlo IV.

The ConFlo IV Interface window, Figure 2-5, displays the basic functionality of the ConFlo IV. It allows adjusting the dilution settings for the sample open split (that is, Sample Dilution) as well as for the reference open split (that is, Reference Dilution).

Figure 2-4. Selecting COM Port of autosampler

Start Acquisition.

Select a suitable configuration that contains the ConFlo IV interface (e.g. ConFlo IV + TC/EA).



• Clicking with the left mouse button onto the Sample Dilution bar or the Reference Dilution bar and keeping the mouse button pressed while moving the mouse up or down will increase or decrease the dilution settings continuously.

• The dilution settings can be adjusted as well by releasing the mouse button on the sample dilution bar or the reference dilution bar. The actual setting will then snap into the nearest possible dilution setting of the incremental helium flow controller.

The dilution is calculated as follows:

0 % dilution means that all valves of the incremental helium flow controller are closed and thus no additional dilution gas is flowing into the open split.

Example: If the flow into the open split is about 5 ml/min and the incremental helium flow controller adds another 10 ml/min helium flow into the open split, dilution amounts to:

In the lower part of the ConFlo IV Interface window the stati of the two reference gas batches are displayed. See Figure 2-6.

Figure 2-5. ConFlo IV Interface window

Dilution 1 gas flow into open split without additional He gasgas flow into open split plus additional He gas

-------------------------------------------------------------------------------------------------------------------–⎝ ⎠⎛ ⎞ 100 %⋅=

Dilution 1 5 mL/min5 mL/min 10 mL/min+---------------------------------------------------------–⎝ ⎠

⎛ ⎞ 100 % 67 %=⋅=



The Ref I batch supports the reference gases H2, N2 and SO2 whereas the Ref II batch supports the gases CO and CO2. For each batch only one reference gas can be selected at a time by clicking on the respective button with the left mouse button.

The button of the selected reference gas will turn into green. Clicking on a particular reference gas button will open or close the respective reference gas valve inside the ConFlo IV. If a reference gas is not selected, the particular reference gas valve will stay closed and thus no reference gas will be consumed. Isodat 2.5 prevents to open two reference gases of one batch at a time. Only one reference capillary of a batch can be selected at a time.

The On/Off button allows moving the reference capillary in and out of the active mixing volume of the open split. The Off status indicates that the reference gas capillary is moved out of the active mixing volume. The On status means that the reference capillary is moved into the active mixing volume such that the reference gas is mixed up with the additional helium flow and the MS capillary sniffs the diluted reference gas into the ion source of the mass spectrometer.

Dynexternals Window

Linearity Tab The Linearity tab shown in Figure 2-7 displays the parameters used for the linearity acquisition script. For the linearity measurement the signal intensity in the mass spectrum is stepped through and the δ values of the measured isotope ratios are recorded for the different intensities. Typically, the linearity should be less than 0.06 ‰/V.

The signal intensities are adjusted by changing the reference gas concentration in the open split. The additional helium gas flow into the open split can be adjusted by the incremental helium flow controller.

Figure 2-6. Status of the two reference gas batches

Clicking on this button allows opening the Dynexternals window to edit parameters specific for ConFlo IV. See Figure 2-7.



Figure 2-7. Dynexternals - linearity parameters

Table 2-1. Linearity tab

Parameterin Figure 2-7

Comment

Intensity Start [mV]

Intensity End [mV]

Together they define the dynamic range over which the linearity measurement should be performed

Steps the number of linearity calibration steps between the defined Intensity Start and Intensity End value.

Isodat 2.5 tries to adjust equidistant values across the dynamic range, however there are some limitations since the spacing of the incremental steps is not equidistant.

Dilution Predelay [s] The linearity measurement is a special standard on/off measurement where signal intensity is stepwise increased. The timing of the procedure is controlled by the parameters Dilution Predelay, Peak Width and Dilution Post Delay.

Dilution Predelay defines the time before the flow becomes stable after a new dilution value is set. During this time, the reference gas capillary is out of the active volume of the open split. See Figure 2-8.

Peak Width [s] time period during which the reference capillary stays within the active volume of the reference open split

Post Peak Delay [s] delay time after the reference capillary is moved out of the active volume of the open split and before the dilution is switched



References Tab The Reference tab, Figure 2-9, allows editing the type of reference gas connected to the ConFlo IV. Usually, the gases shown in Figure 2-9 are the default gases and are not changed. This configuration is true, if the user has installed the reference gases at the rear panel of the ConFlo IV as displayed in Figure 6-2.

However, if special reference gases other than those listed in Figure 2-9 are typed in, the user has to ensure that the gas names are in agreement with the gas names listed in the Gas Configuration Editor.

Figure 2-8. Dilution predelay

switching

off dilutioncapillary

in

capillary

out

ready for new

dilution switch

dilution predelay peak width postdelay

Figure 2-9. Dynexternals - reference gas connections



LF Dil Tab

The parameters in the LF Dil tab, Figure 2-10, depend on the actual flow of the low-flow peripheral connected to the ConFlo IV. For instance, for the GC-C interface as well as for the GasBench, the flow rate entering the sample open split is in the range between 0.5 ml/min and 2 ml/min.

This gas flow can be further diluted by the incremental helium flow controller gas. Sample LF Dilution 1 means the dilution setting with sample dilution valve 1 open and all other valves closed. In this case, 5 mL/min helium flow is added to the flow coming from the GasBench or the GC-C interface. The Sample LF Dilution 1 setting can then be estimated to be:

If only valve 2 of the incremental helium flow controller for the sample open split is open, a helium flow of 10 mL/min is added to the flow coming from the LF peripheral. The Sample LF Dilution 2 value can then be estimated to be:

Figure 2-10. Dynexternals - dilution parameters for low-flow (LF) peripheral

Sample LF Dilution 1 1 1.5 mL/min1.5 mL/min 5 mL/min+-----------------------------------------------------------–⎝ ⎠

⎛ ⎞ 100 % 77 %=⋅=

Sample LF Dilution 2 1 1.5 mL/min1.5 mL/min 10 mL/min+-------------------------------------------------------------–⎝ ⎠

⎛ ⎞ 100 % 87 %=⋅=



In case only valve 3 is open, 35 mL/min are added to the sample open split flow. The Sample LF Dilution 3 is then estimated by:

The actual Sample Dilution values will only change slightly when the flow coming from the peripheral changes. Based on these Sample Dilution settings, Isodat 2.5 will calculate the Sample Dilution values for different valve combinations of the incremental helium flow controller for the sample open split.

The actual Sample Dilution values can be determined experimentally as well. Therefore, four identical samples with identical sample amounts are measured with:

a. No addition of helium, that is all valves of the incremental helium flow controller are closed.

b. Valve 1 is open, all other valves are closed.

c. Valve 2 is open, all other valves are closed.

d. Valve 3 is open, all other valves are closed.

The dilution values can be calculated from the measured intensities relative to the undiluted measurement.

Similarly, the Sample Dilution values for the high-flow peripherals can be determined. Usually, the flow coming from the Elemental Analyzer is in the range between 80 mL/min and 140 mL/min. The inlet ports HF I and HF II of the ConFlo IV for the high-flow peripherals, however are designed to accept a flow in the range between 8 mL/min and 14 mL/min. Hence the flow from the Elemental Analyzer must be splitted by a split ratio of 1:10 before it can be connected to the ConFlo IV (pre-split).

Inside the ConFlo IV, a split valve further splits the Elemental Analyzer flow by a split ratio of 1:16 (post-split). It is used to expand the dynamic range of the sample dilution so that in total a dilution of about 99 % (which equals 1:100) can be achieved. See Table 1-2.

HF I Dil Tab and HF II Dil Tab In the HF-I Dil tab and the HF-II Dil tab (Figure 2-11), two sets of Sample Dilution settings are listed:

a. HF Dilution Settings unsplitted and

b. HF Dilution Settings splitted.

Sample LF Dilution 3 1 1.5 mL/min1.5 mL/min 35 mL/min+-------------------------------------------------------------–⎝ ⎠

⎛ ⎞ 100 % 96 %=⋅=



Table 2-2 and Table 2-3 help to set accurate dilution values. The values are based on a helium fore pressure of 1 bar. Dilution and sample intensity are related by the following two equations:

Figure 2-11. Dynexternals - Dilution parameters for high-flow (HF) peripheral

Table 2-2. Dilution values at EA carrier flows from 80-140 mL/min*

*with helium fore pressure of 1 bar in the ConFlo IV

EA flow[mL/min]

OS flow[mL/min]

V1 (5 mL)[% Dilution]



80 8.0 38 56 81

90 9.0 36 53 80

100 10.0 33 50 78

110 11.0 31 48 76

120 12.0 29 45 74

130 13.0 28 43 73

140 14.0 26 42 71

a

b

Dilution 100 % sample intensity–=

Dilution 1 OS flowVx OS flow+--------------------------------–=



Similar to the sample gas dilution, the reference gas dilution values need to be calibrated as well. The calibration of the reference gas dilution can be performed automatically by starting a predefined script.

The incremental helium flow controller for the reference gas open split is a five-valve system with five different flow restrictions. During the calibration procedure, the dilution for the six basic valve settings is measured.

It starts with all valves closed (dilution = 0 %) and then sequentially opens only one valve starting with V1 to V5. For each of these six basic valve settings, the diluted reference gas intensity is measured and the dilution value is calculated. Based on this basic calibration, the resulting dilution values for any valve combination can be calculated. The reference gas dilution calibration takes about 2 min.

Table 2-3. Dilution values at EA carrier flows from 80-140 mL/min*

*with helium fore pressure of 1 bar in the ConFlo IV

EA flow[mL/min]

OS flowwith PreSplit on[mL/min]




80 0.5 90.9 95.2 98.6

90 0.6 89.9 94.7 98.4

100 0.625 88.9 94.1 98.2

110 0.7 87.9 93.6 98.1

120 0.8 87.0 93.0 97.9

130 0.8 86.0 92.5 97.7

140 0.9 85.1 92.0 97.6

Clicking into the ConFlo IV Interface window (Figure 2-5) with the right mouse button will give access to the entries Determine Reference Gas Dilution and Show Reference Gas Dilution.

When the user selects Determine Reference Gas Dilution, the calibration procedure for the selected reference gas will be started. The selected reference gas will always be the gas defined in the current gas configuration.

Once the reference gas dilution has been calibrated the actual dilution values of the reference gas can be displayed by clicking with the left mouse button onto the command Show Reference Gas Dilution.



Figure 2-12 displays the reference gas dilution values and the reference gas intensities of the main mass.

• The first row of Figure 2-12 shows that the signal of the undiluted N2 reference gas, m/z 28, is about 17.9 V (dilution = 0.00 %; Valves 00000).

• The second row of Figure 2-12 shows that with V1 open, the signal decreases to 12.8 V. This is 28.5 % less than the undiluted intensity (dilution = 28.52 %; Valves 10000).

Figure 2-12. Reference dilution and reference gas intensities


Isodat 2.5Sequence Batcher

Sequence Batcher

Principle The sequence batcher implemented in Isodat 2.5 is a sequence- superordinate tool. It allows automatic execution of several sequences one after another according to a chronological order you specified. This saves time as you don’t need to start each single sequence individually after the antecedent one has been finished. Instead, the entire sequence batch is started only once and then processed without needing any interventions of an operator.

Note Within one and the same measurement, the sequence batcher can automatically switch between different configurations (referring to various peripherals). Thus, it processes even sequences that have been established in different configurations.

A single sequence summarizes all the parameters needed for a complete measurement procedure of several samples. The sequence batcher however, allows composing an extensive series made up of several sequences. It makes it easier to set up and structure a very long sequence by grouping the sequence into sub-sequences.

Editing and executing one very long single sequence can thus be avoided, if instead a short sequence is repeated several times within a batch.

The sequence batcher is used in automated operation, if it is necesssary to:

• run the same sequence several times in succession (e.g. in order to determine reproducibility) or

• run various sequences one after another, e.g. for measuring rather different samples.

Using Sequence Batcher The sequence batcher is part of the Accessories toolbar within the ConFlo IV Interface window. To use the sequence batcher:

1. In File Browser, select the Sequences tab.

2. Mark the sequence(s) of interest. See right side of Figure 2-13.



3. Simply drag&drop them into the sequence batcher. See Figure 2-14.

Note As a special case, you can drag one and the same sequence several times into the sequence batcher. This allows executing it repeatedly (e.g. in case of a zero enrichment test or a linearity test).

Note First, you can drag&drop sequences belonging to a configuration A into the sequence batcher. Afterwards, it is possible to change to other configurations B, C... and drag&drop their sequences in the sequence batcher as well. After the batch is started once, it will automatically be proceeded.

4. The selected sequences appear in the sequence batcher together with their paths. They are now ready to be executed in chronological order.

5. You can add further sequences to the batch by drag&drop from the File Browser. The newly added sequences will appear below the previous ones and be executed after them.

Figure 2-13. Drag&drop of sequences

Figure 2-14. Sequences available in sequence batcher



To change the point in time for a particular sequence to be executed within the batch, modify its position within the sequence batcher. To do so, mark it and drag it to the desired position.

Prior to Sequence BatchExecution

Note When starting a single sequence, a dialog box appears where a lot of result handling parameters must be defined. In automated operation without an operator present, this is obstructive and unwanted. The sequence batcher avoids this as the conditions are defined only once, before the batch is executed (Figure 2-15). This guarantees that the system will not stop during execution requesting for entries.

Before the sequences within the batch will be executed chronologically, define which decision Isodat 2.5 will make, if a fatal sequence error should occur.

To remove a sequence from the sequence batcher, right-click on it in the batch.

• Select Delete, and it will be removed from the sequence batch list. The sequence itself will not be deleted.

• To view its sequence grid, select Open.

Therefore, click on the Properties button of the sequence batcher.

Figure 2-15. Commands for sequence batch execution



Sequence BatchExecution

After the handling of possible error conditions has been defined, all sequences within the batch can finally be executed in chronological order.

Note However, if you start a sequence via the Start button above the sequence grid, only this individual sequence will be executed, but not an entire batch.

Table 2-4. Commands for sequence batch execution

Command Action

Continue automatically

The error will be reported but not paid attention to. The measurement continues with the next sequence.

Ask The fatal sequence error is indicated together with a request about how to proceed (stop or next sequence).

Terminate complete

The entire sequence batch will be stopped.

Click on the Start button of the sequence batcher.


Chapter 3 Reference Gas Measurements

The basic performance of the ConFlo IV interface and the IRMS can be checked by the zero enrichment test and the linearity test. The zero enrichment test documents the stability, and the linearity test the linearity of the system.

Note It is recommended to perform both tests prior to measuring sample sequences.

The linearity measurement specifies the robustness of the isotope ratio measurements against variable signal intensities over a large dynamic range. The zero enrichment test checks the stability of the isotope ratio measurements for constant signal intensities.

The H3 factor calibration is a special case of a linearity measurement. The non-linearity caused by the formation of H3

+ ions is by far the most severe non-linearity. Therefore, it is determined by a linearity measurement, and Isodat 2.5 determines the so-called H3 factor to correct for this non-linearity.

Hence, this chapter treats the following topics:

• “Zero Enrichment Test” on page 3-2

• “Linearity Test” on page 3-9

• “H3 Factor Calibration” on page 3-15


Reference Gas MeasurementsZero Enrichment Test

Zero Enrichment Test The zero enrichment test is often synonymously called standard on/off test. To set up a zero enrichment method, proceed as follows:

Setting up a ZeroEnrichment Method

The method is loaded and shows up with its Instrument tab (Figure 3-2).

1. Open Acquisition.

2. Click on the New button.

Figure 3-1. Creating a zero enrichment method

3. Click on the Method icon.

4. Confirm by a click on OK.



5. Select the gas configuration you are working with, e.g. CO2 (Figure 3-2).

6. For CO2 gas, select the Ref II Capillary reference port at Reference Device (Figure 3-2).

7. At Auto Dilution, mark the Fixed radio button (Figure 3-2).

8. Specify the constant reference intensity you want to use for the test (Figure 3-2).

9. In Time Events tab, set up the time events list in order to define the sequence of on/off pulses during the measurement: the time events list shown in Figure 3-3 defines the timing of ten on/off pulses.

Figure 3-2. Zero enrichment test for CO2 - Instrument tab

step 6

step 8step 7

step 5



Note The off time of the third pulse is 120 s. See arrow in Figure 3-3.

In the Evaluation tab, the reference peak for calculating the δ values is defined. The reference peak is defined by the off time in the chromatogram. In this case, the off time of 120 s specifies the third peak in the time event list. See Figure 3-3 and Figure 3-4.

Note At Ref. Time column, the off time of an arbitrary reference gas peak according to the time events list must be typed in (in this case 120 s as off time of third reference gas peak). See Figure 3-3 and Figure 3-4.

Figure 3-3. Zero enrichment test for CO2 - Time events tab

Figure 3-4. Zero enrichment test for CO2 - Evaluation tab



10. Use the default peak detection parameter of Isodat 2.5.See Figure 3-5.

In Printout tab, the use of printout templates is controlled.See Figure 3-6 and Table 3-1.

11. Save the zero enrichment method as e.g. Zero Enrichment CO2.met.

Figure 3-5. Zero enrichment test for CO2 - Peak detection tab

Figure 3-6. Zero enrichment test for CO2 - Printout tab

Table 3-1. Printout tab

No. Parameter Description

a Single Selects a print template from the Result Workshop for an individual printout per sample.

b Sequence Selects a print template from the Result Workshop for a reduced printout per sample within a sequence summary.

a

b



Sequence and Starting theRun

15. In the Method tab of the appearing sequence grid, select just the IRMS method you created in step 1 to step 11, e.g. Zero Enrichment CO2.met. See Figure 3-8.

16. Start the run.

During the measurement the chromatogram is displayed together with the corresponding result grid. See Figure 3-9 and Figure 3-10.

12. Create a new sequence by first clicking on the New button.

Figure 3-7. Creating a new sequence

Figure 3-8. Selecting IRMS method within sequence grid

13. Then, click on the Sequence icon.




The δ values for 13C/12C and 18O/16O are calculated relative to the reference peak, which in the Evaluation tab has been specified to be the peak with the off time of 120 s. In this case, it is peak 3.

The stability of the zero enrichment test is the standard deviation of the the δ values of all reference peaks. In order to calculate it:

1. Click on the headline of the d 13C/12C column.

2. From the pulldown menu, select Calculate. See Figure 3-11.

Figure 3-9. Zero enrichment test for CO2 - Chromatogram

Figure 3-10. Zero enrichment test for CO2 - Result grid



The stability of the zero enrichment test amounts to 0.038 ‰ for δ13C/12C and to 0.039 ‰ for δ18O/16O. The specification of the stability of δ13C/12C is 0.06 ‰ and 0.08 ‰ for δ18O/16O.

Figure 3-11. Zero enrichment test for CO2 - Calculation of stability

Figure 3-12. Zero enrichment test for CO2 - Calculated stability for δ13C/12C

Figure 3-13. Zero enrichment test for CO2 - Calculated stability for

δ18O/16O


Reference Gas MeasurementsLinearity Test

Linearity Test

General Remarks One reason for non-linearity effects inside the ion source are ion-molecule reactions. In case of CO2, the following ion-molecule reaction with excited H2O+. ions can take place:

In the mass spectrum, the protonated 1H12C16O2+ ion interferes with

the 13C16O2+ ion which will result in a wrong 13C/12C isotope ratio

measurement. Therefore, the measured isotope ratio depends on the conditions inside the ion source.

By a special tuning of the ion source these non-linearity effects can be minimized. The characteristics of the ion source can be monitored by the linearity test. Usually, the non-linearity effects are small (that is, in the range below 0.02 %/nA).

The linearity test requires to measure a series of reference gas pulses with different intensities. It is controlled by a special script which needs to be loaded into the linearity method. The parameters for the linearity test can be edited via the ConFlo IV Interface window. Refer to “Linearity Tab” on page 2-10 and Figure 3-13.

Setting up a LinearityMethod

The linearity method can be set up as follows:

H2O+. CO2+ HCO2+ OH.+→





Figure 3-14. Creating a linearity method

Figure 3-15. Linearity test for CO2 - Instrument tab



step 5step 6

step 7

step 8



The method will be loaded and shows up with its Instrument tab (Figure 3-15).

5. Select the gas configuration you are working with, e.g. CO2 (Figure 3-15).

6. At Acquisition Script, select the script Linearity Determination Acq.isl (Figure 3-15).

7. For CO2 gas, select the Ref II Capillary reference port at Reference Device (Figure 3-15).

8. At Auto Dilution, mark the Dynamic radio button (Figure 3-15).

No entries need to be made in the time events list. The information about the timing of the on/off pulses and the adjustment of the reference gas dilution is read from the Dynexternals parameters defined via the ConFlo IV Interface window at “Linearity Tab” on page 2-10 and Figure 2-7.

In Evaluation tab, the off time of the reference peak for the linearity evaluation has to be specified. In this case, the off time has been selected to be 160 s. See arrow in Figure 3-16.

In Peak Detection tab and Printout tab, use the default peak detection parameters and default printout settings.

9. Save the linearity method as e.g. Linearity CO2.met.

Figure 3-16. Linearity test for CO2 - Evaluation tab




13. In the Method tab of the appearing sequence grid, select just the IRMS method you created in step 1 to step 9, e.g. Linearity CO2.met. See Figure 3-18.

14. Start the run.

During the measurement, the chromatogram of the standard on/off peaks with different intensities is displayed together with the corresponding result grid. See Figure 3-19 and Figure 3-20.

10. Create a new sequence by first clicking on the New button.







Peak 3 is the reference peak. Refer to the peak off time defined in Evaluation tab (Figure 3-16).

The linearity is calculated from the slope in a plot of the δ values of 13C/12C or 18O/16O versus the 12C intensity. To carry out the evaluation, the data need to be exported into Microsoft Excel.

For instance, the export can be performed manually as follows:

Figure 3-19. Linearity test for CO2 - Chromatogram

Figure 3-20. Linearity test for CO2 - Result grid

1. With the left mouse button, click on the headline of the respective column. The column will be highlighted.

2. By pressing the Ctrl-C key, the entries of the grid are copied onto the clipboard and can then be pasted into Microsoft Excel.

3. The data are plotted in Microsoft Excel, and the slope can be calculated. See Figure 3-21.



Figure 3-21 reveals that the linearity of 13C/12C is 0.01 ‰/V over a dynamic range from 888 mV to 19636 mV . Since the amplitude of m/z 44 is measured with a 3*108 Ω amplifier, this is equivalent to 0.003 ‰/nA. The specification for 13C/12C linearity is 0.02 ‰/nA.

Similarly, the linearity for 18O/16O measurements can be evaluated from Figure 3-21 to be about 0.03 ‰/V which is equivalent to 0.01 ‰/nA. The specification for 18O/16O linearity is 0.02 ‰/nA.

Figure 3-21. Linearity test data for 13C/12C and 18O/16O measurements

y = 1E-05x - 0.0209

y = 3E-05x - 0.1362

-0.2

-0.1

0

0.1

0.2

0.3

0.4

0.5

0 5000 10000 15000 20000 25000

delta values

Am

pl

44

[m

V]

d 13C/12C d18O/16O Linear (d 13C/12C) Linear (d18O/16O)


Reference Gas MeasurementsH3 Factor Calibration

H3 Factor Calibration

General Remarks For hydrogen measurements the linearity effect is most severe. This is due to the formation of H3

+ ions in the ion source which interfere with DH+ ions in the mass spectrum. The H3

+ ion formation is due to the following ion-molecule reaction inside the ion source:

The number of H2 molecules and the number of H2+ ions are both

proportional to the partial pressure of H2 gas in the ion source. Hence, the H3

+ ion formation rate is proportional to the square of the H2 partial pressure in the ion source. As a result, the measured ion current ratio can be written as:

with:

I(2): measured ion current on m/z 2

I(3): measured ion current on m/z 3

k: H3 factor

This leads to:

In order to minimize the H3+ ion formation rate, the ion source is

usually operated at 100 % extraction voltage. This minimizes the residence time of the hydrogen ions in the ionization volume of the ion source.

The H3-factor calibration basically is a linearity calibration. The method is set up in the same manner as for the linearity measurement described for CO2 at “Setting up a Linearity Method” on page 3-9. The parameters for the linearity determination script are loaded via the ConFlo IV Interface window. Refer to “Linearity Tab” on page 2-10 and Figure 2-7.

H2+ H2+ H3

+ H+→

I(3)I(2)--------

HD+ H3++

H2+

---------------------------- HD+

H2+

------------k H2

+( )2

⋅

H2+

------------------------+= =

HD+

H2+

------------ I(3)I(2)-------- k I(2)×–=



Setting up a H3 FactorCalibration Method

The H3 factor calibration method can be set up as follows:

The method will be loaded and shows up with its Instrument tab (Figure 3-23).



Figure 3-22. Creating a H3 factor calibration method





5. Select the gas configuration you are working with, e.g. H2 (Figure 3-23).

6. At Acquisition Script, select the script Linearity Determination Acq.isl (Figure 3-23).

7. For H2 gas, select the Ref I Capillary reference port at Reference Device (Figure 3-23).

8. At Auto Dilution, mark the Dynamic radio button (Figure 3-23).

The timing of the on/off pulses is controlled by the script Linearity determination acq.isl, and therefore the time events list is empty.

Figure 3-23. H3 factor calibration method - Instrument tab

step 5step 6

step 7

step 8



In Evaluation tab, the off time of the reference peak needs to be specified. See arrow in Figure 3-24.

Note If the off time of the reference peak for the H3 factor calibration is improperly selected, the H3 factor cannot be calculated properly.

In Peak Detection tab, the default parameters can be used.

Note However, it is important to mark the Overwrite check box! See arrow in Figure 3-25. Otherwise, the H3 factor will not be calculated properly.

Figure 3-24. H3 factor calibration method - Evaluation tab

Figure 3-25. H3 factor calibration method - Peak Detection tab



In Printout tab, use the default printout settings.

9. Save the H3 factor calibration method as e.g. H3 factor calibration.met.


12. In the Method tab of the appearing sequence grid, select just the IRMS method you created in step 1 to step 9, e.g. H3 factor calibration.met. See Figure 3-27.

13. Start the run.

During the measurement, the chromatogram of the standard on/off peaks with different intensities is displayed together with the corresponding result grid. See Figure 3-28 and Figure 3-29.







Figure 3-28. H3 factor calibration - Chromatogram

Figure 3-29. H3 factor calibration - Result grid


Chapter 4 Operating ConFlo IV with EA

This chapter illustrates how ConFlo IV is operated in connection with an Elemental Analyzer (EA). It deals with the following topics:

• “SmartEA™ Function” on page 4-2

• “EA Method” on page 4-5

• “Set Instrument to Standby and Auto-Ready Function” on page 4-10

• “Weight Percent Determination” on page 4-11


Operating ConFlo IV with EASmartEA™ Function

SmartEA™ Function The incremental flow regulation of the ConFlo IV allows automatic adjustment of sample and reference gas amplitudes to predefined intensities (referred to as fixed) or dynamic dilution as a response to the TCD signal of the FlashEA 1112 or the FlashEA 1112 HT. The mode must be defined in the Isodat 2.5 method. The modes below can be chosen:

• Dynamic Dilution

• Fixed

• None

Dynamic Dilution This mode adjusts sample and reference signal to a predefined amplitude. For the sample amplitude the system reacts on the read-out signal of the TCD trace in a FlashEA 1112 for IRMS or a FlashEA 1112 HT. The intensity of the TCD signal is monitored and the dilution in the sample open split (OS) of the ConFlo IV is adjusted in order to reach the desired sample amplitude.

To set the dilution properly in time, the system must be equipped with a special capillary which delays the sample peak on the way to the ConFlo IV. Isodat 2.5 uses the TCD peak intensity to calculate the dilution needed to decrease the signal to the predefined amplitude.

Figure 4-1. Dynexternals - Dilution parameters for high-flow (HF) peripheral

a

b



Isodat 2.5 uses the entries in the Dynexternals dialog (Figure 4-1) to calculate the dilution closest to the predefined amplitude. The values in the dialog depend on the helium fore pressure of the ConFlo IV and on the flow of the Elemental Analyzer.

Table 4-1 and Table 4-2 help to set accurate dilution values at varying EA flows. The values are based on a helium fore pressure of 1 bar. Dilution and sample intensity are related by the following equation:

Table 4-1. Dilution values at EA carrier flows of 80-140 mL/min*

*with helium fore pressure of 1 bar in the ConFlo IV. OS means open split.

EA flow[mL/min]

OS flow[mL/min]




80 8.0 38 56 81

90 9.0 36 53 80

100 10.0 33 50 78

110 11.0 31 48 76

120 12.0 29 45 74

130 13.0 28 43 73

140 14.0 26 42 71

Table 4-2. Dilution values at EA carrier flows of 80-140 mL/min (pre-split on)*

*with helium fore pressure of 1 bar in the ConFlo IV. OS means open split.

EA flow[mL/min]

OS flowwith PreSplit on[mL/min]




80 0.5 90.9 95.2 98.6

90 0.6 89.9 94.7 98.4

100 0.625 88.9 94.1 98.2

110 0.7 87.9 93.6 98.1

120 0.8 87.0 93.0 97.9

130 0.8 86.0 92.5 97.7

140 0.9 85.1 92.0 97.6

Dilution 100 % sample intensity–=



Example If your EA flow is 100 mL/min, your final flow into the open split (OS) of the ConFlo IV will be 10 mL/min, if the pre-split is off.

If your undiluted sample signal were 10 V, Dilution V1 would dilute your sample signal by 33 % to a signal intensity of 6.7 V, dilution 2 by 50 % to a signal intensity of 5 V and so on. The OS flow can be additionally reduced by a pre-split. This additional split inside the ConFlo IV reduces an incoming 10 mL/min to 0.625 mL/min. Together with Dilution V1-V3 another seven dilution steps can be achieved.

Calibrating the TCD-MS SignalRelation

The calibration of the TCD signal and the expected response in the mass spectrometer is done by the entries Start Reference Regression and Add Reference Regression in the Type column of the sequence grid.

• Start Reference Regression will delete previous entries while

• Add Reference Regression will add new entries to the existing calibration.

The response is linear (R2: 0.99-1.00) so that only few entries allow reasonable interpolation and extrapolation.

Note Isodat 2.5 will automatically set the sample dilution to zero, if the type in the sequence grid is set to any other than Sample. Calibration of weight percentage determination, TCD-MS signal calibration and blank determination require measurements without dilution.

Note Varying the helium fore pressure of the ConFlo IV will change the dilution efficiency of Dilution V1-V3. If this is needed, one must determine the dilution efficiency of Dilution V1-V3 with appropriate samples.

Fixed This mode allows predefined settings of reference gas amplitudes and sample dilution. If Isodat 2.5 cannot reach the predefined amplitudes or dilution, it will adjust to the nearest possible amplitude or dilution, which can be slightly higher or lower.

None This mode uses the settings at the start of the analysis. It does not change the settings. The previous sample dilution and reference gas dilution is used.

Note In case of dual measuremets (e.g. N2 and CO2 in one analysis, with Fast Jump), the entry of the intensities of the second gas will be possible not until the Jump has been defined in the time events list.


Operating ConFlo IV with EAEA Method

EA Method The following steps are needed to create a new method.

Instrument Tab

Temperature At Temperature, set the temperatures of the furnaces and the GC oven. See Figure 4-3. The temperatures of the furnaces can be set to 0 or any temperature between 400 °C and 1100 °C. The GC oven can be set to 0 or any temperature between 35 °C and 190 °C.


2. Select a configuration suitable for your ConFlo IV application, e.g. ConFlo IV + FlashEA.

3. Select the appropriate gas configuration for the intended measurement type, e.g. CO2.

4. Press the New button.

Figure 4-2. Creating a new EA method

5. Click on the EA icon.




Note Do not mark the checkbox Set instrument to Standby. The system will be set to standby upon upload of the method. For the standby procedure, refer to “Set Instrument to Standby and Auto-Ready Function” on page 4-10.

Flow/Timing At Flow/Timing, set the carrier flow and the reference flow (used for referencing in the TCD and to purge a solids autosampler). Furthermore, determine the amount of O2 injected for combustion. See Figure 4-4.

Note Unmark the oxygen checkbox when working with a high-temperature conversion reactor in the FlashEA 1112 HT for H and O isotope analysis.

Figure 4-3. Instrument tab - Temperature



Cycle (Run Time) determines the run time of the TCD trace. It starts when Isodat 2.5 triggers the EA (Start EA in the time event list of the Isodat 2.5 method). The run time must be long enough to detect all significant peaks when running in dynamic dilution mode (SmartEA™ function). The SmartEA option has the Part No. 122 7210.

Sampling Delay defines the autosampler start after oxygen injection. In order to allow simultaneous arrival of O2 and sample for accurate and complete combustion in the hot zone of the reactor, the sample must be dropped with a delay. This delay depends on the carrier gas flow, because the carrier gas transports the O2 into the hot zone. The higher the carrier gas flow, the shorter the delay.

Theoretical example: the volume above the reactor filling is approximately 34 mL. Assuming a carrier flow of 100 mL/min or 1.6 mL/s, it would take the oxygen 34 mL/(1.6 mL/s) = 20.4 s to arrive at the hot zone. In practice, it is recommended to drop an empty tin capsule with no delay. Use the peephole in the autosampler to time the arrival of the oxygen at the hot zone which is indicated by a short brighter glowing.

Figure 4-4. Instrument tab - Flow/Timing



Oxygen Injection End defines the duration of the oxygen injection. Together with the oxygen flow, the amount of oxygen (in mL) is determined. Example: the O2 flow is 180 mL/min and the injection end is after 3 s. This results in 9 mL of O2.

The needed amount depends on sample nature and weight (that is, the amount of C, N, S, and H in the sample which will be converted to their oxidized form). It is recommended having an excess of oxygen. For further information about sample oxidation, refer to Sample Oxidation in the FlashEA Operating Manual.

Detector

At Detector, switch the TCD filament off or on. The TCD must be switched on when running in dynamic dilution mode (Smart EA™ function). The SmartEA option has the Part No. 122 7210.

Evaluation Tab The parameters in Evaluation tab define the requirements for peak detection on the TCD trace. See Figure 4-6.

Figure 4-5. Instrument tab - Detector



TCD Control ParameterTab

TCD Control Parameter tab defines the significant peaks in the TCD trace for calibration. The retention time of the sample peak of the TCD trace must fall into the time window given by Peak Start and Peak End.

Isodat 2.5 labels the peaks in the TCD trace with gas name chosen from the pull down menu at Name. This is particularly important for the adjustment during dynamic dilution so that Isodat 2.5 adequately responds to the correct sample peak. The minimum peak height definition allows filtering of small unwanted peaks.

Figure 4-6. Evaluation tab

Figure 4-7. TCD control parameter tab


Operating ConFlo IV with EASet Instrument to Standby and Auto-Ready Function

Set Instrument toStandby and

Auto-Ready Function

After a sequence you can send the EA in a standby mode. Therefore, mark the checkbox Interface Standby after Sequence in the options of your sequence or when starting the sequence. See Figure 4-8.

In this condition, the temperatures of the left and the right furnace are decreased to 50 % of the operating temperatures, and the helium flow on both channels is reduced to 10 mL/min.

Use the Auto-Ready function to get your system back to operating conditions at any time. Therefore, proceed as follows:

1. In the EA Status window, click on the Auto-Ready tab.

2. Check the current date and time of your computer.

3. Enter the desired date and time when the EA shall awake and reset itself to the last operating conditions.

Figure 4-8. Interface standby after sequence checkbox


Operating ConFlo IV with EAWeight Percent Determination

Note The Elemental Analyzer will use the last settings before it was sent to standby. This function works only when the Elemental Analyzer has been sent to standby beforehand.

For additional information, refer to the FlashEA Operating Manual.

Weight PercentDetermination

Both TCD and mass trace can be used to determine the weight percent of an element, e.g. % C in a sample from CO2 produced during combustion in an Elemental Analyzer. In order to achieve accurate results, the system must be calibrated with a known standard (that is benzoic acid, urea, acetanilide etc.) using the entries in the Type column of the sequence. Refer to the EA Operating Manual.

Using the TCD trace for weight percentage determination can be of advantage when working with dilution. TCD signals are undiluted. In order to achieve accurate results, the monitored peaks must be defined at the TCD Control Parameters tab of the Elemental Analyzer method. See Figure 4-7.

Figure 4-9. Auto-Ready tab in Status window of Elemental Analyzer


Operating ConFlo IV with EAWeight Percent Determination

Note Isodat 2.5 will automatically set the sample dilution to zero, if the type in the sequence grid is set to any other than Sample. Calibration of weight percentage determination, TCD-MS signal calibration and blank determination require measurements without dilution.

Due to the low thermal conductivity of H2 the determination of hydrogen weight percentages is restricted with the TCD.

In the EA Status window, use the Detector tab to adjust the TCD. See Figure 4-10.

The TCD operates best under stable conditions. It is recommended to have the GC oven temperature stabilized for several hours. Also the flows of the carrier and reference line must have been set appropriately in time before the TCD signal can be adjusted to 1000 μV.

Note When using the TCD for oxygen and hydrogen measurements with high temperature conversion in a Flash HT, the Polarity shown at the TCD Settings in Figure 2-2 must be changed to Negative.

Figure 4-10. EA Status window - Detector tab


Chapter 5 Operating ConFlo IV with TC/EA

This chapter illustrates how ConFlo IV is operated in connection with a TC/EA.

An EA start cable is needed to run a MAS 200R autosampler on a TC/EA: via the ConFlo IV, the MAS 200R receives an electrical start signal.

The EA start cable (Part No. 210 5590) on the right side of Figure 5-1 and the optoelectronic coupler 3 (Part No. 209 5540) together form the Electronic EA Start Option (Part No. 800 1150).

The Electronic EA Start Option is included in the MAS 200R Upgrade kit (Part No. 072 3182) and will additionally be delivered together with the ConFlo IV for upgrading older instruments.

Figure 5-1. Signal transmission from ConFlo IV to MAS 200R

5

4 3 2 1

9-pole connectoroptoelectronic coupler(Part No. 209 5540)

2-pole connector 25-pole SUB D connectors EA start cable(Part No. 210 5590)

MAS 200R cable


Operating ConFlo IV with TC/EA

The MAS 200R cable on the left side of Figure 5-1 comes together with the autosampler MAS 200R. Together with the driver box and a 24 V power supply, it is part of the MAS 200R Upgrade kit (Part No. 072 3182).

• Connect the two-pole connector 5 to the driver box of the MAS 200R.

• The optoelectronic coupler 3 is directly plugged onto a 25-pole SUB D connector 2. Connect the optoelectronic coupler to the other 25-pole female SUB D connector 4 as shown by the arrows in Figure 5-1.

• Connect the 9-pole connector 1 to External Trigger 2 (that is Ext 2) at the rear panel of the ConFlo IV. See Figure 6-6.

In the time events list of the Isodat 2.5 method, the column Start Sampler provides the point in time when the signal will be transmitted to the MAS 200R. See Figure 5-2.

Figure 5-2. Start Sampler column in time events list


Chapter 6 Technical Information

This chapter provides technical information about the ConFlo IV. It contains the following topics:

• “Installation Kit for ConFlo IV” on page 6-2

• “Connections to ConFlo IV” on page 6-3

• “Incremental Helium Flow Controller” on page 6-16

• “ConFlo IV Diagnosis Window” on page 6-17


Technical InformationInstallation Kit for ConFlo IV

Installation Kit forConFlo IV

The parts needed during installation of the ConFlo IV are contained in the ConFlo IV installation kit. See Table 6-1.

Table 6-1. Selected parts of ConFlo IV installation kit (Part No. 122 2770)

Pos. Designation Part No. Quantity

1 ConFlo IV Operating Manual 122 4730 1

2 sample tray 122 8510 1

3 coupling nut, 202-1/8, brass

(for the connection of reference gas capillaries to the wall outlets)

052 1500 6

4 ferrule 1/8”-1/16”, Teflon

(for the connection of reference gas capillaries to the wall outlets)

067 4790 6

5 open-ended wrench, 5/16x1/4

(needed for installation)

057 1670 2

6 double open-ended wrench, 3/16

(needed for installation)

122 8490 1

7 ferrule; Removal Kit, Valco

(to remove used ferrules)

112 1090 1

8 hexagon socket wrench, SW2.5 (Inbus) 122 8520 1

9 connection to compressed air

(for the connection to the MS)

118 7740 1

10 ferrule FR.1/16” GVF/003 100 4850 5

11 septum, d = 7 mm, SGE

(spare part for later use)

122 5380 5

12 cannula, ID = 0.3 mm, l = 12 mm

(to feed capillaries to the septum seats)

122 8470 1

13 cannula, ID = 0.5 mm, l = 16 mm

(to feed capillaries to the septum seats)

122 8480 1

14 ferrule 1/16” GVF2/003

(to connect the two capillaries to the MS valve seat)

106 0170 2

15 capillary 0.10, fused silica

(replacement capillary from open split to MS)

104 8990 1.6 m

16 capillary 0.05, fused silica

(replacement capillary from open split to MS)

054 3380 1.6 m

17 EA splitter 122 8540 2


Technical InformationConnections to ConFlo IV

Connections toConFlo IV

Table 6-2 summarizes important parts of the basic module (Part No. 122 2760) of the ConFlo IV.

Table 6-2. Parts of basic module of ConFlo IV (Part No. 122 2760)

Pos. Designation Quantity Part No.

1 housing of ConFlo IV 1 122 4330

2 inlet module 1 122 4450

3 1-fold valve cluster (LF) 1 122 2380

4 3-fold valve cluster (HF) 1 122 2350

5 4-fold valve cluster 1 117 5780

6 pressure reducer FR1 2 122 4500

7 Kit for SO2 heater 1 122 6950

8 coupling, B-100-61, 1/16” 3 056 7350

9 ferrule, 1/16” GVF3/004 3 100 4790

10 coupling, M5i-M5i 1 067 4651

11 plug connector 2 117 7150

12 L plug connector 2 117 7320

13 cheese-head screw ISO4762-M4x8-A2 4 104 4420

14 disc ISO7089-4-A4 4 047 0040

17 pressure reducer FR1 3 122 2500

18 pressure reducer FR1 (stainless steel) 1 122 5490

19 Electronics of ConFlo IV 1 800 1130

20 capillary, 0.10, fused silica 3 m 104 8990

21 capillary, 0.18/0.27, fused silica 2.5 m 054 2910

22 capillary, 0.075, fused silica, 2 m 2 104 5480

23 capillary, 0.05, fused silica 1.2 m 054 3380

24 T-piece 1/16” B-100-3 1 052 3460

25 capillary, 1/16”, GC-CII 5 067 4820

26 capillary, 0.32, fused silica 2.75 m 100 4640

27 sulfinert tubing 1/16” x 0.03, stainless steel 3 m 122 6740

29 tubing, 1/16” OD x 0.04” ID 1.2 m 109 7570

30 ferrule, 1/16” GVF/003 7 100 4850

31 ferrule, 1/16” GVF2/003 2 106 0170

32 ferrule, 1/16” GVF/3/003 3 121 6730

33 capillary tube, 0.75 x 0.50 mm 0.1 m 106 8550

34 FS capillary tube, ID = 0.53 mm, deactivated 0.1 m 122 7150

35 T piece, 1/32”, without ferrule ZT.5J 1 104 0440

36 ferrule, FS.5, VICI 2 104 0480

37 ferrule, FS .4, VICI 1 104 0470



Front Panel

40 plate for compressed air connection 2 122 7390

42 distance sleeve for LF valve clusterl 2 122 7400

43 holder for T piece 1 122 7120

47 screw M3x8 DIN7991 (hexagon countersunk H) 4 021 3170

Table 6-2. Parts of basic module of ConFlo IV (Part No. 122 2760), continued


Figure 6-1. Ref 1 batch and Ref 2 batch at front panel

Table 6-3. Parts at front panel of ConFlo IV

Pos. in Figure 6-1

Designation Quantity Part No.

1 pressure reducer, brass knee upward 3 122 2500

2 pressure reducer, brass knee forward 2 122 4500

3 pressure reducer, stainless steel knee forward

1 122 5490

4 PTC heater, 24 V, 32 W 1 122 6690

5 capillary, stainless steel, 1/16” 18 m (6x3 m)

067 4820

2

3

1

H2 He

N2

CO

SO2

CO2

4

5

Ref 1 batch

Ref 2 batch



Table 6-3 summarizes the parts of the front panel that become visible after the front door has been opened. As Figure 6-1 shows, the pressure reducers of the different gases of Ref 1 batch and Ref 2 batch are then accessible. They allow to adjust the pre-pressures of the gases.

Rear Panel All connections to the ConFlo IV are established through the rear panel of its housing. See Figure 6-2.

The five reference gases and helium are directly connected to 1/16”stainless steel capillaries hanging out of the rear panel of the ConFlo IV. The stainless steel capillaries are directly connected to the pressure regulators of the ConFlo IV, which are accessible behind the door at the front panel of the device.

The electrical power to the heater for the SO2 pressure regulator is connected by a plug at the lower left corner of the rear panel.



Rear Panel from Outside Figure 6-2 shows the rear panel of the ConFlo IV, viewed from outside.

Figure 6-2. Rear panel - viewed from outside

H2

HeLF

LF He

N2

CO

Out Air In

MS MS Ref HF 1 HF 2

SO2

CO2

Bakeout

Ext 1 Ext 2

exhaust connection

connection port for low-flow peripheral

outlet for auxilliary helium if no low-flow peripheral is installed

compressed air in

compres-sed airout

connection for HF1 and HF2 peripherals

MS capillary for reference gas

MS capillary for sample gas

ConFlo IV control

trigger out external peripheral 1 trigger out external peripheral 2

heater for SO2

gas connec-tions

gas connec-tions



Table 6-4 summarizes the ports and connector types available at the rear panel of the ConFlo IV.

Connecting Elemental Analyzerby EA Splitter

Table 6-4. Ports, functions and connector types at rear panel

Port in Figure 6-2

Function Type

H2, He, N2, CO, CO2, SO2

gas supply for ConFlo IV stainless steel capillary, 1/16”

exhaust connection

exhaust for consumed gases round opening with nozzle (OD = 60 mm)

Ext 1 trigger out external peripheral 1

(24 V DC)

D-SUB connector, 9 pins, female

Ext 2 trigger out external peripheral 2

(24 V DC)

D-SUB connector, 9 pins, female

ConFlo IV control

control of ConFlo IV D-SUB connector, 37 pins, male

MS MS capillary for sample gas Swagelok connector, 1/16”

MS Ref MS capillary for reference gas Swagelok connector, 1/16”

HF 1 connection for HF 1 peripherals Swagelok connector, 1/16”

HF 2 connection for HF 2 peripherals Swagelok connector, 1/16”

Air Out distributor of permanent compressed air compressed air connector, female

Air In compressed air supply for ConFlo IV compressed air connector, male

Bake Out Heating of SO2 pressure reducer electric connector, 24 VL

LF connection port for low-flow peripheral VICI connector for fused silica capillary

LF He outlet for auxilliary helium if no low-flow peripheral is installed

Swagelok connector, 1/16”

Figure 6-3. EA splitter (Part No. 122 8540)

1

2

toEA

to ConFlo IV

3



The EA splitter, Part No. 122 8540, is shown in Figure 6-3. As a part of the ConFlo IV Installation Kit (Part No. 122 2770) it is listed in Table 6-1.

Table 6-5 lists data of the two capillaries 1 and 2 shown in Figure 6-3.

Note In the future, the parts of the T piece (3 in Figure 6-3) will be made of brass instead of stainless steel.

The EA splitter must be mounted between Elemental Analyzer and ConFlo IV (either to port HF I or to port HF II at its rear panel) as shown in Figure 6-4. The ports HF I and HF II are controlled by Isodat 2.5 according to the ConFlo IV sets that underlie the actual configuration.

In case of two high-flow peripherals, that is an Elemental Analyzer and a TC/EA, one must be connected to port HF I and the other one to port HF II.

The EA splitter realizes the necessary 10:1 split: it reduces the flow of 100 mL/min coming from the high-flow peripheral (that is Elemental Analyzer or TC/EA) to 10 mL/min that finally enter the ConFlo IV. The difference flow of 90 mL/min leaves the system via the purge capillary, 2 in Figure 6-3.

Table 6-5. Capillaries of EA splitter

Pos. in Figure 6-3 Length/mm Inner diameter/mm Part No.

1 90 0.13 116 4040

2 210 0.25 116 4030

Figure 6-4. Connecting Elemental Analyzer to ConFlo IV by EA splitter

to ConFlo IV

to EA

output HF I or HF II at rear panel of ConFlo IV



SmartEA Option In case of the SmartEA option (Part No. 122 7210), a functionally similar splitter, but with a different purge capillary, is used. One end of this SmartEA splitter must be connected to the Elemental Analyzer. The other end is connected to the ConFlo IV via a 20 m long capillary.

Remark on Trigger Outputs When triggering several Elemental Analyzers or GCs of external manufacturers, it is necessary for electronically educated users to know the technical specifications of the trigger outputs that can be expected. This is helpful for estimating the maximum dimensions of the devices that can be connected to the outputs.

In the lower part of Figure 6-6, the outputs Ext 1 and Ext 2 are shown offering two trigger outputs each (that is, totally four individual outputs).

Table 6-6 outlines the specifications of the outputs. The column Maximum Value lists the maximum values the outputs can be loaded with.

Figure 6-5 shows the output stage as a block diagram.

Table 6-6. Parameters for trigger outputs*

*Taken from Data Sheet TLE 6230 GP (V2.1, Page 1, 26. Aug. 2002) from Infineon Technolo-gies AG

Parameter Symbol Maximum Value

Drain source clamping voltage VDS(AZ)max 55 V

On resistance RON 0.75 Ω

Output current (all outp. ON equal) ID(NOM) 500 mA (individually)

1 A

Figure 6-5. Block diagram (output stage)**Taken from Data Sheet TLE 6230 GP (V2.1, Page 1, 26. Aug. 2002) from Infineon Technolo-gies AG

Output Stage



Rear Panel from Inside Figure 6-6 shows the rear panel of the ConFlo IV with the valve groups (viewed from inside).

View Inside ConFlo IV

Inlet Module

Figure 6-6. Rear panel with valve groups - viewed from inside

V1 V2

V1

V4 V3 V2 V1

V3

LF He

In Air Out

MS Ref MSHF 2 HF 1

Ext 2 Ext 1

Figure 6-7. Inlet module (Part No. 122 4450)

470

reference-gassupply-block

He-dilution-block

HFconnectionblock

LF-connection-block

412A

A



Figure 6-7 shows the ConFlo IV in side view. The inlet module can be seen and Table 6-7 summarizes important parts of it.

Table 6-7. Parts of inlet module (Part No. 122 4450)


1 mounting plate 1 122 4470

2 8-fold valve cluster (helium) 1 122 2330

3 5-fold valve cluster (reference gas) 1 122 2360

4 5/2-way valve 1 122 5410

5 lift cylinder 3 122 5420

7 septum holder 4 121 4040

8 reference open split 1 122 5460

9 sample open split 1 122 5470

10 bulkhead union 1/16”, stainless steel 2 116 2400

11 septum, d = 7 mm, SGE 4 122 5380




15 disc ISO7089-2-A4 2 102 6480


17 disc ISO7089-3-A4 1 047 0030



Open Split Module

In Figure 6-8, the mounted open splits and the valve clusters can be seen. The parts are mounted on a single mounting plate that can be dismantled as a whole.

Table 6-8 summarizes the parts of the 5-fold valve cluster for the reference gas (Part No. 122 2360).

Figure 6-8. Open Split module (Part No. 122 4450)

Table 6-8. Parts of 5-fold valve cluster for reference gas (Part No. 122 2360)


1 5-fold valve plate (reference gas) 1 122 0250

2 3/2-way flipper magnet valve, connector 5 122 2310

3 cheese-head screw ISO4762-M1.6x3-A4 20 122 7700

4 nut 1/16” ZN1-10 (VICI) 7 119 6110

5 ferrule 1/16” FS1.25-5 (VICI) 2 122 7440

6 ferrule 1/16” FS1.2-5 (VICI) 5 122 7430

5

9

8

4

10

reference-gassupply-block

He-dilution-block

7

1



Adress List of ConFlo IV

Figure 6-9. Addresses for ConFlo IV

Figure 6-10. Connecting ConFlo IV to DELTA V

Addresses for ConFlo IVDELTA XP/253

Address Bit Plug Addr. Plug Valve Group CF-Conn. Valve Function

0 J6201/2 1 HF-Capillary SAOS

1 J6201/21 2 MS-capillary SAOS

2 J6201/3 3 Ref I-capillary RefOS

3 J6201/22 4 Ref II-capillary RefOS

4 Block 2 J6201/4 J007 1 HF1

5 Block 2 J6201/23 J008 2 HF2

6 Block 1 J6201/5 J009 1 LF

7 Extern2 J6201/24 J6203/9; J005 - EA-Split

0 J6201/7 1 Sample dilution 1



3 J6201/25 4 Reference dilution 1





0 J6201/12 1 Ref II gas- CO

1 J6201/31 2 Ref II gas- CO2

2 J6201/13 3 Ref I gas - H2

3 J6201/32 4 Ref I gas - N2

4 J6201/14 5 Ref I gas - SO2

5 Extern1 J6201/33 J6202/5 - Trigger Out 1

6 Extern1 J6201/15 J6202/9; J006 - Trigger Out 2

7 Extern2 J6201/34 J6203/5 - Trigger Out 3

J004

J

002

J

003

J1104

J1106

J1103

Blo

ck

4(S

MC

)

Blo

ck 8

Blo

ck 5

22A

22B

22C

J521

J522

J

523

DELTA V

32B

32C

32A



Compressed AirConnections

Figure 6-11 shows a schematic of the compressed air connections.

Interconnections Schemeof ConFlo IV

Figure 6-12 shows a schematic of the gas connections, the open splits, the pressure regulators and the valve blocks.

Figure 6-11. Compressed air connections

V2

V3V4

V1

1 3

1

AIRIN

AIROUT

HF

3

MS

REFI

REFII



Figure 6-12. Interconnections scheme of ConFlo IV

CO

CO2

H2

N2

SO2

He

REF-II

REF-I

REF-I

LFHe

reference-gas

supply-b

lock

He-dilution-block

OS-R

EF

OS-S

2)

LF-connection-block

MS

MS/M

SREF

REF-II

HF-connection-block


Technical InformationIncremental Helium Flow Controller

Incremental HeliumFlow Controller

Alltogether, one valve block with eight valves and eight individual restrictions supplies the dilution capillaries of both open splits. The eight valves are installed onto one helium valve block to form the incremental helium flow controller. See Figure 6-14. Table 6-9 summarizes the parts of the incremental helium flow controller.

Figure 6-13. Capillary positions in OS Reference and OS Sample

MS sample

HF capillary

Sample dilution

1 mm2 mm

22 mm

LF connection

Sample Open Split

Ref I and Ref II

MS Ref

Ref. dilution

12 mm

2 mm

Reference Open Split

1 mm

Table 6-9. Parts of incremental helium flow controller (Part No. 122 2330)


1 8-fold valve plate (helium) 1 122 0260

2 2/2-way flipper magnet valve, connector 8 122 4880

3 cheese-head screw ISO4762-M1.6x3-A4 16 122 7700

4 nut 1/16”, ZN1-10 (VICI) 8 119 6110

5 ferrule 1/16” FS1.25-5 (VICI) 5 122 7440

6 screw fitting 1/16”, 5/16”-24 1 122 2560

7 ferrule 1/16” FS1.2-5 (VICI) 3 122 7430

Figure 6-14. Incremental helium flow controller (Part No 122 2330)

4 V1 V2 V3 V4 V5 V6 V7 V8

2


Technical InformationConFlo IV Diagnosis Window

ConFlo IV DiagnosisWindow

In Isodat 2.5, the ConFlo IV Diagnosis window, Figure 6-15, gives access to individual valves of the ConFlo IV.

In its lower part, individual valves of the incremental helium flow controller can be controlled. There are three valves for sample dilution (1) and five valves for reference dilution (2).

Three different sample ports (3) can be opened and closed directly. All five reference gas inlet valves (4) can be opened and closed indivdually as well.

Figure 6-14. Incremental helium flow controller (Part No 122 2330)

1

4,7 4,5

3

4,5 4,7

Figure 6-15. ConFlo IV Diagnosis window

76

3

21

4

58

9


Technical InformationConFlo IV Diagnosis Window

Note No protection mechanism has been implemented in ConFlo IV Extended window.

You may select every valve combination. For instance, you could select all reference inlet valves to be open. As a consequence, a mixture of the selected reference gases would flow through reference capillary 1 and reference capillary 2 into the open split.

Selecting the Reference Capillary buttons Ref I and Ref II (5) will move the reference capillaries in and out of the active volume of the reference open split.

The MS Capillary button (6) in the upper left corner will switch the pneumatic piston of the MS capillary in order to move the MS capillary in or out of the LF capillary. The LF capillary is installed on top of the open split and connects the sample open split to the low-flow peripheral.

The split valve (7) switches between two restrictions in order to split the flow coming from the high-flow peripheral to either 10 % flow or 0.5 % flow.


Glossary

This section lists and defines terms used in our manuals. It also includes acronyms, metric prefixes, symbols, and abbreviations.

A ampere

ac alternating current

ADC analog-to-digital converter

AP appearance potential

APCI atmospheric pressure chemical ionization

API atmospheric pressure ionization

ASCII American Standard Code for Information Interchange

b bit

B byte (8 b)

baud rate data transmission speed in events per second

°C degrees Celsius

CA collision activation

CI chemical ionization

CI/EI combined chemical/electron ionization

cm centimeter

cm3 cubic centimeter

CPU central processing unit (of a computer)

<Ctrl> control key on the terminal keyboard

d depth

Da dalton

DAC digital-to-analog converter

dc direct current

EI electron ionization

<Enter> Enter key on the terminal keyboard

ESA electrostatic analyzer

ESD electrostatic discharge

ESI electrospray ionization

eV electron volt

f femto (10-15)

°F degrees Fahrenheit

FI field ionization

FPGA Field Programmable Gate Array

ft foot

g gram

G Gauss; giga (109)

GC gas chromatograph; gas chromatography

GC/MS gas chromatograph / mass spectrometer

GND electrical ground

GPIB general-purpose interface bus

GUI graphical user interface

h hour

Thermo Electron Corporation ConFlo IV Operating Manual G-1

Glossary: HI

HI high intensity

HPLC high-performance liquid chromatograph

HR high resolution

HV high voltage

Hz hertz (cycles per second)

ID inside diameter

IEC International Electrotechnical Commission

IEEE Institute of Electrical and Electronics Engineers

in inch; 1 in = 25.4 mm

k kilo (103, 1000)

K kilo (210, 1024)

kg kilogram; 1 kg = 2.205 lb

kPa kilopascal; 100 kPa = 1 bar = 14.50 psi

l length

L liter

LAN local area network

lb pound; 1 lb = 0.4536 kilograms

LC liquid chromatograph; liquid chromatography

LC/MS liquid chromatograph / mass spectrometer

LED light-emitting diode

μ micro (10-6)

m meter

m milli (10-3)

M mega (106)

M+• molecular ion

MB Megabyte (1048576 bytes)

MFC mass flow controller

MH+ protonated molecular ion

MID Multiple Ion Detection

MIKES Mass analyzed Ion Kinetic Energy Spectrometry

min minute

mL milliliter

mm millimeter

MPa megapascal

MS mass spectrometer; mass spectrometry

MS MSn power: where n = 1

MS/MS MSn power: where n = 2

MSn MSn power: where n = 1 through 10

m/z mass-to-charge ratio

n nano (10-9)

NIST National Institute of Standards and Technology (USA)

Ω ohm

OD outside diameter

OS Open Split

p pico (10-12)

Pa pascal

PCB printed circuit board

PFK Perfluorokerosene

G-2 ConFlo IV Operating Manual Thermo Electron Corporation

Glossary: PID

PID proportional / integral / differential

P/N part number

P/P peak-to-peak voltage

ppm parts per million

psig pounds per square inch, gauge

PTFE Polytetrafluoroethylene

RAM random access memory

RF radio frequency

RMS root mean square

ROM read-only memory

RS-232 industry standard for serial communications

s second

SIM selected ion monitoring

SRM selected reaction monitoring

T Tesla

TCD Thermal Conductivity Detector

TCP/IP transmission control protocol / Internet protocol

TIC total ion current

Torr torr

u atomic mass unit

V volt

V ac volts alternating current

V dc volts direct current

vol volume

w width

W watt

Thermo Electron Corporation ConFlo IV Operating Manual G-3

Thermo Fisher Scientific Inc.

81 Wyman Street

P.O. Box 9046

Waltham, Massachussetts 02454-9046

United States

www.thermo.com

Part of Thermo Fisher Scientific

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