Overview of the Chemical Characterisation and Analysis Facility

Overview of the Chemical Characterisation and Analysis Facility

Overview of the Chemical Characterisation and Analysis Facility (CCAF) What do we do? CCAF = Chemical Characterisation and Analysis Facility What do we do? CCAF = Chemical Characterisation and Analysis Facility University of Bath researchers External companies and collaborators How do we do it? How do we do it?

State-of-the-art, high-end equipment Highly-skilled Instrument Specialists How do we do it? State-of-the-art, high-end equipment Highly-skilled Instrument Specialists Help frame the analytical question Acquire best possible data Help with data interpretation Knowledge + Meaningful conclusions

Mass spectrometry @ Small molecules Peptides Polymers + + + + + +

+ + Proteins + + What do we use? (Mass Spectrometry) Large range of equipment, including: ESI-TOF + HPLC (3 South) ESI-QTOF + nanoLC (3 South) ESI-UHR-QTOF + 2D-UPLC (5 West) MALDI-TOF-TOF (5 West) ESI-QTOF + glove box (9 West) Open Access System Dedicated, automated, useroperated accurate mass spec. Quick-answers (pdf), 1 2

min for confirmation Register for training sessions, approx. 30min https://goo.gl/qMT7X2 Mass Spectrometry For: ESI QTOF ESI QTOF MALDI U/HPLC - Confirmation of expected formula by accurate mass measurements - Identification of unknowns

- Characterisation of organic and inorganic molecules, including polymers, proteins (native proteins and protein digests) and formulations - Screening and quantification of target compounds in complex matrices e.g. environmental and biological samples - Investigating 2D spatial distributions of molecules by MALDI-imaging (hopefully more soon) ESI QTOF ESI TOF What do we use? (NMR) Large range of NMR machines across campus 300 MHz (1 South)

400 MHz x 2 (1 South and 9 West) 500 MHz x 4 (1 South and 9 West) Most are fully automated Some operated manually Full range of state-of-the-art experiments possible What do we use? (NMR) For: - Characterisation of organic and inorganic molecules, including polymers and formulations - Characterisation of macro-biomolecules, e.g. proteins, DNA and interactions with drugs - Quantification and purity determination - Identification of unknowns - Activity of enzyme assays - Molecular weight estimation via diffusion NMR - Reaction monitoring, kinetics and mechanistic studies

What do we use? (NMR) New this year is a reaction monitoring suite Reactions can be set up in fume cupboard under normal lab conditions and monitored in real time by flowing them into NMR spectrometer 500 MHz with cryoprobe Coupled to other equipment

MS Head space MS UV HPLC What do we use? (X-Ray Diffraction) Powder XRD Single Crystal XRD Powder X-Ray Diffraction BRUKER D8 Advance powder X-ray diffractometer (1 South)

What can we do? (Powder X-Ray Diffraction) X-ray diffraction pattern from Powder Thin Film Membrane Ceramic Foil - Phase identification to compare with literature phase diagrams and determine the presence of mixtures - Determine whether crystalline or amorphous

Typical Powder Pattern Crystalline powder Amorphous powder CuSO4x5H2O 1,2,3,4 80000 70000 60000 d=10.65522 2th=8.291 50000 500

40000 30000 20000 10000 Lin (Counts) 90000 d=1.43401 2th=64.982 100000 600 d=1.61739 2th=56.883

Lin (Counts) 110000 700 d=2.02419 2th=44.735 120000 d=2.41813 2th=37.151 130000 d=2.86682 2th=31.173 140000

d=3.98280 2th=22.303 150000 d=3.69906 2th=24.039 160000 d=4.72426 2th=18.768 d=5.73950 2th=15.426 170000 400 300

200 100 0 0 5 10 20 30 40 50

60 70 80 90 100 2-Theta - Scale CuSO45h2o - File: coppersulfateovernightnew.raw - Type: 2Th/Th locked - Start: 5.000 - End: 110.004 - Step: 0.016 - Step time: 6728.3 s - Temp.: 21 C - Time Started: 17 s - 2-Theta: 5.000 - Theta: 2.500 - Chi: 0.00 - Phi: Operations: Import 110 4

10 20 30 40 50 60 2-Theta - Scale 1 - File: 1.raw - Type: 2Th/Th locked - Start: 4.000 - End: 90.022 - Step: 0.025 - Step time: 403.5 s - Temp.: 20 C - Time Started: 14 s - 2-Theta: 4.000 - Theta: 2.000 - Chi: 0.00 - Phi: 0.00 - X: 0.0 mm - Y: 0.0 Operations: Import Y + 10.0 mm - 2 - File: 2.raw - Type: 2Th/Th locked - Start: 4.000 - End: 69.999 - Step: 0.025 - Step time: 403.5 s - Temp.: 20 C - Time Started: 12 s - 2-Theta: 4.000 - Theta: 2.000 - Chi: 0.00 - Phi: 0.00 - X: 0. Operations: Import

Y + 20.0 mm - 3 - File: 3.raw - Type: 2Th/Th locked - Start: 4.000 - End: 69.999 - Step: 0.025 - Step time: 403.5 s - Temp.: 20 C - Time Started: 13 s - 2-Theta: 4.000 - Theta: 2.000 - Chi: 0.00 - Phi: 0.00 - X: 0. Operations: Import Y + 30.0 mm - 4 - File: 4.raw - Type: 2Th/Th locked - Start: 4.000 - End: 69.999 - Step: 0.025 - Step time: 403.5 s - Temp.: 21 C - Time Started: 12 s - 2-Theta: 4.000 - Theta: 2.000 - Chi: 0.00 - Phi: 0.00 - X: 0. Operations: Import 70 Case Study: (the Struvite nuisance) SS4 6000 5000 Lin (Counts)

4000 3000 NH4MgPO46H2O 2000 1000 0 12 20 30 40

50 60 70 2-Theta - Scale SS4 - File: SS4new.raw - Type: 2Th/Th locked - Start: 4.000 - End: 79.994 - Step: 0.016 - Step time: 403.5 s - Temp.: 20 C - Time Started: 13 s - 2-Theta: 4.000 - Theta: 2.000 - Chi: 0.00 - Phi: 0.00 - X: 0.0 m Operations: Y Scale Add 292 | Import 01-071-2089 (C) - Struvite - MgNH4PO4(H2O)6 - Y: 55.70 % - d x by: 1. - WL: 1.5406 - Orthorhombic - a 6.94100 - b 6.13700 - c 11.19900 - alpha 90.000 - beta 90.000 - gamma 90.000 - Primitive - Pmn21 (31) - 2 - 477. 80 How do I get access to powder XRD? Do you have the occasional sample? We do it for you Do you have frequent samples?

You get trained Involves some paperwork, Booking possible via Calpendo upon approval Subscription to the X_ray-facility users list with currently 115 members Single X-Ray diffraction Xcalibur single crystal diffractometer SuperNova dual wavelength single crystal diffractometer (1 South ) 1000 10 20 30 d=2.64193 2th=33.904

40 d=1.66155 2th=55.240 d=1.61645 2th=56.919 50 Phase identification / comparison d=1.55781 2th=59.270 60 d=1.27466 2th=74.360 d=1.29550 2th=72.967 d=1.32826 2th=70.892

d=1.37034 2th=68.406 d=1.44601 2th=64.377 d=1.42740 2th=65.320 d=1.49986 2th=61.805 d=1.48072 2th=62.694 d=1.58164 2th=58.291 d=1.54011 2th=60.021 d=1.80439 2th=50.542 2000 d=1.70916 2th=53.576

d=1.92356 2th=47.213 d=1.99988 2th=45.309 d=2.10754 2th=42.876 d=2.22140 2th=40.579 d=2.30103 2th=39.116 d=2.55251 2th=35.129 d=2.51346 2th=35.693 d=3.16719 2th=28.152 d=2.96768 2th=30.088 4000

d=2.86049 2th=31.244 Lin (Counts) 3000 d=3.06544 2th=29.107 d=3.70582 2th=23.994 d=4.19276 2th=21.173 d=8.70358 2th=10.155 d=2.96991 2th=30.065 Powder XRD vs single crystal XRD ZrO2

d=1.81858 2th=50.121 Crystallisation ZrO2 - File: ZrO2new.raw - Type: 2Th/Th locked - Start: 10.000 - End: 80.041 - Step: 0.016 - Step time: 672.5 s - Temp.: 21 C - Time Started: 7 s - 2-Theta: 10.000 - Theta: 5.000 - Chi: 0.00 - Phi: 0.00 - X: 0.0 Operations: Import 70 Unit Cell: a,b,c, a, b, g, b, gb, g, b, gg Intensity Data Collection

Data Reduction 0 2-Theta - Scale 80 Structure Solution Structure Refinement Tables Graphics What can we do? (Single crystal XRD) Full structural analysis atomic positions in 3-D interatomic bond lengths and angles packing models hydrogen bonding

Determination of absolute structure (chirality), relevant for chiral and pharmaceutical compounds Investigation of phase transitions in crystals as function of temperature Determination of polymorphs electron density studies Single crystal X-ray structure Asymmetric Unit Unit Cell P 21/n What do we use? (Thermal, Elemental and Materials analysis) Differential Scanning Calorimetry (DSC) (1 South) Atomic Absorption (AA) Spectrometer (1 South) CHN Elemental Analyser (out-sourced) Gel Permeation Chromatography (GPC)

Dynamic Mechanical Analyser (DMA) Thermogravimetric-Differential Thermal-Evolved Gas Analyser (TGA-DTA-EGA) Microcalorimeter Surface area and porosity analyser (All in 5 West) What do we use? (Materials Characterisation) Thermal and Mechanical Analysis: TGA + Mass Spec for evolving gas analysis + DTA/DSC Microcalorimeter Dynamic Mechanical Analyser Gel Permeation Chromatography Surface & Porosity Analyser (BET) (all in 5 West) What do we use? (Materials Characterisation)

For the characterisation of: - Thermal stability and decomposition with temperature - Thermodynamic properties: heat capacity, melting point, glass transition - Quantity of remaining moisture/solvent - Pore size distribution and surface area - Mechanical properties (stiffness, damping) in temperature or humidity conditions - Molecular weight distribution of a polymer CCAF team CCAF team Mass spectrometry: Anneke Lubben (5 West), Shaun Reeksting (5 West and 3 South), and Christian Rehbein (5 West) NMR: John Lowe (1 South), Catherine Lyall (1 South), and Tim Woodman (9 West) X-ray diffraction:

Gabriele Kociok-Khn and Alan Carver (both 1 South) Thermal and elemental analysis: Alan Carver (1 South) Materials characterisation: Rmi Castaing (5 West) Admin: Wai Wolfe CCAF team Mass Spectrometry: 25 years+ of experience Anneke Lubben, Shaun Reeksting, Christian Rehbein NMR: 50 years+ of experience John Lowe, Catherine Lyall, Tim Woodman X-Ray Diffraction: 25 years+ of experience Gabriele Kociok-Khn and Alan Carver Thermal and elemental analysis: 15 years+ of experience Alan Carver Materials Characterisation: 5 years+ of experience Rmi Castaing (5 West and 1 South)

How do I get access to all of this? How do I get access to all of this? Talk to us! And then get trained to use them.. How do I get access to all of this? Talk to us! 01225 384173 www.bath.ac.uk/ccaf Individual CCAF team members, or [email protected] How do I get access to all of this?

Talk to us! Anneke Lubben: [email protected], 5W 2.33 Shaun Reeksting: [email protected], 5W 2.31a Christian Rehbein: [email protected] John Lowe: [email protected], 1S 0.46 Catherine Lyall: [email protected], 1S 0.46 and 9W NMR suite Tim Woodman: [email protected], 5W 3.4 Gabriele Kociok-Khn: [email protected], 1S 1.35a Alan Carver: [email protected], 1S 1.35a Rmi Castaing: [email protected], 5W 2.31a

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