GC Detector

Detectors
In This Section, You Will Learn:

Identifying the most common GC detectors used Identifying detector response characteristics Identifying the operational consideration of the TCD Identifying the operational considerations of the FID Comparing the response of the TCD and FID detectors
GC Detector: A Definition
A GC Detector is a device which senses the presence of a component different from the carrier gas, and converts that information to an electrical signal. Thermal Conductivity Detector (TCD) Flame Ionization Detector (FID) Electron Capture Detector (ECD) Nitrogen Phosphorus Detector (NPD) Flame Photometric Detector (FPD) Electrolytic Conductivity Detector (ELCD, HALL) Photoionization Detector (PID) Mass Selective Detector (MSD) Infrared Detector (IRD) Atomic Emission Detector (AED)
Detector Response Characteristics
Sensitivity:
The response per amount of sample, that is, the slope of the response/amount curve. The minimum amount on the curve is defined as the minimum detectable level (MDL). A measure of which categories of compounds will give a detector response.
Selectivity:
Dynamic Range: The range of sample concentrations for which the detector can provide accurate quantitation.
Comparison Of GC Detectors
TCD FID ECD AED PID NPD (N) NPD (P) FPD (S) MSD ELCD ELCD 10-15 fg pptrillion 10-12 pg ppb 1 ppm = (SIM) (X) (S or N) 10-9 ng ppm 1 ng 1 L = 10-6 g ppthousand 1 mg Liter = 10-3 mg percent 1 L Liter (SCAN) IRD
Increased Sensitivity With Capillary Columns
Packed Columns Area = 2600 Height = 5 Noise = 1
Capillary Columns Area = 2600 Height = 10 Noise = 1 Sensitivity = Signal/Noise Ratio
S/N = 5
S/N = 10
Capillary Columns and Detector Selectivity
FID
ECD
NPD (P)
Dynamic Range
Dynamic range is a measure of response vs. Quantity Response is the signal produced by the sample.
Dynamic Range Response increases reproducibly with increased quantity.
Response
Quantity
Linear Dynamic Range Response increases proportionally with increased quantity. Response
Quantity
Non-linear response, as long as it is reproducible, can be dealt with using non-linear calibration techniques.
8
Operating Conditions For Detectors

Sensitivity Range
Detector
Typical Samples
Gas Flow Rates (mL/min.) Carrier + Make-up Hydrogen 30-40 n.a. n.a. Air 200-500 n.a. n.a.
FID TCD ECD
Hydrocarbons Anything other than carrier gas Organohalogens Chlorinated solvents & pesticides Organonitrogen & Organophosphorus
10-100 pg 10 ppb-99%
20-60
5-100 ng 15-30 10 ppm-100% 0.05-1 pg 30-60 50 ppy-1 oom 0.1-10 pg 20-40
NPD
1-5
70-100
Thermal Conductivity Detector
The TCD is a nondestructive concentration sensing detector. A heated filament is cooled by the flow of carrier gas.
FLOW
When the carrier gas is contaminated by sample, the amount of cooling changes. The difference in cooling is used to generate the detector signal.
10
Single Filament TCD
COLUMN flow enters the center of three ports. AUXILLARY, or make-up flow sheathes the column minimizing diffusion at the end of the column. REFERENCE flow is directed to either one of the outside ports into the detector cell. Which port is determined by the SWITCHING SOLENOID.
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Selecting the Reference Gas Flow Rate
12
Operating the TCD

Recommended Flow Rates
Gas Type Carrier Gas (hydrogen, helium, nitrogen) Reference (same gas type as carrier) Capillary Makeup (same gas type as carrier) Flow Range Packed, 10-60 mL/min. Capillary, 1-5 mL/min. 15-60 mL/min. See previous page to select value. 5-15 mL/min. capillary columns 2-3 mL/min. packed columns
Recommended Detector Temperature If < 150 C, cannot turn on filament. 150 C to 200C - filament is at low setting >/= 200 C - filament is at high setting. Detector temp should be 30 - 50 C > highest oven temp.
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Typical Pressure/Flow Relationships
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TCD Troubleshooting/Maintenance
Check Pressures/Flows Thermal Cleaning:
TCD can become contaminated with deposits from column bleed or dirty samples. Symptoms include:
wandering baseline increased noise level changes in response of reference sample
Replace the detector.
15
Flame Ionization Detector Schematic
Air Inlet Capillary Column End-Position (1-2 mm from Top of Jet) H2 Inlet + Make-Up
FID Detector Assembly
Jet
Exit End of Column

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Flame Ionization Detector

+ CHO H0 2 + CHO CO 2 H0 2 H0 2 CO 2 H0 2 CHO+ + CHO CO 2 + CHO
2 2
H CH CH CH CH CH 4
2 2
The FID is a destructive, mass sensing detector. Cations generated in the flame are counted and produce the detector signal. Analytes that have the greatest number of low oxidation state carbons produce the largest signal.
H H H H H
H 4 H 4 4 4 4 H H H
2 2 2
2 2
Column
2 2
CH 2
Jet
17
Compounds with Little or No FID Response
Rare Gasses Nitrogen Oxides Silicon Halides H2O Perhalogenated cpds
NH3 H2 CO CO2
CS2 COS O2 N2
HCOH HCOOH
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FID Response
en To
10
lu
ol
io n
Fo
H H C H OH H
rm
Ac id Ac et ic
ic
H C H
H C H OH H
M et ha no l Et ha n
Pr op
Relative Response (by wt.)
ic
ta n
an o
ex
ic
H C H
H C H
ol Bu
H C H
H C H OH
Methanol
Ethanol
Butanol
Response is proportional to the number of carbon-hydrogen bonds.

19
ex
an o
FID Variables
Kr
Carrier Gas Selection Sensitivity vs. MW of Gas
Ar He
N2
Gas (mw)
Sensitivity vs. Hydrogen Flow (Carrier Gas and2Air Held Constant)
H2 Flow
Sensitivity vs. Air Flow (Carrier Gas and Hydrogen Flow Held Constant)
Air Flow
20
FID Pneumatics (EPC)
21
Operating the FID

Recommended Flow Rates
Gas Type Carrier Gas (hydrogen, helium, nitrogen) Packed Columns Capillary Columns Detector Gasses Hydrogen Air Column plus Capillary Makeup 10-60 mL/min. 1-5 mL/min. 24-60 mL/min. 40 mL/min. Flow Range Suggested Flow
200-600 mL/min. 450 mL/min. 10-60 mL/min. 50 mL/min.
Recommended Detector Temperature If < 150 C, flame will not light. Detector temp should be 20 C > higher than oven temp.
22
Typical Pressure/Flow Relationships for the FID
23
FID Exploded View
24
FID Jet Selection

Jets for the Capillary-Optimized FID
Jet Type Capillary High-Temp (use with simulated distillation) Part No. G1531-80560 G1531-80620 Jet Tip I.D. 0.29 mm (0.011 in.) 0.47 mm (0.018 in.)
Jets for the Adaptable FID

Jet Type Capillary Packed Packed Wide-Bore (use with high-bleed applications) High-Temperature (use with simulated distillation) Part No. 19244-80560 18710-20119 18789-80070 Jet Tip I.D. 0.29 mm (0.011 in.) 0.47 mm (0.018 in.) 0.030 in.
19244-80620
0.47 mm (0.018 in.)

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FID Troubleshooting and Maintenance

Typical Problems
Flame Out Spiking Low Sensitivity Noise Drift
FID Troubleshooting
Check Pressures/Flows Check Background signal Inspect Flame Check Electrometer Connections (spring) Check O-Rings
FID Maintenance
Clean or replace the jet Clean the collector Replace the igniter assembly
26
Lab Exercises
The Students should perform the following lab exercises: Lab 1: Lab 2: Thermal Conductivity Detector Performance Flame Ionization Detector Performance
27

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Detectors

In This Section, You Will Learn:

Detector Response Characteristics

Increased Sensitivity With Capillary Columns

Packed Columns Area = 2600 Height = 5 Noise = 1

Capillary Columns Area = 2600 Height = 10 Noise = 1 Sensitivity = Signal/Noise Ratio

Capillary Columns and Detector Selectivity

Operating Conditions For Detectors

FID TCD ECD

5-100 ng 15-30 10 ppm-100% 0.05-1 pg 30-60 50 ppy-1 oom 0.1-10 pg 20-40

Thermal Conductivity Detector

Single Filament TCD

Selecting the Reference Gas Flow Rate

Operating the TCD

Typical Pressure/Flow Relationships

Replace the detector.

Flame Ionization Detector Schematic

FID Detector Assembly

Exit End of Column

Flame Ionization Detector

Compounds with Little or No FID Response

Rare Gasses Nitrogen Oxides Silicon Halides H2O Perhalogenated cpds

Relative Response (by wt.)

Response is proportional to the number of carbon-hydrogen bonds.

Carrier Gas Selection Sensitivity vs. MW of Gas

Sensitivity vs. Hydrogen Flow (Carrier Gas and2Air Held Constant)

FID Pneumatics (EPC)

Operating the FID

200-600 mL/min. 450 mL/min. 10-60 mL/min. 50 mL/min.

Typical Pressure/Flow Relationships for the FID

FID Exploded View

FID Jet Selection

Jets for the Adaptable FID

0.47 mm (0.018 in.)

FID Troubleshooting and Maintenance

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