2 Use of the User Manual
Contents
1. SN in sn 35 7 2 PERIODIC MAINTENANCE one alt 35 7 3 NEEDLE REPLACEMENT ice 37 8 SPARES AND CONSUMABLES 39 9 TROUBLESHOOTING DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 3 of 45 1 About Da Vinci Laboratory Solutions As a versatile partner for analytical applications and authorized distributor of world leading instrument manufacturers Da Vinci Laboratory Solutions DVLS is able to provide an expert advice and offers an extensive range of chromatographic systems software services and supplies For information visit www davinci ls com or contact us at Da Vinci Laboratory Solutions Cairostraat 10 3047 BC Rotterdam The Netherlands Postbus 12103 3004 GC Rotterdam The Netherlands T 31 0 10 258 1870 F 31 0 10 258 1879 solutions davinci ls com Note In no event will Da Vinci Laboratory Solutions be liable for any loss or damage including incidental indirect special or consequential damages arising from the use of DVLS Liquefied Gas Injector Note Information descriptions and specifications in this publication are subject to change without notice DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 4 o2. 16 5 1 PR PARINGTHE GC ct line ot 16 5 2 PREPARING THE PRESSURE STATION SR Ne etat tnt tent Ted 16 5 3 PREPARING THE CONTROLLER 20 5 4 SIS et nine 23 6 APPLICATION 1 RESIDUE IN anne 27 6 1 nt D 27 6 2 LElCONTROLLERSETIINGSE SE E 27 6 3 G CONFIGURATION A EE EE 28 6 4 COLUMN INSTALLATION PROCEDURE 30 6 5 CHROMATOGR AW Cana 31 6 6 INTEGRA TION 31 6 7 CALIBRATION a dos nie 32 6 8 CALCULATION OF UNKNOWN 33 DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 2 of 45 6 9 CALCULATION OF THE RECOVERY OF THE MINERAL OIL FRACTION ccccceccceccecceccecccceccceucecceaceas 34 7 USER MAINTENANCE tune recevant sen 35 7 1
3. between brackets are the values entered in the Setup screens Selecting the Rinse N button will immediate start the rinsing process N times according to the setup details entered DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 20 of 45 Setup 1 amp 2 screens Setup 1 OVE High Pressure Injector Rinse pulse GDI Rinse cycles Rinse interval Inject pulse GDI Com Co Co jm Co jm Setup 2 OVE High Pressure Injector Vent open Los Inject pre delay o 5 Los Inject post delay Help Screen Serialnumber FW version GUI version Refer to User Manual DVLS LGI 2 User Manual Copyright 2014 v5 0 Comments In the Setup 1 menu rinse settings and inject pulse time are configured In the Setup 2 menu the vent time and injection pre and post delay are entered The pulse cycle interval etc figures can be changed directly using touch screen functionality Comments Selecting the Help button will show the serial number and the firmware and GUI version of the Controller It also refers to the manual in the current version of the software no online help is available Page 21 of 45 Diagnose screen Comments Diagnostics DVE High Pressure Injector Diagnostics are available by selecting the Diag button on the Main screen The functionality of the various buttons is described in the following table Ex Needle Will bring the GDI in a position abo
4. ASTM D1265 Practice for Sampling Liquefied Petroleum LP Gases LPG Material Safety Data Sheet usually to be obtained from the LPG supplier 3 3 Training and Usage The LGI should be used by trained users only Perform cleaning and maintenance as described in the chapter on Maintenance Refer to qualified service personnel for servicing Use of the instrument in a manner not specified by the manufacturer or use for another application than described in this manual may result in a safety hazard If parts are substituted or unauthorized modifications are performed this may result in a safety hazard 3 4 Injector The Injector has moving parts and a needle These instructions must be followed Wear safety glasses while operating the LGI Turn off the power before removing the Injector tower or during maintenance The needle is sharp Never open the Cover when the Injector is in operation When the instrument is unattended never leave the needle in the Ex Needle position Make sure the needle is in the needle waste vessel by Initialization via the Controller Initialization is performed by pressing the Init button in the Diagnose screen please refer to the operational chapter for details on the Controller The Injector can be stopped at any time by pressing the red button on the Controller All electronic wires and connections are shielded by covers Only trained and authorized personnel are allowed to open the covers DVLS LG
5. Typical Chromatographic parameters DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 29 of 45 6 4 Column installation procedure 1 Connect all columns according to Figure 25 and 26 In general it is important to make a clean straight cut on the column Most GC suppliers have ceramic cleaving wedges or other specific capillary column cutters available After installing the column nut and ferrule on the column cut the column and inspect the top of the column using a magnifier Secondary verify that LGI needle smoothly fits in the column without any obstruction straighten the column if required Install the column in the GC inlet according to the manufacturer s manual If the Agilent Cool on Column inlet is used insert the column until the spring is completely compressed Slightly tighten the column nut Mark the column and pull down the column 6 to 7 mm Tighten the column nut further More information on the column connection can be found in the Troubleshooting chapter of the User Manual DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 30 of 45 For a leak tight connection of the Sulfinert tubing to the 1 16 Swagelok union part no SS 100 6 replace one of the stainless steel ferrules of the union by a 0 53 mm SilTite ferrule part no DVE 029797 For tightening use the procedure described in paragraph 5 1 for connection of the bleed capillary to the vent valve 2 Allow at least 30 minutes of
6. Working with pressurized and highly extremely flammable liquids holds certain risks Read and use the following safety instructions Potential dangerous voltages can exist on All LGI and GC electronic boards and electrical connections e All LGI and GC AC power supplies and electrical connections All electronic boards and connections are shielded by covers Unless specifically instructed to never remove the cover Contact your Da Vinci service representative for assistance and instructions Note It is not allowed to make changes to the instruments or setup without consulting Da Vinci Laboratory Solutions B V Note All information in this manual applies to set up of the instrument for analysis of LPG Warning Use of the instrument in a manner not specified by the manufacturer or use for another application than described in this manual may result in a safety hazard If parts are substituted or unauthorized modifications are performed this may result in a safety hazard Warning Using the LGI with other sample matrices than LPG e g Butadiene or Condensate will require certain modifications to the instrument for safe operation Note Always wear safety glasses during operation of the LGI DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 6 of 45 3 2 LPG LPG is a flammable mixture all safety precautions must be taken If the LGI is used for LPG injection please refer to the following international guidelines
7. make sure the needle valve On Off switch is in the On position Allow approximately 5 minutes rinsing with Nitrogen Rinse the needle with Nitrogen by selecting the Rinse N button Turn the Pressure switch Off Turn the Bypass switch On Wait until the pressure gauge reads 0 bar psi Turn the Bypass switch Off Verify that the pressure gauge remains 0 bar psi wait if necessary 10 Verify that the rotameter flow reads 0 5 4 3 Sample analysis On the Pressure Station 1 After the pressure and the rotameter flow have dropped to 0 remove the Flexible hose from the Sample Input Quick connector 2 Install the sample cylinder on the Sample Input quick connector 3 Install the earth clamp on the cylinder not on the cylinder valves Quick connectors or eventual adapter pieces but on the cylinder itself DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 23 of 45 Cylinder with earth clamp O eS Sf 12 15 16 17 Install the earth clamp not on the cylinder valves quick connect or eventual adapter pieces but ON THE CYLINDER ITSELF Connect the Flexible hose to the top of the cylinder Verify that the Depressurize valve is closed on top of the Pressure Station Close the flow Controller needle valve vaporizer completely Turn the Pressure switch On Open the top valve of the cylinder Open the bottom valve of the cylinder Now the Pressure Stat
8. back of the Pressure Station Warning Always connect the earth clamp to the sample cylinder to prevent build up of static electricity DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 8 of 45 3 6 Controller e Power sockets must be fused with min 16A and all power sockets must have protective earth e Never replace the power cord with another type e The Injector can be stopped at any time by using the red button on the Controller e All electronic boards and wires are shielded by covers Only trained and authorized personnel is allowed to open the covers 3 7 Gas Chromatograph Please refer to the GC manufacturer s manual 3 8 Symbols Warnings in the manual or on the instrument must be observed during all phases of operation service and repair of this instrument Failure to comply with these precautions violates safety standards of design and the intended use of the instrument Da Vinci holds no liability for the customer s failure to comply with these standards See accompanying instructions for more information Crush hazard keep hands clear Hot surface Earth ground terminal DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 9 of 45 4 Introduction 4 1 Sample introduction Gasoline Direct Injection GDI The liquefied sample introduction principle used in the LGI is based on the Gasoline Direct Injector GDI technique commonly used in car engines The GDI is filled with sample un
9. flushing of the columns with carrier gas before oven heat is applied 3 Condition the columns according to the manufacturer s instructions 6 5 Chromatogram The chromatography should look like the chromatogram shown below Verify whether the solvent peak is separated from the C10 the first component of the total of the residue 50 ppm mineral oil o z r r r i 0 5 10 15 20 25 Example chromatogram of 50 ppm residue in LPG 6 6 Integration Integrate the total area between C10 and C40 Refer to the data acquisition software manufacturer s manual for details on total area integration DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 31 of 45 6 7 Calibration e N Alkane standard Determine the retention time of C10 and C40 by analyzing an LPG standard spiked with C10 and C40 or by analyzing a dedicated Alkane standard mixed with pentane C10 is the first component to be determined as residue e LPG calibration standard Analyze an LPG standard with a matrix close to the matrix of the unknown samples The recommended concentration of the mineral oil is 50 ppm The response factor can be calculated with the following formula Rf area where Rf Response factor Conc Concentration of mineral oil in LPG Area Summed area of C10 C40 after subtraction of a blank e Pentane validation sample A mixture of mineral oil in pentane is a good validation standard Seve
10. operation if required Details on the various Controller commands are described in the operational chapter of this manual Typical Controller settings DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 14 of 45 Controller on Agilent GC DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 15 of 45 5 Operating instructions Note In case of an emergency or in case pressure flow or temperature readings are different from normal operation first make sure the sample cylinder is closed stop the LGI immediately push the red stop at the front panel of the Controller Note Always wear safety glasses 5 1 Preparing the GC Using your GC data acquisition system download the required GC set points If required start one or more blank analysis by starting the GC directly without the LGI in order to clean the GC columns prior to injection The signal is considered stable when the start and end signal value pA of two consecutive blank runs are within 5 deviation An unstable baseline can be caused by a leak detector gases or by high boiling point components not completely eluted from the columns In general the signal height at the end of a calibration validation or routine sample run should be similar to signal from a blank run Refer to the Application chapter or the GC manufacturer s manual for specific GC details 5 2 Preparing the Pressure Station e For PTS3 Pressure Station type 3 with vaporizer switch o
11. the system via the Waste exit on the back of the Pressure Station connected to a suitable waste system see the Installation Manual for suggestions e In PTS2 the needle valve is the part until where the sample is pressurized After the needle valve pressure becomes atmospheric and the LPG liquid vapors In PTS3 the vaporizer is the part until where the sample is pressurized The LPG liquid is vaporized by the heated vaporizer e The needle valve vaporizer can be bypassed by opening the Bypass Switch to quickly release leftover sample e sample flow is controlled via rotameter which also allows for visual inspection of the sample flow e The Pressure Station has a safety pressure relieve valve which opens when the pressure in the system exceeds the set maximum pressure for example 35 bar 507 DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 13 of 45 psi to make sure the pressure does not exceed the maximum pressure of the rotameter Details on the function and operation of the Pressure Station switches connections needle valve PTS2 and vaporizer PTS3 are described in the operational chapter of this manual 4 4 Controller The Controller unit contains the electronics to control the GDI and to start the GC In some applications a GC valve is programmed as well The Controller is operated via a touch screen except for the start and stop buttons The stop button on the Controller immediately stops the Injector
12. G These residues can lead to troublesome deposits that will accumulate and corrode or plug the LPG fuel filter the low pressure regulators the fuel mixer or the control solenoids LPG can become contaminated by oily residues during its production or transport Transport contamination can come from shared pipelines valves and trucks used for the distribution of other products Production sources such as the desulfurization process may contribute sulphur absorbent oil to the LPG stream 6 2 LGI Controller settings The following table shows the typical Controller settings for the Residue in LPG analysis under the conditions described in Chapter 6 3 w Inject pulse GDI Inject post delay DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 27 of 45 6 3 GC configuration For residue analysis the GC is equipped with an On Column Inlet and solvent vent The sample is injected on a 5 m coated stainless steel capillary This retention gap is connected to a 3 non polar retaining column which is routed to the solvent vent for flushing the LPG light ends Subsequently the vent is closed and the flow is switched to the non polar analytical column for residue separation by boiling point DVE 01716 Solvent vent valve Stainless Steel Tubing SS 100 6 Cool on column inlet DVE 095196 ait Swagelok Detector Sulfinert tubing SS union 20 cm 0 53 mm ID ute splitter a mK DVE 001818 MN LGI SilFlo
13. I 2 User Manual Copyright 2014 v5 0 Page 7 of 45 3 5 Pressure Station e Wear safety glasses while operating the Pressure Station e Never leave the LGI instrument unattended while the sample cylinder is installed and under pressure e Ensure the pressure rating for the sample cylinder cylinder valves and quick connector of your choice the choice of quick connector usually depends on the company standard will withstand the factory set 35 bar 507 psi pressure at which the pressure relief valve is installed e Never use a charging pressure higher than 25 bar 363 psi unless the Pressure Station is specifically set up for a higher maximum pressure e Read the pressure on the Pressure Station gauge when the cylinder with liquid gas is opened and make sure this pressure is maintained after closing the flow A drop in pressure may be an indication of a leak in the flow system e Open the sample cylinder only to supply high pressure Nitrogen to purge and to inject the sample Close the cylinder immediately after purging and injection e Refer to the manufacturer s manual for specific details on the quick connectors e Do use the Pressure Station for anything outside the scope of the validated application Note Never try to disconnect quick connectors if the system is still under pressure The Nitrogen pressure must be released first Note The Pressure Station must be connected to protective earth using the protective earth on the
14. User Manual DVLS Liquefied Gas Injector Series 2 Date 8 26 2014 v5 0 Table of Contents 1 ABOUT DA VINCI LABORATORY SOLUTIONS 4 2 USE OF THE USER MANUAL cecccccccccccccccccccccccccccccncccccccsacssccccsnsensccsecsucenseuscenuentevens 5 3 SAFETY AND REGULATORY INFORMATION 6 3 1 GENERALE a dane a a 6 3 2 A EG da naa eae wie ee Cala 7 3 3 RAINING AND USAGES ne tn nes AA a A 7 3 4 INE GTO Ria A Se Need 7 3 5 PRESSURE du en lle a tetes ont terne Aid 8 3 6 CONTROLLER a aa ee de Uni 9 3 7 GAS CHROMATOGRA PE eee RE LR 9 3 8 SYMBOLS west nn le EE le ide eue 9 AY choice ret rect a dae nan A ante 10 4 1 SAMPLE INTRODUCTION VIA GASOLINE DIRECT INJECTION GDI iii 10 4 2 INJECTOR rerainan RG un 11 4 3 PRESSURE ON de T 12 4 4 CONTROLLER EE E ee 14 5 OPERATING 5
15. cause Carrier gas impurities contaminated column leaks Suggested solution Inspect the carrier gas purity install filters if required Inspect the column connection in the GC oven for leaks Carry out a pressure test if needed Condition or replace the column s Comments The following chromatograms show 50 ppm oil in LPG results The first run is resulting in excessive column bleed at higher oven temperatures The second chromatogram was obtained using a well conditioned column set and leak tested instrument 180 160 140 120 100 Detector signal 60 at oven temperature e of 315 C 60 40 20 0 I r r r 0 5 10 15 20 25 120 100 80 60 40 Detector signal 15 at an oven temperature of 315 C Agilent 7890 GC 20 0 0 5 10 15 20 i 25 min DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 43 of 45 Symptom Unexpected hydrocarbon peaks in the C10 C20 area Possible cause Production oil present in the GDI valve Suggested solution Execute GDI cleaning procedure using pentane Comments Although the GDI valves are cleaned before shipment GDI production oil may be visible in a blank pentane run usually in the first runs after a new GDI valve is installed To clean the GDI valve after installation pressurize the Injector with pentane and rinse the LGI 99 times with a pulse time of 999ms Then re analyze the n pentane sample to verify that the issue is resol
16. der pressure After activation of the solenoid the sample is injected through a needle either to waste to purge or to a GC column for analysis b Injection Injection Y Injection cycle of the GDI a The GDI is filled with the liquid sample under pressure b After activation of the solenoid the sample is pushed through the needle c After injection the position returns to start position A complete LGI system consists of e The Injector which is the injection device that holds the GDI e The Pressure Station e The Controller DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 10 of 45 The combination of the Injector Pressure Station and Controller is hereafter referred to as the Liquefied Gas Injector LGI Complete LGI application Residue in LPG analysis via GC is a proved application where the LGI is used as described in subsequent chapters The required GC configuration column inlet detector etc used may vary depending on the analysis needed 4 2 Injector The Injector consists of the GDI mounted in a housing a stepper motor for movement of the GDO and a waste vessel e Injector is placed on top of a GC using a specific mounting post e stepper motor moves the GDI into position either for injection or purge to waste A needle is attached to the GDI allowing injection into a GC e sample flows from the Pressure Station into the GDI e The function of the wa
17. e into the surrounding area If the previous sample is not completely removed from the Pressure Station and a new sample cylinder is pressurized with Nitrogen Pressure while the Depressurize valve is open then the previous sample is forced via the Flexible hose into the sample cylinder Bypass Switch The needle valve vaporizer can be bypassed by opening the Bypass Switch to quickly release leftover sample DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 19 of 45 5 3 Preparing the Controller Prepare the Controller as follows e Put the power plug into the socket e Switch on the Controller by pressing the On Off switch on the back e Familiarize with the Controller screens as described on the next pages e Load the typical Controller settings for your application Startup screen Comments OVE High Pressure Injector By pressing the Accept button the user is WARNING asked to confirm to study the manual before Before operation read the User Manual first starting to operate the LGI system Injector will initialize after acceptance Vinci Europe loborotory solutions Main screen Comments Main OVE High Pressure Injector This is the default Controller screen which will Injector NOT READY 0 show after initialization It shows the actual GC NOT READY bli CLOSED OFF 0 status of the Injector GC and vent valve re delay Post delay controlled by the LGI if applicable The values
18. f 45 2 Use of the User Manual This guide is intended for users of the Da Vinci Liquefied Gas Injector LGI It describes the routine operational procedures of the LGI The information in this guide not only applies to operation of the LGI but contains information on the use of the LGI in certain applications as well for instance residue analysis in LPG Additionally using the LGI with other sample matrices not described in this manual e g Butadiene or Condensate will require certain modifications to the instrument Details on the use of the Gas Chromatograph GC and data acquisition software is not described in this document but available from the manufacturer s manuals Note There are several important safety notices to keep in mind when using the LGI as described in Chapter 3 Note Make sure you have read and understood all safety information before starting to use the instruments Note Da Vinci does not hold liability for any personal damage that is caused by the use of the LGI For extra information which may not be found in this guide we refer to the Da Vinci website or your local Da Vinci representative DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 5 of 45 3 Safety and regulatory information 3 1 General These instruments are designed to pressurize extremely flammable liquefied gasses and highly flammable volatile liquids and to inject an amount of this sample under pressure an analyzer
19. for 1 16 nut Pe 10pcs DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 39 of 45 LGI consumables Part number Description Recommended quantity DVE 093725 Injector needles 6pcs requires 6x DK 800183 DK 800183 Teflon o ring special for LGI 2x6 DVE 095196 Sulfinert Tubing 17ft x 0 53mm ID DVE 090002 Solvent valve bleed capillary 10m DVE 094424 12744 SILFLOW FINGERTITE FERRULES 0 75MM ID PK DVE 094425 123743 SILFLOW FINGERTITE FERRULES 0 55MM ID PK DVE 029795 Siltite ferrules 0 25 10pcs DVE 029797 Siltite ferrules 0 53 10pcs DVE 095191 RIVM mineral oil 1 ampoule 3 DVE 044764 Manual syringe 50ul LPG calibration gas On request DP LG XX TC Sample cylinder to prepare liquid calibration 1 10 samples with QTM4 quick connectors for use with Pressure Station with QTM4 quick connectors Available with other connectors on request DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 40 of 45 DK 095191 Residue in LPG analytical column MXT 5 30m x 0 32mm ID 9 Troubleshooting Symptom LPG Solvent peak tailing Possible cause Bad column cut column height in the inlet Suggested solution Re cut and inspect the column Adjust the column height Comments Although the LPG or other solvent is mostly vented a part of it will remain in the system The peak shape is depending on the column fit but also on the position of the needle in the column If the needle depth is too far LPG expansion may become difficu
20. he sample contains high concentrations of heavier hydrocarbons amines or other strong absorbing components it is recommended to test for carry over in between analyses using pentane cylinders In such cases these steps should be followed 1 Clean and prepare a sample cylinder with pentane 2 Analyze the pentane according to the procedure under 5 4 3 DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 25 of 45 Note Carry out an additional rinsing sequence prior to injection Rinse N 3 If memory of components of interest is visible in the chromatogram repeat steps 1 2 until the system 15 clean Note In case the LGI system is not only used for injection of liquefied gasses but also for injection of fluids that are in the liquid phase at atmospheric pressure beside vapor also liquid sample will elute from the Waste exit As a consequence care should be taken that the waste lines Pressure Station waste and Injector waste remove the liquid efficiently and quickly so that no accumulation of liquid occurs If it is expected that accumulation of liquid will occur the customer should make a facility to safely remove the liquid For suggestions of how to connect the waste exit to different waste facilities refer to the LGI Installation Manual DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 26 of 45 6 Application 1 Residue in LPG 6 1 Background Control over the residue content is essential in end use applications of automotive LP
21. ion will fill with gas and subsequently liquid which is observed at the rotameter Slowly open the flow Controller needle valve vaporizer to establish a flow of 5 10 ml min Purge the system for 1 2 minutes During the purging time select the Rinse N button Note The accuracy of the actual flow reading is depending on the type of Controller used On some models it can be difficult to establish a stable flow of 5 10 ml min Use a lower flow set point but longer time in this case Close the flow Controller completely After the rotameter ball has dropped to 0 select the Rinse button 13 Repeat 2 times with intervals of 10 seconds After the last rinse cycle wait for 10 seconds and press the Start button on the Controller After injection close the bottom valve of the cylinder Close the top valve of the cylinder Turn the Pressure switch Off DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 24 of 45 18 Release the Nitrogen pressure opening the Depressurize valve on top of the Pressure Station Wait for 5 seconds then close the Depressurize valve again Note Before opening the Depressurize valve make sure the valves of the sample cylinder and the Pressure switch are closed Note Always make sure that the Depressurize valve is closed after the Depressurization is finished Note If the Depressurize valve is left open and Nitrogen Pressure is applied for removing the sample waste f
22. lies high pressure Nitrogen to the sample cylinder Connection to the Sample cylinder with quick connect 2 Can be directly connected to the Sample Input Quick Connect for rinsing Pressure Station and injection needle with Nitrogen Vaporizer PTS3 only Sample flow control Heats and vaporizes the sample The LPG sample is pressurized and in liquid phase until the vaporizer After the vaporizer the sample becomes atmospheric and 15 directed to waste Needle valve amp Sample flow control Needle valve On The LPG sample is pressurized and in liquid phase until the Off Switch PTS2 only vaporizer After the needle valve where pressure becomes atmospheric the LPG liquid vapors and is directed to waste Flow meter Rotameter type flow meter for flow control Allows visual inspection of the sample flow Depressurize valve Opening this valve releases the Nitrogen Pressure from the Flexible hose Note Before opening the Depressurize valve make sure the valves of the sample cylinder and the Pressure switch are closed Note Always make sure that the Depressurize valve is closed after the Depressurization is finished Note If the Depressurize valve is left open and Nitrogen Pressure is applied for removing the sample waste from the Pressure Station then part of the sample waste will be forced via the Depressurize valve into the Flexible hose This sample will not be disposed via the waste exit but is blown out via the Flexible hos
23. lt which could result in peak tailing LPG Solvent peak tailing has a negative impact on integration and the repeatability of the area The following example shows the relation between needle depth and LPG tailing on the Agilent Cool on Column inlet The blue chromatogram shows the result of an analysis with the column all the way up in the injection port The other chromatograms correspond to tests with a lowered column position 700 Main LPG peak Start of Oil fraction 600 column inserted to far DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 41 of 45 Symptom Bad repeatability between successive analyses of the same sample Possible cause Oil residue between GDI valve and waste vessel Suggested solution Rinse the needle between successive analyses Follow the Standard Operating Procedure for LGl Comments Oil residue may accumulate in the needle between analyses as a result of slight leakage in the GDI If the GDI is not rinsed between analyses this residue will be injected with the next sample on the column If the needle is rinsed before the next injection the needle residue will be removed 50 ppm oil in LPG Run 2 no needle rinses Run 1 amp 3 needle rinses 9x999 ms g p i 0 2 5 5 7 5 10 12 5 15 17 5 20 DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 42 of 45 Symptom High column bleed signal Possible
24. n the vaporizer by inserting the Pressure Station power cord into the socket e Allow the vaporizer to heat up for several hours the vaporizer can be left on overnight and is usually only turned off when the system is not used for a longer period of time e Familiarize with the Pressure Station parts as described on the next pages DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 16 of 45 Needle valve On Off Switch Pressure Bypass Needle valve Complete front view of PTS3 left in PTS3 flow is controlled via a vaporizer Front view of the flow controlling part of PTS2 right in PTS2 flow is controlled via a needle valve DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 17 of 45 Pressure a 25 bar N2 Depressurize N2 pressure Depressurize t Pressure Relief Pressure Relief sample Input to Waste Quick Connect Pressure __ Gauge i Filter Rotameter Rotameter a Bypass __ Switch Bypass Needle valve lt Switch Vaporizer 98 Off Switch Schematic overview of 53 left in PTS3 flow is controlled via a vaporizer Schematic overview of the flow controlling part of PTS2 right in PTS2 flow is controlled via a needle valve other parts are the same as for PTS3 DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 18 of 45 Sample Input Quick Connection for sample cylinder Connect Flexible hose 1 Supp
25. or 2 Remove the needle and make sure both Teflon O rings are removed from the GDI housing Needle configuration 3 Assemble the Teflon O rings on the new needle and finger tighten the needle nut on the house of the GDI Needle and finger tight needle nut connection DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 37 of 45 4 Close the transparent Cover of the Injector housing 5 Press Init in the Diagnose screen of the Controller This will move the needle into the needle waste Note The LGI injection is time based The amount of sample injected depends on the length of the inject pulse the pressure of the sample and the restriction in the system If the needle is exchanged the restriction may change slightly because of minimal differences in needle ID Therefore recalibration is required DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 38 of 45 8 Spares and Consumables LGI spare parts Part number Description Recommended quantity DM LG IN GK GDI injector for LGI version 2 12 DVE 095192 Solvent vent valve 3 2 24V DVE 095193 Connector for solvent vent valve DVE 095194 Adapter 1 16 M5 for solvent vent valve 1 1 DVE 095195 Sealing washer M5 for solvent vent valve DVE 001818 Liquefied Gas Injector splitter union complete incl ferrules SS 100 6 Stainless steel 1 16 union 1 DVE 017176 Stainless steel 1 16 tubing 1 0mm ID 10m DVE 007002 Stainless steel front back ferrule set
26. ral concentrations can be prepared It is recommended to fill a clean sample cylinder with the standard and inject under equal conditions as to regular LPG samples Note In case the LGI system is not only used for injection of liquefied gasses but also for injection of fluids that are in the liquid phase at atmospheric pressure beside vapor also liquid sample will elute from the Waste exit As a consequence care should be taken that the waste lines Pressure Station waste and Injector waste remove the liquid efficiently and quickly so that no accumulation of liquid occurs If it is expected that accumulation of liquid will occur the customer should make a facility to safely remove the liquid For suggestions of how to connect the waste exit to different waste facilities refer to the LGI Installation Manual DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 32 of 45 6 8 Calculation of unknown samples Calculate the concentration of residue in the validation standard or the unknown sample as follows Note If the matrix of the calibration sample e g pentane is different from the unknown sample a density correction should be applied according to ASTM D 7756 DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 33 of 45 Concentration area Rf where Concentration Mineral oil content in ppm weight Area Summed area of the area of C10 C40 after subtraction of the blank Rf Concentration of the mineral oil in the calibra
27. rom the Pressure Station then part of the sample waste will be forced via the Depressurize valve into the Flexible hose This sample will not be disposed via the waste exit but is blown out via the Flexible hose into the surrounding area Note If the previous sample is not completely removed from the Pressure Station and a new sample cylinder is pressurized with Nitrogen Pressure while the Depressurize valve is open then the previous sample is forced via the Flexible hose into the sample cylinder 19 Release the sample pressure by turning the Bypass valve On When the pressure has dropped to 0 turn the bypass valve Off and open the flow controller needle valve vaporizer In case of PST2 make sure the Needle valve On Off switch is in the On position 20 Wait until the pressure and rotameter flow have completely dropped to zero This may take a few minutes depending on the type of sample injected 21 Disconnect the Flexible hose remove the earth clamp and remove the cylinder 22 Close the flow controller needle valve vaporizer In case of PST2 make sure the needle valve On Off switch is in the Off position 5 4 4 Standby preparation 1 Follow the Cleaning and depressurization procedure described in paragraph 5 4 2 2 After depressurization leave the Flexible hose connected to the Sample Input Quick connector to avoid dust particles will enter this Quick Connector 5 4 5 Additional pentane rinsing procedure If t
28. ste vessel is to collect the sample that comes out of the needle during needle rinsing The sample is disposed via tubing attached to the DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 11 of 45 waste vessel The sample either liquid vapour coming out of this tubing should be disposed appropriately e When the Injector is initialised via the Controller the needle moves initially to the waste vessel e After activation of the GDI the sample is pushed in discrete bursts through the needle initially to waste but in a later stage to the GC inlet Injector 4 3 Pressure Station For a representative analysis the sample must remain in the liquid phase during the injection process this is especially required for LPG or other chemicals that are gaseous at ambient pressures To keep the sample under pressure a device is used that adds high pressure Nitrogen to the sample cylinder and controls the outlet pressure and flow This device is referred to as the Pressure Station Two types of Pressure Stations are available PTS2 and PTS3 In PTS2 the flow is controlled via a needle valve In PTS3 the flow is controlled via a vaporizer DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 12 of 45 Pressure Station type 52 with sample cylinder e When the sample cylinder is opened the liquid sample flows through the Pressure Station and subsequently to the GDI and back to the Pressure Station e Waste sample leaves
29. t DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 35 of 45 Daily Weekly Monthly Annually Verify the pressure level of the supply gases to the instrument Replace with new cylinders if required Run control sample and apply statistical quality control procedures The exact frequency of the control sample depends on internal guidelines and on the average number of routine samples Replace the septum of the GC inlet Perform a leak check on the column connections inside the GC oven Perform a leak check of the Pressure Station and Injector as described in the Installation Manual Verify there is no abnormal pressure drop monitor the pressure on the pressure gauge no 3 Vacuum any dust found inside the housing of the Injector on and around the GDI Clean the exterior of the instrument using a damp not wet lint free cloth Do not use chemical cleaners Replace the Sulfinert retention gap Replace the Pressure Station particle filter Replace more often than once a year in case the samples measured on the system frequently contains particles Replace the LGI needle DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 36 of 45 7 3 Needle replacement 1 Press Ex Needle in the Diagnose screen of the Controller This will move the needle upwards allowing to remove the needle Note Never put the GDI in the Ex Needle position when sample under pressure is present in the Pressure Station and Inject
30. tion gas divided by the area 6 9 Calculation of the recovery of the mineral oil fraction To maintain a quality control chart for this application it is recommended to monitor the recovery of the validation standard over time The optimum recovery is 100 Mineral Oil content in LPG in ppm weight theoreticaWDPM measured 100 where ppm theoretical the recorded weight of mineral oil ppm measured the result of the chromatographic analysis DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 34 of 45 7 User Maintenance 7 1 General Note Before performing any maintenance first check the instrument s safety guidelines and make sure the system is purged and in standby position 7 2 Periodic maintenance The following table describes the recommended actions required to ensure good performance of the LGI application For GC routine maintenance please refer to the GC manufacturer s manuals To prevent carry over from previous samples it is recommended to purge the instrument with Nitrogen when the system is in standby Note Before performing maintenance items marked with switch off the Controller and remove the power plug from the socket Note Before performing maintenance items marked with remove the power plug of the Pressure Station from the socket applies only to PST3 PST2 does not have any electrical power connections switch off the Controller and remove the power plug of the Controller from the socke
31. ve the waste vessel to replace the needle Note Never put the GDI in the Ex Needle position when sample under pressure is present in the Pressure Station and Injector Note Always return the GDI to the Init position afterwards Init Will bring the GDI to its initial and default position needle in waste vessel Ex GDI Will bring the GDI in a position in which the connections on the Y piece can be easily accessed E g to leach check these connections and to enable exchanging the GDI GDI Will open the GDI valve once according to the Inject pulse GDI setup 1 configuration Rinse 1 Will open the GDI valve once according to the Rinse pulse GDI setup 1 configuration Will manually switch the vent valve if present Beep Switches on and of the touch sound of the Controller buttons GC Start Starts the GC program without starting the Injector DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 22 of 45 5 4 Sample analysis 5 4 1 Configuration if required Using the Controller setup 1 menu 1 Set the Rinse pulse to 400 ms 2 Set the Rinse cycle to 10 3 Set the Rinse interval to 2 5 5 4 2 Cleaning and depressurization prior to injection On the Pressure Station 1 Connect the Flexible hose to the Sample Input Quick connector and turn the Pressure switch On if not already 2 Establish a rotameter flow of approx 20 40 ml min by turning the needle valve PST2 or vaporizer PST3 In case of PST2
32. ved pA 60 50 30 GDI production oil 20 10 DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 44 of 45 Symptom Excessive signal increase over the complete range of the chromatogram Possible cause A particle inside the GDI valve Suggested solution Rinse the GID 99 times with a Rinse time of 20ms Comments A particle inside the GDI valve may cause a continuous sample flow through the GDI and into the waste vessel and injection port If rinsing does not resolve the issue the GDI should be replaced To verify if the issue is resolved fill and pressurize the LGI with pentane Put the Injector in the lt Ex Needle gt position No visible sample should flow from the needle DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 45 of 45
33. w Wafer A Wy W AU Retention gap Retaining precolumn Analytical column DVE 095196 Sulfinert tubing 5 0 53 mm ID Schematic configuration of GC columns and connectors for residue analysis of LPG Tubing to vent nn pr a ce fi AL a Pre column o Analytical column i 0 32mm 0 32mm Retention gap 4 column N 0 53mm 0 32mm LGI SilFlow Wafer configuration DVLS LGI 2 User Manual Copyright 2014 v5 0 Page 28 of 45 Oven initial temp 35 Inlet initial temp 55 Oven initial time 3 min Inlet initial time 3 min Oven rate 25 C min Inlet rate 25 C min Oven final temp 325 C Inlet final temp 325 C Oven final time 20 min Inlet final time 20 min Detector Air flow 350 ml min Detector Hydorogen 35 ml min flow Detector make up flow 20 ml min Detector temp 325 C Pressure mode Constant flow Column Flow 6 ml min Septum purge flow 12 ml min Vent flow vent valve gt 40 ml min On Purge flow vent valve lt 1 ml min Off Retention gap Sulfinert coated SS capillary 5m x 0 53 mm ID Pre column 5 3 m x 0 32 mm ID x 1 00 um film thickness Analytical column MXT 5 27 m x 0 32 mm ID x 1 00 pm film thickness Split bracket union Sulfinert coated SS capillary 15 cm x 0 53 mm ID tubing Union vent valve Stainless steel OD 1 16 ID 1 0 mm tubing Residue in LPG application
Download Pdf Manuals
Related Search