SCION™ GC-MS - nemc.us on Method... · • SCION GC-MS Environmental Methods Manual for USEPA...

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



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



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



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



Axial Ion Source- Inert by Design

SCION

Non-inert

SCION

Pentachlorophenol

Non-inert

Difenoconazole



SCION SQ Select- 1% Diesel Fuel Injections

Injection # 1 SCION Select

Injection # 300 SCION Select

Robust Operation for routine applications!



Axial Ion Source- Tune Stability • DFTPP PASSES after 500 soil extract injections over 14 days without source cleaning

Inj. #1 Inj. #500

Matrix Sample



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



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



EDR Detection System- Linear Range

• Excellent sensitivity without sacrificing linear dynamic range

Calibration curve 1 to 200 ppm for Hexachlorocyclopentadiene



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



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



Fast Pump-down-Ready for use

TIC Before Source Removal TIC After 25 min Pump Down



Software Innovation

Tuned for Productivity



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



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!



EasySIM™ + Compound Based Scanning • From full scan method- Click ‘Make SIM Method’

Full Scan



EasySIM™ + Compound Based Scanning • CBS creates complex SIM/Scan method

Original Full SCAN segment

SIM segments added and optimized automatically by CBS



EasySIM™ + Compound Based Scanning • Data handling and acquisition tables auto-updated

• Simply acquire your SIM/Scan data files!

SIM/Scan



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.



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)



SCION™ GC-MS Method 8270

Environmental Sample Analysis



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?



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



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



8270 Sludge Extract

PCP injection 1

PCP injection after 35

Left- Blank Extract; Right-Sludge Extract



Heavy Matrix Injections-Soil Extract Full Scan

TIC of highly contaminated soil extract from EPA 8270.



Good Full-scan sensitivity

Full Scan of 75 ppb calibration standard (Top) and extracted ion chromatogram (bottom) for the trichlorophenols



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



SIM/Scan segments for 55 8270 targets compounds

30



SIM/Scan 75 ppb

31



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



Remember our Full Scan Extract…

Find and quantitate the needles!



Q1

Q3

q2

291

291

Parathion

Matrix Interference

109

MS/MS in future for Method 8270



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



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



See our Poster- 8270 with Hydrogen



Thank You

www.scionhasarrived.com

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SCION™ GC-MS - nemc.us on Method... · • SCION GC-MS Environmental Methods Manual for USEPA...

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