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USEPA Methods 8270 and 8260 on a Single
GCMS Without Changing Columns
Richard Whitney, Laura Chambers, Clifford Taylor
Shimadzu Scientific Instruments, Inc.
Columbia, MD
Spotlight on Method
8270 Instrumentation
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USEPA Methods 8270 and 8260 on a Single
GCMS Without Change Columns
Richard Whitney, Laura Chambers, Clifford Taylor
Shimadzu Scientific Instruments, Inc.
Columbia, MD
Spotlight on Method
8270 Instrumentation
Venting the MS to . . .
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• Small laboratory
• Limited budget
• Multiple applications
• No time
Problem
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The Big Bang Theory – CBS.com
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• 8260 and 8270
• Single GCMS
• Two inlets, two columns
• No venting
Solution
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The Big Bang Theory – CBS.com
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What We Did
Instrument configuration
Optimize method parameters
Analytical results (aka data)
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Instrument Configuration
GCMS-QP2010 SE
Production Workhorse 6
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Instrument Configuration
GCMS-QP2010 SE
Production Workhorse 7
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Instrument Configuration (cont.)
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GCMS Twin Line Kit
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Instrument Configuration (cont.)
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Instrument Configuration (cont.)
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Instrument Configuration (cont.)
58 L/sec (He)
Pfeiffer TMP (Rotary pump 30 L/min)
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Instrument Configuration (cont.)
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Instrument Configuration (cont.)
13
Ecology Mode saves ~26%
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Instrument Configuration (cont.)
Parameter EPA Method 8260 EPA Method 8270
Sample introduction Purge-and-trap Liquid syringe
Liner Shimadzu multi-purpose
split liner, no glass wool
Shimadzu multi-purpose
split liner, no glass wool
Injection conditions Split 75:1 Split 10:1
Column Rxi-624Sil MS
20 m x 0.18 mm x 1.4 µm
Rxi-5Sil MS
20 m x 0.18 mm x 0.18 µm
Maximum column
temperature Program = 320 °C Program = 350 °C
Carrier gas Helium, constant linear velocity mode
MS pump Single stage TMP, max flow 4 mL/min (He)
MS interface 225 °C
Ion source EI, 200 °C
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Instrument Configuration (cont.)
Born in Kyoto
Made in the USA
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• Primary objectives
1. Keep total column flow rate
below 4 mL/minute
2. Keep maximum oven
temperature below 320 °C
3. Keep GC run time as short
as practical
Method Optimization
16
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Method Optimization (cont.)
Parameter Method 8260
Primary
Method 8270
Inactive
Column constant
linear velocity
45 cm/second
~0.8 mL/min
30 cm/second
~0.5 mL/min
Maximum total
column flow ~1.3 mL/minute
Oven program
35 °C (5 min)
20 °C/min to 220 °C
(hold 2.5 min)
NA
GC run time 12.5 minutes NA
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Method Optimization (cont.)
Parameter Method 8260
Inactive
Method 8270
Primary
Column constant
linear velocity
30 cm/second
~0.5 mL/min
40 cm/second
~0.7 mL/min
Maximum total
column flow ~1.2 mL/minute
Oven program NA
45 °C (0.5 min)
25 °C/min to 315 °C
(hold 4.2 min)
GC run time NA 16 minutes
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Why Constant Linear Velocity?
Van Deemter Plot
Linear Velocity – Isothermal Oven
Optimal LV for
each carrier
Gas
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Why Constant Linear Velocity? (cont.)
Head Pressure (kPa)
Flow (ml/min)
Linear Velocity (cm/sec)
Oven Temp
With temperature programming:
1. Viscosity of gas increases
2. Gas expands
3. Flow rate and LV drop
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Why Constant Linear Velocity? (cont.)
Linear Velocity
Linear Velocity
Oven Temp
Head Pressure
Flow
Linear Velocity
Constant
Pressure
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Why Constant Linear Velocity? (cont.)
Linear
Velocity
Linear
Velocity
Head Pressure
Flow
Linear Velocity
Oven Temp
Constant
Flow
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Why Constant Linear Velocity? (cont.)
Constant
Linear Velocity
Head Pressure
Linear Velocity
Flow
Oven Temp
Linear Velocity
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Why Constant Linear Velocity? (cont.)
Constant Flow
Linear velocity = 20 cm/sec
Constant Pressure
Linear velocity = 15 cm/sec
Constant Linear Velocity
Linear velocity = 30 cm/sec
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Analytical Results
BFB Spectrum
EPA Method 8260
BFB Tune Criteria
Passed
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Analytical Results (cont.)
EPA Method 8260
10 µg/L calibration standard
TIC – 66 compounds resolved
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Analytical Results (cont.)
DFTPP Spectrum
EPA Method 8270
DFTPP Tune Criteria
Passed
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Analytical Results (cont.)
DDT Breakdown
DDT (expanded)
DDE DDD
Benzidine and Pentachlorophenol Tailing
Benzidine
Pentachlorophenol
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Analytical Results (cont.)
DDT Breakdown
DDT (expanded)
DDE DDD
Benzidine and Pentachlorophenol Tailing
Benzidine
Pentachlorophenol
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Analytical Results (cont.)
EPA Method 8270
50 µg/mL calibration standard
TIC – 66 compounds resolved
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Analytical Results (cont.)
EPA Method 8270 Calibration
Range 8 points, 0.4 – 160 µg/mL
6 Internal Standards Acenaphthene-d10, Cyrysene-d12, 1,4-Dichlorobenzene-d4,
Naphthalene-d8, Perylene-d12, Phenanthrene-d10
40 µg/mL each
Response Factor 54 compounds < 15% RSD
Min. RF = 0.132, Pentachlorophenol
Max. RF = 3.966, bis(2-chloroisopropyl)ether
Linear Curve 12 compounds > 15% RSD
Min r = 0.997, 2,4-dinitrophenol
Max r = 0.999, 8 compounds
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Analytical Results (cont.)
2-Nitrophenol (2 µg/mL)
r = 0.999
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Benzo(b&k)fluoranthenes (1 µg/mL)
Analytical Results (cont.)
RSDb = 6.1%
RSDk = 12.0%
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Analytical Results (cont.)
0.0
2.0
4.0
6.0
8.0
10.0
12.0
%R
SD
% Relative Standard Deviation (0.4 µg/mL*, n = 8)
62/66 RSD < 8%
39/66 RSD < 4%
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Analytical Results (cont.)
0.0
20.0
40.0
60.0
80.0
100.0
120.0
Ave
rag
e %
Re
co
ve
ry
Average % Recovery (0.4 µg/mL*, n = 8)
57/66 Recovery 80 – 120%
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Analytical Results (cont.)
0.00
0.10
0.20
0.30
0.40
0.50
0.60
0.70
0.80
IDL (
µg
/mL
)
Statistical Instrument Detection Limit (0.4 µg/mL, n = 8)
60/66 IDL < 0.2 µg/mL
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Analytical Results (cont.)
DCM carryover < 1.0 ppb
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Analytical Results (cont.)
Acetone carryover ~ 1.0 ppb
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• Two methods
• Two intro techniques
• Two injection ports
• Two columns
• One MS
• All method criteria passed
• One happy customer
• Shimadzu application
note GCMS-1302
Summary
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Acknowledgements
Richard R. Whitney, Ph.D.
Configuration insight and
all the hard work!
Julie Kowalski
Advice re column and conditions
Columns and standards
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Shimadzu Scientific Instruments
Products – People - Passion
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