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IST16 User manual

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Version 8.0

SRA

INSTRUMENTS

210 rue des Sources
69280 Marcy l'Etoile
FRANCE

T : 04.78.44.29.47
F : 04.78.44.29.62
[email protected]
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. 9 / 59

3.3.2

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.

The injection sequence then allows injecting these samples into a chromatograph (optionally coupled to a
mass spectrometer) in an automated way.

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Summary of Contents for IST16

Page 1: ...ces 69280 Marcy l Etoile FRANCE 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 Storage Interface IST16 User manual ...

Page 2: ..._________ 10 4 1 Preparation for the installation _____________________________________________________ 10 4 2 Modification of the GC carrier gas system_____________________________________________ 11 4 3 Installation of the capillary on the GC injector _________________________________________ 12 4 4 Installation of the transfer line on the TGA____________________________________________ 13 4 5 V...

Page 3: ...__________ 33 10 MAINTENANCE OPERATIONS__________________________________________________ 34 10 1 Maintenance schedule ___________________________________________________________ 34 10 1 1 After each experiment ________________________________________________________ 34 10 1 2 Every week _________________________________________________________________ 34 10 1 3 Every month _______________________...

Page 4: ..._______ 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 _____________________________________...

Page 5: ...ract are neither extended nor limited by the content of this manual 2 Safety instructions Important information This instrument is designed for use in very specific conditions If the equipment is used in a manner not specified by 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 i...

Page 6: ... is above 100 C Do not open the electronic box Eliminate from the environment of the instrument vibrations magnetic effects and explosive gases The IST16 must be used indoors only it is designed for use at room temperature and under conditions where no condensation can occur Install the IST16 on a rigid and stable surface 3 Description 3 1 Presentation The IST16 is an interface for storing gases d...

Page 7: ...eating zones to maintain the temperature up to 250 C Each of these 2 heating zones is coupled with an independent safety device which switches off the power if the threshold is exceeded 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...

Page 8: ...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 8 59 3 3 1 Storage mode This storage mode is not available on IST1 For this latter refer to appendix IV chapter 17 ...

Page 9: ...731 00054 Code TVA FR 40342068731 p 9 59 3 3 2 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 The injection sequence then allows injecting these samples into a chromatograph optionally...

Page 10: ...31 p 10 59 This software is optimized for operation under Microsoft Windows 7 or 10 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 1 power supply 237 VAC 16 A Approximately 40 cm wide on the right side of the GC Us...

Page 11: ...screwdriver 1 electronic leakage detector Allen key 9 64 and Allen key 7 64 1 electronic flowmeter The following cables are supplied with the IST16 TGA remote Ethernet 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...

Page 12: ...ning to ensure the best seal A leak control with electronic detector is recommended periodically to check for leakage that can degrade the analysis and create overconsumption of carrier gas The use of hydrogen carrier gas for IST16 is not recommended It is better to use helium for safety reasons 4 3 Installation of the capillary on the GC injector The transfer line on the Split Splitless injector ...

Page 13: ...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 We recommend the use of a transfer tube of 1 8 diameter Depending on the type of connection and type of thermo balance it may be desirable to mechanically maintain the transfer line in order to no...

Page 14: ...ned Select the file Setup exe right click on this file and select the menu Run as Administrator 3 A welcome window is displayed click on Next 4 Then accept the terms of the license agreement so that you can go on with the installation 5 In the window Destination location select the folder where the application files will be stored by entering its name or by clicking on Browse 6 In the window Selec...

Page 15: ...guration of the IST16 must not be used by people not trained When you have entered the password select the Interface Configuration Ip address menu 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 mes...

Page 16: ...the interface is used in Storage mode You can also use the Gas sampling valve or Multi injection modes which will be described in chapter 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 The Automatic wash checkbox allows the user to activate the request f...

Page 17: ...t programmed time 2 Second step loops are injected and analyzed one after the other 3 Third step loops are cleaned with the flowing gas coming from the TGA at the end of the GC analysis sequence The storage sequence can only be started when the interface oven temperature is steady Before each injection of a loop the software checks that the gas chromatograph is in a ready state green color The GC ...

Page 18: ...e changed in the Method Temperatures menu The following window appears 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 ...

Page 19: ...2 068 731 APE 4669B SIRET 342 068 731 00054 Code TVA FR 40342068731 p 19 59 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 A fraction of the emitted gas typically 250 μL will be stored in one of the 16...

Page 20: ...8 731 00054 Code TVA FR 40342068731 p 20 59 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 If you click on the Yes button the software corrects the values and displays again the window If you click on the Cancel button it dis...

Page 21: ...fication or for the study of the composition of a mixture It is indeed customary to set up the storage sequence with a very short time on the first loop of the series in order to start storing the first compounds of interest on the second loop of the series 6 5 Washing parameters After the analysis sequence you must flush the injection loops A washing time common to all the loops used is accessibl...

Page 22: ...njected and analyzed 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 The checkbox Run the inject sequence after the storage sequence allows to start the injection cycle as soon as the storage cycle is finished If the Running by external start checkbox is...

Page 23: ...42 068 731 APE 4669B SIRET 342 068 731 00054 Code TVA FR 40342068731 p 23 59 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 aft...

Page 24: ...1 APE 4669B SIRET 342 068 731 00054 Code TVA FR 40342068731 p 24 59 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 The parameters can be changed via the Method Injection menu The ...

Page 25: ...cts 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 8 Dialog with the interface Two menus allow either to load the method from the application to the interface Load method or to retrieve the method of the interface Upload method These two actions ...

Page 26: ...ich 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 X GC Not Ready O GC Ready By clicking on the arrow at the top left of the screen the Control page is displayed From this page it is possible to switch on the heating of the o...

Page 27: ...cess the screens to perform different control or maintenance This mode is protected by a password The password is 2947 From this page you can switch on either the oven only or the heated lines You can control the atmospheric pressure release valve and monitor the temperature of the oven and of the safety sensor as well as the status of the logic inputs The following screen allows you to view the A...

Page 28: ...f 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 This page also displays the IP address of the interface To change this address refer to chapter 9 2 The last page of this mode allows to control the position of the different valves 9 2 Changing the IP address of the interface When power is tu...

Page 29: ...the MainUnit tab a new screen gives access to different buttons Press the Ethernet button From the new screen it is possible to change the IP address and the Subnet Mask Keep the port value at 8000 The bottom right arrow displays the Mac address of the interface and the fields for changing the GateWay address When you have modified the IP address click on the Exit button to reset the interface the...

Page 30: ...50 000 RCS Lyon B 342 068 731 APE 4669B SIRET 342 068 731 00054 Code TVA FR 40342068731 p 30 59 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 9 3 1 Analysis parameters ...

Page 31: ...80 Marcy l Etoile FRANCE 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 31 59 9 3 2 Storage parameters 9 3 3 Washing parameters ...

Page 32: ...PE 4669B SIRET 342 068 731 00054 Code TVA FR 40342068731 p 32 59 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...

Page 33: ... Oven Ready message This means that the oven temperature has been reached and the storage sequence can be performed Oven Not Ready Message This means that the oven temperature is changing Heating stopped message This means that the heating is stopped and that no storage cycle can be performed Heating alarm message This message appears if there is a heating fault in the oven o Either the oven does ...

Page 34: ...tion valve is not recognized loss of ID power off or faulty Inject valve default message This message appears if the injection valve is not recognized loss of ID power off or faulty This information is also displayed in the software At the end of the cycle the IST16 resets these parameters and checks the presence of the valves 10 Maintenance operations 10 1 Maintenance schedule 10 1 1 After each e...

Page 35: ... 10 2 Typical cleaning after an experiment IST16 a Check all the removable fittings between the input transfer line and the TGA and if necessary clean them with ethanol or isopropanol b 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 recom...

Page 36: ... p 36 59 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 4 Operate the storage valve from the software to disengage the rotor from the valve body 5 Note the direction in which the rotor is positioned and ca...

Page 37: ...o remove any residue 3 Also be careful to remove any fiber left during the cleaning 4 Visually check the inside of the valve body The conical surface must be smooth The presence of a scratch between the holes can lead to leakage in this case the valve body must be replaced 10 3 3 Clean the rotor 1 Carefully grasp the rotor tip taking care not to damage the metal or polymer 2 Immerse it briefly in ...

Page 38: ...3 turns by hand 4 Push the tubing so that it gets in place this is essential for proper connection with zero dead volume 5 Turn the nut manually until you can tighten it by hand 6 Use the appropriate wrench and screw the nut of a turn 90 after the point where the ferrule begins to touch the tubing 11 Locate the origin of the problem TGA IST16 GC MS coupling is a complex and powerful solution havin...

Page 39: ... au capital de 150 000 RCS Lyon B 342 068 731 APE 4669B SIRET 342 068 731 00054 Code TVA FR 40342068731 p 39 59 Most common problems Paragraph No flow in GC No pressure in GC GC can t hold the pressure 11 1 No peak Small peak Flow restriction TGA oven back pressure 11 2 Memory effect 11 3 High level of air in MS 11 4 Problem with oven display and multi position valve number 11 5 ...

Page 40: ...heck your carrier gas pressure level Is it correct 5 bar on Agilent GC Change your cylinder or open the valve until the correct pressure is reached Lower the GC injector temperature to 50 C Disconnect the IST16 transfer line and turn the 3 way manual valve to let the carrier gas flow directly into the GC Let the split flow at a ratio of 1 3 and the GC oven at the maximum temperature of the analyti...

Page 41: ...he 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 5 Use the IST16 interface to help you find the leak Maintenance menu Sampling valve screen Step 1 Legend Inactive Active In this configuration of the IST16 the leak may be On the GC septum side change the septum if necessary Chec...

Page 42: ... 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 If the GC holds the pressure in this position go to step 2 Step 2 Legend Inactive Active In this configuration of the IST16 the leak may be Between the injection valve connection and the isolation valve connection check for leaks and replace tub...

Page 43: ...e loop and check if the leak has disappeared replace it if necessary On the rotor of the storage valve clean the rotor paragraph 10 3 replace it if necessary On the connection between the isolation valve and the storage valve check for leaks and replace tube and ferrules if necessary On the atmospheric pressure release valve inspect the plastic vent located on the rear panel if you detect helium a...

Page 44: ...m Check the flow 50 mL min at the TGA inlet Then with the TGA oven closed check the flow at the IST16 outlet Both flows must be very close Is it the case Conclusion There is a leak or a restriction Disconnect the IST16 and run a cleaning method on the TGA Check the condition of the union and Teflon tube change them if necessary In this case clean the sampling transfer line with a solvent see 11 2 ...

Page 45: ... C line and oven and use a nitrogen flow to push slowly a small volume of solvent isopropyl alcohol inside the system 2 A contaminated loop or a transfer line can also be replaced The rotor must be cleaned after this operation Place an evacuation at the outlet of the IST16 in a recovery vial products may come out in liquid form Exothermic reactions may occur at this stage 3 At the end of the clean...

Page 46: ...rom the IST16 transfer line Clean it with a solvent Run storage and analysis again If there is really a significant contamination it is possible to change a loop or the transfer line If the memory effect decreases run after run it means that the problem comes from the TGA oven Run some blanks and storages with an empty crucible using your current TGA method 11 4 Problem of high level of air in MS ...

Page 47: ...ulti position valve number Change the IP address if necessary and confirm with the OK button If you see this The indication No configured means that the connection with the IST16 has been lost Close the application and switch off the IST16 Then switch it on and restart the application If the connection is still not established enable configuration with the Interface Configuration menu using the Co...

Page 48: ... the oven display and the multi position valve number two possibilities 1 After refreshing if you still observe an unknown status for both multi position valve and heated zone 2 After refreshing if you still observe an unknown status for the multi position valve only Check the LAN communication with the IST16 by performing a ping with its address The valve may have lost its identifier or is probab...

Page 49: ...f valves 3 injection storage isolation with automatic management Heated zones 2 electronically regulated Loop volume 250 µL in standard customized volumes on demand Heated transfer lines Small internal diameter x 1 15 meter in SulfinertTM stainless steel Tmax 300 C Valve box temperature 250 C as standard working temperature 300 C can be reached for specific applications Ethernet port Ethernet port...

Page 50: ...h 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 220 VAC Instrument Fuses T4AH 250 VAC 110 VAC Instrument Fuses T6 2AH 110 VAC To change them turn off the power and unplug the power cable 12 6 Inputs Outputs Refer to ap...

Page 51: ...s 69280 Marcy l Etoile FRANCE 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 51 59 14 Appendix I IST16 Remote outputs I O ...

Page 52: ...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 52 59 15 Appendix II Connecting the IST16 transfer lines The power cable depends on the voltage of your IST16 ...

Page 53: ...orage interface Agilent 7890A GC 5975C MSD Pre treatment None Sample preparation See respective figures 16 2 Instrument parameters 16 2 1 TGA Reactive Purge gas 30 mL min N2 grade 5 0 Protective gas 20 mL min N2 grade 5 0 Method 500 C to 1000 C at 20 C min Pan Alumina 70 µL Sample mass around 10 mg 16 2 2 IST16 Transfer lines and valves temperature 250 C 16 2 3 GC Inlet port temperature 280 C Spli...

Page 54: ...ss is shown in black and the DTG curve is shown in red The DTG curve corresponds to the first derivative of a TGA curve In a DTG curve a TGA step is displayed as a peak This makes it easier to determine the limits for the TGA step evaluation The sample exhibits one decomposition step of about 44 in the studied temperature range under nitrogen atmosphere It starts at about 600 C and has its maximum...

Page 55: ...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 Based on figure 1 gas storage temperatures were set according to table 2 below Table 2 Storage loop numbers at selected temperatures After collection of the loop 11 the samples stored in the 11 loops had...

Page 56: ... and the GC acquisition method is only 7 5 minutes As it can be observed in figure 3 CO2 is still detected even the decomposition process is finished This can be resolved by either using a lower sample mass such as e g 5 mg a bigger reactive gas flow such as e g 50 or 70 mL min or a bigger split ratio such as e g 10 1 or 20 1 The same test should be repeated using other columns delivered with the ...

Page 57: ...l configuration because it is equipped only with a high temperature transfer valve see diagram with two positions the loading position left and the injection position right The installation and configuration of the software are similar to the IST16 Only the Gas sampling valve default and Multi injection modes are available For maintenance operations the recommendations are the same as for the IST1...

Page 58: ...The injection parameters are available under the Method Injection menu The following window is displayed 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 ...

Page 59: ...n ensured by applying the following standards 1 Directive 2014 35 EU Low voltage NF EN 61010 1 A1 2019 Safety requirements for electrical equipment for measurement control and laboratory use Part 1 General requirements NF EN 61010 2 081 2015 Safety requirements for electrical equipment for measurement control and laboratory use Part 2 081 Particular requirements for automatic and semi automatic la...

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