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Chemical Engineering and Methods: Analytical Procedures and Materials Treatment

This section provides qualitative and quantitative chemical analyses, develops new analytical procedures, and offers expertise in radiation chemistry, materials compatibility, and surface treatments. It also conducts chromatography analyses and provides support for chemical analysis needs in the MME Group and CERN community.

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Chemical Engineering and Methods: Analytical Procedures and Materials Treatment

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  1. TS / MME – CEM: Chemical Engineering and Methods • MANDATE • STRUCTURE AND MANPOWER • INSTRUMENTS • TWO EXAMPLES OF MAIN WORK FOR PH • FUTURE ? V.Vuillemin / TS-MME – LEAF 28.10.05

  2. TS-MME-CEM Section: Mandate Realize qualitative and quantitative inorganic and/or organic chemical analyses, develop new analytical procedures and methods following the users demands, provide support on general chemistry for MME Group and CERN community. Offers expertise and consultancy in radiation chemistry, ageing and materials compatibility and reactivity, purification of gaseous mixtures and fluids. Assures a complex range of metallic surface treatments: cleaning for UHV applications; chemical&electrochemical degreasing, plating, etching and polishing using DC or pulsed current. Assures the outsourcing, when necessary, for different surface treatments and for plastic and resins works. Produce prototypes, pieces or parts in different types of resins and realize special gluing, as, for example for cryogenic, magnetic or high voltage applications for LHC and/or HEP detectors.

  3. TS-MME-Chemical Engineering and Methods (CEM section) Chef de section : S.Ilie Atelier Traitement de surface Atelier Résines et Polymères Laboratoire de Chimie Sorin Ilie Delphine Létant Benoit Teissandier Leonel Ferreira M. A. Jacky Carosone Colette Charvet Serge Forel Marina Malabaila Marc Thiebert Jean Francois Ecarnot Sebastien Clement + FSU

  4. Chromatography analyses • Instruments used: • Gas Chromatograph coupled with a mass spectrometer • GC Agilent 6890 Plus; Mass Spectrometer Detector HP 5973; • Gas Chromatograph • GC HP 5890; Thermal Conductivity Detector; GC-TCD HP 5890A GC Agilent 6890 – MS Agilent 5973

  5. Spectrometry facilities • UV-Vis Spectrophotometer • Agilent 8453; • FT-IR Spectrometer • Bruker IFS 66; IR-TF spectro Bruker IFS 66 UV-VIS spectro Agilent 8453

  6. Liquid analysis • Flame Atomic Absorption Spectrophotometer • AAS Perkin Elmer AAnalyst 300; • Inductively Coupled Plasma Optical Emission Spectroscopy • ICP-OES Perkin Elmer Optima 2000; ICP-OES Perkin Elmer Optima 2000 AAS Perkin Elmer AANalyst 300 MME-CEM

  7. Avalanche mode Streamer mode Resistive Plate Chambers (RPC) Used for the muons triggering for ATLAS, CMS and ALICE, experiments at LHC ATLAS CMS

  8. Ar The nominal composition of the RPC’s gaseous mixture in LHC experiments Example of a GC-MS chromatogram (standard gas mixture RPC – ATLAS)

  9. GC-MS identification of some radiolytic products Zoom 1 ALICE (Id. 19) Example: RPC – ALICE (Id.19)

  10. Cleaning tests of the irradiated gas mixture • The HF is totally eliminated • The filters reduce the total impurities content (~50%) Mixture before filters Mixture after filters

  11. 100 80 Mineral grease 60 Transmittance [%] 40 Copper 1 cm x 2 cm 20 Silicon grease Stainless Steel 0 3500 3000 2500 2000 1500 1000 Wavenumber cm-1 Evaluation of the presence and nature of greases over metallic surfaces TS / MME-CEM Solubilisation in 2 drops n-hexan Spectrometer FT-IR Brucker Vertex 70

  12. Typical IR spectrum of a silicon grease CH3 asymmetric deformation of Si-CH3 2905.60 Si-C stretching and CH3 rocking 1412.53 CH stretching of CH3 Si-O-Si stretching vibrations CH3 symmetric deformation of Si-CH3 2963.46

  13. Chemical Engineering and Methods Section Reports are different activities of the CEM Section are available on the EDMS server: htpps://edms.cern.ch Example of Reports Identification of oils and greases on metallic surfaces by FT-IR spectroscopy https://edms.cern.ch/file/410969/1/oils_and_greases.pdf Electropolissage du Tungstene https://edms.cern.ch/file/317887/1/tungstene.doc Resine Epoxy type VANTICO: Tests de tenue mecanique, de pression et de vieillissement https://edms.cern.ch/file/351635/1/Vantico.pdf Radiation induced chemical effects on some fluorocarbon used as cooling fluids Spain SHIM 2002 The analyse of radiation induced chemical effects on the working gas in HEP detectors Portland - Oregon - USA 2003 NSS-IEEE https://edms.cern.ch/file/411401/1/2003NSS.ppt

  14. FUTURE: • Do the LHC experiments need analysis during • tests / commissioning / running of: • Gas composition • Radiolytic components in gas (efficiency of filters) • Presence or not of HF in gas • Presence of silicon oil in installed chamber circuits • Cooling fluids composition [CnFm] • Radiolytic components in cooling (efficiency of filters) • Presence or not of HF in cooling fluids • Or any other chemical analysis performed in TS-MME-CEM ? • And to which extent?

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