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Standard Operating Procedure

Agilent 7890B Gas Chromatography with Gas Sampling Valve

This customized Agilent 7890B Gas Chromatography system is equipped with a gas sampling valve at the inlet which is designed for direct gas sample tests. Two detectors, Thermal Conductivity Detector (TCD) at the back and Flame Ionization Detector (FID) at the front, are dedicated for detecting most permanent gases excluding the carrier gas and most organic compounds (e.g., hydrocarbons), respectively.

1.0 Safety Precautions

General Laboratory Precautions

 Avoid leaks in the carrier gas lines. Use leak-checking equipment to periodically check for hydrogen leaks.

 Eliminate from your laboratory as many ignition sources as possible (open flames, devices that can spark, sources of static electricity, etc.).

 Do not allow hydrogen from a high pressure cylinder to vent directly to atmosphere (danger of self-ignition).

 Provide proper system ventilation as described in the Site Prep manual.

Operation Precautions

 Turn off the hydrogen at its source every time you shut down the GC.  Turn off the hydrogen at its source if a power failure occurs.

 If a power failure occurs while the GC is unattended, even if the system has restarted by itself: 1. Immediately turn off the hydrogen at its source.

2. Turn off the GC.

3. Eliminate all potential sources of ignition in the room. 4. Open the vacuum manifold of the GC to atmosphere. 5. Wait at least 10 minutes to allow any hydrogen to dissipate. 6. Start up the GC as normal.

 When using hydrogen gas, check the system for leaks to prevent possible fire and explosion hazards based on local Environmental Health and Safety (EHS) requirements. Always check for leaks after changing a tank or servicing the gas lines. Always make sure the vent line is vented into a fume hood.

Measuring Hydrogen Gas Flows

 Do not measure hydrogen together with air or oxygen. This can create explosive mixtures that may be ignited by the automatic ignitor.

 To avoid this hazard, turn the automatic ignitor off before your begin and always measure gases separately.

 When measuring gas flows on a detector using hydrogen for the detector flame or carrier gas, measure the hydrogen flow separately. Never allow an air stream to enter when hydrogen is present in the flow meter.

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Uncombusted Hazardous Gases

 During normal operation of the GC with many detectors and inlets, some of the carrier gas and sample vents outside the instrument through the split vent, septum purge vent, and detector exhaust. If any sample components are toxic or noxious, or if hydrogen is used as the carrier gas, these exhausts must ben vented to a fume hood. Place the GC in the hood or attach a large diameter venting tube to the outlet for proper ventilation.

1.1 System Start-up

1. Double-click the icon “7890GC Gas Sampling (online)” on the right side of Desktop 2. Select “Download to Instrument”

3. When the software is opened, the GC system will initiate automatically and ignite the FID flame (you will hear the sound of ignition). The status should show a “Ready” in green. 4. In the file browser, find the directory of your method “C:\Chem32\2\Methods\[Your Name]”,

and create a new subfolder using the current date

5. There is a template method (Template for GC training.M) in “C:\Chem32\2\Methods”. Copy and paste it into your new subfolder and rename the method.

6. On the left column of the software, select “Method and Run Control” tab, and you will see the new subfolder and the copied method in this tab

7. Double-click this copied method, its name will appear in the second line of the software (Fig. 1). It is now loaded as the current method.

Figure 1. Display the current method

1.2 Edit Your Method

8. On the top line of the software, click Method  Edit Entire Method  check “Method information” and “Instrument/Acquisition”  click OK  click OK again

9. If you wish to manually inject the gas sample, select Manual and select Front as the injection location  click OK; If you wish to automatically introduce the gas sample, select GC Valve and select Valve 1 as the injection location  click OK

10. The Setup Method screen will pop out

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11. In the Valves tab, Valve #1 is the Gas Sampling Valve. Set up the Load Time and Inject Time (Fig. 2). This is the time for the gas sample to be loaded in the TCD and FID loops if you select to automatically introduce the gas sample. If you select to manually inject the gas sample, this time doesn’t matter. Keep the Heater temperature at 150 °C (max 225 °C).

Figure 2. Edit the Valves tab

12. In the Inlets tab, set up CAP SSL inlet and PPI inlet settings separately (Fig. 3 and Fig. 4) 1) CAP SSL inlet (for FID gas line):

 Set Heater temperature at 250 °C (max 300 °C)  Keep the Pressure value unchanged

 If split ratio = 20:1, Total inlet flow = Column flow (HP-5) x 20 + Column flow (HP-5) + Septum purge flow

Figure 3. CAP SSL inlet settings (for FID gas line)

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2) PPI inlet (for TCD gas line):

 Set Heat temperature at 250 °C (max 300 °C)

 Total inlet flow = Column flow (HayeSep) + Septum purge flow  Keep Control Mode as Flow

Figure 4. PPI inlet settings (for TCD gas line)

13. In the Columns tab, set up HP-5 column and HayeSep column separately (Fig. 5 and Fig. 6) 1) HP-5 column (for FID gas line):

 Set the Column flow and keep the other settings unchanged  Make Column flow = Post Run flow

 Select “Constant Flow” mode

Figure 5. HP-5 column settings (for FID gas line)

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2) HayeSep column (for TCD gas line):

 Set the Column flow and keep the other settings unchanged  Make Column flow = Post Run flow

 Select “Constant Flow” mode

Figure 6. HayeSep column settings (for TCD gas line) 14. In the Oven tab, set up the temperature ramp program

 Maximum Oven Temperature = 290 °C  Equilibrium Time = 0.5 min

 Post Run temperature = 50 °C or the starting temperature of the ramp program

Figure 7. Oven temperature ramp program

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15. In the Detectors tab, set up FID (Front) and TCD (Back) settings, separately (Fig. 8 and Fig. 9) 1) FID detector (Front):

 Set the Heater temperature at 300 °C (max 300 °C)

 Air flow = 400 ml/min; H2 fuel flow = 30 ml/min; Makeup flow (He) = 25 ml/min  Check “Constant Makeup and Fuel Flow”; Check “Flame”

Figure 8. FID detector (Front) settings 2) TCD detector (Back):

 Set the Heater temperature at 300 °C (max 300 °C)  Makeup flow (He) = 5 ml/min, Constant Makeup Flow  Reference flow = Makeup flow + Column flow (HayeSep)  Check “Filament”

Figure 9. TCD detector (Back) settings

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16. In the Events tab, set Time = 0.1 min, Event Type = Valve, Position = Valve 1, Setpoint = On (Fig. 10). This setting makes the GSV to open/close in 0.1 min after the test is started.

Figure 10. Events settings 17. In the Signals tab, set up FID and TCD signals separately (Fig. 11)

#1: Front Signal (FID): select 50 Hz / 0.004 min, check Save to record data #2: Back Signal (TCD): select 5 Hz / 0.04 min, check Save to record data

Figure 11. Signals settings 18. Click Apply and then click Ok to close the Setup Method screen

19. Click Save Current Method in the second line of the software to save the changes (Fig. 12)

Figure 12. Save Current Method icon

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Sequence Table: 7890GC Gas Sampling

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1.3 Start the Measurement

20. If you wish to manually run the samples one by one:

1) On the top line of the software, click Run Control  Run Method 2) The status shows “Run in Progress/Waiting for Injection” in purple 3) Walk to the GC and manually inject your gas sample into the inlet 4) Press the Start button on the GC front panel

5) After 0.1 min, you will hear the gas sampling valve is closed

6) The status shows “Run in Progress/Data Acquisition” in blue as well as the elapsed time 21. If you wish to automatically introduce the samples and run in sequence:

1) On the top line of the software, click Sequence  Sequence Table 2) A “Sequence Table: 7890GC Gas Sampling” screen will pop out (Fig. 13)

Figure 13. “Sequence Table: 7890GC Gas Sampling” screen 3) Fill the Sample Name for each sample

4) Select the desired method in the Method Name drop list

NOTE: If the desired method is not included in the Method Name drop list, click the “Browse Method” icon to open the desired method (Fig. 14), then you can find it in the Method Name drop list

Figure 14. Browse Method icon

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5) Keep the other parameters as below: Injector Location = Front; Injection Source = As Method; Inj/Loc = 1; Sample Type = Sample

6) Click Apply and then click OK to close the Sequence Table screen

7) On the top line of the software, click File  Save As  Sequence Template 8) A “Save Sequence as: 7890GC Gas Sampling” screen will pop out (Fig. 15)

Figure 15. “Save Sequence as: 7890GC Gas Sampling” screen

9) In the file browser, find the directory of your sequence “C:\Chem32\2\Sequence\[Your Name]”, and create a new subfolder using the current date

10) On the right side of the “Save Sequence as: 7890GC Gas Sampling” screen, locate the new subfolder you have just created and double-click it

11) On the left side of the “Save Sequence as: 7890GC Gas Sampling” screen, input the name of your sequence (e.g., xxxxxx.S) in the File Name field

12) Click OK to close the “Save Sequence as: 7890GC Gas Sampling” screen

13) The sequence directory will appear in the second line of the software (Fig. 16). It is now loaded as the current sequence.

Figure 16. Display the current sequence

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Start Run: 7890GC Gas Sampling

Waiting for Ready ...

Press Start Run to Override

2tart Run ~bort Run

14) On the top line of the software, click Run Control  Run Sequence 15) A “Waiting for Ready” screen will pop out (Fig. 17)

Figure 17. Waiting for Ready screen 16) The status shows “Sequence Running/Data Acquisition” in blue

17) The GSV opens at 0.1 min to start loading the gas sample automatically. It will automatically close after a certain period of time to start the test run. This time duration is determined by your method setting for Load Time and Inject Time in the Valves tab.

1.4 Post-run Procedures

22. After a test run is completed, a .pdf report will automatically pop out

23. The data will be automatically stored in the folder of “C:\Chem32\2\Data”. You need to create a new subfolder with directory “C:\Chem32\2\Data\[Your Name]”, move the newly reported data into your subfolder, and rename it.

24. After all the test runs are completed, close the “7890GC Gas Sampling (online)” software 25. Walk to the GC, on the GC front panel:

1) Press the “Front Inlet” button

2) Use the downward arrow button to select “Pressure” 3) Press the “Off/On” button to turn it OFF

4) Press the “Back Inlet” button

5) Use the downward arrow button to select “Total flow” 6) Press the “Off/On” button to turn it OFF

NOTE: You can double-click the icon “7890GC Gas Sampling (offline)” on the right side of Desktop to open the offline software to view and analyze the data in the “Data Analysis” tab.

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2.0 Specifications

 System components:

 Thermal Conductivity Detector (TCD) at the back  Flame Ionization Detector (FID) at the front

 Gas sampling valve with 0.5 ml TCD loop and 0.25 ml FID loop  PPI inlet (purged packed inlet) for TCD gas line

 CAP SSL inlet (capillary split/splitless inlet) for FID gas line  HayeSep packed column for TCD gas line

 HP-5 capillary column for FID gas line  OpenLAB CDS ChemStation software  Carrier gas: helium

 Electronic pneumatic control (EPC) modules  Maximum oven temperature: 290 °C

 Thermal Conductivity Detector (TCD):  Linear dynamic range: > 105 _{± 5%}  Maximum temperature: 300 °C

 Standard EPC for 2 gases (He, H2, or N2 matched to carrier gas type)  Make-up gas: 0 to 12 ml/min

 Reference gas: 0 to 100 ml/min  Flame Ionization Detector (FID):

 Linear dynamic range: > 107 _{± 10%}  Maximum temperature: 300 °C

 Standard EPC for 3 gases (air, H2, make-up gas)  Air: 0 to 800 ml/min

 H2: 0 to 100 ml/min

 Make-up gas: 0 to 100 ml/min  HayeSep packed column:

 Temperature range: -60 °C to 290 °C

 Feature: 3 m x 1/8 inch x 2 mm; packed with HayeSep DB 80-100 Mesh  In: PPI inlet; Out: TCD detector at the back

 HP-5 capillary column:

 Temperature range: -60 °C to 325 °C  Feature: 30 m x 320 µm x 0.25 µm

 In: CAP SSL inlet; Out: FID detector at the front

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3.0 User Requirements

The Agilent 7890B GC with GSV must be used by authorized personnel only. All authorized users are expected to read and understand this SOP and follow the operation instructions carefully. No unauthorized user may operate this GC with GSV unless accompanied by an authorized user. All visitors must be briefed on proper safety protocol and must wear appropriate personal protective equipment. To become an authorized user, one must:

1. Complete the New User Scope of Work Form

2. Read and sign the Materials Characterization Laboratory (MCL) Governance Document 3. Complete Environment, Health & Safety (EH&S) training class

4. Take the basic MCL orientation session

5. Receive training on the operation of this GC with GSV by the MCL staff 6. Read and fully understand this SOP

7. Sign the training certificate form and receive the Google Calendar for online reservation

4.0 General Safety

4.1 Required Personal Protective Equipment

Users must wear lab coats, safety glasses, and gloves. Shorts, open-toed shoes, high heels, and skirts, are forbidden.

4.2 Emergency Procedures and Contacts

For non-life threatening emergencies: notify the MCL facility manager and your PI immediately.

Facility manager: Zongmin (Shirley) Bei, Ph.D.

Office: 109B Furnas Hall, Tel: (716) 645-5165, Cell: (585) 354-5623 Email: [email protected]

or for police / ambulance, call 645-2222

In case of fire or other life threatening emergency: Exit the laboratory through an emergency exit door. Pull one of the fire alarms located in the main hallway. Dial campus police / ambulance at 645-2222.

4.3 Power outage: If there is a power outage, turn off the GC with GSV system according to

the shutdown procedure to avoid a hazardous situation when power is restored. If there is an emergency, leave the MCL immediately and either return after emergency to shut down the GC with GSV system or contact the facility manager.

4.4 University after hours laboratory use policy

No working alone, use the buddy system!

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# Revised by Date Modification

1 Zongmin (Shirley) Bei 01/29/2020 Document initial release 2

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