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State Institute for Chemical and Veterinary Analysis of Food CVUA Freiburg Dual Data Acquisition Experiences and Application at the CVUA Freiburg / EURL for halogenated POPs 38th International Symposium on Halogenated Persistent Organic Pollutants (POPs) Thermo Lunch Seminar: DFS Magnetic Sector GC-HRMS Krakow, August 26 – 31, 2018 State Institute for Chemical and Veterinary Analysis (CVUA ) Freiburg European Union Reference Laboratory (EURL) for Halogenated POPs in Feed and Food Freiburg, Germany Alexander Schächtele, Helmut Winterhalter

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Page 1: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg 1 / Pork-Lard PT 2012

Dual Data Acquisition

Experiences and Application

at the CVUA Freiburg / EURL for halogenated POPs

38th International Symposium on Halogenated

Persistent Organic Pollutants (POPs)

Thermo Lunch Seminar: DFS Magnetic Sector GC-HRMS

Krakow, August 26 – 31, 2018

State Institute for Chemical and Veterinary Analysis (CVUA ) Freiburg

European Union Reference Laboratory (EURL) for Halogenated POPs in Feed and Food

Freiburg, Germany

Alexander Schächtele, Helmut Winterhalter

Page 2: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Content

Configuration

Analytes and methods

Sensitivity and chromatography

Recoveries of internal standards

Practical issues

Page 3: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Configuration

DFS

2 x Trace 1310 GC

with PTV, SSL injector

2 x TriPlus RSH

Dual Data XL

(Installation: end of 2016)

MCD

Page 4: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Configuration

Instrument methods Alternating staggered Dual Data Sequence

Single Sequences (only one side) with micro fluidic channel

device (MCD)

Single Sequences (only one side) with column direct into ion

source (without MCD)

Page 5: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Configuration

Single run

Normal sequence

Dual data sequence

Page 6: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Analytes of interest

Current analytes of interest on Dual Data XL DFS:

PCDD/Fs

PCBs

NDL-PCBs (indicator PCBs)

WHO-PCBs

mono-ortho-PCBs

non-ortho-PCBs

PBDEs

Extracts for GC-HRMS measurement:

(1) PCDD/Fs

(2) non-ortho-PCBs

(3) mono-ortho-PCBs + indicator PCBs

(4) PBDEs

Page 7: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Methods

PCDD/Fs

Mono-ortho-PCBs + Indicator PCBs

Non-ortho-PCBs

Injektor PTV, 5 µl injection (solvent vent)

Column DB-5MS (60m, 0.25 mm ID, 0.25 µm film)

Flow: 1.5 ml/min

GC run time ca. 36 min

Injektor SSL, 1 µl splitless injection

Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film)

Flow: 1.5 ml/min

GC run time ca. 40 min

Injektor SSL, 1 µl splitless injection

Column DB-5MS (60m, 0.25 mm ID, 0.25 µm film)

Flow: 1.5 ml/min

GC run time ca. 38min

Page 8: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Methods

PBDEs

Injektor PTV, 5 µl injection (solvent vent)

Column RTX-5 (15m, 0.25 mm ID, 0.25 µm film)

Flow: 2.0 ml/min

GC run time ca. 30 min

Injektor SSL, 1 µl splitless injection

Column RTX-5 (7m, 0.25 mm ID)

Flow: 4.0 ml/min

GC run time ca. 16 min

Page 9: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Dual Data Acquisition

Dual data acquisition:

PCDD/Fs + PCDD/Fs

PCDD/Fs + non-ortho-PCBs

Mono-ortho-PCBs/Indicator PCBs

+ non-ortho-PCBs

PCDD/Fs + PBDEs (15m, 7m column)

Page 10: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Dual Data Acquisition

Sample throughput (in same timeframe)

Normal sequence Dual data sequence

PCDD/Fs

Mono-ortho-PCBs/

Indicator PCBs

+ non-ortho-PCBs

PCDD/Fs + PBDEs

Page 11: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Sensitivity and chromatography

Sensitivity (20 fg 2,3,7,8-TCDD)

Without dual

data acq. /

MCD

With dual

data acq. /

MCD

S/N 302:1 S/N 305:1

Page 12: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Sensitivity and chromatography

GC column in ion source,

without dual data acq. / MCD

With dual data acq. / MCD

Page 13: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Recoveries of internal standard

Calculation of receoveries of ratio of recovery standard(s) and

internal standards

Reeovery standard(s) for PCDD/Fs:

Originally 13C12-1,2,3,4-TCDD

Since 2017: Multi-standard with recovery standard for each

chlorination degree for dioxins and furans

13C12-1,2,7,8-TCDF 13C12-1,2,3,4-TCDD 13C12-1,2,3,4,6-PeCDF 13C12-1,2,3,4,7-PeCDD 13C12-1,2,3,4,6,9-HxCDF 13C12-1,2,3,4,6,8-HxCDD 13C12-1,2,3,4,6,8,9-HpCDF 13C12-1,2,3,4,6,7,9-HpCDD

Page 14: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Recoveries of internal standard

Runs with column direct in source (without MCD)

Runs with MCD

Runs with MCD (Calculation with Multi-Std.)

100 %

Page 15: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Practical issues

Setup of sequence list

GC column exchange

Handling of the MCD wafer in routine

Potential leakage

Cleanliness / contamination of source

Page 16: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Sequence setup

Setup of staggered sequence necessary

Manual setup of DualData sequence lists with Xcalibur Sequence Setup more complex and

time-consuming than forsingle sequences

Setup in Excel and import in Xcalibur highly recommended

Page 17: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

GC column exchange

Column changing possible without venting the ion

source and cooling down the ion source and the

transfer line

Increase of helium flow during column exchange

No significant air entrance into ion source

No significant negative effects on ion source vacuum

Page 18: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

GC column exchange

Opening of connection

between column and MCD

Page 19: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Handling in routine

Additional connections and tubings for Dual Data

Page 20: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Handling in routine

MCD wafer with 4 connectors

Handling more difficult and tricky

than for configuration without

dual data

Page 21: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Potential leakage

Additional possible leakage Problematic leakage source

(also without dual data)

Page 22: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Summary

DFS in Dual Data acquisition mode routinely applied for

PCDD/Fs, PCBs and PBDEs

Considerably higher sample throughput possible

No negative effects on sensitivity, chromatography or

recoveries observed

User-friendly setup of Dual Data methods (high flexibility)

Sequence setup and handling in routine more complex

Additional leakage sources

Page 23: Dual Data Acquisition · Flow: 1.5 ml/min GC run time ca. 36 min Injektor SSL, 1 µl splitless injection Column MXT-500 (60m, 0.25 mm ID, 0.15 µm film) Flow: 1.5 ml/min GC run time

State Institute for Chemical and

Veterinary Analysis of Food

CVUA Freiburg

Thank you very much for

your attention !

Contact: [email protected]


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