Transcript Analysis of Chlorinated Pesticide, Herbicide, PCBs by GC

An Optimized Dual Column System for the
Analysis of Chlorinated Pesticides,
Herbicides and PCBs by GC-ECD
Cameron George
Technical Support Engineer
26 April 2001
Cameron George
Applications Chemist
April 26, 2001
An Optimized Dual Column System for the
Analysis of Chlorinated Pesticides,
Herbicides and PCBs by GC-ECD
11:00 a.m. EST
Telephone Number: 904-779-4715
Chair Person: Lisa Lloyd
Cameron George
Applications Chemist
April 26, 2001
An Optimized Dual Column System for the
Analysis of Chlorinated Pesticides,
Herbicides and PCBs by GC-ECD
11:00 a.m. EST
Telephone Number: 904-779-4715
Chair Person: Lisa Lloyd
Starts in Five Minutes
Cameron George
Applications Chemist
April 26, 2001
An Optimized Dual Column System for the
Analysis of Chlorinated Pesticides,
Herbicides and PCBs by GC-ECD
11:00 a.m. EST
Telephone Number: 904-779-4715
Chair Person: Lisa Lloyd
Starts in One Minute
AREAS OF FOCUS
• Injector
• Detector
• Column (including guard column)
CLP Pesticides B-0447
March 8, 2001
TRACE ANALYSIS INJECTION
TECHNIQUES
5-2000 pg On-Column
• Megabore direct
• Splitless
• PTV
• On-Column (cold & hot)
• Large volume
CLP Pesticides B-0447
March 8, 2001
SAMPLE INJECTION
Goals
• Introduce sample into the column
• Reproducible
• No efficiency losses
• Representative of sample
CLP Pesticides B-0447
March 8, 2001
INFLUENCE OF INJECTION EFFICIENCY
Short
Concentrated
Solute Bands
Long
Diffuse
Same column, same chromatographic conditions
CLP Pesticides B-0447
March 8, 2001
FIRST, SOME BASIC DEFINITIONS:
Regarding Inlets
• Backflash
• Discrimination
CLP Pesticides B-0447
March 8, 2001
A FEW WORDS ABOUT BACKFLASH
Definition:
In a vaporization injection, a phenomenon wherein a
portion of the sample expands beyond the boundary
of the injection port liner towards the septum face
and incoming gas line
CLP Pesticides B-0447
March 8, 2001
BACKFLASH
Effects
• Ghost peaks
• Erratic quantitation
• Poor accuracy
CLP Pesticides B-0447
March 8, 2001
BACKFLASH
Causes
• Highly volatile solvent
• Excessive inlet temperature
• Excessive injection volume
• Small liner volume
CLP Pesticides B-0447
March 8, 2001
BACKFLASH
Preventative Measures
• Lower inlet temperature
• Less volatile solvent
• 1-2 µL injection volume
• Chambered liner
• Using pulsed split or pulsed splitless
CLP Pesticides B-0447
March 8, 2001
INJECTION PORT LINERS
Splitless
Yes
CLP Pesticides B-0447
March 8, 2001
NO!!!
INLET DISCRIMINATION
• Injected sample  Sample into the column
• Due to compound volatility differences
• Higher volatility = More into the column
CLP Pesticides B-0447
March 8, 2001
INLET DISCRIMINATION
In Pesticide Analyses
Generally inlet discrimination is not a concern for
pesticide analyses when utilizing appropriate GC
inlets such as Splitless, Pulsed Splitless and PTV
CLP Pesticides B-0447
March 8, 2001
OTHER INLET CONSIDERATIONS
• Silylation
• Using glass wool
• Cleaning and reusing liners
CLP Pesticides B-0447
March 8, 2001
A FEW WORDS ABOUT RESIDUES
• Semivolatile vs nonvolatile
• Worst offenders
• Sample prep
CLP Pesticides B-0447
March 8, 2001
GUARD COLUMNS
Use 0.53mm Or 0.32mm ID Deactivated Tubing
• Fit all inlets
• Enhanced deposition of residues
• Easy to work with
• Minimum 1 meter
CLP Pesticides B-0447
March 8, 2001
GUARD COLUMN
Traps non-volatile sample residues
Injector
Detector
Deactivated
Fused Silica
Tubing
Union
Column
Usually 1-5 meters long and same diameter as the column
CLP Pesticides B-0447
March 8, 2001
COLUMN CONNECTORS
Thermal Mass, Inertness, Seal Integrity
• Stainless steel
• VU-Tight
• Press-fits
• Integral guard columns (Duraguard)
CLP Pesticides B-0447
March 8, 2001
ANALYTE DETECTION
Let’s Be Sensitive
CLP Pesticides B-0447
March 8, 2001
SENSITIVITY
Analytical Definition
The minimum amount of an analyte that can
still be confidently identified as a peak (S/N >
4)
CLP Pesticides B-0447
March 8, 2001
SENSITIVITY
Analytical Definition
• Detector Sensitivity: No sample influence (standard)
• Method Sensitivity: Matrix influence (sample)
CLP Pesticides B-0447
March 8, 2001
RESPONSE TO A CONSTANT ANALYTE
AMOUNT
2 Cases
Sx
S
N
N
"Normal" response
1. High noise, detector, background
2. Absorption, breakdown of analyte
3. Sample prep losses
"Improved" response
1. High quality circuit components
and reagents
2. Inertness
3. Method optimization
CLP Pesticides B-0447
March 8, 2001
HP 6890 Series Micro-ECD Design
Comparison of HP 6890 ECDs
Standard
MDL
< 0.040
> 10^4
Dynamic range
Linear range
Micro-ECD
< 0.008
pg/sec lindane
> 5 x 10^5 lindane
no spec. > 5 x 10^4 lindane
Linear Range,
CLP pesticides
Maximum data rate
5 - 80
1 - 500
5
50
pg (ppb)
Hz
Break Number 1
For Questions and Answers
Press *1 on Your Phone to
Ask a Question
CLP Pesticides B-0447
March 8, 2001
LETS GET TO THE CHROMATOGRAPHY
CLP Pesticides B-0447
March 8, 2001
WHAT EXACTLY ARE WE TRYING TO
ACHIEVE
• The best resolution possible
• Minimize analysis time
• Get MDLs as low as possible
CLP Pesticides B-0447
March 8, 2001
RESOLUTION VS SEPARATION
• Separation: Time between the 2 peaks
• Resolution: Describes how well 2 peaks are
separated with regard to their widths
CLP Pesticides B-0447
March 8, 2001
WHICH PAIR OF SOLUTES HAVE
BETTER SEPARATION?
11.24
12.72
(tm = 95.5)
10
11
11.14
12
13
14
15
13
14
15
11.61
(tm = 95.5)
10
CLP Pesticides B-0447
March 8, 2001
11
12
RESOLUTION VS SEPARATION
Better Separation
11.24
12.72
a
= 1.17
Rs
= 0.6
K = 6.07
10
11
11.14
K = 7.00
12
13
14
15
14
15
11.61
Better Resolution
a
= 1.05
Rs
K = 6.00
= 2.7
10
CLP Pesticides B-0447
March 8, 2001
11
K = 6.30
12
13
RESOLUTION AND ANALYSIS TIME
• Improving resolution often results in the opportunity
to shorten analysis times
• Many variables can affect resolution
CLP Pesticides B-0447
March 8, 2001
RESOLUTION
Rs =
N  k   a - 1



4  k + 1  a 
N
=  (L, rc)
k
=  (T, df, rc)
a
=  (T, phase)
CLP Pesticides B-0447
March 8, 2001
IMPROVING RESOLUTION
Retention
The column must provide sufficient retention of
the early eluting compounds without excessive
retention of the late eluting compounds
CLP Pesticides B-0447
March 8, 2001
IMPROVING RESOLUTION
Film Thickness
Decreasing Film Thickness Results In:
• Increased efficiency
• Elution of analytes at lower temperatures
• Decreased analysis time
• Decreased bleed interference
• Increased column activity
• Decreased capacity
CLP Pesticides B-0447
March 8, 2001
IMPROVING RESOLUTION
Efficiency
• High column efficiency is necessary to resolve large
numbers of compounds
• Improperly operated injectors and/or improperly
optimized carrier gas can result in efficiency losses
CLP Pesticides B-0447
March 8, 2001
IMPROVING RESOLUTION
Column Length
Increasing Column Length Results In:
• Increased efficiency
• Increased analysis time
• Increased bleed
• Big increase in cost
CLP Pesticides B-0447
March 8, 2001
IMPROVING RESOLUTION
Column Inner Diameter
Decreasing Column Inner Diameter Results In:
• Increased efficiency
• Increased head pressure
• Decreased capacity
• Decreased carrier gas flow rates
CLP Pesticides B-0447
March 8, 2001
IMPROVING RESOLUTION
Stationary Phase
• Stationary phase selectivity has the largest impact on
separation, thus resolution
• Optimization of stationary phase selectivity should be
approached cautiously
CLP Pesticides B-0447
March 8, 2001
For Years Environmental
Laboratories Have Suffered With
Pesticide Analyses Using NonOptimal Stationary Phases
CLP Pesticides B-0447
March 8, 2001
TRADITIONAL STATIONARY PHASES
•5% Phenyl-methylpolysiloxane
•35-50% Phenyl-methylpolysiloxane
•Trifluoropropyl-methylpolysiloxane
•14% Cyanopropylphenyl-methylpolysiloxane
CLP Pesticides B-0447
March 8, 2001
PROBLEMS WITH TRADITIONAL PHASES
•Long analysis times (Over 30 minutes!)
•High bleed resulting in decreased sensitivity
•Poor resolution and confirmation capabilities
•Poor inertness of some phases
CLP Pesticides B-0447
March 8, 2001
TRADITIONAL PESTICIDE COLUMNS
Coelution of
peaks 10 & 11
608 Type
Phase
1701 Type
Phase
Poor peak shape
for Endrin aldehyde
High Bleed
at 280°C
40 min
0
10
CLP Pesticides B-0447
March 8, 2001
20
Time (min.)
30
40
0
10
20
Time (min.)
30
40
EFFORTS TO IMPROVE PESTICIDE
ANALYSES
Application Specific Phases
Stationary phases designed with a primary
focus placed upon maximizing separation (a)
for a specific group of target analytes
CLP Pesticides B-0447
March 8, 2001
APPLICATION SPECIFIC PHASES
Common CLP Pesticide Phases
Phase 1
Trifluoropropyl-dimethylpolysiloxane
CH 3
Si
C2 H4CF3
Si
O
CH 3
m
Phase 2
O
CH3
n
Trifluoropropyl-diphenyl-dimethylpolysiloxane
C2 H4CF3
Si
Si
O
m
Dimethyl functionality of Phase 2 not shown
CLP Pesticides B-0447
March 8, 2001
CH3
O
n
EFFECT OF PHASE POLARITY
Polarity
Thermal
Stability
CLP Pesticides B-0447
March 8, 2001
DRAWBACKS OF APPLICATION SPECIFIC
PHASES
•Limited thermal stability resulting in longer
analysis times and hampered sensitivity
•Excessive column conditioning times
leading to increased column activity
•Decreased column lifetimes
CLP Pesticides B-0447
March 8, 2001
PHASES DESIGNED WITH OPTIMUM
PERFORMANCE IN MIND
Arylene Phase Technology
CLP Pesticides B-0447
March 8, 2001
LOW BLEED STATIONARY PHASES
Arylene Structure
Biphenyl
O
CH 3
Si
O
CH 3
CH 3
Si
Si
O
CH 3
CH 3
Si
CH 3
CLP Pesticides B-0447
March 8, 2001
O
Si
CH 3
O
CH 3
Si
CH 3
Si
Si
CH 3
O
CH 3
CH3
Arylene
CH 3
CH 3
LOW BLEED STATIONARY PHASES
DB-35ms vs. DB-35
DB-35ms
320°C
8.00
10.00
12.00
14.00
16.00
18.00
20.00
DB-35
8.00
300°C
10.00
CLP Pesticides Analysis
CLP Pesticides B-0447
March 8, 2001
12.00
14.00
16.00
18.00
20.00
STATIONARY PHASE AFFECT ON
SENSITIVITY
S/N =10
DB-35ms, 320°C
Both 30 m x 0.25 mm I.D., x 0.25 µm
5 ng Decachlorobiphenyl
CLP Pesticides B-0447
March 8, 2001
S/N =3
DB-35, 300°C
LOW BLEED STATIONARY PHASES
Spectral Purity
DB-35ms
498
DB-35
253
Primary Ion
207
Primary Ion
78
498
377
428
315 331
253
135
156
214
207
78 96 119 144
315
250
428
356 377
346
52
197
286
405
51
281
197
470
405
96 119
451
249
470
455
m/z-->
356
m/z-->
50
100
150
CLP Pesticides B-0447
March 8, 2001
200
250
300
350
400
450
500
50
100
150
200
250
300
350
400
450
500
BENEFITS OF LOW BLEED STATIONARY
PHASES
• Improved sensitivity
• Improved spectral purity
• Reduced analysis times
• Potential increase in column lifetimes
• Rigorous inertness testing
• Less Detector maintenance
CLP Pesticides B-0447
March 8, 2001
Break Number 1
For Questions and Answers
Press *1 on Your Phone to
Ask a Question
CLP Pesticides B-0447
March 8, 2001
DEMANDING PESTICIDE APPLICATIONS
BENEFIT FROM ADVANCED PHASE
TECHNOLOGY
DB-35ms and DB-XLB capillary columns
contain second generation arylene stationary
phases giving them enhanced thermal
stability
CLP Pesticides B-0447
March 8, 2001
DB-35MS PRIMARY COLUMN
CLP Pesticides
•Should provide adequate resolution of all 22
CLP Pesticides and surrogates
•Short analysis time ideal
•Easily realized analysis conditions preferable
•Should give minimal column bleed
CLP Pesticides B-0447
March 8, 2001
CLP PESTICIDES
Column:
P/N:
Carrier:
Oven:
Helium at 45 cm/sec (EPC in constant flow mode)
110°C for 0.5 min
110-320°C at 15°C/min
320°C for 2 min
Splitless, 250°C
30 sec purge activation time
50 pg per component
µECD, 350°C
Nitrogen makeup gas
(column + makeup flow = 30 mL/min constant flow)
DB-35ms
Injector:
30 m x 0.32 mm I.D., 0.25 µm
123-3832
Detector:
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
4
Tetrachloro-m-xylene (SS)
a-BHC
 -BHC
-BHC
Heptachlor
-BHC
Aldrin
Heptachlor epoxide
 -Chlordane
a-Chlordane
Endosulfan I
4,4’-DDE
Dieldrin
Endrin
4,4’-DDD
Endosulfan II
4,4’-DDT
Endrin aldehyde
Endosulfan sulfate
Methoxychlor
Endrin ketone
Decachlorobiphenyl (SS)
2
3
7
8
1
12
13
Short Analysis Time
9 10
11
15 16
5
21
6
18 19
14
4
22
17
Low Bleed
At 320ºC
20
6
8
10
12
14
16
6
8
10
12
14
16
CLP Pesticides B-0447
March 8, 2001
DB-XLB CONFIRMATION COLUMN
With Regard To The Primary Column
•Should resolve any co-elutions
•Needs to provide adequate resolving power when
run under the same analytical conditions
•Should possess at least equivalent thermal stability
•Should provide a different relative elution pattern
•Ideally, elution order changes should be realized
CLP Pesticides B-0447
March 8, 2001
4
CLP PESTICIDES
Column:
Carrier:
Oven:
DB-XLB
30 m x 0.32 mm I.D., 0.50 µm
123-1236
P/N:
Helium at 45 cm/sec (EPC in constant flow mode)
110°C for 0.5 min
110-320°C at 15°C/min
320°C for 2 min
Splitless, 250°C
30 sec purge activation time
50 pg per component
µECD, 350°C
Nitrogen makeup gas
(column + makeup flow = 30 mL/min constant flow)
Injector:
Detector:
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
Tetrachloro-m-xylene (SS)
a-BHC
 -BHC
-BHC
Heptachlor
-BHC
Aldrin
Heptachlor epoxide
 -Chlordane
a-Chlordane
Endosulfan I
4,4’-DDE
Dieldrin
Endrin
4,4’-DDD
Endosulfan II
4,4’-DDT
Endrin aldehyde
Endosulfan sulfate
Methoxychlor
Endrin ketone
Decachlorobiphenyl (SS)
2
1
7
3
100% Confirmation In
Under 16 Minutes
12
8
13
910
11
16
15
21
6
14
5
18
19
4
22
17
20
6
6
CLP Pesticides B-0447
March 8, 2001
8
8
10
10
12
12
14
14
16
16
min
OPTIMIZING FOR SPEED WITHOUT
SACRIFICING ANALYTE RESOLUTION
•Use Hydrogen as the carrier gas
•Set linear velocity at 65 cm/sec (3.4 mL/min)
•Increase oven ramp rate from 15°/min to 25°/min
CLP Pesticides B-0447
March 8, 2001
CLP PESTICIDES USING HYDROGEN CARRIER GAS
Column:
DB-35ms
Carrier:
Oven:
30 m x 0.32 mm I.D., 0.25 µm
123-3832
P/N:
Hydrogen at 65 cm/sec (EPC in constant flow mode)
110°C for 0.5 min
110-320°C at 25°C/min
320°C for 2 min
Splitless, 250°C
30 sec purge activation time
50 pg per component
µECD, 350°C
Nitrogen makeup gas
(column + makeup flow = 30 mL/min constant flow)
Injector:
1
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
Detector:
Tetrachloro-m-xylene (SS)
a-BHC
-BHC
-BHC
Heptachlor
-BHC
Aldrin
Heptachlor epoxide
-Chlordane
a-Chlordane
Endosulfan I
4,4’-DDE
Dieldrin
Endrin
4,4’-DDD
Endosulfan II
4,4’-DDT
Endrin aldehyde
Endosulfan sulfate
Methoxychlor
Endrin ketone
Decachlorobiphenyl
3
CLP Pesticides B-0447
March 8, 2001
12
7
Baseline Resolution In
Under 9 Minutes!
2
8 9
3
10
13
11
22
14
16
15
5 6
18
19
21
17
4
20
44
55
6
7
8
9
10
10
3
CLP PESTICIDES USING HYDROGEN CARRIER GAS
Column:
DB-XLB
Carrier:
Oven:
30 m x 0.32 mm I.D., 0.5 µm
123-1236
P/N:
Hydrogen at 65 cm/sec (EPC in constant flow mode)
110°C for 0.5 min
110-320°C at 25°C/min
320°C for 2 min
Splitless, 250°C
30 sec purge activation time
50 pg per component
µECD, 350°C
Nitrogen makeup gas
(column + makeup flow = 30 mL/min constant flow)
Injector:
1
Detector:
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
Tetrachloro-m-xylene (SS)
a-BHC
-BHC
-BHC
Heptachlor
-BHC
Aldrin
Heptachlor epoxide
-Chlordane
a-Chlordane
Endosulfan I
4,4’-DDE
Dieldrin
Endrin
4,4’-DDD
Endosulfan II
4,4’-DDT
Endrin aldehyde
Endosulfan sulfate
Methoxychlor
Endrin ketone
Decachlorobiphenyl
4
CLP Pesticides B-0447
March 8, 2001
Excellent Resolution
And Confirmation In
Under 10 Minutes
12
7
2
10
13
8
9
11
3
14
16
15
6 5
22
21
18 19
17
4
20
5 5
6 6
77
88
99
10
10
OTHER COMMON ECD APPLICATIONS THAT
THIS DUAL COLUMN SHOULD BE ABLE TO
PERFORM
•EPA 8151A (Phenoxy acid herbicides)
•EPA 508.1 (Pesticides)
•EPA 552.2 (Haloacetic acids)
•EPA 8082 (PCB congeners and Aroclors)
CLP Pesticides B-0447
March 8, 2001
EPA 8151A PHENOXY ACID HERBICIDES
11
DB-35ms
8
5
2
1
4
3
2
4
2
6
4
8
6
8
C784
18
12 13
1415
6 7
9 10
16
10
10
Time (min)
20
19
17
12
14
12
16
14
16
DB-XLB
11
8
12 13
14
15
5
2
1
2
2
C785
CLP Pesticides B-0447
March 8, 2001
3
44
66
88
4
10
10
Time (min)
910
6 7
12
12
18
19
20
16 17
14
14
16
16
min
EPA 8151A PHENOXY ACID HERBICIDES
DB-35ms
30m x 0.32 mm I.D., 0.25 µm
P/N: 123-3832
DB-XLB
30m x 0.32 mm I.D., 0.50 µm
P/N: 123-1236
Carrier: Helium at 45 cm/sec (EPC in constant flow mode)
Oven: 50°C for 0.5 min
50-100°C at 25°C/min
100-320°C at 12°C/min
320°C for 2 min
Injector: Splitless, 250°C
30 sec purge activation time
50 pg per component
Detector: µECD, 350°C
Nitrogen makeup gas
(column + makeup flow = 30 mL/min constant flow)
CLP Pesticides B-0447
March 8, 2001
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
Dalapon
3,5-Dichlorobenzoic acid
4-Nitrophenol
Methyl-2,4-dichlorophenylacetate (SS)
Dicamba
MCPP
MCPA
4,4´, Dibromooctafluorobiphenyl (IS)
Dichloroprop
2,4-D
Pentachlorophenol
2,4,5-T,P
2,4,5-T
Chloramben
Dinoseb
2,4-DB
Bentazone
DCPA
Picloram
Acifluorofen
EPA 508.1 PESTICIDES
7
6
1516
11
DB-35ms
13
21,22 25 28
24 27
20
26
17
18
1
9,10
4
2
32
30 31 33 35
12
36
23
3
14
5
34
19
8
8
10
16
14
12
10
8
12
14
16
Time (min)
C786
38
37
29
22
20
18
18
20
22
24
24
min
76
DB-XLB
1516
9,11
25 28
24 27
22
26
20
13 17
1
12
4
32
30 31 33
18
35
2
3
8
8
C787
CLP Pesticides B-0447
March 8, 2001
10
10
12
12
14
8,10
5
14
14
16
19 23
16
Time (min)
21
34
36
38
37
29
18
18
20
20
22
22
24
24
min
EPA 508.1 PESTICIDES
1.
DB-35ms
2.
3.
30m x 0.32 mm I.D., 0.25 µm
4.
P/N: 123-3832
5.
6.
7.
DB-XLB
8.
30m x 0.32 mm I.D., 0.50 µm
9.
P/N: 123-1236
10.
11.
Carrier:
Helium at 45 cm/sec (EPC in constant flow mode) 12.
Oven:
75°C for 0.5 min
13.
75-300°C at 10°C/min
14.
300°C for 2 min
15.
Injector: Splitless, 250°C
16.
30 sec purge activation time
17.
50 pg per component
18.
Detector: µECD, 350°C
19.
Nitrogen makeup gas
20.
(column + makeup flow = 30 mL/min constant flow)
CLP Pesticides B-0447
March 8, 2001
Hexachloropentadiene
21. 4,4´-Dibromobiphenyl (SS)
Etridiazole
22. Heptachlor epoxide
Chloroneb
23. Cyanazine
Trifluralin
24. g-Chlordane
Propachlor
25. a-Chlordane
Hexachlorobenzene
26. Endosulfan I
a-BHC
27. 4,4´-DDE
Atrazine
28. Dieldrin
Pentachloronitrobenzene (IS) 29. Chlorobenzilate
Simazine
30. Endrin
g-BHC
31. 4,4´-DDD
b-BHC
32. Endosulfan II
Hepatachlor
33. 4,4´-DDT
Alachlor
34. Endrin Aldehyde
d-BHC
35. Endosulfan sulfate
Chlorothalonil
36. Methoxychlor
Aldrin
37. cis-Permethrin
Metribuzin
38. Trans-Permethrin
Metolachlor
DCPA
EPA 552.2 HALOACETIC ACIDS
12
11
9
DB-35ms
7
8
2,3
5
1
10
4
6
4
5
4
6
5
7
6
Time (min)
8
7
min
8
C788
DB-XLB
12
11
8,9
7
3
5
2
4
1
C789
CLP Pesticides B-0447
March 8, 2001
10
6
4
5
4
5
6
6
Time (min)
7
7
8
8
min
EPA 552.2 HALOACETIC ACIDS
DB-35ms
30m x 0.32 mm I.D., 0.25 µm
P/N: 123-3832
DB-XLB
30m x 0.32 mm I.D., 0.50 µm
P/N: 123-1236
Carrier:
Oven:
Helium at 45 cm/sec (EPC in constant flow mode)
40°C for 0.5 min
40-200°C at 15°C/min
200°C for 2 min
Injector: Splitless, 250°C
30 sec purge activation time
50 pg per component
Detector: µECD, 350°C
Nitrogen makeup gas
(column + makeup flow = 30 mL/min constant flow)
CLP Pesticides B-0447
March 8, 2001
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
Chloroacetic acid
Bromoacetic acid
Dichloroacetic acid
Dalapon
Trichloroacetic acid
1,2,3-Trichloropropane (IS)
Bromochloroacetic acid
Bromodichloroacetic acid
Dibromoacetic acid
2,3-Dibromopropionic acid (SS)
Chlorodibromoacetic acid
Tribromoacetic acid
EPA 8082 PCB CONGENERS
1415
2
19
18
101112
DB-35ms
8
5
7
20
17
13
16
9
21
6
3
4
1
6
8
6
10
8
12
10
14
12
16
14
min
16
Time (min)
C790
2
15
14
DB-XLB
17
10
1112
7
5
8
19
18
16
20
13
9
6
3
21
4
1
6
6
C791
CLP Pesticides B-0447
March 8, 2001
8
8
10
12
10
12
Time (min)
14
14
16
16
min
EPA 8082 PCB CONGENERS
DB-35ms
30m x 0.32 mm I.D., 0.25 µm
P/N: 123-3832
DB-XLB
30m x 0.32 mm I.D., 0.50 µm
P/N: 123-1236
Carrier:
Oven:
Helium at 45 cm/sec (EPC in constant flow mode)
110°C for 0.5 min
110-320°C at 15°C/min
320°C for 5 min
Injector: Splitless, 250°C
30 sec purge activation time
50 pg per component
Detector: µECD, 350°C
Nitrogen makeup gas
(column + makeup flow = 30 mL/min constant flow)
CLP Pesticides B-0447
March 8, 2001
1. IUPAC 1
2. Tetrachloro-m-xylene (IS/SS)
3. IUPAC 5
4. IUPAC 18
5. IUPAC 31
6. IUPAC 52
7. IUPAC 44
8. IUPAC 66
9. IUPAC 101
10. IUPAC 87
11. IUPAC 110
12. IUPAC 151
13. IUPAC 153
14. IUPAC 141
15. IUPAC 137
16. IUPAC 187
17. IUPAC 183
18. IUPAC 180
19. IUPAC 170
20. IUPAC 206
21. Decachlorobiphenyl (IS/SS)
WHAT DOES THIS MEAN FOR
ENVIRONMENTAL LABORATORIES?
•Improved productivity
•Increased sample throughput
•Superior results
•Total solution for ECD systems
CLP Pesticides B-0447
March 8, 2001
CONCLUSION
DB-35ms and DB-XLB provide excellent
resolution and confirmation for CLP Pesticides
and other critical GC/ECD methods providing
total performance:
•Excellent selectivity
•Exceptional inertness
•Superb thermal stability
CLP Pesticides B-0447
March 8, 2001
CONCLUSION
When optimized columns are combined with
effective injector setup and detector design
improved testing results are realized while
sample throughput and laboratory efficiency
are improved dramatically
CLP Pesticides B-0447
March 8, 2001
AGILENT’S J&W TECHNICAL SUPPORT
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www.agilent.com/chem
CLP Pesticides B-0447
March 8, 2001
Wrap-up E-Seminar Questions
Thank you for attending Agilent e-Seminars.
Our e-Seminar schedule is expanding, please
check our website frequently at:
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CLP Pesticides B-0447
March 8, 2001