Presentation of the TRACE LABORATORY. Petra Přibylová Head of Trace laboratory

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1 Presentation of the TRACE LABORATORY Petra Přibylová Head of Trace laboratory

2 Laboratory of the trace analysis - accreditation "Accredo - put faith in"» Matrices: - Outdoor / indoor air - Surface water - Sediments, soils - Food, foodstuffs - Cell tissues - Secretions and excretions incl. Breast milk Analytes: - PCDDs/Fs, dl-pcbs, ind. PCBs - PBDEs GC/ HRMS

3 Samples flow

4 Struktura Stopové laboratoře Vedoucí: Petra Přibylová Odborný garant: Anton Kočan Manažer kvality: Rostislav Červenka Inetrní auditoři: Rostislav Červenka Iva Poláková Metrolog: Rostislav Červenka Laboratorní specialista I: Iva Poláková Lenka Vaňková Laboratorní specialista II: Ondřej Audy Jitka Bečanová Eliška Čechová Jiří Kohoutek Rostislav Červenka Pavlína Karásková Tono Kočan Petr Kukučka Jan Kuta Petra Přibylová Marta Seifertová Šimon Vojta Technik: Lída Tupová Eva Krejčí

5 PEOPLE WORKING IN THE LAB Tono Kočan Petra Přibylová Rosťa Červenka Eva Krejčí Trace Lab Staff: Roman Prokeš Jiří Kohoutek Lenka Vaňková Iva Poláková Lída Tupová Tono Kočan Petr Kukučka Šimon Vojta Jitka Bečanová Jiří Kohoutek jr. Jan Kuta Rosťa Červenka PhD. Students working on the projects: Ondřej Audy Pavlína Karásková Eliška Čechová Marta Seifertová Non-trace lab staff, entrance just for measurements: Zdeněk Šimek, Brano Vrana, Lisa Melymuk, Lucie Bláhová SELECTED STUDENTS UNDER CONTROL OF THEIR SUPERVISORS!!!! IN INSTRUMENTAL ROOMS ONLY!!!!

6 Laboratory of the trace analysis Equipment: 2 x GC/HRMS dl-pcbs, PCDDs/Fs, pyrethroids, BFRs = PBDEs, NBFRs 4 x GC/MS/MS ind.pcbs, OCPs, cyclodiene pesticides (including endosulphane), PAHs, N-PAHs, OPFRs 3 x GC/MS - PAHs, musks, personal care products GC/ECDxFID alkalnes, OCPs HPLC/ MS alkylphenols, estrogens HPLC/ MS/MS CUPs, pharmaceuticals, HBCDs, PFCs, microcystins, oxidative stress markers ICP / MS metals GC (LS)/ ICP/MS speciation analysis AAS - Hg

7 GC/ECD + FID Jaromír Literák (responsible person) Tono Kočan (the second floor 212)

8 GC 7890 / FID/ECD (Agilent) Tono Kočan, Jaromír Literák GC/ECD PCBs + OCPs (Tono Kočan) Enantioselective measurements (Jaromír Literák) GC/FID Aliphatic hydrocarbons Alkyl-PAHs PAHs (Jaromír Literák)

9 Organic and inorganic carbon determination Ondřej Mikeš (responsible person) Rosťa Červenka (analysis for TL) (the second floor 212)

10 Organic and Inorganic carbon determination Room: 212 Persn.: Ondřej Mikeš (Klára Šmídová, Rosťa Červenka) High temperature digestion of the sample Liquids 0 60,000 mg/l in liquids % in solids NDIR detection Solids LOD 6 μg/l (ppb) - liquids reagent water drinking water waste water sea water saline solutions electrolytes particles suspensions soils slurries residues solids Next- Organic and elementar carbon in the air samples

11 Structure of the trace lab Sampling Samples preparation Analysis

12 SAMPLE PREPARATION IN THE TRACE LAB Samples evidence Iva Poláková, Lenka Vaňková, Lída Tupová Cleaning (preextraction) of the sampling media before the exposure (Soxhlet extraction) Extraction of the samples (Automated hot solvent extractors Büchi B-811, SPE) Analytical clean-up (adsorption column chromatography on the different sorbents, GPC) Groups of compounds: - PCBs, OCPs, Drin pesticides, PBDEs, HBCDDs, PBBs, NBFRs, PAHs - NEWLY: PCDDs/Fs - FUTURE PFCs, CUPs

13 GC 7890 / MS-MS Triple Quadrupole 7000B (Agilent) Petra Přibylová (responsible person) Ondra Audy Petr Kukučka (the second floor 232)

14 Group of compounds: PCBs + OCPs, PAHs native and 13C labeled -Monitoring: AIR (MONET projects 2900 analysis/year), Košetice projects 130a/y) Water (Košetice RW 240 a/y) Soil, sediment, needles, moss (Košetice 100a/y) -Projects Gerhard s project (~1300a/y), ArcRisk/Monairnet, Fluvisoils, Anděl autoroute monitoring, Mokrá cement factory, Luca s projects, Water s group projects (~1700 a/y) -Calibration studies (~1200 a/y) -Indoor studies (? a/y) - Samples for the methods validation (~200s/y) Capacity samples/day ~ 8000 analysis / 2014

15 GC-LRMS: GC 6890N / MSD 5975 (Agilent) Single quadrupole EI (SIM, SCAN) Brano Vrana (responsible person) Petra Přibylová Tono Kočan Petr Kukučka Ondra Audy (the second floor 233)

16 Until NOW: PAHs measurements - Monitoring (MONET projects, Košetice projects) - Projects Monairnet, Fluvisoils, Anděl, Karla s samples, calibration studies, some student s projects) -NEAR FUTURE: -PAHs for Brano -Methods development - MUSK compounds - Alkyl phosphates? - Pyrethroids? Projects of Brano Capacity samples/day

17 GC/MS-MS Quattro Micro GC (Waters) Petr Kukučka (responsible person) (the second floor 232)

18 Until NOW: PCBs + OCPs, cyklodiene pesticides measurements - Monitoring (MONET projects, Košetice projects) -NEAR FUTURE: MS/MS Methods development -CI ionization possible - MUSK compounds - Alkyl phosphates? - Pyrethroids?

19 GC 7890 / APGC MS-MS XEVO TQ-S (Agilent-Waters) Petr Kukučka (responsible person) Ondra Audy (the second floor 232)

20 Projects only New method development Substituted PAHs Alkyl phospates? Organophosphorus flame retardands SCCPs/MCCPs?

21 High Resolution GC/MS THERMO Scientific DFS Tono Kočan (responsible person) Eliška Čechová Marta Seifertová Šimon Vojta (the basement 1S05)

22 High Resolution GC/MS THERMO Scientific DFS PCDD/Fs 60m Rtx-Dioxin 2 column (Restek) dl-pcbs 60m DB5-MS UI column (Agilent) Pyrethroids Predicted capacity of 1500 samples per year in accreditation mode (QA/QC assurance)

23 High Resolution GC/MS AutoSpec Premier (Waters) Petr Kukučka (responsible person) Šimon Vojta Tono Kočan Ondra Audy (the basement 1S31)

24 AutoSpec Premier, Agilent 7890A PBDEs, PBBs Novel BFRs 15m DB5 column, (Restek 1614, to be delivered), S/SL inlet, PTV inlet (Gerstel CIS3), short GC runtime sample throughput on average ~20-40 samples/day

25 LC-MS/MS Agilent 1290 and ABSciex QTRAP 5500 Waters Acquity and XEVO TQ-S (QqQ) unit resolution Agilent 1290/7890 and 6550 (Qtof) high resolution Jiří Kohoutek (responsible person) Jitka Bečanová Zdeněk Šimek Lucie Bláhová (the second floor 229, 231)

26 LC-MS/MS analysis Analysis: PFCs (perfluorinated compounds) HBCD (hexabromocyclododecane) Chlordecone CUPs (currently used pesticides) and degradation products Estrogens, Pharmaceuticals, Sweeteners Secondary metabolites of cyanobacteria and conjugates Fytoestrogenes Matrices: water, sediment air samples - PUF/QUARTZ/XAD materials, biological samples Instrumentation: Agilent 1290 and ABSciex QTRAP 5500 Capacity: cca analyses per year

27 Target and non-target LC-MS analysis (Jiří Kohoutek, Zdeněk Šimek) - quantitative and qualitative analysis of organic compounds - various matrices (water, sediment, biological samples, ) - LC (NP, RP, HILIC) and GC (SPME option) separation techniques - ESI, APCI and APPI ionization Instrumentation: Waters Acquity and XEVO TQ-S (QqQ) unit resolution Agilent 1290/7890 and 6550 (Qtof) high resolution

28 Analysis of metals, speciation analysis Jan Kuta Rosťa Červenka Blanka Maňáková (the second floor 214)

29 Analysis of metals, speciation analysis Jan Kuta, Rostislav Červenka, Blanka Maňáková Analysis of total content of elements (a large part of the periodic table) in various matrices e.g. sediment and soil samples, biota samples, air samples (dust on nitrocelullose filters)... Metals in specific leachates from soils and sediments Speciation of selected elements using hyphenated methods LC/GC-ICP-MS - As, Se, Hg (Cr, organo-sn) Instruments ICP-MS: Agilent 7500ce, Agilent 7700x HPLC: Agilent 1100 GC: Agilent 6890

30 Analysis of metals, speciation analysis Jan Kuta, Rostislav Červenka, Blanka Maňáková Hg analysis Altec AMA254 solid sampling AAS Hg analyzer Contact persons: Rostislav Červenka, Jan Kuta Solid sampling AAS total content without sample extraction (grinded sample) Sample preparation Contact persons: Jan Kuta, Rostislav Červenka, Blanka Maňáková Microwave digestion system MW3+ Berghof Ball Mill Retsch MM301 for grinding of samples Thermoblock, horizontal shaker, hot plates system for sub-boil distillation of acids, centrifuge...

31 Direct cooperation between teams of TL and GENASIS GENASIS: on-line processing of data (www.genasis.cz) Data analyses Interactive risk assessment case studies GIS visualization and space-time modelling

32 Thank you for your attention!

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