Introducing the DSQII

Terry Jeffers

Agenda
Update on Thermos Environmental Initiatives
Discussion on new approaches to the challenges of 8270
Introducing Thermo Electrons Productivity Kits
EnviroLab Forms 2.0 High Throughput Quatification
New application note: Rapid Analysis of 8270

Thermo Electron: Environmental Initiative

Focus on Environmental Laboratory needs:
Requirement for Productivity
Need for good work flow in Generating, Reviewing and Reporting
data
Benefit from guides for operation, maintenance and troubleshooting
specific Methodologies

Thermo Electron: Environmental Initiative

ProductSalesSpecialist
EnvironmentalDemoChemist
EnvironmentalSeedChemist
Newhardware:DSQII
ProductivityKits:

8270and525
8260and524

Pitt Falls for Method 8270

Those little things that stop everything

Activity in the GC/MS system

Activity
These sites can be everywhere
Injector, column, source
SPCC compounds are used to show good system

Nitrophenols are some of the best compounds to find active sites

Minimizing Effects of Activity

Deactivated liners
Good column that shows no active sites
High flow rates to reduce the residence time of any active
compound.
Balance temperature zones to reduce activity and thermal break
down.

Chromatography

How important is it really?

GC and Autosampler
Separations accomplished with slow chromatography
Common GC methods for 8270

Fast injection
250 - 300 0 C injector temperature
1 mL/min flow rate
30 m x 0.25 mm ID column
Oven ramps between 5 0 and 10 0 C/min from 35 0 to 300 0 C

Separations accomplished with fast chromatography

Alternate GC method for 8270

Hot needle injection

250 0 C injector temperature
3 mL/min flow rate
30 m x 0.25 mm ID x 0.5 m column
Oven stepped ramps to provide the critical pair separations.

Hot Needle Injection: Run at Lower Inlet

Temperature: Fewer Replacements of Liner

Increase the Mobile Phase:

3 mL/min vs 1mL/min
Increase capacity of stationary
No fronting of peak shape for 160 ng/uL PNA

Decrease the irreversible absorption of active species

Pentachlorophenol < 10%RSD
(5-160 ng/uL)
0.1 ng/uL MDL
replicates at 1 ng/uL 4.7%RSD

Minimal breakdown for endrin or 4,4-DDT

Provide Gaussian shape peaks for the most volatile

No solvent skewing of NDMA and pyridine

Shorter run times: 17 minutes

10

Effects of increased flow rates

Why increase the flow rate to 3.0 mL/min
Learned from applications developed for the analysis of explosives.
Decrease the residence time of the compounds in potential active
areas.
Decreases the run time without higher temperatures that could
potentially damage thermally labile compounds.
Do not need to expose the column to higher temperatures that will
damage it.
Provides better separations and narrower peak widths.
This is balanced with a 20:1 split flow ratio.

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Injection: Choice of Liner

12

PNAs ( 5 ng and 160 ng)

Relative Abundance

RT: 17.32 - 18.34

RT: 17.45
AA: 1357507
BP: 276.1
100

NL:
4.27E5
m/z=
275.5276.5 F:
MS ICIS
031706_b_0
03

RT: 18.05
AA: 1192699
BP: 276.1

80
60
40
20
0
100

RT: 17.47
AA: 38042327
BP: 276.1

NL:
1.14E7
m/z=
275.5276.5 F:
MS ICIS
031706_b_0
08

RT: 18.07
AA: 32375912
BP: 276.1

80
60
40
20
0
17.4

13

17.5

17.6

17.7

17.8
17.9
Time (min)

18.0

18.1

18.2

18.3

NDMA and Pyridine

RT: 1.71 - 5.17

Split

Relative Abundance

100
80

4.94 5.05 NL:

3.81

3.19

2.46

1.79E8
TIC F: MS
C07

60

4.10
2.42

40

3.29

20

2.71

0
100

3.12

4.45

3.62

3.44

3.97

4.13

4.50 4.84
4.99

80

Splitless

60

4.87

40
20

4.52

0
2.0

14

2.5

3.0

3.5
Time (min)

4.0

4.5

5.0

NL:
8.09E6
TIC F: MS
A07

Two Methods: Splitless and Split

RT: 0.00 - 30.08
5.85

Relative Abundance

100

9.50

80

40

5.05

14.74

5.40

15.18

17.10

20
17.87 19.87 21.84

0
100

NL:
1.37E8
TIC F: MS
A07

9.42

80

8.10

60

8.22

7.49

40

7.34

20

6.37 6.90
4.87

0
0

15

12.89

8.92

8.72

60

NL:
5.80E8
TIC F: MS
C07

13.53

12.12
11.32

13.34
14.74 15.10
15.82

10

15
Time (min)

17.41

18.73 22.26

20

25.26

25

26.19
30

TRACE Ultra DSQ II GC/MS

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Source materials and geometry

New DuraBriteTM Source Open Geometry
Passive Collector
Extends Dynamic Range
Improves Robustness

Optional Closed EI Ion Volume

Constructed of new proprietary material for enhanced
inertness
Protects Lens 1 from ion burn

17

New DynaMax XR Ion Detection System

SGE ETP AF635 Electron Multiplier

Detector linear range
output current >30A
Simple snap out replacement of
multiplier assembly

18

New Linear/Log Hybrid Electrometer

Extends output current to 70A
Provides dynamic range to >106
No loss of response or precision at the lower
sample/analyte levels

Expected Results

Results I can get, you can get them too.

Calibration Curve
First page of the calibration
curve report
All SPCC and CCC
requirements met
Average of all RSD calibration
curves of 7.46%

20

SPCCs (5ng to 160 ng min >0.05)

21

2,4-dinitrophenol

0.11

4-nitrophenol

0.19

hexachlorocyclopentadiene

0.212

N-nitroso-di-n-propylamine

0.688

CCCs < 30% RSD for Initial Calibration Curve

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BNAs

%RSD

Acids

%RSD

1,4-dichlorobenzene

2.2

2,4-dichlorophenol

8.6

acenaphthene

1.6

4-chloro-3methylphenol

3.9

benzo(a)pyrene

7.1

2-chlorophenol

5.1

Di-n-octylphthalate

14

pentachlorophenol

9.1

diphenylamine

1.9

phenol

4.7

fluoranthene

3.8

2,4,6-trichlorophenol

11

hexachlorobutadiene

2.6

2-nitrophenol

8.5

Quantitated Data File

First page of the Quantitation
Report
This shows the quantitation of
the 20 ng/uL sample for the
calibration curve
Meets the requirements of the
internal standards and
surrogates
Meets all ion ratio requirements
No manual integrations were
required

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Robustness: Split (2gr sediment/2mL methylene

chloride + 25 uL diesel fuel)
RT: 0.00 - 17.11
8.33

100

7.77

90

Relative Abundance

9.36
9.83

7.18

80
70

10.28
10.71

6.53
5.01 5.82

60

NL:
1.08E9
TIC F: MS
rep96

8.87

11.12

4.04

50

11.51
40
30

2.34

20

11.90
3.97

12.26
12.61
12.96

1.40 1.70

10
0
0

8
Time (min)

10

12

2.5000
2.0000
1.5000
1.0000
0.5000
0.0000
1 3 5 7 9 11 13 15 17 19 21 23 25

24

14.00 14.87
14

16

Phenol(CCC) 2%
1,4-Dichlorobenzene(CCC) 1%
2-Nitrophenol(CCC) 2%
2,4-Dichlorophenol(CCC) 1%
Hexachlorobutadiene(CCC) 2%
4-Chloro-3-methylphenol(CCC) 2%
2,4,6-Trichlorophenol(CCC) 1 %
Acenaphthene(CCC) 1%
Pentachlorobenzene(CCC) 2%
Diphenylamine(CCC) 2%
Pentachlorophenol(CCC) 2%
Fluoranthene(CCC) 2%
Di-n-octylphthalate(CCC) 3%
Benzo(a)pyrene(CCC) 1%

How can we prove it

Productivity Solutions

Productivity Solutions

Integrating the DSQ II with Software, Methods,

and Consumables to Get Productive, Quickly

Productivity Solutions
Provide all of the necessary material to run the method
Proven Thermo Column
Deactivated Liners
Standards
Snap and shoot prediluted for entire method validation

All other consumables for about 2 weeks

Provide all of the software

EnviroLab Forms 2.0
Interactive Reference CD
All of the methods, sequences,

Validation data used to generate all of what you see here and in the
manuals

Two Boxes full of materials, manuals, and CDs.

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Productivity Kit
SOP manual for method
How to Guide
Quick Start Guide
Provide consumables for running method
Standards, liners, septa, syringes, column,

Instrument method, processing method, reporting package

CD deliverable
SOP
Data from method validation
Instrument method
Processing method
Reporting software with templates

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Pieces of the Productivity Kit

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Quick Start Guide

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8270C/D Productivity Solution

Customers system can be taken from installation sign off to
method IDLs in as little as 2 days!
8270 is a value added product which will sell for ~ $3000 US
Add on service provided by Thermo FSEs
US Field Service Engineers are being trained on the 8270 PS
Kits serve as a great tool for training aides for the lab

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Productivity Solutions are a Win-Win

Good for customers
Improves overall experience
Increases satisfaction
Eases transition to Thermo GC/MS
Gives optimal performance for the DSQ II

Good for Thermo

Easy to support these solutions

Helpsthecustomerandsupportbyestablishingaknown
setofcriteriatoachievesuccess.
Addressthenewlabenvironmentlesshighlyskilledusers
withhigherthroughputrequirements

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ftw
So

t
Ki

ar
e

Redefining the Way We Look at GC/MS

Hardware
Productivity Solutions target routine GC/MS applications to offer value to
the customer
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EnviroLab Forms v 2.0

High Throughput Quantification

EnviroLab Forms v 2.0

An entirely new data processing and reporting system running
as a layer over Xcalibur 1.4
While targeted towards environmental laboratories and
applications, it has been shown to be valuable for any
laboratory performing high-throughput quantification
Adds a significant complement of capabilities that Xcalibur
Ion ratio calculations
Peak integration
Reporting

Integrated data review and reporting

No more batch reprocessing to re-generate reports of edited results

Fully automated while still allowing sophisticated manual review

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Data Review

36

Report View

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EnviroLab Forms v 2.0

Brand new workflow oriented user interface
Substantially improved ion ratio review and editing support
Comprehensive set of textual and graphical reports
Fully automated, fully manual or any combination in between
Can be used as a high-throughput quantification engine for
any application
Simply turn off or dont use those options which arent relevant for a
given user

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Conclusion
The DSQ II system provides updates to hardware and
software that make it easy to use
The Productivity Solution for method 8270 provides a method
that has been validated across multiple DSQ II systems.
All of this allows a new operator to be productive immediately
The proven changes to the method allow an increased
amount of productivity and throughput for the analyst and the
laboratory.

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Questions?
ThankYou

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