Eliminating the Fear Factor

Flame Ionization Detector

Agilent Technologies

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The Flagship GCs from Agilent

8860 8890 Intuvo

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Agilent 8860/8890 Series GC Features – Detectors

• AUX 1 Detector (TOP) can be TCD or FPD+

• AUX 2 Detector (SIDE) can be TCD, FID, or ECD

YES! This means you can have up to 4 detectors on your 8890 GC or 3 detectors on your 8860 GC!

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Agilent Intuvo GC Features – Detectors

D1 Position
• FID
• TCD
• uECD
• FPD+
• NPD
• XCD D2 Position
• FID
• TCD
• uECD

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Common GC Detectors

• Flame Ionization Detector (FID)*

• Thermal Conductivity Detector (TCD)*
• Nitrogen-Phosphorous Detector (NPD)* Today’s topic is
• Electron Capture Detector (ECD) the FID!
• Flame Photometric Detector (FPD)
• Chemiluminescence Detectors (XCD)
• Mass Selective Detector (MSD)

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 GC Detectors
Let’s focus on the FID

TCD
FID
µECD
sim MSD scan

NPD (N)
NPD (P)
FPD (S)
FPD (P)

SCD
NCD
10-15 g 10-12 g 10-9 g 10-6 g 10-3 g
fg pg ng µg mg
1 ppt 1 ppb 1 ppm 0.1% %

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Flame Ionization Mechanism
+
CHO
H 20 • The FID is a
CO2
H20 +
CHO+ DESTRUCTIVE, mass
CHO
CO2 CO2 sensing detector
H20
H20 CHO
+ SELECTIVITY
CHO
+ • Cations generated in • The FID will respond to ORGANIC
the flame are counted compounds (C-H Bonds)
and produce the
detector signal • There is little or NO response for the
following:
H H
2 CH 2
• Analytes that have the • Inert Gases
4
H H • H2O
2 CH 2 greatest number of low • CO2
4
H H oxidation state carbons • CO
2 CH 2
4 produce the LARGEST • N2
H
2 CH H
2
signal • O2
4
Column • CS2
H CH
4 H • Heavily halogenated compounds
2 2
Jet
H CH H
4
2 2

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Agilent FID Theory of Operation

• H2 / Air = Flame
• Sample is burned producing
positively charged ions
• Positive Ions are attracted to
the negative voltage on the
collector
• Collector current is converted
to FID output in the
Electrometer

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FID Detector Cutaway

Ignitor
Insulators Collector

Air
Jet
H2 and Make-Up
gas

Column nut

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FID Detector Bases

• 6890/7890 GC –
Capillary optimized FID base
OR
Packed FID base with
capillary adapter included

• Intuvo GC –
Capillary optimized FID base only
-no packed column capabilities on Capillary columns Adapters are available
Intuvo only for capillary columns or
1/8” Packed Columns
• 8860/8890 GC –
Capillary optimized FID base only ¼” Packed columns
A packed column adapter is can be installed
included without an adapter

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Agilent 6890/7890/8860/8890/Intuvo FID Jets

Adaptable FID Jets – 6890/7890

Jet Type Part# Jet Tip ID
0.29 mm
Capillary 19244-80560
0.011 in.
0.47 mm Intuvo/8860/8890 FID Jet
Packed 18710-20119
0.018 in.
Jet Type Part# Jet Tip ID
0.79 mm
Packed Wide Bore 18789-80070
0.030 in. Jet G4591-20320 0.011 in.
0.47 mm
High Temp G1531-80620
0.018 in.

Capillary-Optimized FID Jets – Agilent’s NEW

6890/7890 FID Jet Design!
Jet Type Part# Jet Tip ID
Backwards
0.29 mm
Capillary G1531-80560
0.011 in.
Compatible back
to 6890 GC
0.47 mm
High Temp G1531-80620
0.018 in.

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FID Setup - Column Installation - FID

Column Installation – From Troubleshooting and Maintenance Manuals

Capillary Optimized FID Adaptable FID

01m 0 20 30 40 50

m0 10 20 30 40 50 60 70
4
8
m
m
6
8
m
m 1
m
m

General Rule:
Push column up to inside the tip
of the jet and then pull back 1 mm

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FID – Optimizing Gas Flows for Sensitivity

O
p
t
i
mu
mh
y
d
r
og
e
nf
l
ow
ra
t
e
ve
rs
u
s
ca
r
r
ie
r
f
lo
wr
a
t
e
5
0 Gas Flow Guidelines:
Hydrogen Flow (ml/min or kPa)
(
1
56
)
Hydrogen 30-35 ml/minute
4
0

(
1
32
)
Carrier + Makeup 30-35 ml/minute
Air – 400 ml/minute
3
0

(
1
07
) Nitrogen is the recommended makeup gas

2
0
H2-to-Air ratio should be between 8-12%
(
7
5)

2
0 3
0 4
0 5
0 6
0
Total Inert Gas should have ~1:1 ratio to H2
C
a
r
r
i
er
Fl
o
w (
N
2)
,m
l
/
mi
n

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FID Makeup Gas Modes
Method Editor Menu in Software

AKA: Column + Fuel = Constant

Select if using Hydrogen Carrier
The detector sees Constant Hydrogen Flow if carrier flow changes.
AKA: Column + Makeup = Constant
Best for Column – “Constant Pressure” Mode
Makeup is ramped during the run to compensate for dropping
carrier flow – Detector sees constant Column + Makeup flow
AKA: Constant Makeup & Fuel Flow
Best for “Constant Flow” mode on the Column (He or N2)
Makeup Gas and Hydrogen Control are independent of the Carrier
and remain constant throughout the analysis

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FID – Tips and Tricks

• It is best to operate the FID at 300oC or hotter – But always 20oC hotter than the highest
GC Oven Temp
Gas Flow Guidelines:

• Optimizing Flows 1:1 ratio of Carrier + Makeup to H2 flow Hydrogen 30-35 ml/minute

• Nitrogen is the recommended makeup gas Carrier + Makeup 30-35 ml/minute (≈1:1 ratio to H2)
Air – 400 ml/minute

• Make sure you check the base of the FID for any chunks of graphite when changing the column or
jet to prevent those chunks from getting into the jet and causing a partial blockage

• Check your Lit Offset. Default is 2pA and sometimes with very clean gases the baseline will drop
below 2pA causing your GC to think the flame is not it.

• Use the right jet for your application

• High oven temps, bleeding columns, or clogging jets often – try the High Temp FID Jet

Wider opening to help prevent clogging

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FID Troubleshooting
Flame Won’t Light - Jet Diagnostic Test – 7890 Series GC

Pass Fail
• Set H2 Flow to 75 ml/minute
• Turn the Makeup Gas “OFF”
• Monitor Makeup Gas “Actual Flow”
➢ Low flow reading/minimal change – Jet is clear!
➢ High Flow reading/big change - indicates Jet Plugging…

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FID Jet Restriction Test – How does it Work?
H2 Makeup Air

Plugged Jet Tip

Makeup and H2
Flows

• Turn Makeup Gas Off

• Set H2 to 75 ml/minute
• Monitor Makeup Gas -

An increase in the Makeup Gas flow reading indicates pressure backing up from the jet

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Jet Diagnostic – Built into 8860/8890/Intuvo GC

Now the GC has the ability to run the Jet Restriction test from the front panel and generate a pass or fail.

A quick, easy, un-intrusive test

that can be run from the GC or
the browser interface.

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FID Troubleshooting
Baseline Spiking

Possible Causes:
• Contamination of the jet, collector, and/or the base by particulates, stationary phase, graphite
- Clean and Sonicate or Replace the Jet
- Thoroughly clean the collector and chimney assembly
- Thoroughly clean the base of the FID – especially if ferrule chunks are visible

• Electronic Noise – much less likely

- Vibration
- Electrical – Grounding problems, Power line disturbances, Power Line conditioners
- Strong RF Interference

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#19
FID Troubleshooting
Baseline Drift and Wander

New!
Smart
Gas Clean
Sensor

Possible Causes:
• Contaminated/Saturated Gas Supply Traps
• Buildup of high MW sample contamination in the GC Column
• Column Bleed
• Contamination in the Base of the Detector
• Gas Leaks
• Column Fitting Leaks

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Baseline Evaluation – Intelligent GCs

• Blank Evaluation allows

you to set up expected
signal levels at the start
and end of the run and
confirms they are as
expected.

• When you run a blank,

your smart GC monitors
the blank and returns
either a log entry if the
blank is not blank, or
stops the sequence.

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FID Troubleshooting
Measuring Flows

Gather your flowmeter and adapter tube first!

• Set oven temp to Ambient (35C)
• Turn off column flow
• Shut off all detector gases
• Turn off FID flame
• Cool detector
• Connect adapter to detector by inserting into
FID as far as possible
• Turn on one detector flow at a time allowing the
gas to equilibrate in the flowmeter tubing before
taking a measurement

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FID Maintenance

Cleaning Kit: G1531-67000

Includes Small Parts:
• Teflon Collector Insulators
• Silicone Rubber Base Gasket
• Ignitor
• Cleaning brushes for Collector
Rebuilding Kit: G1531-67001 • Cleaning Wires for Jet
Entire Collector Assembly for
Extremely corrosive applications

Note: The FID Jet must always be ordered separately

Now let’s step through a complete FID

Maintenance/Rebuild Procedure together!

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FID Maintenance Procedures
Ignitor Replacement

Disconnect the Ignitor

Remove with 5/16” wrench

Install the new Ignitor with

Copper Washer –
Tighten with 5/16” wrench

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FID Maintenance Procedures
Collector Removal

Loosen 3-T20 Screws

A common mistake people make is NOT removing the three screws
FIRST. This makes getting to the jet quite difficult and you can damage the
interconnect assembly and spring. Make sure you remove the screws first.

Pull the Collector Assembly straight up

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FID Maintenance Procedures
Collector Disassembly and Cleaning

Unscrew the knurled nut Remove the castle

Remove/replace the
Remove the collector and silicone rubber gasket
Upper/lower PTFE Insulators
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FID Maintenance Procedures
Jet Removal, Collector Removed

Using a ¼” Nut Driver,

FID Jet Loosen the Jet

Remove the Jet

Be careful not to damage the

Interconnect Spring

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FID Maintenance Procedures
Check for Graphite Chunks in the Detector Base
Indicator ….Was the Column hard to remove or to re-install?

Shine a flashlight up
From the oven to check Look for graphite chunks
For impacted graphite Clean out the Detector Base – Top down falling into the oven
A syringe plunger works well

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FID Maintenance Procedures
Jet Cleaning or Replacement

Jet sealing surface – if this is

Compromised, replace the jet

If the jet is plugged you can clean

with a .010” cleaning wire
Agilent recommends
Jet Cleaning Wire (0.010”) 9301-0985
replacing the Jet

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FID Maintenance Procedures
Jet Installation

FID Jet
Interconnect
Spring

Using a ¼” Nut Driver,

Tighten the FID Jet 1/6th of
A turn past Hand Tight
(For a New Jet only)

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FID Maintenance Procedures
Re-install the Collector

Position the cleaned or replacement collector

directly over the detector base and push
straight down.
The interconnect spring will “pop” into place!

Tighten 3-T20 Screws evenly and firmly

Re-connect Ignitor electrical cable

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Intelligent GC Features – Self Guided Maintenance

These on-board
procedures take you
through common
maintenance operations,
guiding you step-by-step,
cooling the instrument
zones that are necessary,
and even updating logs
and EMF counters when
finished!

These are accessed by

way of the “perform
maintenance” link in the
maintenance tab.

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 For more information regarding Agilent’s Gas Chromatography, please visit the website at:
https://www.agilent.com/en/products/gas-chromatography

Videos for Simple Maintenance and Theory can be found on the Agilent YouTube page:
https://www.youtube.com/user/agilent/

Checkout Agilent Communities where you can get answers and share insights:
https://community.agilent.com/welcome

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A Sample of Customer Education Courses – GC

e-Learning Agilent University Course Code Course Name

GC-MULTI-2100e Advanced Operation of the Multi Mode Inlet (MMI)

GC-0GEN-1012s GC Inlets Theory and Operation

GC-0GEN-1013s GC Detectors Theory and Operation

SI-7696-1100s Agilent 7696A Sample Prep WorkBench Operation

GC-MULTI-1240zs Making Productivity Happen: an Agilent GC eLearning Series

SI-7693-1100s Agilent 7693A ALS Basic and Advanced Operation and Maintenance

SI-7697-2100fs Running Start for Agilent 7697A Headspace Sampler

Classroom Agilent University Course Code Course Name

GC-0GEN-2000V2 Practical Gas Chromatography – 4 Day (R1915A)

GC-7890-2100cV4 Agilent 7890A/B GC and OpenLAB ChemStation Operation – 5 Day (R1778A)

GC-7890-2200cV3 Agilent 7890A/B GC Maintenance & Troubleshooting – 4 Day (R1914A)

GC-9000-2101cV3 Agilent 7890/9000 GC with OpenLAB 2.3 Essential and Advanced Operation – 4 Days

GC-9000-2103c Agilent Intuvo 9000 GC with OpenLAB CDS ChemStation Operation – 4 Days

GC-8890-2100c Agilent 8890 GC Operation with OpenLAB CDS ChemStation Edition – 4 Days

Enroll at Agilent University: http://www.agilent.com/crosslab/university/

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