Research_

# Chemistry facilities

State-of-the-art facilities for research and experimentation
Our chemistry facilities provide support and instrumentation for a wide range of research projects.

Housed within the School of Chemistry, our research infrastructure is supported by dedicated high-level professional and technical expertise.

### Mass Spectrometry Facility

The Mass Spectrometry Facility in the School of Chemistry provides analytical services for researchers within the school, other researchers at the University of Sydney, as well as users outside the University.

There are six mass spectrometers in the Facility and low resolution and high-resolution spectra can be obtained by most ionisation techniques. Two instruments are jointly administered with other departments.

Bookings for the Facility (including requests for training to run samples yourself) can be made through the online booking system (internal access only) or by contacting Dr Nick Proschogo.

### Bruker amaZon SL mass spectrometer (ESI, APCI, direct probe)

The amaZon is a quadrupole ion trap mass spectrometer obtained in 2015. The mass range of this instrument is m/z 50-4000 and the ion trap is ideally suited for MS/MS and MSn experiments with fast polarity switching.  Ionisation modes available include ESI, APCI (liquid and direct probe) and will include APPI (liquid and direct probe) in late 2018. The mass spectrometer can be connected to an Agilent 1100 HPLC with binary pump, diode array detector and column heater.

### Perkin Elmer Clarus 680 SQ 8 C GC/MS GC/MS (EI, CI)

The Clarus SQ 8 C is a quadrupole mass spectrometer obtained in 2016 with a mass range of m/z 4-1000 in full scan or selective ion mode. Ionisation modes include EI and CI using methane as the reactive gas. The mass spectrometer is connected to a Clarus 680 GC which can perform automated liquid injections, manual headspace and manual SPME injections.

### Bruker autoflex speed LRF MALDI-TOF mass spectrometer

This Matrix Assisted Laser Desorption Ionization – Time of Flight (MALDI-TOF) mass spectrometer was obtained in 2015. This instrument can operate in linear (1-300,000 Da) or reflectron mode. The mass spectrometer is equipped with a TLC-MALDI holder and flexImaging software to allow MALDI-imaging experiments for TLC/tissue samples prepared in Sydney Mass Spectrometry. It is capable of performing high energy MS/MS experiments using post source decay either with or without a collision cell. Polymerix software to aid in co-polymer interpretation and biotools for proteomic analysis are also available.

### Bruker Apex Qe 7T Fourier Transform Ion Cyclotron Resonance Mass Spectrometer (FTICR)

The 7 Tesla FTICR was purchased with an ARC LIEF grant in 2008. This high resolution instrument has an actively shielded, refrigerated superconducting magnet allowing a mass accuracy of <2ppm. It will be equipped with an ESI/MALDI dual source and capable of APCI (dissolved and solid probe) ionisation methods either via syringe infusion or connection with an Agilent 1100 HPLC with binary pump, diode array detector and column heater. Fragmentation options include CID (in source, in collision cell or in ICR cell) and ECD.

### Perkin Elmer Nexion 350X Inductively Coupled Plasma Mass Spectrometer (ICPMS)

The Perkin Elmer Nexion 350X Inductively Coupled Plasma Mass Spectrometer was purchased and commissioned in 2015 by the School of Geosciences and is jointly administered between the School of Geoscience and School of Chemistry. It is an instrument used to measure trace concentrations of metals and some non-metals. This instrument is set-up to handle liquid samples; therefore most samples will require pre-treatment/acid digestion and/or dilution prior to analysis. The benefits of this instrument include rapid multi element quantitative analysis, very low limits of detection, isotopic analysis and a wide dynamic range. It is equipped with universal cell technology and has Kinetic Energy Discrimination (KED) available to allow removal of molecular interferences. It is equipped with a 240 sample position autosampler for 10mL sample tubes.

### Perkin Elmer Nexion 2000B Inductively Coupled Plasma Mass Spectrometer (ICPMS)

The Perkin Elmer Nexion 2000B Inductively Coupled Plasma Mass Spectrometer was purchased and commissioned in 2018 by Sydney Nano, and is jointly administered between Sydney Nano and School of Chemistry. It is an instrument used to measure trace concentrations of metals and some non-metals. This instrument is set-up to primarily handle nanoparticles (characterisation of particle size distributions), cell culture samples (determination of attogram abundance of a metal in individual cells) or bacteria cultures. It is equipped with an ESI SC-µ DX autosampler capable of running samples off a 96 well plate or 2mL tubes.

### (Coming soon) Bruker Solarix 2xR 7T Fourier Transform Ion Cyclotron Resonance Mass Spectrometer (FTICR)

The 7 Tesla FTICR will be commissioned in late 2018. This high resolution (450,000 @ 1Hz and 400 m/z, 20,000,000 maximum resolving power) instrument has an actively shielded, refrigerated superconducting magnet allowing a mass accuracy of 600ppb. It will be equipped with an ESI/MALDI dual source and capable of nanospray (Captivespray nanoBooster source), APCI and APPI (dissolved and solid probe) ionisation methods either via syringe infusion or connection with a Waters Acquity UPLC H-Class with PDA detector. Fragmentation options include CID (in source, in collision cell or in ICR cell), ECD and ETD. SciLS software will be available to allow visualisation of MALDI-FTMS imaging experiments for TLC/tissue samples prepared in Sydney Mass Spectrometry.

#### How to submit samples

The Mass Spectrometry Facility provides analytical services for organic compounds, biochemical compounds and organo-metallic compounds. To submit a sample, please fill out the Sample Submission Form and send it with the sample to the Mass Spectrometry Facility, Room 223, Madsen Building, F09 The University of Sydney, NSW, 2006  by mail or in person.

To obtain a mass spectrum, the sample must first be ionized. The ionization techniques available in the Unit are EI, CI, MALDI, ESI and APCI at present. Each technique has its own advantages and limitations. Please consult the staff in the facility if you cannot decide which of the techniques would be suitable for your sample.

Samples should be submitted in a sample screw-cap vial or 1.5 mL Eppendorf tube labelled with a sample identification code. About 0.1 mg to 1 mg of solid or liquid samples is required. For normal EI or CI MS, solvent free and pure samples are preferred because solvents or impurities may suppress the peaks of interests and complicate the structure analysis. For MALDI, ESI, APCI, GC/MS or LC/MS, please specify solvent. For samples requiring GC/MS analysis, a GC trace and the column conditions should be provided, if possible.

#### How much does it cost?

The charges (per sample) for services performed by the Mass Spectrometry Facility are listed below:

 School of Chemistry The University of Sydney Non-University of Sydney Low resolution ESI/APCI/APPI/Solid probe/EI/CI/GCMS $15$30 $60 Low resolution MALDI$20 $40$75 High Resolution (Accurate Mass) ESI/APCI/APPI/Solid Probe/MALDI1 $50$75 $100 ICPMS2$5 $10$20

1Special rates will also apply for investigators involved in the ARC LIEF grant used to obtain the FTICR.

2NexION 350X School of Chemistry price is also for School of Geoscience. NexION 2000B School of Chemistry price is also for all members of Sydney Nano and this cost does not include calibration standards required for analysis.

Other services such as extensive sample preparation, data interpretation, LC/MS, MS/MS, MALDI imaging etc. will be charged by the hour in negotiation with Mass Spectrometry staff. External invoices will include an additional 10% GST charge. The costs of analysis may be discussed with the staff of the Mass Spectrometry Facility.

Non-University of Sydney charges apply to all external users, whether affiliated to the School/University or not. They also apply to any contract research or consultative work performed by members of the School or University. If in doubt, it may be discussed with the staff of the Mass Spectrometry Facility.

### Nuclear Magnetic Resonance Facility

The primary role of the Nuclear Magnetic Resonance (NMR) Facility is to provide research support to School of Chemistry staff and students, however its services are available to anybody. The NMR Facility operates a number of modern high-field NMR Spectrometers, supported by a host of ancillary infrastructure. Staff of the NMR Facility provide a range of consulting services, technical assistance and training.

Training seminars are held periodically throughout the year for NMR users covering a range of topics aimed at introductory and intermediate levels. This includes spectrometer operation and software applications.

We are able to provide consultation and assistance in experimental design, data processing and interpretation for your NMR experiments. Staff have expertise in a wide range of chemical applications, with particular interests in organic, organometallic, bioorganic and phosphorus chemistry.

Bookings for the Facility can be made through the online booking system (internal access only) or by contacting Dr Ian Luck.

#### Instruments

• nmr200 : Bruker AVANCE I 200 NMR Spectrometer
• nmr300 : Bruker AVANCE I 300 NMR Spectrometer
• nmr400 : Bruker AVANCE III 400 NMR Spectrometer
• nmr500 : Bruker AVANCE III 500 NMR Spectrometer

#### How to submit samples

Samples can be sent to us for analysis by NMR Spectroscopy. This service is not limited to School of Chemistry researchers, and we welcome enquires from all disciplines within the University, and the wider community.

All samples submitted to the NMR Facility Analysis Service should be appropriately packaged and accompanied by a sample submission form. Each sample submitted should have a unique sample code.

Please try to fill out all sections of the form, taking care to ensure that sample code information on the sample container matches that supplied on the submission form. Samples must be fully soluble in the nominated solvent for analysis to be possible. Please speak to NMR Staff if you have doubts about the solubility or correct choice of solvent for your samples.

NMR Facility Analysis Service: Sample Submission Form (PDF 7.9MB)

Samples being sent from outside the School of Chemistry should be addressed to:

NMR Facility
School of Chemistry, F11
The University of Sydney NSW 2006

#### How much does it cost?

Costs for services provided by the NMR Facility operate on a three-tiered recovery basis, covering external (non-University of Sydney), University of Sydney and School of Chemistry users. All services are charged at an hourly rate, and additional costs may be incurred for solvents and tubes.

School of Chemistry users (internal) are charged on a cost-recovery basis according to spectrometer usage and reservation logs, with solvents and tubes supplied at cost.

 External (non-University of Sydney) Analysis Service (Routine Analysis) $150 per hour Additional Processing (no data collection)$100 per hour Methods Development / Advanced methods contact for quote Consultation and Educational Services $150 per hour External (University of Sydney) Analysis Service (Routine Analysis)$50 per hour Spectrometer use by licensed users $10 per hour Training and licensing for spectrometer use$250 per person
 Solvent Cost CDCl3, CD3OD, Acetone-d6, DMSO-d6, water-d2, Acetonitrile-d3 Included in base rate High level deuterated solvents ("100%-d") $40 per sample DMF-d7, THF-d8$50 per sample

## Separations Facility

The separations facility provides chromatography support and instrumentation for a wide range of research projects. We also offer technical and analytical consulting services as well.

Bookings for the Facility can be made through the online booking system (internal access only) or by contacting Dr Cody Szczepina.

### High Performance Liquid Chromatography (HPLC) systems

Available for automated analysis and separation of complex mixtures in quantities ranging from milligram to gram scale.

Types of separation techniques available:

• Reverse phase (typically hydrophobic compounds)
• Normal phase (typically for hydrophilic compounds)
• Chiral separation (for both hydrophilic and hydrophobic compounds)
• Size exclusion (for large compounds, eg peptides and proteins)

### Liquid Chromatography-Mass Spectroscopy (LCMS)

Provides high throughput analysis including separation of mixtures and mass data of each component.

School of Chemistry users, please login via the  HPLC Separation Facility website.

Note: All users must be trained and certified before use.

### Thermophysical Properties Facility

The primary role of the Thermophysical Properties Facility (TPF) is to provide research support to School of Chemistry staff and students. TPF services are also available to external clients.

The TPF operates a number of specialist instruments capable of measuring diverse physical properties over a large range of temperatures including: Magnetic Susceptibility, Heat Capacity, Electrical Resistivity, ThermoGravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC) and Isothermal Titration Calorimetry.

Staff of the TPF provide a range of consulting services, technical assistance and training. Samples can be submitted for a range of magnetic or calorimetric measurements.

Bookings for the Facility can be made through the online booking system (internal access only) or by emaling us at: chemistry.tpf@sydney.edu.au

#### Instruments

Quantum Design Physical Properties Measurement System (PPMS) with sample measurement from 2 to 400 K in magnetic fields up to 9 T. This system is equipped with the following accessories: Vibrating Sample Magnetometer (VSM), VSM oven (measurement up to 1,000 K), AC Magnetic Susceptibility (ACMS), Heat Capacity and Resistivity options.

Quantum Design Versalab with sample measurement from 50 to 400 K in magnetic fields up to 3 T with a Vibrating Sample Magnetometer (VSM), a VSM oven (measurement up to 1,000 K), Heat Capacity and Resistivity options.

TA Instruments Discovery Thermogravimetric Analyser (TGA). Capable of collecting sample mass change from ambient to 1,200 °C with a 4-channel gas blending system and 10-7g resolution.

Perkin Elmer Pyris 1 Thermogravimetric Analyser (TGA) with a measurement range from ambient to 1000°C and 10-7g resolution. This instrument is capable of performing TGA measurements with static and dynamic gas atmospheres.

TA Instruments 2920 Differential Scanning Calorimeter (DSC) with a data collection range from 100 °C to 600 °C is capable of collecting data without the use of liquid nitrogen.

Mettler Toledo Differential Scanning Calorimeter (DSC) 823e. This instrument has a measurement range from -165 °C to 600 °C and is used to measure heat flow in a sample which can yield information about glass transition temperatures, melting and crystallisation events, oxidative stability and much more. Capable of collecting modulated DSC data.

MicroCal Isothermal Titration Calorimeter (iTC200) with a measurement range from 2 to 80 °C is used to study low volume, in solution biomolecular interactions.

#### How much does it cost?

The facility operates on a subsidised cost recovery basis for Australian academic and government clients, and on a full cost recovery basis for others. The PPMS is charged in 24 hour blocks (10am-10am) or part thereof.

The other instrument charges are per peak hour, Mon-Fri, 9am-5pm. After hours/weekend (building access only available to University of Sydney Chemistry staff and students) rates are half peak hour rates. Overnight (5pm-9am) costs the same as two peak hours. Charges listed below are for instrument use only. Extra Staff Scientist's time for training in use of the instruments and services such as running your samples for you, filling nitrogen dewars, etc. will be charged at $50/h for University of Sydney users and$100/h for external clients.

 User category PPMS daily Versalab hourly TGA DSC ITC USyd chemistry Staff/students $150$20 $9$9 $9 Other USyd users$200 $40$15 $15$15 External clients (+GST) $450$60 $30$30 $30 A relatively small extra charge, our cost price, may need to be applied for clients who use substantial quantities of consumables (e.g. PPMS VSM sample tubes are$11 each, DSC pans are $4 each. Most DSC measurements require LN2. One 50L dewar will support several measurements - 50 litre, LN2 dewar$50 – including Staff Scientist time to fill it.

All charges apply regardless of the "success" of the experiment.