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Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
SCION™ GC-MS A Highly Sensitive, Robust, and Easy-to-Use GC/MS
Spotlight on Method 8270 Instrumentation NEMC 2013, San Antonio, Texas
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Method 8270- The Lab Pain Points
holding times Start up costs reporting
downtime sustained sensitivity
productivity
competition
Cost of ownership
turnover
Ease of use
dynamic range
throughput
flexibility
automation
connectivity
run time
new methods
sample matrix
support data review
bench space
Tune stability
data integrity
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
SCION™ SQ Innovations
• Hardware • Robust Axial Ion Source- High Productivity, Maximize Uptime
• Curved Optics with lens-free design- Noise Elimination = High Sensitivity
• EDR-Extended Dynamic Range- Increased Working Range
• Large capacity turbo pump – Get up and running fast
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Axial Ion Source- Inert by Design
• Laminar flow-through source
• Reduces contact of ions with hot surfaces
• Uniquely designed to avoid matrix build-up on ion source parts
• Dual filaments for high productivity
• 300L/s pumping capacity
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Axial Ion Source- Inert by Design
SCION
Non-inert
SCION
Pentachlorophenol
Non-inert
Difenoconazole
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
SCION SQ Select- 1% Diesel Fuel Injections
Injection # 1 SCION Select
Injection # 300 SCION Select
Robust Operation for routine applications!
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Axial Ion Source- Tune Stability • DFTPP PASSES after 500 soil extract injections over 14 days without source cleaning
Inj. #1 Inj. #500
Matrix Sample
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Curved Ion Optics: Extreme FS Sensitivity
• 90 Degree Curved q0
• Reduces neutral noise for trace level GC/MS analysis
• Results are– higher S/N, excellent library match, and stable ion ratios !
To Quadrupole
From Ion
source
SCION SQ response for 1,2,3-Trichloropropane at 0.03 ppb by Purge and Trap -Ion ratios consistent across the peak.
Spectrum 1A
Spectrum 2A
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Added sensitivity- Active focusing q0 option
Benzene Hexachloro Hexachloro- cyclopentadiene
128% 71%
He Off
He On
From Ion
Source
To Q1
Patented rf couplers to improve transmission (part of Lens-Free architecture)
Ceramic heater circuit
Small amount of He added to sealed q0 slows down ions for better focusing and transmission to the mass filter
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
EDR Detection System- Linear Range
• Excellent sensitivity without sacrificing linear dynamic range
Calibration curve 1 to 200 ppm for Hexachlorocyclopentadiene
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
EDR Detection System- Quality Spectra
• Avoid detector saturation at high concentrations, get quality spectral library matches
200 ppm calibration standard for 8270 spectrum taken at peak apex
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Best-in-class high-capacity turbo pump
• Enables fast pump-down for higher productivity
• CI ready (can handle high gas loads)
• New high-capacity 300/400 **L/s design (Leybold-Turbovac series)
• MTBF is 8yrs
User Benefit: Higher Productivity
Fast Pump-down and CI field-upgradeable
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Fast Pump-down-Ready for use
TIC Before Source Removal TIC After 25 min Pump Down
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Software Innovation
Tuned for Productivity
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
SCION SQ Software innovations
• Software • EasySIM™- Covert full scan to SIMs , combine with CBS
• Compound Based Scanning (CBS)- Easy method development and maintenance
• EnviroPro™ Reporting Software
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
EasySIM™ - Adding SIM to FS Methods
• Step 1- Load Existing Full Scan Method File
• Step 2- Select “Convert to SIM/Scan” with EasySIM™
• Step 3- Let CBS fill in your tables with optimized conditions
Single ion monitoring SIM is an acquisition mode that greatly increases sensitivity for all or any target components. Changing full scan methods to include mixed mode FS-SIM can be very tedious and time consuming. Many systems require a complete method rebuild. EasySim make this a snap!
……Acquisition table and data handling table updated simultaneously ……..SIMs automatically optimized for best sensitivity ……………………Simply view the segments and run your sample!
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
EasySIM™ + Compound Based Scanning • From full scan method- Click ‘Make SIM Method’
Full Scan
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
EasySIM™ + Compound Based Scanning • CBS creates complex SIM/Scan method
Original Full SCAN segment
SIM segments added and optimized automatically by CBS
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
EasySIM™ + Compound Based Scanning • Data handling and acquisition tables auto-updated
• Simply acquire your SIM/Scan data files!
SIM/Scan
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
EnviroPro™ - Turning Data into Invoices
• Delivers reports that meet your customer’s requirements
• EPA reporting protocols, such as tune check, CLP program, tentatively identified compound (TIC) reports etc.
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Bruker – Getting you going from the Start
• SCION GC-MS Environmental Methods Manual for USEPA Methods
GC-MS Environmental Manual and Methods CD The CD contains method and data files for EPA method 524.3, 525.2 and 8270D
GC-MS Environmental Manual Only (PDF)
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
SCION™ GC-MS Method 8270
Environmental Sample Analysis
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Method 8270 Challenges
• Wide variety of acids, bases, and neutrals
• Strict quality control guidelines
• Market desire for lower reporting limits, even in very dirty matrices
• Addition of mixed-mode scanning
• Need for managing large number of SIMs
• Desire to calibrate and report lower limits in full scan of targets and TICs
• This challenges inertness of the entire GC/MS system- how can I keep it running longer with minimal maintenance?
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
8270 GC/MS Conditions
GC Column Conditons
Temp Rate (C/min) Hold(min) Total Time(min)
45 3 3
120 30 1 6.5
310 10 5 30.5
MS Full Scan Conditions
Mass Range: 45-450 da
Scan Time: 200 ms
Resolution: Unit
Fil. Delay: 2.0 min
Source Temp: 300 C
Trans Line Temp: 280 C
Injector Temp: 250 C
Pressure pulse: 40 psi for 0.25 min
Column flow: 1 ml/min
Column: BR-5ms, 30 M x 0.25mm x 0.25 um
Pulsed-split injection
Method for semi-volatile compounds in waste water and sludge/sediment samples
Desired FS CAL Range: 75 ppb to 30 ppm
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Advantage of Pulsed-Split Injection
High pressure in (40 psi) during injection
During the pulsed-split injection, the inlet is set to 40 psi with split vent at 70:1. Under this condition, the column flow is near 5 ml/min, allowing rapid transport of analytes to column. The actual split ratio is near 14:1.
Split flow out
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
8270 Sludge Extract
PCP injection 1
PCP injection after 35
Left- Blank Extract; Right-Sludge Extract
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Heavy Matrix Injections-Soil Extract Full Scan
TIC of highly contaminated soil extract from EPA 8270.
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Good Full-scan sensitivity
Full Scan of 75 ppb calibration standard (Top) and extracted ion chromatogram (bottom) for the trichlorophenols
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Passing method QC requirements
Compound Method 8270 Criteria
(Min RRF)
RRF on SCION SQ Cal Range 0.075-30ppm
N-nitroso-di-n-propylamine 0.05 0.109
Hexachlorocyclopentadiene 0.05 0.138
2,4-Dinitrophenol 0.05 0.149
4-Nitrophenol 0.05 1.03
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
SIM/Scan segments for 55 8270 targets compounds
30
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
SIM/Scan 75 ppb
31
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Calibration Statistics- Full Scan
32
75 ppb-30 ppm Full Scan
Overall Calibration Statistics-100 compounds total: Average % RSD = 11.62 % Average Correlation Coefficient =0.9989
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Remember our Full Scan Extract…
Find and quantitate the needles!
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
Q1
Q3
q2
291
291
Parathion
Matrix Interference
109
MS/MS in future for Method 8270
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
MS/MS for Method 8270
MS/MS on SCION in soil extract, 15-20 pg injected on column – pulsed-split
MS/MS on same Extract Previous Slide
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
MS/MS Precision Examples: 100 Injections at 100 ppb in Sludge Extract
1-Chloronaphthalene
%RSD = 5.7%
0
10000
20000
30000
40000
50000
60000
70000
0 20 40 60 80 100 120
Injection Number
Raw
Peak A
rea
Series1
2,4-Dichlorophenol
%RSD = 4.7%
0
1000
2000
3000
4000
5000
6000
7000
8000
9000
10000
0 20 40 60 80 100 120
Injection Number
Raw
Peak A
rea
Series1
4-Bromophenoxy Ether
%RSD = 6.6%
0
2000
4000
6000
8000
10000
12000
14000
16000
18000
20000
0 20 40 60 80 100 120
Injection Number
Raw
Peak A
rea
Series1
Copyright 2012 Bruker Corporation. All Rights Reserved.
C h e m i c a l a n d A p p l i e d M a r k e t s
See our Poster- 8270 with Hydrogen