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Chromatography in the Fast Lane
Mark SinnottApplication EngineerDecember 13, 2018
1
Fast GC
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Questions to Ask
What information do you need from your analysis?
Do you have more baseline than you need between your peaks?
Do you need to resolve all of the components?
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•Stationary Phase
•Temperature Programming
•Carrier Gas: type and linear velocity
•Shorten Column Length
•Decrease Film Thickness
•Decrease Internal Diameter
Variables for Shortening Run Times
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Resolution
RN k
ks =
4 1
1
+
−
Factors effecting Rs
Efficiency N = (gas, L, rc)
Retention k = (T, df, rc)
Selectivity = (T, phase)
Variables
L Length
rc radius
df film thickness
T Temperature
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Resolution
RN k
ks =
4 1
1
+
−
Factors effecting Rs
Efficiency N = (gas, L, rc)
Retention k = (T, df, rc)
Selectivity = (T, phase)
Variables
L Length
rc radius
df film thickness
T Temperature
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Stationary Phase - Common Types
Siloxane polymers
Poly(ethylene) glycols
Porous polymers
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Selectivity
Relative spacing of the chromatographic peaks
The result of all non-polar, polarizable and polar interactions that cause a stationary phase to be more or less retentive to one analyte than another
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Optimizing Selectivity
Match analyte polarity to stationary phase polarity
-like dissolves like(oil and water don’t mix)
Take advantage of unique interactions between analyte and stationary phase functional groups
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Start with the Right Phase
Time (min.)
0 2 4 6 8 10 12 14
Time (min.)
DB-1
15m x 0.32mm, 0.25µm
Oven:
40°C for 2 min
40-120°C at 5°C/min
0 1 2 3 4 5
DB-Wax
15m, 0.32mm, 0.25µm
Oven:
80-190°C at 20°C/min
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Resolution
RN k
ks =
4 1
1
+
−
Factors effecting Rs
Efficiency N = (gas, L, rc)
Retention k = (T, df, rc)
Selectivity = (T, phase)
Variables
L Length
rc radius
df film thickness
T Temperature
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Column Length and Efficiency (Theoretical Plates)
0.25 mm IDn/m = 4630 (for k = 5)
Length (m) n
15 69,450
30 138,900
60 277,800
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Column Length and Resolution
Length X 4 = Resolution X 2
R n L
t L
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Column Length VS Resolution and Retention: Isothermal
Double the plates, double the time but not double the the resolution
15 m 60 m30 m
R=0.84
2.29 min
R=1.68
8.73 min
R=1.16
4.82 min
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BTEX
Carrier: Helium, 36 cm/sec at 40°c
Oven : 40°C for 3 min, 5°/min to 100°C
1. Benzene
2. Toluene
3. Ethylbenzene
4. m,p-Xylene
5. o-Xylene
.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.00.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 7.50 8.00 8.50 9.00
1
2 3
4
5
DB-5
30 m
0.53 mm I.D., 0.5 µm
DB-5
15 m
0.53 mm I.D., 0.5 µm
0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00 4.20 4.40 4.60 4.80 5.00 5.20 5.40 5.60 5.801.0 2.0 3.0 4.0 5.0
1 2 3
4
5
6.0
DECREASE THE LENGTH
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Column Length and Cost
15m30m
60m
$ $ $ $ $ $ $
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Length Summary
If you Decrease Length:
Efficiency Decrease
Resolution Decrease
Analysis Time Decrease
Pressure Decrease
Cost Decrease
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Resolution
RN k
ks =
4 1
1
+
−
Factors effecting Rs
Efficiency N = (gas, L, rc)
Retention k = (T, df, rc)
Selectivity = (T, phase)
Variables
L Length
rc radius
df film thickness
T Temperature
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Column Diameter - Theoretical Efficiency
I.D. (mm)
0.05
0.10
0.20
0.25
0.32
0.45
0.53
0.18
n/m
23,160
11,580
5830
4630
3660
2840
2060
6,660
30 m
20 m
10 m
k = 5
5 m
N ~ 112,000
N ~ 112,000
N ~ 112,000
N ~ 112,000
Total Plates
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Different Column I. D. Equal Phase Ratios
Time (min)0 5 10 15 20
Column : DB-62430 m, 0.32 mm, 1.8 m
Carrier:Oven: 65°CInjection: SplitDetector: FID
Helium, 40(cm/sec)
Column : DB-62430 m, 0.53 mm, 3 m
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PHASE RATIO ()Film Thickness
Column Dimensions Phase Ratio β
30 m x .53 mm x 3.0 m 44
30 m x .32 mm x 1.8 m 44
KC = k β
r2df
β =
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Column Diameter and Capacity
Like Polarity Phase/Solute0.25 µm film thickness
I.D. (mm) Capacity (ng)
0.05 1-2
0.18 25-55
0.20 35-70
0.25 80-160
0.32 110-220
0.53 1000-2000
0.45 600-800
0.10 6-13
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Column Diameter - Inlet Head Pressures (Helium)
30 metersHydrogen pressures x 1/2
I.D (mm) Pressure (psig)
0.10 90-130
0.20 25-40
0.25 15-25
0.32 10-20
0.45 3-7
0.53 2-4
0.18 30-45
0.05 275-400
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Column Diameter and Carrier Gas Flow
Lower flow rates: Smaller diameter columns
Higher flow rates: Larger diameter columns
Low flow rates : GC/MSHigh flow rates: Headspace, purge & trap
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Diameter Summary
If you decrease the inside diameter:
Efficiency Increase
Resolution Increase
Pressure Increase
Capacity Decrease
Flow rate Decrease
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Combining a change in Length with a change in Diameter
Eff
icie
nc
y
Analysis Time
Decrease Length
Decrease Diameter
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Carrier Gas ConsiderationsBest velocity?
Optimal range of velocities
Too low or high results in loss of resolution
Balance resolution and analysis time
BUT... there is no LAW against going FASTER
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60
Excessive Diffusion
Poor Mass Transfer
Carrier Gas Considerations
Van Deemter Curve
10 20 30 40 50 60
0.25
0.50
0.75
1.00
u (cm/sec)
H (
min
)
He
N2
H 2
uopt
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Carrier Gas ConsiderationsUtilizing Computer Controlled Flow Ramping (EPC)
Lonely Late Eluters? = P
Decrease retention and overall run time by increasing pressure
(speed up the gas!)
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Fast Detector Electronics – 6890 FID
200 Hz
100 Hz
50 Hz
20 Hz
10 Hz
Proper peak quantitation typically requires a minimum of 10 data points per peak
10 Hz data rate: (peaks less than one second wide will have less than 10 data points)
200 Hz data rate: (peaks as narrow as 50 msec can be handled reliably)
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Easy Options with Method Translation Software
Different Column Dimensions
Switch He to H2 Carrier Gas and Try Faster Velocities
Same Column & Gas Type but Faster Velocities
Combination of all of the above
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Temperature Programming
30m, 0.25mm ID
Temperature
10m, 0.1mm ID
Temperature
Temperature program must be modified to give same temperature of elution (i.e. faster ramps, shorter hold times)
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2 . 0 0 4 . 0 0 6 . 0 0 8 . 0 0 1 0 . 0 0 1 2 . 0 0 1 4 . 0 0 1 6 . 0 0 1 8 . 0 0
1 e + 0 7
2 e + 0 7
3 e + 0 7
4 e + 0 7
5 e + 0 7
6 e + 0 7
7 e + 0 7
8 e + 0 7
9 e + 0 7
1 e + 0 8
1 . 1 e + 0 8
1 . 2 e + 0 8
1 . 3 e + 0 8
1 . 4 e + 0 8
1 . 5 e + 0 8
1 . 6 e + 0 8
1 . 7 e + 0 8
1 . 8 e + 0 8
1 . 9 e + 0 8
T i m e
R e s p o n s e _
G C 3 - 6 7 0 7 . D \ E C D 2 B
22
21
20
19
18
17
16
1514
13
12
11
10
9
8
7
5,6
4
3
2
1
Column: DB-XLB30m x 0.32mm i.d., 0.25µm
Carrier: He, constant flow, 38 cm/s at 120°CInjector: Pulsed Splittless, 220 °C
Pulse pressure & time: 35psi for 1.15min2µL, 50ppb
Oven: 120°C for 1.17min120°C to 160°C at 25°/min160°C to 260°C at 10°/min260°C to 300°C (4min) at 15°/min
Detector: µ-ECD, 320°CAr/CH4 (P5) makeup gas at 60mL/min
<16 minutes
CLP-Pesticides - Original “Improved” Method 0.32mm I.D., Helium Carrier Gas
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Input Original Method Parameters
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New Velocity
New Temp. Program
Same Column and Gas TypeFast Analysis (OPGV)
Transfer same dimensions
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Only Time!
<14 minutes
No Real Changes in Resolution!
Same Column and Gas TypeFast Analysis (OPGV)
2 . 0 0 4 . 0 0 6 . 0 0 8 . 0 0 1 0 . 0 0 1 2 . 0 0 1 4 . 0 0 1 6 . 0 0 1 8 . 0 0
1 e + 0 7
2 e + 0 7
3 e + 0 7
4 e + 0 7
5 e + 0 7
6 e + 0 7
7 e + 0 7
8 e + 0 7
9 e + 0 7
1 e + 0 8
1 . 1 e + 0 8
1 . 2 e + 0 8
1 . 3 e + 0 8
1 . 4 e + 0 8
1 . 5 e + 0 8
1 . 6 e + 0 8
1 . 7 e + 0 8
1 . 8 e + 0 8
1 . 9 e + 0 8
T i m e
R e s p o n s e _
G C 3 - 6 7 0 7 . D \ E C D 2 B
Before
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Same Column, Hydrogen Carrier GasTranslate Only
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Same Column, H2 Carrier GasTranslate Only
33% faster!
11 minutes
No Real Changes in Resolution
2 . 0 0 4 . 0 0 6 . 0 0 8 . 0 0 1 0 . 0 0 1 2 . 0 0 1 4 . 0 0 1 6 . 0 0 1 8 . 0 0
1 e + 0 7
2 e + 0 7
3 e + 0 7
4 e + 0 7
5 e + 0 7
6 e + 0 7
7 e + 0 7
8 e + 0 7
9 e + 0 7
1 e + 0 8
1 . 1 e + 0 8
1 . 2 e + 0 8
1 . 3 e + 0 8
1 . 4 e + 0 8
1 . 5 e + 0 8
1 . 6 e + 0 8
1 . 7 e + 0 8
1 . 8 e + 0 8
1 . 9 e + 0 8
T i m e
R e s p o n s e _
G C 3 - 6 7 0 7 . D \ E C D 2 B
Before
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New Column Dimensions, H2 Gas, Translate Only
Input NEW dimensions
New Velocity
New Temp. Program
Close enough (got lucky)
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New Column Dimensions, H2 Gas, Translate Only
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10
11
5
6
New Column Dimensions, H2 Gas, Translate Only
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New Velocity
New Temp. Program
New Column Dimensions, H2 Gas, Fast Analysis
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0 . 5 0 1 . 0 0 1 . 5 0 2 . 0 0 2 . 5 0 3 . 0 0 3 . 5 0 4 . 0 0 4 . 5 0 5 . 0 0 5 . 5 0 6 . 0 0 6 . 5 0 7 . 0 0 7 . 5 0
2 0 0 0 0 0 0
3 0 0 0 0 0 0
4 0 0 0 0 0 0
5 0 0 0 0 0 0
6 0 0 0 0 0 0
7 0 0 0 0 0 0
8 0 0 0 0 0 0
9 0 0 0 0 0 0
1 e + 0 7
1 . 1 e + 0 7
1 . 2 e + 0 7
1 . 3 e + 0 7
1 . 4 e + 0 7
1 . 5 e + 0 7
1 . 6 e + 0 7
1 . 7 e + 0 7
1 . 8 e + 0 7
1 . 9 e + 0 7
2 e + 0 7
2 . 1 e + 0 7
2 . 2 e + 0 7
2 . 3 e + 0 7
2 . 4 e + 0 7
2 . 5 e + 0 7
2 . 6 e + 0 7
T i m e
R e s p o n s e _
G C 8 - 3 3 4 5 . D \ E C D 2 BNew Column Dimensions, H2 Gas, Fast Analysis
Better Resolution and Faster Analysis!
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New Column Dimensions, H2 Gas, Higher Velocities
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105 cm/sec
95 cm/sec
85 cm/sec
<6 minutes
5.5 minutes!?
New Column Dimensions, H2 Gas, Higher Velocities
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0 . 5 0 1 . 0 0 1 . 5 0 2 . 0 0 2 . 5 0 3 . 0 0 3 . 5 0 4 . 0 0 4 . 5 0 5 . 0 0 5 . 5 0 6 . 0 0 6 . 5 0 7 . 0 0
2 0 0 0 0 0 0
4 0 0 0 0 0 0
6 0 0 0 0 0 0
8 0 0 0 0 0 0
1 e + 0 7
1 . 2 e + 0 7
1 . 4 e + 0 7
1 . 6 e + 0 7
1 . 8 e + 0 7
2 e + 0 7
2 . 2 e + 0 7
2 . 4 e + 0 7
2 . 6 e + 0 7
2 . 8 e + 0 7
3 e + 0 7
3 . 2 e + 0 7
3 . 4 e + 0 7
3 . 6 e + 0 7
T i m e
R e s p o n s e _
G C 8 - 3 3 6 7 . D \ E C D 2 B
22
21
20
19
18
17
161514
13
12
11
109
8
7
6
5
4
3
2
1
Column: DB-XLB20m x 0.18mm i.d., 0.18µm
Carrier: H2, constant flow, 77.3cm/s at 120°CInjector: Pulsed Splittless, 220 °C
Pulse pressure & time: 35psi for 0.5minFlow ramp at 6.25min of 99mL/min2 to 3mL/min2mm i.d. liner0.5µL, 50ppb
Oven: 120°C for 0.49min120°C to 160°C at 59.4°/min160°C to 260°C at 23.7°/min260°C to 300°C (1.69min) at 35.6°/min
Detector: µ-ECD, 320°CAr/CH4 (P5) makeup gas at 60mL/min
Final Method Used at EPA
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0 . 5 0 1 . 0 0 1 . 5 0 2 . 0 0 2 . 5 0 3 . 0 0 3 . 5 0 4 . 0 0 4 . 5 0 5 . 0 0 5 . 5 0 6 . 0 0 6 . 5 0 7 . 0 0
2 0 0 0 0 0 0
4 0 0 0 0 0 0
6 0 0 0 0 0 0
8 0 0 0 0 0 0
1 e + 0 7
1 . 2 e + 0 7
1 . 4 e + 0 7
1 . 6 e + 0 7
1 . 8 e + 0 7
2 e + 0 7
2 . 2 e + 0 7
2 . 4 e + 0 7
2 . 6 e + 0 7
2 . 8 e + 0 7
3 e + 0 7
3 . 2 e + 0 7
3 . 4 e + 0 7
3 . 6 e + 0 7
T i m e
R e s p o n s e _
G C 8 - 3 3 6 7 . D \ E C D 2 B
DB-XLB
0 . 5 0 1 . 0 0 1 . 5 0 2 . 0 0 2 . 5 0 3 . 0 0 3 . 5 0 4 . 0 0 4 . 5 0 5 . 0 0 5 . 5 0 6 . 0 0 6 . 5 0 7 . 0 0
2 0 0 0 0 0 0
4 0 0 0 0 0 0
6 0 0 0 0 0 0
8 0 0 0 0 0 0
1 e + 0 7
1 . 2 e + 0 7
1 . 4 e + 0 7
1 . 6 e + 0 7
1 . 8 e + 0 7
2 e + 0 7
2 . 2 e + 0 7
2 . 4 e + 0 7
2 . 6 e + 0 7
2 . 8 e + 0 7
3 e + 0 7
3 . 2 e + 0 7
3 . 4 e + 0 7
3 . 6 e + 0 7
T i m e
R e s p o n s e _
G C 8 - 3 3 6 7 . D \ E C D 1 A
V i e w M o d e : I n t e g r a t i o n
DB-17ms
22
21
20
19
18
17
161514
13
12
11
1098
7
6
5
4
3
2
1
22
21
20
19
1817
1615
14
1312
11
1098
7
6
5
4
32
1
Final Method Used at EPA
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Food/Fragrance – Method translation
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Food/Fragrance – Method translation
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Spearmint Oil
Δ -9.7 min (0.18 mm, He Carrier)
Δ -16.8 min (0.18 mm, H2
Carrier)
10.6 min
17.7 min
3 8 13 18 23 28
(0.25 mm, He Carrier)
Time (min)
27.4 min
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10.6 min
17.7 min
3 8 13 18 23 28
27.4 min
(0.25 mm, He Carrier)
Δ -9.7 min (0.18 mm, He carrier)
Δ -16.8 min (0.18 mm, H2 Carrier)
Spearmint Oil – Resolution Check
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Practical Fast GC Applications with Capillary GC ColumnsMay 19, 2009
Page 55
Resolution Maintained
Compound Resolution
Compounds 0.25 mm
Helium
0.18 mm
Helium
0.18 mm
Hydrogen
Sabinene
β-Pinene1.52 1.59 1.56
α-Terpinene
p-Cymene1.61 1.73 1.86
Speed Gain N/A 35% 61%
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CONCLUSIONSStationary Phases – Chosen for optimized selectivity
Diameter – Smaller allows shorter length but has less capacity
Make Small Changes – Again think capacity
Carrier Gas – Hydrogen, high velocity, but can still go fast with He
Temperature Program – Scale properly to preserve elution pattern
Method Translation Software – FREE, reliable
Flow Ramp – Increase at end of run for late eluters (if necessary)
System Upgrades – LTM, Capillary Flow Devices (back flush)
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The New Agilent Intuvo 9000 GC System
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Common frustrations with GC
• Measuring column length correctly
• Cutting your column correctly
• How tight it too tight?
• Clipping columns to deal with active sites, then updating retention times
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Common Care and Maintenance Scheme for GC Columns
1. Cut off 6”-1ft of the inlet end of the column.
2. Bake out the column for no more than 2 hours.
3. Cut off more column. (repeat as necessary)
Guard Column
Intuvo…
Change the guard chip
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Innovating the GC Flow Path
Click-and-run direct
connections
To detector
To detector
Conventionalflow path
Intuvoflow path
Inlet Inlet
Guard chip
Intuvo planar column
Gold seal
Nuts and ferrules
Classic capillarycolumn
Flow chip
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Easier and faster maintenance with Intuvo
• No more ferrules
• Direct face seal connections
• Audible and tactile click lets
you know connection is made
• Less unplanned downtime
• Fewer batch reruns and
precious samples lost
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No More
- measuring
- over-tightening
- trimming
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A New Portfolio of GC Consumables
UI Inlet LinersGuard Chip
No-trimcolumn
Intuvo Flow Chips
Smart Keys
Tools & Accessories
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No More:
- Measuring
- Over-tightening
- Trimming
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Tips to Assure a Good Column Installation
1. Finger tighten until only 1 thread on each of the two nuts is showing.
If more than 1 thread is showing, wiggle or re-position the column into place to further finger tighten the nuts to 1 thread.
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Tips to Assure a Good Column Installation
2. Check that the small integrated column nuts on the column are in form fitted place on the heater in the instrument.
3. Click and Run!!
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Smart Key Technology
• Smart chip tells your Intuvo
what you have
• Sets temperature limits for
you
• Keep track of performance
with read/writeable Smart Key
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Where Does it Get Dirty?
Here
Here
Here
Here
Here
Here
Page 78
Not the Column!
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New Autonomous Leak Checking