System Description and Operations

TRACE LC-GC System Description and Operations

Release B March 2006

TRACE LC/GC System Description and Operations

List of Contents

TRACE LC-GC System.......................................................................................................................3 Introduction ................................................................................................................................................. 3

System Description..............................................................................................................................4 Pneumatics ................................................................................................................................................... 4

LC/GC System Composition....................................................................................................................................... 4 Injection, Back-flush and Optional Switching Valve.................................................................................................. 8 LC/GC Advanced Configuration................................................................................................................................ 8 Example of LC/GC Advanced Configuration............................................................................................................. 9

Pump Rear Panel....................................................................................................................................... 12 Transfer Line Connection......................................................................................................................... 13 Electrical Connections............................................................................................................................... 14 Conditions for a Correct Automatic Operation with the TriPlus and the GC .................................... 15 New Parameters Programmable Through the Phoenix 40 Keyboard and Display............................. 15

Control of the Pump..........................................................................................................................16 Controlling and Programming the Phoenix via Keyboard and Display............................................... 16 Time Programming of the Valves ............................................................................................................ 17 Programming the Transfer Valve on the GC.......................................................................................... 18 Programming the SVE Valve ................................................................................................................... 21 Control of the Carrier Purge Line of the Transfer Valve...................................................................... 22

Aux Purge ................................................................................................................................................................ 22 Start up....................................................................................................................................................... 22 Preparing the GC Oven Temperature..................................................................................................... 23 Controlling and Programming the Pump Through RS232 and Hyper Terminal ............................... 23

Pump Programming Through the Terminal....................................................................................24 Commands Syntax..................................................................................................................................... 24

Setting the Hyper Terminal to Correctly Control the Pump ..........................................................27

Control of the TriPlus Sampler ........................................................................................................31

Analytical Testing .............................................................................................................................32 Conditions .................................................................................................................................................. 32

TRACE GC Method: ................................................................................................................................................ 32 Pump Program......................................................................................................................................................... 33

Chromatograms......................................................................................................................................... 33 Appendix: TriPlus LC Installation...................................................................................................34

Sampler Supports Assembling ................................................................................................................. 34 Installation on the GC ............................................................................................................................... 34


TRACE LC-GC System Introduction The LC-GC Instrument is constituted of the following main components:

1. Phoenix 40 Pump, specialized for this application with up to 3 electrically actuated valves (Injection, Back-flush, Switching)

2. Trace GC Ultra equipped with a dedicated On-Column Injector (OC), on the left,

connected to an electrically actuated 6-port valve mounted on the top of the GC close to the OC Injector. The GC oven is equipped with a Solvent Vapor Exit valve (SVE) connected to the wide bore pre-column in the same way as it is done for the OC Large Volume Injection (Chapter 9 of the Trace GC Ultra Operating Manual). The GC is also equipped with the suitable DPFC for the carrier gas control for the OC injector and the pressurizing gas for the HPLC BKF solvent bottle.

3. Triplus LC Sampler is also available as optional component of the system. For the installation of the TriPlus LC sampler, please refer to Appendix: TriPlus LC Installation.

NOTE: The LC detector is not furnished in the package and must be selected according to the applications.

Figure 1: PH 40 Pump with 3 valves mounted and the TriPlus LC sampler.


System Description Pneumatics

Figure 2: PH 40 Pump with 2 syringe pumps installed

LC/GC System Composition Figures 3a, 3b, 3c, 4a-4b show the composition of the LC-GC system, including the UV Detector (Optional) that can be mounted in between the HPLC valve/column and the transfer valve on the GC. There are two possible injection valves:

Pump Controlled Injection valve This valve, schematically shown in figure 3b, is used when autosampler is not available.

Autosampler Injection Valve

This valve, schematically shown in figure 3c, is installed on the TriPlus LC sampler. Figures 4a and 4b schematically shown the LC-GC system where the Autosampler Injection Valve is considered. NOTE: A third additional pump can be added at any time to realize more complex configuration as shown in figure 7. Refer to paragraph . LC/GC Advanced Configuration


1 = GC Control Unit 2 = Syringe Pump 3 = TriPlus LC Sampler 4 = Sampler Injection Valve (6/10 ports) 5 = Pump Controlled Injection Valve 6 = Backflush Valve 7 = Optional 6-port Switching Valve 8 = Transfer Valve 9 = On-Column injector 10 = Solvent Vapor Exit Valve 11 = LC Detector (optional) 12 = GC Detector 13 = MS Detector Interface

Figure 3a: TRACE LC-GC System


LOAD INJECT

4

6

5

MobilePhase

Column

Sample Loop

Sample

Waste

4

6

5

16

54

3

2

MobilePhase

Column

Sample Loop

Sample

Waste

Default Position

12

3

45

6

Figure 3b: Pump Controlled Injection Valve Schematic Diagram

LOAD INJECT

4

6

5

16

54

3

2

MobilePhase

Column

Sample Loop

Sample

Waste

4

6

5

16

54

3

2

MobilePhase

Column

Sample Loop

Sample

Waste

Default Position

Figure 3c: Autosampler Injection Valve Schematic Diagram


4

6

5

4

6

5

16

54

3

2

MobilePhase fromPHOENIX 40

Sample Loop

Sample

110

3

2

4

56

7

8

9

20 uL

1 mLLoop

HPLCColumn

N2 From GC

1

2

3

4

5 6

Detector

Solvent

INJVLV

BKFVLV

TR VLV

Capillary Column

Carrier

Sample Load and elution

on HPLC column

Fraction transfer to

the capillary column

On-ColumnInjector

F.S. Transfer Lineto the GC

Restrictor

AUTOSAMPLER

Figure 4a: TRACE LC-GC Schematic Diagram (1)

4

6

5

4

6

5

16

54

3

2

MobilePhase fromPHOENIX 40

Sample Loop

Sample

110

3

2

4

56

7

8

9

20 uL

1 mLLoop

HPLCColumn

N2 From GC

1

2

3

4

5 6

Detector

On-Column injector

Solvent

INJVLV

BKFVLV

TR VLV

Capillary Column

Carrier

Column Backflush

Purge

Restrictor

AUTOSAMPLER

Figure 4b: TRACE LC-GC Schematic Diagram (2)


Injection, Back-flush and Optional Switching Valve Figure 5 shows the injection and back-flush valves.

Figure 5: Injection and Back/flush Valves

When TriPlus LC is used, the sample injection is performed through the sampler injection valve. For this

reason, the pump controlled injection valve, shown in Figures 3 and 5, must be disconnected and insulated from the pneumatic circuit. The sampler injection valve must be mounted and connected to the port 9 of the BKF valve as shown in Figure 4. An optional 6-port valve, shows in figure 6, can be installed as switching valve and controlled by the PH40 pump.

Figure 6: Optional 6-port Switching Valve

The Switching Valve can be used and programmed for more complex multi-dimensional set-up. LC/GC Advanced Configuration This is a case of the configuration of figure 7 that includes up to three pumps where two of them are used for the gradient while the third one is used for the BKF of the pre-column. To realize this configuration two “subsets” must be programmed and the second one must be linked to the first as described in the configuration of the pump.


Figure 7 shows the Injection, BKF and Switching valves using an HPLC pre-column and column with 2 or 3 pumps.

1. AS LC Injection Valve 2. Optional 6/port Valve 3. Pump Controlled Injection Valve 4. Transfer Valve

Figure 7: LC-GC Advanced Configuration

Example of LC/GC Advanced Configuration In the following example, a configuration for the analysis of mineral oil products in various food stuffs is considered. (Courtesy of M. Biedermann – Kantonales Labor Zürich). Figures 7a to 7d schematically shown the schematic and timing diagrams.

4

6

5

4

6

5

16

54

3

2

MobilePhase fromSyringe Pump A(or A+B)

Sample

1

2

3

4

5 6

Detector

On-Column injector

INJVLV

TR VLV

Pre-columnCarrier

Sample Loop

110

3

2

4

56

7

8

9

BKFVLV

RES. Column

4

6

5

16

5

43

2

SVVLV

MobilePhase fromSyringe Pump C

Column 1Column 2

1

Figure 7a: Schematic Diagram 1


4

6

5

4

6

5

16

54

3

2


Sample

1

2

3

4

5 6

Detector

On-Column injector

INJVLV

TR VLV

Pre-columnCarrier

Sample Loop

110

3

2

4

56

7

8

9

BKFVLV

4

6

5

16

5

43

2

SVVLV


Column 1Column 2

RES. Column

Column Backflush

2

Figure 7b: Schematic Diagram 2

4

6

5

4

6

5

16

54

3

2


Sample

1

2

3

4

5 6

Detector

On-Column injector

INJVLV

TR VLV

Pre-columnCarrier

Sample Loop

110

3

2

4

56

7

8

9

BKFVLV

RES. Column

4

6

5

16

5

43

2

SVVLV


Column 1Column 2

3

Figure 7c: Schematic Diagram 3


0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 153.5

TIME (min)

1 minINJ VLV

HPLCInj.

BKF VLV4 min

8 minSW VLV

PUMP A

PUMP C33 min

300 mL/min

300 mL/min

0 mL/min0 mL/min33 min

Figure 7d: Schematic Diagram 4

The detailed programming is reported in the table below:

Pump A, subset 1 Pump C, subset 3 Lines Lines Minute Flow µL/min A % Minute Flow µL/min C % 0.0 300 100 0.0 0 100 33.0 300 100 3.4 (*) See NOTE 0 100 --- --- --- 3.5 300 100 --- --- --- 8 300 100 --- --- --- 8.1 0 100 --- --- --- 33.0 0 100 Times Times Stand-by 0.2 min Stand-by 0.2 min Post run 0.5 min Post run 0.5 min Add target 0.0 MPa Add Target 0.0 MPa Injection valve (duration) 1.0 min --- --- Bach-flush time 4.0 min --- --- Back-flush duration 4.0 min --- --- Switching valve time 7.0 --- --- Switching valve duration 15.0 --- ---

Both Pumps GC-Transfer Modes Pressures Transfer Valve External Events Contr flow Minimum 0.0 MPa EV 6 0.0 min OFF Not quiet Maximum 12.0 MPa EV 5 3.5 min ON Full load Target 4.0 MPa EV 5 4.6 min OFF Cont run 0 --- EV 6 4.61 min ON

Solvent Vapor Exit Valve (*) NOTE

SVE Temperatyure 150 “C To keep constant the flow at 0.0 µL/min before a change tp 300 µL/min at 3.5 min, a time 3.4 min must be programmed.

SVE duration 4.8 min


Pump Rear Panel The rear panel of the pump is shown in figure 8. The rear panel includes the BKF solvent bottle (1), the solvent recovery bottle (2), a restrictor (3), the ports for the electrical connections. See Figure 9.

Figure 8: Pump Rear Panel The solvent bottle is pressurized with the carrier gas taken from the right manual carrier gas control of the TRACE GC. The relieve valve can discharge the pressure in case of obstruction or excessive pressure setting. Figure 9a shows the Pressure/Flow Control for the pressurization of the back-flush solvent bottle while the figure 9b shows the discharge bottle located on the TRACE GC rear panel.

a b

Figure 9: Pressure/Flow Control and Discharge Bottle


Transfer Line Connection Connect the transfer line between the transfer valve and the on column injector by using the proper fittings as schematically shown in figure 10.

Figure 10: Transfer Line Connection

Figure 11 shows the pre-column and column assembly with solvent vapor exit carried out into the GC oven..

Figure 11: GC Oven Internal View


Electrical Connections All the connections are the same as described in the PH 40 instruction Manual except for:

The new 15 connector (1), marked SW Valve, used for the optional Switching Valve. The strip connectors (2) marked “Autosampler GC” that are use to connect the GC

Autosampler DIN connection cable with the Start and Ready connection of the pump.

Figure 12: New Connections of the Back Panel

The following tables report the 15-pin and the strip connectors pin-out.

SW Valve 15-pin Connector Pin 6 DGND Pin 9 VLV pos B (Out) Pin 13 VLV pos B (In) Pin 14 VLV pos A (In) Pin 15 VLV pos A (Out)

Autosampler GC Strip Connector

+ Start GC Start - Start GND

+ Ready GC Ready - Ready GND

Each valve is electrically supplied by a 24 Vdc external portable power supply connected through the power line and the relevant “jack” marked Left Valve or Right Valve located on the rear panel of the Valve Box as shown in figure 13.


1-2-3 = 24 V dc Jack

Figure 13 Valve Box – Rear View

The electrical characteristics of the power supply are:

AC Input = 100 V-240 V; 1.3 A max; 50/60 Hz DC Output = 24 V; 2A

Conditions for a Correct Automatic Operation with the TriPlus and the GC Connect the cables as described in figure 14.

SamplingRS232Sub 1

GC

Valves

RS232

Autosampler

Events

Autosampler GC

COMPUTER

Transfer Valve

ValcoInterfaces Valves

TRIPLUSSampler

PHOENIX 40

TRACE GC

ValcoInterface

Figure 14: LC-GC System Connections New Parameters Programmable Through the Phoenix 40 Keyboard and Display If LC-GC is set to ENABLE, the pump will display a series of new parameters that are available in different pages on the display of the pump. The same parameters are also available through the RS 232 communication protocol.


Control of the Pump The pump can be controlled and programmed either through:

Keyboard and display PC via RS232 and Hyper Terminal

Controlling and Programming the Phoenix via Keyboard and Display The following page menu shows the normal setting of the pump when operating as an independent syringe pump in a stand-alone micro HPLC system. In this operation mode the pump will control the Injection Valve and the Enrichment Valve, if enabled, as described in the Phoenix 40 Pump Instruction Manual.

SYSTEM CONFIGURATION MAIN MENU OVENOFF TEMP00 AUTO-RUN IN SUBSET AUTO-INJECT: YES 1 NO 2 NO 3 YES ENRICHMENT: YES DEVICE #: 1 LC-GC: DISAB PRESSURE UNIT: MPa BAUD RATE: 9600

The following parameters are available:

Injection Time Enrichment Time Enrichment Delay

PROGRAM TIMES PROGRAMMING SUBSET 1 MAIN MENU STAND-BY 0.0 ADD TARGET 0.5 POST-RUN 1.0 ENRICHMENT 1.0 ENR DELAY 2.0 INJECTION 0.6 PMP_A PMP_B PMP_C STOP STOP

The following submenus have been modified to allow full control of the pump for the LC-GC mode of operation. Setting LC-GC to ENABLE the system will permit full programming of the three valves (Injection, BKF and Switching) available in any timing combination with start from the Run of the pump.

SYSTEM CONFIGURATION MAIN MENU OVENOFF TEMP00 AUTO-RUN IN SUBSET AUTO-INJECT: YES 1 NO 2 NO 3 YES BKF VLV: YES DEVICE #: 1 LC-GC: ENAB PRESSURE UNIT: MPa BAUD RATE: 9600 SW VLV: YES

The following parameters are available:


Injection Time BKF Time BKF Duration Switching Valve (SV)Time Switching Valve (SV) Duration

PROGRAM TIMES PROGRAMMING SUBSET 1 MAIN MENU STAND-BY 0.0 ADD TARGET 0.0 POST-RUN 1.0 BKF TIME 2.0 SV TIME 0.7 BKF DURAT. 1.0 SV DURAT. 1.2 INJECTION 0.6 PMP_A PMP_B PMP_C STOP STOP

In the Manual Controls submenu it is possible to move the three valves in any of the two positions when the pump is not running.

MANUAL CONTROLS LIVE DISPLAY SAMPLE VALVE LOAD INJ

BKF VALVE OFF SWITCH VALVE POS A

PMP_A PMP_B PMP_C STOP STOP

The actual position of the Injection Valve and BKF Valve are indicated by the corresponding LED present in the valve box close to the valve (Inj, Load). The actual position of the Switching Valve is indicated in the Manual Controls submenu. Time Programming of the Valves To program the PH 40 from the control panel refer to the Phoenix 40 Pump Instruction Manual and consider the following modifications:

1. The pump can be programmed to operate in the LC-GC mode selecting in the CONFIGURATION, the option LC-GC = ENABLE. In this mode of operation the Pump is able to communicate with GC through the Autosampler GC connection cable such that the GC will inhibit the pump Run if the GC is not ready and it is not in the Sampling Status. As a consequence of that also the TriPlus LC sampler, if present, will not start the injection sequence until the pump and the GC are ready to start.

2. The valves are freely programmable with the following behavior. Consider that the origin of

the valves timing and the pump run is the injection valve movement from LOAD to INJECT position or the moment at which the TriPlus is injecting. GC will also start at the moment of the injection.

3. In LC-GC mode up to three valves can be programmed completely independently one from

the other. A general timing that can be realized is shown in figure15.


Figure 15: Valves Timing Schematic

4. The pumps can operate in gradient mode or independently or in a combination of both.

5. Even if independent (with different subsets) the pumps can be started simultaneously

selecting the LINK to1 mode in the Configuration page.

6. Valves and pumps will start at the beginning of injection and will continue to operate up to the end of run.

7. The timing will be repeated up to the end of the cycles programmed.

Programming the Transfer Valve on the GC The transfer valve is positioned at the back of the OC Injector and is actuated through a VICI electrical motor connected to the Actuator Control Module, triggered by the Manual Valve Control (a box with two buttons and LEDs for Pos A and Pos B) or programmed through the Time Events of the TRACE GC via the Time Events connection cable shown in figure 14. Figure 16 shows an example of the Transfer Valve programming via the GC keyboard and display.


RUN TIME EVENT 0.00 Ext Ev#6 Off<1.00 Ext Ev#5 On 2.00 Ext Ev#5 Off2.00 Ext Ev#6 On

Add run time events

DEFAULT CONDITIONS Ext. event #5 OffExt. event #6 On Ext. event #7 Off<

Figure 16: Transfer Valve Programming via GC Figure 17a shows Transfer Valve, On-Column interface, SVE valve and Purge line connected to the DPFC on purge connection while the figure 17b shows the same Transfer Valve but with the purge line controlled with a Needle Valve (default configuration). See 1 of figure 17b.

a b

Figure 17: Valves View The most suitable programming parameters for the Valve on the TRACE GC control Data System (e.g. Chrom Card, ChromQuest, Xcalibur) is shown in figure 18.

Figure 18: GC External Events Programming Page C


The valve is controlled with two time events:

External Event 6 set to ON = To move the valve in Pos A. Corresponding to the valve position that divert the HPLC eluent to the waste (see figure 9b)

External Even 5 set to ON = To move the valve in Pos B. Corresponding to the valve position that transfer the HPLC eluent into the pre-column through the FS transfer line

Note that to be able to move the valve in any of the two positions, the opposite time event must be in OFF E.g. to move the valve from position A to position B, External event time 6 must be in OFF and at the same time External Event 5 must be in ON. To be sure that when the GC is in St-by and in Prep Run the valve remain in position A (no sample is injected into the pre-column) the Initial Values for External Event 6 must be checked. Figure 19 shows an example of special external events programming for the Transfer Valve to leave the valve free for activation at any time.

Figure 19: Special External Events Programming If a more flexible operation of the valve is required, through the Manual Valve Control box, the events driving the valve must be set OFF immediately after the actuation has been realized. In this way in any moment the valve can be manually positioned where it is required. The actual position of the injection and BKF valve is indicated by the two LEDs present in the Valve box. The actual position of the switching valve is shown on the display of the pump.


Figure 20: Top of the GC with Manual Valve Control Box for the Transfer Valve Programming the SVE Valve The Solvent Vapour Exit present in the TRACE GC for the LC-GC instrument is the same as installed on the TRACE LV OC instrument. This means that all the setting defined in the relevant section of the TRACE GC Operating Manual are valid also for the LC-GC.

Figure 21: Example of SVE Parameters

Attention: When Data System is used, uncheck the Link to Large Volume assistant program box on

the TRACE GC Configuration Inlet page. The SVE valve, if programmed, is ON at the Prep Run of the GC and remain ON up to the end of the SVE Duration. The SVE Duration is set according to the duration programmed for the External Event 5 plus a time that correspond to the time required for the Partial Evaporation of the transferred mobile phase into the pre-column.

Figure 22: Programming Page for the SEV and AUX Purge on Chrom-Card


Control of the Carrier Purge Line of the Transfer Valve The purge line of the Transfer Valve on port number 4 of figure 7 can be controlled using the purge valve of the DPFC installed on the GC (figure 16) or through a Needle Valve directly connected to the Transfer Valve as shown in figure 17 (default condition). Aux Purge The aux purge is a programming possibility present on the OC Inj. page that allows to set a specific time for controlling the OPEN/CLOSE position of the purged line present in the transfer valve and that is connected to the DPFC. If Constant Purge is unchecked and Stop Purge Time is different from zero, the ON/OFF valve present in the DPFC module is opened for the time programmed (normally up to the end of analysis) This allows the purge be present for the whole analysis time or for the time required. (The purge flow is normally low and it is independent from the pressure of the carrier gas). At the end of the programmed time the valve will be closed and will remain closed until the next Prep Run phase is activated. If the purge is not required the Aux Purge must be programmed to Constant Purge. Start up To be ready for the HPLC injection with the sampler and for the fraction transfer, the following settings of the pump, sampler and GC must be assured:

Phoenix 40 AUTORUN= NO, AUTOINJECT = YES, CYCLE = At least 1

TriPlus LC ENABLE INPUT = H > L INJECT OUT = H > L

TRACE GC

READY OUT = WHEN HIGH

AUTO PREP RUN = ON

1. At pump start and when Sampling phase has been reached the pump will display the message WAIT GC IN 1.

2. Pressing prep run on GC or automatically if auto prep run has been selected on the GC

oven configuration, the sampler will start and according to the TriPlus setting the pump will go in run together with the GC.

NOTE: To avoid the switching of the pump controlled injection valve, the INJ TIME = 0 must be set.

3. The transfer valve, if correctly configured the External events 5 (set to ON move the valve

in TRANSFER) and External event 6 (set to ON move the valve back to LOAD position).


4. The SVE must also be programmed to remain open up to the end of the transfer time and this is programmed in the OC control page of the GC.

5. Also the Auxiliary purge, if connected to the DPFC and to the Transfer Valve in position 4,

must be correctly programmed on the OC page of the data system or keyboard.

6. The following sequence of messages are visible on the display: ST-BY >> WAIT GC IN 1 >> WAIT RUN IN 1 >> WAIT INJ IN 1 >> SAMPL >> RUN >> POST RUN

Preparing the GC Oven Temperature Oven temperature must be kept constant during the whole LC time before transfer and during transfer and SVE delay time to allow the solvent to evaporate in suitable temperature conditions according to the LC eluent used. Controlling and Programming the Pump Through RS232 and Hyper Terminal To program and control the pump with the PC a generic Terminal program is needed. Here under is described the use of the “HyperTerminal” available in any Windows operating systems. For details refer to Pump Programming Through the Terminal.


Pump Programming Through the Terminal The pump can be programmed from the Hyper Terminal using a series of commands listed below and that can be seen in any moment just writing “HELP” followed by ENTER. The syntax must be the one described in section 5 of the PH 40 Instruction Manual. Before starting the Hyper Terminal must correctly set as described in paragraph Setting the Hyper Terminal to Correctly Control the Pump. Commands Syntax HELP LIne T=.. {X=..} {A=..} {B=..} {C=..} {F=..}/{P=..} {E} %Filled %Work ?A ?B ?C ?Flow ?P[:Z] ?PVerbose ?Status ?Time ACtive ADump AINjct 0/1 ARUn 0/2 ATTime = BKDurat. = BKFvlv 0/1 BKN on BKO off BKTime= COFlow COPress CRun 0/1/2 CYcles= DElete:Z DISplay ECho 0/1 ENable:Z ERich 0/1 ERDelay= ERTime = EVBypass EVOnline FIle FUll_load HALt HElp HOld[:W] INTime= LC -gc 0/1 LFIle n LLIst LREad n LWRite n MAPress= MFill:Z= MIPress= NAMe = NEw OVEnab 0/1 OVTemp = PArt_load PRTime= PSI 0/1 PURge[:Z/W]QUiet 0/1 RST[:W][=] RUN[:W] SBTime= SSet= STArt[:W] STOp[:Z/W] SVInject SVLoad SWA PosA SWB PosB SWDura = SWTime = SWValve 0/1TAPress= VErsion XOnset 0/1 ** Z = A, B, C or @ (all pumps) - W = 1, 2, 3 or @ (all subsets) ** A series of new COMMANDS have been added to control and program the additional features of the pump. The new commands are highlighted in blue and are: LC-gc 0/1 : “0” set the operating mode of the pump as it is defined in the PH40 instruction manual.

“1” set the operating mode of the pump as “LC-GC” and in this mode the pump allows the programming and the actuation of the pumps and valves as suitable for LC-GC (e.g. waiting the GC before starting the Run), programming all the 3 valves independently one from the other, showing the specific dialog for the programming of the valves.

SWValve 0/1 : To Enable (1) or Disable (0) the installation of the Switching Valve. BKFvlv 0/1 : “0” disable the BKF valve, “1” allows the programming and the actuation of the BKF valve. ARUn 0/1/2 : With 2 all the subset are LINK to subset 1 so that only when all the linked subsets are in SAMPLING status the injection can be performed (manually or with sampler) and all the pumps start simultaneously at the injection moment. ARUn=2 can only be programmed from a subset different from 1


BKDurat. : Set the time at witch the BKF valve will move to the ON position. BKN on : Direct command to move the valve in the ON position. BKO off : Direct command to move the valve in the OFF position. BKTime= : Duration of the BKF time. SVInject : Direct command to move the Injection valve in the Inject position. SVLoad : Direct command to move the Injection valve in the Load position. SWA PosA : Direct command to move the Switching valve in Position A. SWB PosB : Direct command to move the Switching valve in Position B. SWDura = : Duration of the Switching time with valve in position B. SWTime = : Time at witch the Switching valve will move to position B. Below a Series of Programming Dialogs Using the New Commands: File command with the highlighted valve parameters programmed: FI SS = 1 NAME = TEST______ COF FULL_LOAD QUIET 0 ATT = 0.0 SBT = 0.0 PRT = 1.0 MAP =30.0 MIP = 0.1 TAP = 1.7 NEW DELETE:@ ENABLE:A ENABLE:C LINE T = 0.0 X = 0 A = 100.0 C = 0.0 F = 118 LINE T = 1.0 X = 0 A = 100.0 C = 0.0 F = 120 LINE T = 2.0 X = 0 A = 20.0 C = 80.0 F = 150 LINE T = 3.0 X = 0 A = 100.0 C = 0.0 F = 120 MFILL:A = 100.0 MFILL:C = 100.0 CYCLES = 5 INT = 0.5 BKT = 0.5 BKD = 1.2 SWT = 0.7 SWD = 1.2 Display command, to control in real time the status of many parameters of the selected subset and also the status of the GC ready status. DISP (when pump is performing the target) SS = 1 PRESSURES (MPa) - TIME - FLOW - CYCLE -FLOW SHARING(%) - VALVES - OVEN A B C (min) (ul/min) # A B C SAMP BKF SWV (°C) STATUS 4.9 0.0 0.0 0.5 0 0 0.0 0.0 0.0 LOAD OFF A OFF TARG DISP (when pump is waiting the GC ready signal) SS = 1


PRESSURES (MPa) - TIME - FLOW - CYCLE -FLOW SHARING(%) - VALVES - OVEN A B C (min) (ul/min) # A B C SAMP BKF SWV (°C) STATUS 2.3 0.0 0.0 1.1 118 0 100.0 0.0 0.0 LOAD OFF A OFF WT_GC The valve parameters can be programmed at any time before and during the run. If the programmed time is over there will be an error message or the parameter will be executed the next run. At the end of run, or when a STOp:@ command is given, all the valves and pumps will return in the stand-by position. With the STOp or STArt commands only, the selected subset will performs the selected operation. INT = 0.5 BKT = 5 .4 BKD = 1.5 SWT = 3.3 SWD = 2.5 ?ST STOP COF CRUN 0 QUIET 0 XONSET 0 PSI 0 ARUN 0 BKF 1 AINJ 1 OVEN 0 LC 1


Setting the Hyper Terminal to Correctly Control the Pump To correctly control the PH 40 the Hyper Terminal, available in the Accessories folder of the Windows Operating System, must be lunched.

1. Select Program >> Accessories >> Communication >> Hyper Terminal. The following window is displayed.

2. This is the first window of the Hyper Terminal where a name for the connection can be entered. Click on OK, the following window is visualized.

3. In the window the COM Port of the computer is selected (e.g. COM 1) then click on OK. The following window is visualized.


4. This window allows to define the parameters of the COM port to match the requirement of the RS 232 port of the Phoenix 40 (in this case: baudrate 9600). Click on OK, the following Hyper Terminal main window is visualized.

5. In File menu select Properties. The following window is visualized.

6. Select Setting to open the following page.


7. Select ASCII Setup the following page is visualized.

8. In ASCII Setup page set the ASCII parameters as follows: Line delay to 50 milliseconds Character delay 2 milliseconds Uncheck all the ASCII Receiving parameters boxes.

9. Click on OK to return to Hyper Terminal main window.

NOTE: Now you can type the programming parameters of the pump and the direct command through the Notepad.


10. Open the Notepad available in the Accessories folder of the Windows Operating System selecting Program >> Accessories >> Notepad.

11. Type the suitable pump program following the correct syntax as described in the paragraph

Commands Syntax.

12. Type the desired program for the pump payi ng attention to r espec t the correct commands syntax. Se.

NOTE: After the last command has been typed, press ENTER to move the cursor to start a new paragraph.

13. Save the file with extension .TXT; e.g. 4_Test.txt. 14. Send the file to the pump operating as follows:

In the Hyper Terminal main window select Transfer menu then Send text file. Select the file previously saved; e.g. 4_Test.txt.


The transfer of the text lines to the pump is visualized on the Hyper Terminal main window. Wait for the complete transfer.

15. To save a file present on the memory of the pump operate as follows:

Recall the file by using command FI for each Subset. By using the pointer of the mouse select the text lines with the exclusion of the first line FI. Click on the right button of the mouse and select the Copy.

Paste on a new Notepad file. Save the file.

Control of the TriPlus Sampler TriPlus sampler can be controlled through:

Stand/alone program Chrom/Card Xcalibur or ChromQuest Data processing system.

Operate as normally done with a GC programming and control.


Analytical Testing Carry out the following analysis to test the performance of the system. Conditions Solution of 1ng/µL of PAHs in hexane Injection volume: 20 µL Detector: UV; 254 nm HPLC Mobile Phase: 90% n-pentane / 10% methyl t-butyl ether (GC grade) HPLC Column: Hypersil Silica 100 mm; 2.1 mm ID (Provided with instrument) Pre-column: Uncoret 15 m; 0.53 mm ID; 0.25 µm f.t. (Provided with instrument) Column: Silica Phase 15÷30 m; 0.25/032 mm ID; 0.25 µm f.t. (Not included) TRACE GC Method: Oven Method Initial Temperature (°C): 55 Initial Time (min): 3.00 Rate #1 (deg/min): 15.0 Final Temperature #1 (°C): 320 Hold Time #1 (min): 5.00 Left LVOCI Method SVE Temperature (°C): 150 SVE Duration (min): 1.70 Left Carrier Method Mode: Programmed Pressure Initial Value (kPa): 80.00 Initial Time: 3.00 Rate #1 (kPa/min): 20.0 Final Value #1 (kPa): 220.00 Hold Time #1 (min): 0.00 Left FID Method Base Temperature (°C): 330 H2 Flow (ml/min): 35 Air Flow (ml/min): 350 Makeup Gas Flow (ml/min): 30 Run Table External Event #1 Prep-Run Default: Off External Event #2 Prep-Run Default: Off External Event #3 Prep-Run Default: Off External Event #4 Prep-Run Default: Off External Event #5 Prep-Run Default: Off External Event #6 Prep-Run Default: On External Event #7 Prep-Run Default: Off External Event #8 Prep-Run Default: Off 0.00 min - External Event #6: Off 0.50 min - External Event #5: On 1.50 min - External Event #5: Off 1.50 min - External Event #6: On


Pump Program SS = 1 NAME = __________ COF FULL_LOAD QUIET 0 ATT = 0.0 SBT = 0.3 PRT = 5.0 MAP =30.0 MIP = 0.0 TAP = 1.1 NEW DELETE:@ ENABLE LINE T = 0.0 X = 0 A = 90.0 C = 10.0 F = 400 LINE T = 5.0 X = 0 A = 90.0 C = 10.0 F = 400 LINE T = 5.1 X = 0 A = 90.0 C = 10.0 F = 50 LINE T = 15.0 X = 0 A = 90.0 C = 10.0 F = 50 MFILL:A = 100.0 MFILL:C = 100.0 CYCLES = 2 INT = 1.5 TAP=0.5 Chromatograms Figures 23 and 24 respectively shown the PAHs LC fraction chromatogram and the related GC chromatogram.

(min)

(mV

off)

Inje

ctio

n

End

of F

ract

ion

Figure 23: LC Fraction Chromatogram

Figure 24: GC Chromatogram of the PAHs Fraction


Appendix: TriPlus LC Installation This appendix provides the instruction to install the TriPlus LC Sampler on the TRACE GC Ultra. Sampler Supports Assembling With reference to Figure 25, proceed as follows

1. Support Bar 2. Support Leg 3. Mounting Clamps 4. Support Leg Holes 5. Leg Fixing Screws 6. Support Bar Fixing Holes for the GC

Figure 25: Support Assembling

1. Insert the provided fixing screw into each hole present on the support bar.

2. Place the support leg on the support bar paying attention that the fixing screw of the leg is frontally turned.

3. Tighten the fixing screws.

Installation on the GC To properly install the sampler supports on a TRACE GC Ultra, proceed as follows:

1. From the GC upper cover remove the plastic caps covering the corresponding fixing holes.

2. Insert into each holes present on the support bar the provided fixing screw.

3. Mount each sampler support on the GC paying attention to have the support leg turned toward the back of the GC as shown in Figure 26.


Figure 26: Sampler Supports Installation on a TRACE GC Ultra

4. Guide the fixing screws into the corresponding fixing holes.

5. Tighten the fixing screws.

6. Install the crossrail X of the TriPlus LC sampler on its support and continue the installation as described in Chapter 3 of the TriPlus LC Operating Manual

a b

Figure 27: Sampler and Injection Valve Installation

7. Install the sampler injection valve paying attention to install the sampler injection valve as

shown in Figure 4b. 8. Disconnect and insulate the pump controlled injection valve from the pneumatic circuit. 9. Connect the sampler injection valve to the port 9 of the BKF valve as shown in Figure 3a.

System Description and Operations

Documents

Transcript of System Description and Operations