Solvent Expansion Calculation

101
Split Flow Diagram: Liner Overload
(SEPTUM)
PURGE VENT
TOTAL FLOW

= CARRIER GAS SPLIT VENT

= SAMPLE MOLECULES
= SOLVENT MOLECULES
(INLET)
PURGE
VALVE

A large injection of a solvent with a large

expansion volume can cause an overload of
the injection port liner.

This can result in loss of sample out the PURGE

VENT as well as contamination of the incoming
carrier gas line.

COLUMN

102
Injection Processes

• Reduce residence time by raising inlet pressure:

For a 900µuL Liner:
15 psi = 0.6 mL/min = 1.5 minutes
60 psi = 3.0 mL/min = 0.3 minutes
• Increase Injection Volume
EXPANSION = 22,400 x A x C x 15/( P + 15)

For Methanol:
A = .79 / 32
C = ( 275 + 273)/273 = 2
At 15 psi Head Pressure:
Expansion = 555
At 60 psi Head Pressure:
Expansion = 222
103
Pressure In GC

• Higher pressures will always improve GC results.

• At higher pressures, there is less residence time of analytes on

surfaces (liners, columns and gold seals) which will enhance the
symmetry and efficiency of peak shapes.

104
Various Capillary Liners

105
Split/Delayed Split Liners
Syringe In

deactivated, low pres drop, 870uL split 5183-4647

deactivated, 900uL splitless 5181-3316

deactivated, 2mm ID, 250uL direct 5181-8818

general purpose, 870uL split/splitless 5183-4711

deactivated, 900uL splitless 5062-3587

deactivated, 800uL splitless 5181-3315

1.5mm ID, 140uL direct 18740-80200

2mm ID, 250uL direct 18740-80220

4mm ID, glass wool, 990uL split 19251-60540

empty pin & cup, 800uL split manual 18740-80190

packed pin & cup, 800uL split manual 18740-60840

Column Out
106
Delayed Split Injection

107
Delayed Split Injection

108
Delayed Split Injection

109
 Delayed Split Flow Diagram
• Purge valve closed during injection (No split vent flow).
• At a specified time after injection, the purge valve opens to sweep remaining
vapors out of inlet .

110
When To Use Delayed Split Injections

For delayed split (splitless) injection, a conventional split injector is operated in

a non-splitting mode by closing the split valve during injection for only a few
seconds. The sample is flash-vaporized in the liner, and sample vapors are
carried into the column by the carrier gas where they are recondensed at
temperatures below the boiling point of the solvent. After most of the sample
has been transferred into the column, vapors remaining in the liner are cleared
by opening the split vent which remains open from that point on for the duration
of the run.

The most important benefit of delayed split injection is that a majority of the
injected sample is introduced into the column; this results in much higher
sensitivity than can be normally achieved using split injection. Delayed split
injection is routinely used in areas such as environmental analysis, pesticide
monitoring of foods, and drug screening where low levels (low ppm levels) of
target analytes need to be detected. In certain applications, sample clean up
may be necessary since more “raw” sample is introduced into the column. So
column protection becomes as important as sensitivity.

111
Delayed Split Mode Problems
Several of the problems with split inlets have parallels for
splitless inlets. These include peak shape distortions due 1
to poor column installation techniques and liner/gold seal
1
contaminations. Liner volume overload can occur more 91 2
4
easily due to more sample being present longer in the 1
5 67 1
inlet. Leaks will also plague the inlets when in splitless 8
0
mode.
Unique to delayed split injections are problems
associated with improper purge times (when split flows
are initiated) and incorrect initial oven temperatures that
are at or not below the boiling point of the solvent. The
optimum purge times and purge (split) flows need to
always be experimentally verified for the sample that is
being analyzed. The chromatograms on the right show
the results for no purging at all (above) and the purge flow
being turned on at 0.75 minutes (below).
Since more of the sample is introduced into the inlet for
longer periods of time during delayed split injections,
overall inlet contamination effects are going to be more
severe. This also can cause column overloading. Column
overload peak shapes are very conspicuous, exhibiting
front tails (also called shark fin shapes). This is shown on
the next chromatogram. Such peak shapes seriously
compromise integration as well as reproducibility.

112
 Flow versus Temperature
• One physical property of gases is that their viscosity
increases with and increase in temperature. This has a
number of effects on gas chromatography.
• For isothermal analyses all inlet flows should be set with the
column at the analysis temperature. If the flows are set at a
lower temperature and then the temperature is raised to the
analysis temperature the column flow will be decreased,
which can alter resolution, run time, and ultimately
precision. For split injections reducing column flow will
also increase split vent flow, altering the split ratio.
• For temperature programmed analyses the variation in
column flow with temperature means linear velocity cannot
be optimized through the entire run if the inlet is set in the
constant pressure mode. The column flow will decrease
with elevated oven temperature.
• The new generation of GC’s allows a constant flow setting,
which compensates for this.

113
 Changes in Column Flow versus Temperature

Carrier Gas: Helium

Outlet Pressure: 1 atm
20 2
Column Flow A, mL/min

Column Flow B, mL/min

15 1.5
Column A, 15 m x 0.53 mm, 5.3
psi Inlet Pressure
10 1
Column B, 30 m x 0.25 mm, 12
psi Inlet Pressure
5 0.5

0 0
0 50 100 150 200 250 300 350 400
Temperature degrees C

114
Operating Modes For EPC Systems

• Older generation GC’s operated only at constant pressure.

• Newer GC’s like the 6890 and 7890 can now operate with
constant flow as well.

• The user can now also utilize pressure programming. This may
or may not establish a constant flow mode. This is typically
used with isothermal column oven conditions.

115
Improvements to the Capillary Split/Delayed Split
Inlet for the 7890

116
6890’s Insert Weldment Assembly

• Inlet tubing on the left-hand side.

• Screw cap design to seal the liner
“O” ring.
• Requires inlet wrench.
• Special care to avoid breaking liner.

117
Now Easier Access to the Inlet

118
7890A Insert Weldment

• Inlet tubing on the right-hand side.

• Twist the locking tab to access the
liner and o-ring. No wrench
required at safe temperatures.
• No guessing about how tight to
prevent a leak.
• No more broken liners.

119
Benefit of Septum Purge

• Septum purge prevents

Cap off the
septa volatiles from getting septum purge. S/SL inlet
into the column.
FID detector
• Used in 4 inlets: SSL, COC,
and PTV.
Turn on the
septum purge.

120
6890 Septum Purge
Vent to atmosphere
Septum purge
gas
mechanical forward fixed resistor
pressure regulator (fixed)

• Fixed septum purge flow =

~3mL/min.
• Fixed flow rate implemented with a
restrictor.
• Vented to atmosphere.
• Flow will vary with atmospheric
pressure.

121
 New 7890A Version
Split Carrier Supply
Septum Purge

EPC Module
Frit Frit
Valve Valve Valve
PS
FS
PS

Septum
PS = Pressure Sensor
FS = Flow Sensor

Split vent trap Inlet Weldment

• Control the septum purge flow. Ferrule

• Design includes:
– a proportional valve
– a pressure sensor Column

– a fixed restrictor

122
 Septum Purge
Design includes:

EPC Module

Vent Frit
Valve
Proportional valve
PS

Septum

Pressure sensor

123
Control the Septum Purge Flow

• The default value is 3 mL/min.

• For all inlets the range is 0 to 30
mL/min.

124
Program the Septum Purge Flow

• New item in Run Time Event list.

• You can program it from the
keyboard using the Run Time
Table.

125
The Heart of a GC – The Column

126
Things to Know: Typical Capillary Column

127
Separation is a Partitioning Process

128
Capillary Columns

129
Separation Mechanisms

Applies to 90% of applications:

• Separation by partitioning or differential solubility in stationary phase.

• Components are separated based upon differences in polarity
(interaction of dipole forces).

Generally:
Like dissolves like
or
Polar interacts with polar

Example: Alcohols are polar.

Carbowax is polar liquid phase.

130
Cause – Analyte Polarity

131
Packed GC Columns

132
Column Separation Characteristics

Efficiency: Ability of the column to produce sharp peaks.

Resolution: Ability of the column to separate two peaks from
each other.
Selectivity: Ability of the column to determine chemical and/or
physical difference in two peaks.

GOOD GOOD
POOR POOR
133
Capillary Column Efficiencies

134
Calculating Efficiency

We would like to know the actual time the

Solute component spends in the stationary phase.

t ' 2
t ' = t - t n = 5.545 R
Start R R m
Wh

Inert Gas t R ' = Corrected Retention Time.

tm t 'R Time
tR n = effective theoretical
plates.
Let's relate “n” to the length of the column.
n
Plates per meter (N) = or
L
L
Height equivalent to a theoretical plate (HETP) =
n

Thus, the more efficient the column, the bigger

the "N" the smaller the "HETP“.

135
Measuring Linear Velocity and Flow Rate

column length (cm)

Linear Velocity =
Retention time of inert gas (sec)

Estimate the column length by using the formula Length = Πdk

where d = the diameter ( in meters) across the cage holding the
column k = the number of turns of the column on the cage
Π = 3.14.

The retention time of an inert gas can be estimated by:

• Using the retention of the solvent if it is the first component that elutes.
• Injecting 100 ul of methane and using the retention time using gas standards that
can be purchased (i.e. 100 ppm methane in helium).

136
 Efficiency & Carrier Gas Linear Velocity

• Efficiency is a function of the carrier

B
HETP = A + +Cμ gas linear velocity or flow rate.
μ

• The minimum of the curve represents

the smallest HETP (or largest plates
HETP

per meter) and thus the best

MOLECULAR
DIFFUSION
B{
}C RESISTANCE TO MASS TRANSFER
efficiency. "A" term is not present
for capillary columns.
} A EDDY DIFFUSION

μ ( opt μ)

• Plot of HETP versus linear velocity is know as the Van Deemter

plot.
• The linear velocity value at the minimum of the curve is the
optimum value for achieving the best efficiency.

137
Optimum Flow Rate

Generally the following guidelines may be used for finding the

optimum values for a particular column:
Optimum Carrier Optimum Carrier
Column Diameter Flow Rate Linear Velocity
1/
4” 50-60 ml/min. 2.6-3.2 cm/sec.

1/
8” 20-30 ml/min. 4.2-6.3 cm/sec.

Capillary Column
HP Series 530 (megabore) 3-5 ml/min. 22-38 cm/sec.

0.320 mm (wide bore) 1-3 ml/min. 20-41 cm/sec.

0.200 mm (narrow bore) .5-1 ml/min. 21-32 cm/sec.

0.100 mm (high speed) .2-.5 ml/min. 42-106cm/sec.

138
How To Improve Column Efficiency

1. Use smaller diameter column.

2. Use a lower % or thinner film of stationary phase.
3. Use smaller sample size.
4. Use longer column.
5. Use faster temperature programming.

139
For Capillary Columns:

140
Comparison of Columns of Different
Dimensions

141
Isothermal vs. Temperature Programming

142
Column Temperature Operation

• Isothermal:
– Oven is maintained at a constant temperature throughout the analysis.
– Stop time is set with the initial time.
– Rate is set to zero.
– Excessive broadening of later eluting peaks.

• Temperature Programmed:
– Used when components have a wide range of boiling points (>100°).
– Reduces analysis time and produces sharper peaks.
– Increased column bleed causing baseline drift.
– Can have Multiple Ramps.
– 6890 can "Fast Ramp" up to 120°/min. at temperatures between 50°C
and 70°C. Even at temperatures above 300C, ramp rates are 35C/min.

143
Peak Efficiency

144
 Resolution

• Resolution is a measure of the

RT = 4.41
ability of a column to separate two

RT = 4.59

RT = 5.10
6.0E5 peaks.
• Resolution is measured in terms of
5.0E5
two adjacent peaks which we want
4.0E5
to separate. Generally, the most
Abundance

difficult pair is chosen; if these can

3.0E5 be pulled apart successfully then all
of the others will be resolved as
2.0E5
well.
1.18 ( RT - RT1 )
1.0E5 2
R= (W + W )
1 2
4 4.5 5 5.5 6

R = 1.5 Results in Baseline Separation

Time ( Min.)

145
Decreasing Run Time

Column Parameters: Instrument Parameters:

• Shorter column length • Different carrier gas

• Smaller column i.d. • Faster temp program rate
• Thinner liquid phase • Higher Temp Isothermal analysis
• Higher carrier gas flow rate

146
Using Fast GC
toluene
C8 C9 plus aromatics
aromatics
0.32 mm i.d., helium
benzene
0.5탅, 200/1

naphthalenes

5 min 18.2 min

0.10 mm i.d., hydrogen

0.1탅, 800/1

1.2 min 3.5 min

147
Using Fast GC: Constant Pressure
70C at 17C-min to 170C, 15psi

C14,15,16 in hexane
FID2 B, (JML\SIG20151.D)

1.059
1.072
1.120

6.065
pA

6.890
Conventional GC
800

700
Parameters (i.e. slow
temperature program, long
column, low column

7.891
600

pressure/flow)
500

With ample resolution

400

300 being present, considerable

adjustments can be made R=14.3 R=18.7
200
to speed up the analysis.

6.770
1.177

5.815
0.998

100

1 2 3 4 5 6 7 8 min

HP5 30m x 0.32mm ID x 0.25um 148

Using Fast GC: DB-5 (15 meter x0.25 mm ID, 0.25 um)
210C, 65 psi, 12.5 ml/min, 186 cm/sec

FID2 B, (PITTCON\PITTCO12.D)
pA
C14,C15,C16 in hexane

9
21
0.
700
Less than 17 seconds

43
2
0.
600

8
27
0.
500

R=4.3
400

Even with the

augmented linear
300

velocity, resolution 200

factors remain better

than baseline resolved. 100
0. 0
2
19
20
0.

0.2 0.3 0.4 0.5

149
Using Fast GC: DB-5 (15 meter x0.25 mm ID, 0.25 um)
210C, 87 psi, 20.6 ml/min, 243 cm/sec

FID2 B, (PITTCON\PITTCO14.D)
pA

72
1000

1
0.
C14,C15,C16 in hexane

0
19
0.
Less than 13 seconds
800

7
21
0.
At higher pressures 600

(and consequently
higher column flows
and linear velocities),
R=5.8
400
good resolution is
maintained and in
fact, improved.
200

8
15
0.

0.2 150
 Type of Carrier Gas Effect on Efficiency and
Resolution

HETP C17 at 175º C Nitrogen Helium Hydrogen

(mm) (58 cm/sec)
k' = 4.95
(58 cm/sec) (58 cm/sec)
1.2 N2 WCOT Column

OV-101 0.4µ
1.0
25 m x 0.25 mm
He 15 m x 0.25 mm
.8
Glass WCOT
.6 SE - 52
H2
.4 Isothermal, 150º C

.2

10 20 30 40 50 60 70 80 90
R = 1.17 R = 1.37
Average Linear Velocity (cm/sec)

Efficiency curves for a 25 m x 0.25 mm id Effect of carrier gas on the resolution of n-

WCOT column with 0.4 um of OV-101. heptadecane and pristane.

151
Reformate Gasoline

Hydrogen carrier gas speeds up analysis.

A 30m x 0.32, 0.5탆 HP-Wax

helium

0 5 10 15 min

10m x 0.10, 0.2탆 HP-Wax

B helium

0 1 2 3 4 5 min

10m x 0.10, 0.2탆 HP-Wax

C hydrogen

0 1 2 3 4 min

152
Column Selectivity

153
Considerations In Column Selection

• Phase coating
• Column diameter
• Film thickness
• Length

154
Column Polarity
Dispersion Interaction

155
Film Thickness

156
What is a GC Detector?

• A GC detector is a device that senses the presence of a

compound different from the carrier gas and converts this
information to an electrical signal.

157
Detector Types

• Flame Ionization Detector (FID).

• Thermal Conductivity Detector (TCD).
• Electron Capture Detector (ECD).
• Nitrogen-Phosphorous Detector (NPD).
• Flame Photometric Detector (FPD).
• Photo Ionization Detector (PID).
• Electrolytic Conductivity Detector (ELCD).
• Infrared Detector (IRD).
• Mass Selective Detector (MSD).

Items in red covered in this course

158
Detector Sensitivity Comparison

ELCD (S or N)

ELCD (X)

AED

TCD
FID
µECD

NPD (N)
NPD (P)

FPD (S)
PID

IRD
(SIM) (SCAN)
MSD

Sensitivity 10-15 10-12 10-9 10-6 10-3

fg pg ng ug mg
1 ppt 1 ppb 1 ppm 0.1% 100%
159
Flame Ionization Detector (FID)

• FID Theory of Operations.

• FID Hardware Identification.

• FID Maintenance and Troubleshooting.

160
7890 Flame Ionization Detector
Theory of Operation

• H2 – Air Flame
• Sample is burned in
flame.
• Charged Ions
produced.
• Ions attracted to
collector.
• Collector current
converted to output
via Electrometer.

161
FID Detector Cutaway
Igniter

Insulators Collector

Air
Jet

H2 and Make-Up gas

Column nut
162
FID Response/Selectivity CHO+
CO2 He H2O
N2 CHO+ N2
CHO+
CHO+ He CO2
H2O CHO+
N2
Air N2 He Air
He

N2 He H2
Air FID air supply CH
H2 He 4
CH4 Methane in sample N2 N2
He
CHO+ Methyl cations H2 H2
CH4
H2 FID hydrogen N2 N2
He
He Carrier gas H2 H2
CH4
H2O Water N2 N2
He
N2 Makeup gas H2 H2
CH4

H2 and Makeup H2 and Makeup

Carrier and Sample 163

7890 Flame Ionization Detector

Compounds with little or no FID

response
Rare Gases NH3 CS2
Nitrogen Oxides H2 COS

Silicon Halides CO O2

H2O CO2 N2
Perhalogenated HCOH HCOOH
compounds

164
7890 Flame Ionization Detector

• Dynamic Range 1 x 107.

• Sensitivity 10 to 100 picograms of an organic sample

dependent on the molecular structure.

• Selectivity Responds to all organic compounds with H-C

bond except those that do not burn or ionize in
the H2- Air flame.

• Little or no Response H2O, CO, CO2, N2, O2, CS2, COS, NH3, and all
inert gases. Formaldehyde and heavily
halogenated compounds give little response.

165
7890 Flame Ionization Detector Jets
Adaptable FID Jets
Jet Type Part# Jet Tip ID

0.29 mm
Capillary 19244-80560
0.011 in.

0.47 mm
Packed 18710-20119
0.018 in.
0.79 mm
Paced Wide Bore 18789-80070
0.030 in.
0.47 mm
High Temp G1531-80620
0.018 in.

Capillary-Optimized FID Jets

Jet Type Part# Jet Tip ID
0.29 mm
Capillary G1531-80560
0.011 in.

0.47 mm
High Temp G1531-80620
0.018 in.

166
FID Parameters

FRONT DET (FID)

Temp 250 250 <
H2 flow 30.0 30.0
Air flow 400.0 400.0
Mkup 30.0 30.0
Flame Off
Output 0.0

CONFIGURE FRONT DET

Mkup gas type N2 <
Lit offset 2.0
Electrometer On

167
FID Flow Rates

Gas Type Flow Range Typical Flow

30 ml/min
Packed columns 10 – 60 ml/min
Carrier (1/8” column)
Gases
(H2, He, N) 1.5 ml/min
Capillary columns 0.5 – 5 ml/min
(0.32 mm column)

Hydrogen 24 – 60 ml/min 40 ml/min

Detector
Air 200 – 600 ml/min 450 ml/min
Gases

Column + Makeup 10 – 60 ml/min 50 ml/min

168
 FID Pressure/Flow Relationships

800 80

Hydrogen Flow (ml/min)

Air Flow (ml/min)

600 60

400 40

200 20

100 200 300 400 500 20 100 150 200 250

Pressure (kPa) Pressure (kPa)

169
Exploded Parts View of the FID

170
7890 Flame Ionization Detector

171
7890 Flame Ionization Detector EPC Flow
Module

172
FID EPC Module

173
FID EPC Module Replaceable Parts

Valves
“O” Rings
Fittings
Restrictors

Valves

174
Thermal Conductivity Detector (TCD)

• TCD Theory of Operations.

• TCD Hardware Identification.

• TCD Maintenance and Troubleshooting.

175
7890 Thermal Conductivity Detector

Thermal Conductivity Values of Common Gases/Solvents.

Compound Relative Thermal Conductivity

Carbon Tetrachloride 0.05

Benzene 0.11

Hexane 0.12
Argon 0.12
Methanol 0.13
Nitrogen 0.17
Helium 1.00
Hydrogen 1.28

Thermal Conductivity Relative to Helium.

176
 Thermal Conductivity Basics
The TCD is a nondestructive, When the carrier gas is contaminated
concentration sensing detector. by sample , the cooling effect of
A heated filament is cooled by the gas changes. The difference in
the flow of carrier gas . cooling is used to generate the detector
signal.

Flow
Flow

The TCD will respond to any substance different from

the carrier gas as long as its concentration is
sufficiently high enough. 177
7890 Thermal Conductivity Detector
5 Hertz Pneumatic Switching
COLUMN flow enters the center of
three ports.

REFERENCE flow is directed to

either one of the outside ports into
the detector cell. The port entered
is determined by the SWITCHING
SOLENOID.

AUXILIARY, or make-up, flow

passes along the outside of the
column and merges with the
column flow prior to entering the
detector’s center port.

178
7890 TCD - Theory of Operation

The filament
current is set to
keep the filament
at a fixed Constant
Current
temperature above Supply
the block
temperature.

Filament

Heater/Sensor for Block

Temperature Control

Column Reference

179
7890 TCD - Theory of Operation

As a peak elutes, the

filament heats up and
the resistance
increases. - Constant
Filament drive Current
Supply
voltage is increased
to keep current
constant.

Filament

Heater/Sensor for Block

Temperature Control

Column Reference

180
 TCD Normal Flow Ratio

20 ml/min
Col + MUG
+ 30 ml/min
Reference Sample
Filament

Filament
10 ml/min Ref Reference
Reading Reading

20 ml/min
Reference 20 ml/min
Col + MUG

30 ml/min 30 ml/min
Reference 20 ml/min 20 ml/min Reference
Column + MUG Column + MUG

Signal (+ polarity) = Sample - Reference

181
 Reference Flow Too High

10 ml/min
Col + MUG
+ 24 ml/min
Reference Sample
Filament

Filament
14 ml/min Ref Reference
Reading Reading

16 ml/min 10 ml/min
Reference Col + MUG
+
6 ml/min Ref

30 ml/min 30 ml/min
Reference 10 ml/min 10 ml/min Reference
Column + MUG Column + MUG
The low column flow, relative to reference flow, causes the carrier to be diluted with reference
flow. This decrease in concentration reduces the size of the TCD signal.
182
Reference Flow Too Low
8 ml/min
Reference
+
18 ml/min 10 ml/min
Col + Col +
Reference Sample
Filament

Filament
MUG MUG
Reading Reading

10 ml/min 12 ml/min
Reference Col + MUG
+
2 ml/min
Col + MUG

10 ml/min 20 ml/min 20 ml/min 10 ml/min

Reference Column + MUG Column + MUG Reference

The loss of column flow to the bypass channel does not alter the concentration of sample
in the filament channel. Therefore, no significant change in the sample reading, but the
reference flow is contaminated with sample increasing the size of the reference reading.
183
TCD Parameters

FRONT DET (TCD)

Temp 55 Off<
Ref flow0.0 Off
Mode: Col + mkup = const
Combined flow 0.00 Off Turn Filament on and off.
Mkkup (He) 0.0 Off
Filament Off
Detector Output
Output 0.0
Neg polarity Off
1 unit = 25uV.

Set polarity to + or -.

CONFIGURE FRONT DET

Mkup/ref type He <
Set reference gas type.

184
TCD Flow Rates

Gas Type Flow Range

Carrier Packed columns 10 – 60 ml/min

Gases
(H2, He) Capillary columns 1 – 5 ml/min

Reference 15 – 60 ml/min
Detector
Gases Packed MUG 2 – 3 ml/min
(H2,He)
Capillary MUG 5 – 15ml/min

185
 Choosing Reference Flow Rate
Ratio of Ref flow to Column + MUG.
3.5

2.5

1.5

0.5
0 5 10 15 20 25 30 35 40 45 50 55 60 65 70

Column + Makeup flow (ml/min).

Column + MUG Flow = 10 ml/min.

Ref flow = 2.3 X 10 = 23 ml/min.

186
7890 TCD EPC Flow Diagram

187
7890 TCD EPC Module
Reference Gas Line.

Switching Valve.

Make Up Gas Line.

188
 7890 TCD Filament Drive - Delta T Sensor
500 ΔT 50C
400

Response Filament 300

Temp C
200
ΔT135C
100

100 200 300 400 100 200 300 400

Detector Temp (body temp) C
Detector response versus detector temperature. Filament Temperature versus Block Temperature.

189
 TCD Board
TCD Board Connections

Filament
Connections

PRT sensor
Connections

Filament nor PRT sensor wires have “polarity”, but

DO NOT swap connections between the two on the board.

190
TCD Parts Explosion

Detector Cover
Insulation
PRT Sensor
To EPC Module.
Heater/Sensor Assembly.
TCD Cell.

PRT Wires to Board.

Filament Wires to Board.
Column Adapter.

191
Thermal Conductivity Detector Cell

Filament Wires to
Detector Board.

Sensor Slot. TCD Cell

Assembly.

Heater Slot.

PRT Sensor Slot.

192
Electron Capture Detector

• ECD Theory of Operations.

• ECD Hardware Identification.

• ECD Maintenance and Troubleshooting.

193
ECD Theory of Operation

Detector Anode -
Pulse frequency increases
to maintain constant current.
Secondary Emission
of Electrons. Gas Exit.
-e
-e -e
X
N2 -e -e As electronegative
-e
X
-e -e sample enters cell -
-e
X -e free electron population
is depleted.
Ni63
Source.

Makeup Gas -
N2 or ArMe. Column - He, N2 or H2
Carrier.

194
7890 uECD Cell

Anode Purge Vent Anode

Vent
Cell

Ni63

Fused Silica Make Up Adapter.

Make Up Gas Inlet.

Column
195
7890 ECD Detector Sensitivity

Chemical type Relative Sensitivity

Hydrocarbons 1

Ethers,esters 10

Aliphatic alcohols,ketones,amines,mono-Cl,mono-F compounds 100

Mono-Br,di-Cl and di-F compounds 1000

Anhydrides and tri-Cl compounds 10^4

Mono-I,di-Br and nitro compounds 10^5

Di-I,tri-Br,poly-Cl and poly-F compounds 10^6

196
7890 µECD

197
7890 Electron Capture Detector
µECD Gas Flows

Gas Type Recommended Flow

Range
Carrier gas 30 to 60 ml/min
Packed Columns
(nitrogen or argon -
methane)
Capillary Columns 0.1 to 20 ml/min
(helium, hydrogen, depending on diameter
nitrogen or argon-methane)

Capillary makeup 10-150 ml min.

(nitrogen or argon - (30-60ml/min typical)
methane)

198
7890 µECD EPC Module

Vent

Ni63

Makeup Gas Adapter.

199
ChemStation Configuration

200