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IST16 User manual – Version 8.0
SRA
INSTRUMENTS
210 rue des Sources
69280 Marcy l'Etoile
FRANCE
Storage Interface IST16
User manual
T : 04.78.44.29.47
F : 04.78.44.29.62
info@sra-instruments.com
www.srainstruments.com
SAS au capital de 150.000 €
RCS Lyon B 342 068 731
APE 4669B
SIRET: 342 068 731 00054
Code TVA FR 40342068731
p. 1 / 59
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Table of Contents
Summary of Contents for SRA IST16
- Page 1 IST16 User manual – Version 8.0 Storage Interface IST16 User manual INSTRUMENTS T : 04.78.44.29.47 SAS au capital de 150.000 € 210 rue des Sources F : 04.78.44.29.62 RCS Lyon B 342 068 731 69280 Marcy l'Etoile info@sra-instruments.com APE 4669B FRANCE www.srainstruments.com...
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Page 2: Table Of Contents
4.3 Installation of the capillary on the GC injector _________________________________________ 12 4.4 Installation of the transfer line on the TGA ____________________________________________ 13 4.5 Vents __________________________________________________________________________ 14 5. INSTALLATION AND CONFIGURATION OF THE IST16 SOFTWARE ______________________ 14 5.1 Software installation _____________________________________________________________ 14 5.2 Configuration of the IST16 _________________________________________________________ 14 5.3 Advanced options ________________________________________________________________ 16... - Page 3 11.1 Flow/pressure problem with GC ___________________________________________________ 40 11.1.1 Find the origin of the problem __________________________________________________ 40 11.1.2 There is a leak on the IST16 side _________________________________________________ 41 11.2 Problem of flow restriction _______________________________________________________ 44 11.2.1 Find the problem _____________________________________________________________ 44 11.2.2 Clean the inside of the IST16 ____________________________________________________ 45...
- Page 4 12.6 Inputs/Outputs _________________________________________________________________ 50 12.7 Recycling ______________________________________________________________________ 50 13. ABOUT ____________________________________________________________________ 50 14. APPENDIX I: IST16 REMOTE OUTPUTS & I/O _____________________________________ 51 15. APPENDIX II: CONNECTING THE IST16 TRANSFER LINES_____________________________ 52 16. APPENDIX III: INSTALLATION CHECKOUT SAMPLE _________________________________ 53 16.1 Sample and conditions ___________________________________________________________ 53 16.2 Instrument parameters __________________________________________________________ 53...
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Page 5: Introduction
SRA Instruments, the protection provided by the equipment may be impaired. Moreover, it is the responsibility of the customer to inform SRA Instruments after-sales service if the IST16 has been used for the analysis of hazardous samples, prior to any instrument service being performed or when an instrument is being returned for repair. -
Page 6: For Experiments
These fractions can then be injected separately into GC-MSD for a detailed analysis. Thanks to IST16, the duration of the analysis is no longer a limitation for the study of TGA profiles. 3.2 Principle of operation The interface consists of: 1. -
Page 7: Fluid Flow Diagram
The alarms on the front panel are then active and it is recommended to contact the after-sales support in this case. 3.3 Fluid flow diagram The IST16 is equipped with 3 high temperature switching valves. The 16 loops of the storage valve have a default volume of 250 µL and have an external tube diameter of 1/16 inch. -
Page 8: Storage Mode
IST16 User manual – Version 8.0 3.3.1 Storage mode This storage mode is not available on IST1. For this latter, refer to appendix IV chapter 17. INSTRUMENTS T : 04.78.44.29.47 SAS au capital de 150.000 € 210 rue des Sources F : 04.78.44.29.62... -
Page 9: Injection Mode
This injection mode is not available on IST1. For this latter, refer to appendix IV chapter 17. 3.4 Automated control software The IST16 software has been developed to control the IST16 storage interface. The storage sequence can trap up to 16 samples. -
Page 10: Installation
4. Installation 4.1 Preparation for the installation The installation of the IST16 is performed by an SRA Instruments technician or a recognized partner. To be able to set up the equipment in your laboratory, it is necessary to provide: •... -
Page 11: Modification Of The Gc Carrier Gas System
GC remote Power Supply 4.2 Modification of the GC carrier gas system In order to supply the IST16 with carrier gas, a 3-way valve will be mounted on the GC. This valve allows switching the carrier gas: • Through the storage interface for the TGA/IST16/GC-MS mode, allowing injection with the IST16. -
Page 12: Installation Of The Capillary On The Gc Injector
Swagelok 1/16" union GC S/SL injector The carrier gas connection to the IST16 is located on the back of the upper panel. The fitting is 1/16‘’ Swagelok type. We recommend that you use new ferrules during installation and follow the coupling manufacturer’s recommendations for tightening to ensure the best seal. -
Page 13: Installation Of The Transfer Line On The Tga
IST16 User manual – Version 8.0 We recommend to possibly put a mark to adjust the depth once the line is in place. 4.4 Installation of the transfer line on the TGA The transfer line is normally supplied with the connection corresponding to your TGA model. This can be a DN16 flange (Mettler case) or a simple double ring fitting (TA, Setaram cases...). -
Page 14: Vents
Before launching the entire installation of the application, you can check the data entered by clicking on the Back button and correct any mistake. 8. In the new window, check the box “Launch IST16” to launch the application as soon as you exit the installation. - Page 15 The following window is displayed: Enter the IP address and validate with Ok; the software automatically tries to connect to the interface. When connecting to the IST16 and if a method has already been loaded, the following message may be displayed: This message means that the parameter values of the IST16 method are different from those of the method loaded in the application.
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Page 16: Advanced Options
7. When the 'Manual mode' checkbox is checked, the user can work manually with the IST16 and has access to the method parameters. For more information on the manual mode, please refer to chapter 9.3. -
Page 17: Operate With The Ist16 Software
GC cycle time must correspond to the GC analysis time. It is used to adjust the delay between two injection loops. 6.1 Washing The washing sequence can be started when the IST16 is idle by checking the Washing option and clicking on the Start button. INSTRUMENTS T : 04.78.44.29.47... -
Page 18: Temperatures
The temperature can be set between 150 and 250 °C. Click on "Apply" to send values to the storage interface, then click on "Ok" and save in the IST16 method. Note that when the temperature from 150 to 250 °C is applied, the storage interface will start its own heating procedure and will automatically trigger the switch valves during the temperature raise. -
Page 19: Storage Time
IST16 User manual – Version 8.0 6.4 Storage time During the storage sequence of an experiment, the multi-position valve allows each loop to be flushed with the emitted gas for a period of time. This time is defined in the window below accessible from the Method\Storage Time menu. - Page 20 IST16 User manual – Version 8.0 Note that if a set time is not correct, the input value is displayed in red. When all changes are made, click on the “OK” button to confirm. The software checks the values and if there is an error, it reports it with the message: •...
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Page 21: Washing Parameters
The checkbox 'Stop heating after cycle' allows you to stop heating the oven and the lines when the washing cycle is finished. This is useful when the operation is finished and you want to put the IST16 in standby mode. -
Page 22: Options
It is also important to check the box 'Running by external start' so that the IST16 waits for the signal from the TGA at the end of the analysis of the last loop to restart the next storage cycle. -
Page 23: Gas Sampling Valve (Without Multi-Injection)
IST16 User manual – Version 8.0 7.1 Gas sampling valve (without multi-injection) The interface will inject only once into the chromatograph for each analysis. The parameters can be changed via the Method\Injection menu. The following window appears: The injection will be carried out after the indicated sampling time and the analysis cycle will be started after the injection. -
Page 24: Multi-Injection
IST16 User manual – Version 8.0 You can repeat the cycle several times. If the 'Running by external start' option is checked, the IST16 will wait for the TGA to start before performing the sampling. 7.2 Multi-injection The interface will inject several times in the chromatograph during the same analysis. -
Page 25: Dialog With The Interface
IST16 User manual – Version 8.0 In the example above, the interface injects every 30 seconds during the TGA experiment, with the first injection after 20 seconds of loop flushing. If the option is checked, the cycle will only start after receiving the external start from the TGA. -
Page 26: Storage Interface
IST16 User manual – Version 8.0 9. Storage interface The storage interface is equipped with a touch screen from which various operations can be performed. From the 'Monitoring' page, it is possible to view the status of the interface. The display shows the various faults present or alarm, the status of the logic inputs and the oven temperature. -
Page 27: Control And Maintenance
IST16 User manual – Version 8.0 9.1 Control and maintenance The Tools button in the bottom right corner of the 'Control' screen allows you to access the screens to perform different control or maintenance. This mode is protected by a password. -
Page 28: Changing The Ip Address Of The Interface
IST16 User manual – Version 8.0 The Analog input 2 value is only used if the IST16 pressure reading option is enabled. Indeed, it could be considered to equip the IST16 with a pressure sensor and this input would allow to read it. -
Page 29: Manual Mode
IST16 User manual – Version 8.0 In the upper left corner, the button gives access to the low level resources of the PLC. Press this button. After a beep, the PLC goes into low level configuration mode, the display of the 'Home' tab shows the firmware version of the Proface. -
Page 30: Analysis Parameters
IST16 User manual – Version 8.0 The Run button is used to start the storage cycle or the injection cycle when the storage mode has been completed. Press the Wash button to start the washing cycle. An additional button is displayed on the 'Control' screen. This button gives access to the parameters of the method. -
Page 31: Storage Parameters
IST16 User manual – Version 8.0 9.3.2 Storage parameters 9.3.3 Washing parameters INSTRUMENTS T : 04.78.44.29.47 SAS au capital de 150.000 € 210 rue des Sources F : 04.78.44.29.62 RCS Lyon B 342 068 731 69280 Marcy l'Etoile info@sra-instruments.com APE 4669B FRANCE www.srainstruments.com... -
Page 32: Options
IST16 User manual – Version 8.0 9.3.4 Options 9.3.5 Gas sampling parameters When the IST16 is configured in Gas Sampling mode, the 'Storage parameters' screen is not available and is replaced by the 'Gas Sampling' screen. 9.3.6 Multi-injection parameters When the IST16 is configured in Multi-injection mode, the 'Storage parameters' screen is not available and is replaced by the 'Multi-injection' screen. -
Page 33: Error And Fault Messages
IST16 User manual – Version 8.0 9.4 Error and fault messages The various error or fault messages are displayed on the 'Monitoring' screen. Different information can be displayed: Oven Ready message: This means that the oven temperature has been reached and the storage sequence can be performed. -
Page 34: Maintenance Operations
➢ Check air and water levels using the MSD signal with carrier gas flowing through IST16, in standby mode. If the level is too high, check for leaks throughout the entire configuration. ➢ Clean the sample path of the IST16 with a solvent (≈ 20 mL) if you don't use a Teflon protective tube. -
Page 35: Every 6 Months
You can also replace the Teflon® protective tube if necessary. c. The programmable IST16 cleaning sequence is used to clean the loops after a sequence (a total cleaning time of at least 5 minutes for each loop is recommended). -
Page 36: Clean The Valve And Rotor
IST16 User manual – Version 8.0 10.3 Clean the valve and rotor 10.3.1 Disassembly the valve 1. Shutdown IST16 heating. 2. Wait until the oven temperature is around 50 °C, otherwise the preload assembly thread may become permanently blocked. 3. Unscrew totally the preload assembly. -
Page 37: Clean The Inside Of The Valve Body
IST16 User manual – Version 8.0 10.3.2 Clean the inside of the valve body 1. After taking out the rotor, wet a cotton stab with methanol or isopropyl alcohol. 2. Clean gently by dabbing the inside of the valve body to remove any residue. -
Page 38: Change Tubing Or Fitting
11. Locate the origin of the problem TGA/IST16/GC-MS coupling is a complex and powerful solution having 3 independent devices: a TGA, an IST16 and a GC-MS. Each device can have a problem and therefore affect the results given by the other 2 devices. - Page 39 IST16 User manual – Version 8.0 Most common problems Paragraph No flow in GC No pressure in GC 11.1 GC can’t hold the pressure No peak Small peak 11.2 Flow restriction TGA oven back pressure Memory effect 11.3 High level of air in MS 11.4...
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Page 40: Flow/Pressure Problem With Gc
The GC can’t hold pressure and flow Everything works normally. Conclusion: There is a problem on the GC side. Conclusion: There is a leak on the IST16 side Check the septum, the column connection and (See next paragraph). the tube leaks. -
Page 41: There Is A Leak On The Ist16 Side
3. Let the split flow at a ratio of 1:3 and the GC oven at the maximum temperature of the analytical method. 4. Lower the temperature of the IST16 to 50 °C. Make sure that the 3-way manual valve is in the IST16 position. - Page 42 IST16 User manual – Version 8.0 In the IST16 oven, located between the rear panel of the IST16 and the injection valve → check for leaks and replace tube and ferrules if necessary. On the rotor of the injection valve → clean the rotor (see paragraph 10.3); replace it if necessary.
- Page 43 Change the atmospheric pressure valve. Contact SRA Instruments or your TGA support company for the next steps. INSTRUMENTS T : 04.78.44.29.47 SAS au capital de 150.000 €...
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Page 44: Problem Of Flow Restriction
In this case, clean the sampling transfer Use a standard gas cylinder instead of a TGA line with a solvent (see § 11.2.2) sample for sampling/storage. It will help you to validate the IST16/GC/MS system. INSTRUMENTS T : 04.78.44.29.47 SAS au capital de 150.000 €... -
Page 45: Clean The Inside Of The Ist16
Exothermic reactions may occur at this stage. 3. At the end of the cleaning, run a wash sequence from the IST16 software using a nitrogen flow (5 minutes wash per loop) for 2 hours. 4. After the cleaning: start a GC-MS analysis using storage with nitrogen to check the memory effect. -
Page 46: Problem Of Memory Effect
Check the condition of the union and Teflon® tube; change them if necessary. Disconnect the IST16 from the TGA. Connect your reactive gas directly to the IST16 without passing through the TGA. Run storage and analysis with 3 to 16 loops. Clean the TGA oven with a dedicated method. -
Page 47: Problem With Oven Display And Multi-Position Valve Number
IST16 User manual – Version 8.0 11.5 Problem with oven display and multi-position valve number If you see this : Close the application and switch off the IST16. Then switch it on and restart the application. If the connection is still not established,... - Page 48 The valve may have lost its identifier or Check the LAN communication with is probably blocked if you hear an the IST16 by performing a 'ping' with unusual noise from the motor. its address. Follow the procedure for resetting the ID or the one for rotor cleaning.
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Page 49: Technical Data
Ethernet port IEEE 802.3u 10/100 BASE-T fast Ethernet Compatible 12.4 Utilities The SRA IST16 interface must be located between TGA and GC. This requires a space of at least 40 cm wide. Power: 220-240 VAC; 1000 W max GC specification •... -
Page 50: Carrier Gases
The IST16 is compatible with helium, nitrogen, and argon, with Swagelok fittings. 12.4.2 Repeatability Typical RSDs at constant temperature and pressure including SRA MPA system: ≤ 5 % 12.5 Fuses Presence of 2 fuses on the back of the instrument at the bottom right. -
Page 51: Appendix I: Ist16 Remote Outputs & I/O
IST16 User manual – Version 8.0 14. Appendix I: IST16 Remote outputs & I/O INSTRUMENTS T : 04.78.44.29.47 SAS au capital de 150.000 € 210 rue des Sources F : 04.78.44.29.62 RCS Lyon B 342 068 731 69280 Marcy l'Etoile info@sra-instruments.com... -
Page 52: Appendix Ii: Connecting The Ist16 Transfer Lines
IST16 User manual – Version 8.0 15. Appendix II: Connecting the IST16 transfer lines The power cable depends on the voltage of your IST16: INSTRUMENTS T : 04.78.44.29.47 SAS au capital de 150.000 € 210 rue des Sources F : 04.78.44.29.62... -
Page 53: Appendix Iii: Installation Checkout Sample
IST16 User manual – Version 8.0 16. Appendix III: Installation checkout sample 16.1 Sample and conditions • Sample: Calcium carbonate (CaCO • Measuring cell: TGA/DSC 3+ with SDTA sensor, IST16 storage interface, Agilent 7890A GC / 5975C MSD. • Pre-treatment: None •... -
Page 54: Results
), the theoretical calculated weight loss is 44 %. The effect observed at about 900 °C corresponds to IST16 position change from storage mode to injection mode (after collection of the last loop) and is not related to a thermal effect. -
Page 55: Tga/Ist16/Gc-Ms
0.8 mL/min. Scan mode from m/z 35 to m/z 55 and an EMV gain of 1 were used for the MS detector. The IST16 interface transfer lines and oven were set to 250 °C. A PTFE filter tube is placed between the TGA outlet and the IST16 transfer line to protect the interface. -
Page 56: Conclusion
Figure 3: TGA curve and m/z 44 evolution profile 16.4 Conclusion Calcium carbonate (CaCO ) can be used as a standard for the TGA-IST16-GC/MS system proof of concept for on-site verification. CaCO decomposes to CaO and CO . The mass loss measured by the TGA should be 44 % →... -
Page 57: Appendix Iv: Ist1
(default) and Multi-injection modes are available. For maintenance operations, the recommendations are the same as for the IST16. Note that it is possible to upgrade from an IST1 MONO version to an IST16 version by returning the unit to the manufacturing plant. -
Page 58: Injection Parameters - Gas Sampling Mode
The parameter 'GC Run time' must correspond to the analysis time of the GC method. It is possible to launch several cycles; each cycle can start on receipt of an external start from the TGA. The recommendations are the same as for use with an IST16. 17.2 Injection parameters – Multi-injection mode The injection parameters are available under the Method\Injection menu. -
Page 59: Eu Declaration Of Conformity
IST16 User manual – Version 8.0 18. EU declaration of conformity SRA Instruments 210 Rue des Sources 69280 MARCY L'ETOILE FRANCE As a manufacturer, declare under our sole responsibility that the instrument type IST16 Storage interface for gas to which this declaration relates, meets the Essential Health and Safety Requirements applicable to it and which are...
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