Standard Operating Procedure Agilent 7890B Gas ...

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"% Shared Instrumentation Laboratories

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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~1~111, 0 Columns Oven

_L X Events Signals Configuration

VaJve r,,,. Postion

Ga,5-'!, V,Jve NIA

112 Not..,,.aled NIA

#3 Not..,,.aled NIA

114 Not..,,.aled NIA ... #5 Not..,,.aled NIA

m; Not..,,.aled NIA

If] Not nstaled NIA

#8 Not ..,,.aled NIA

Vl/Jve Bax

Actual

r{] Heater

150'C 150'C

I Ii Readiness GC Calculators

Load Tme inn)

N/A

N/A

NIA

N/A

N/A

N/A

N/A

_L X ~ ~l1i l,Q, Oven Detectors Ev ents Signals Configuration

SSL - Front I pp - Back I Split -Splitless Inlet Select Liner. .. A Liner has not been selected.

Gas Saver: Setpoint Actual

~ Heater: 250 'C 250'C 20mUmin

~ Pressure: 12071 psi 12.1 psi

Total Flow: 66 mU min 66mUmin

~ Septum Purge Flow: 3 ml/min 3mUmin

Septum Purge Flow Mode: § andard ___:)

Mode: Split Ratio:

20 :1 Split Flow 60mU min

~

r-;ectTmejn;n)

NIA

NIA

NIA

N/ A

NIA

NIA

NIA

mu Readiness GC Calculators

After: 2 rrun

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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~ ~111 1,20< Oven Detectors Events Signals

SSL - Front PP - Back ]

Purged Pocked Inlet Select Liner. .. A Liner has not been selected.

Setpoint Actual

['.l] Heater: 250 'C 250'C

['.l] Flow: 23 mUmin 23mUmin

Control Mode: [ Row .. I ['.l] Septum Purge Flow: 3 mU min 3mUmin

'\© i 1Ql t1 ~ ~ 1,__ X

X i Configuration Readiness GC Calculators

la ALS Valves Inlets ~ Oven Detectors Events Signals Configuration Re:adiness GC Calculators

# Selection Control Mode

l:t) On

Flow

Pressure

Average Velocity

Holdup Time

I Constant Row

Setpoint

3mUmin

12.071 p~

43. 715 an/sec

11438min

Post Run: 3 mUmin

ColLrm #1 Configuration

Actual

3 mUmin

12.1 p~

(Initial): Omin He @ 30 'C Oven Ou: lvnbtent Pressure 30 mx320µ,,x0.25µn

I Change Column . 11 Calibrate Column... 11 Lock Column ...

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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'



© i3 ~ X I i ALS Valves Oven Detectors Events Signals Configuration Readiness GC Calculators

II Selection Corool Mode

0 0 n

Flow

1 Constant Row

Setpoint

20mUmin

Post Run: 20ml../min

Coum #2 Corf,gcration

I Change C-Olumn... I r

Actual

20mUmin

222p~

(htial): 0 rrin He @ 30 'C Oven Ou: "'1bent Pressure Ui<nown

t, C Lock Coiunvi ...

I 150 ~===========================================---l 20

3

- Oven: °C*

~ 1: ( lO i - Col.,m2 He: ml/,rin

~---~----~---~----~---~---~~---~---~----~------+O

~

' © -ij O~ r ~ 10 12 14 16

Run Time, min

_1,__ X I Iii ALS v, tves Inlets Columns ~ Detectors Events Signals Configu ration Readiness GC Calculators

,/ OvenTempOn

SO 'C

Equilibrabon Time

O.Smi"l

Actual

30'C

Maxunum Oven Temperature

290'C

!!:I Override ColurM Max: 290 •c

(Iii.al)

Ran<> 1

► Ran<> 2

*

Rale 'C/nw,

Post Run: 50 "C

Post Run Time· 0 mi1

10

10

Vu 'C

50

120

140

Hoid Tme .., fb>Tme ..,

18 20

17

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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,©i ALS Valves Inlets

FIO ·R-ont l rCD ·Badtl FID

111 Heater:

111 A,r Flowe

111 H2Fuel Flow:

111 Makeup Flow: (He)

Carrier Gas Flow Conection

Colu,m Flowe (He)

0 Columns

t'.) Coll#M + Fuel • Constant

Coll.WM + Makeup • Constant

(o Constant Makeup and Fuel Flow

Setpoint

JOO'C

400ml./mi,

30mllrni"I

25mL./mi,

3mL./mi,

Actual

JOO'C

400ml./nw,

30mUnw,

25mUrrai

_L X Signals Configuration

0 Flome

FID

I 11m Readiness GC Calculators

Subtroct &om Signal.

a (No<hino)

--' Column Compensation CLWVe 1'1 Colu,m Compensation C...-ve :2

' © i 0 ~ ~ 'P ~ _L X

2pA

ALS Valves Inlets Columns Ovon Detectors Events Signals Configuration Readiness GC Calculators

FID ·Front TCD · Back I TCD

0 Heater:

~ Reference Flow:

0 Makeup Flow: (He)

C UITVl + "1a1<ec;, C

@ Constant Makeup Flow

0 Filament

EJ Negative Polarity

Setpoint

300'C

25mUm

5ml./nw1

Actual

300'C

l OmUm

5mUm

1 (25 µV)

TCD Subtract from Signal:

Q ( Nothing)

ColUJM Compensation Curve #1

v Coll.nm Co,npensation Curve #2.

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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' © ALS ValvH



1) 0 0t:~ l~I ~. X

Inlets Columns Ov,n Configuration I

ReadinHs

Runtime Events

1~ TmefrWI)

Delete Events

Even Tw,e

·•~ v ...

=I

Oven Detectors

Dual Signal Source

F #1: Front Signal (FID)

B #2: Back Signal (TCD)

B #3: Diagnostics: Test Plot

B #4: Diagnostics: Test Plot

I Hide Dual Injection Signal Assignments I

Signal Evert Table

[ Signal Source n me. min

\01-28-2020\jiquid injection.M ... Sequences

I NMffil;H,N

liiil [rl] GC Calculators

~ 1- 1 ·- - ~1 v ... ,

=I

X Configuration Readiness GC Calculators

Data Rate / Min Peak Width Zero Save

... 50 Hz / 0.004 min . □ ~

... S Hz / 0.04 min . □ ~ ,.. lso Hz / 0.004 min . □ ... [ SO Hz / 0.004 min . □ □

Signal Event

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

. u:- c--~ 2 Te,15-2

T~eforGCUWW\O

T~e forGCU'ari'\g

T~eforGCtrainng

o,Loc-. -Souce _ v....,. . - __:]h.Melhod

• ,. Method

• ,. Melhod

Method Name

Template for GC training

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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Save Seque nce as: 7890GC Gas ~mpling

fie~: T ..-.,late for GC tranng .S

Save fie as type:

I 5equence,.s>

7890GC Gas Som

File RunControl Instrument

[ M.thods 4!J Q Terrc,iate for GC tr....,_.M

Ready

Foidef>: c: \. .. \2\seq.Jence 'be,

l~c, ~ CHEM32

~2SEOUENCE

CJ 01-29-2020 CJ 05-02-2019 CJ ll>ro-2019 CJ -2019

c-fves:

li!l c: W...OS • [ Netwo,L I

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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Sta rt 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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mailto:[email protected]



# Revised by Date Modification

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

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