1

Sophisticated Analytical Instrumentation Facilities (SAIF) Centre

(Sponsored by Department of Science and Technology, Govt. of India, New Delhi) in

UNIVERSITY SCIENCE INSTRUMENTS CENTRE (USIC), KARNATAK UNIVERSITY, DHARWAD (KUD). INDIA.

Phone : +91-0836-2215275, Fax : +91-0836-

e-mail : usicofficekud@rediffmail.com or ________________, website :kud.ac.in or ______________

About SAIF Centre, USIC, KUD.

USIC, KUD was established in 1976 with the initial support of UGC. After the completion of successful FOUR decades in globalised and liberalized modern Indian scientific research era, the USIC, KUD spreading the support and services and extended scientific R&D culture in North Karnataka region of South India. Further requirement or demand with higher end sophisticated instruments for R&D activities KUD taking decision for future vision for expansion or up gradation of USIC, KUD with support or sponsorship of DST, New Delhi. Main purpose of SAIF program is solve the problem of non-availability of sophisticated instruments in respective institutes may not come in the way of Researchers/scientists in pursuing R&D activities requiring such facilities and the able to keep pace with developments taking place globally. Also SAIF centre is to provide facility of data collection from sophisticated analytical equipments to scientific community for their advanced research with nominal charges. The facility has grown into a major centre for spectral measurements, molecular and crystal structure determination and materials characterization. KUD SAIF centre having high end equipments such as Filed Emission Gun Scanning Electron Microscopy (FEG-SEM), Environmental Scanning Electron Microscope with EDAX, Transmission Electron Microscope (TEM) 200kV, X-Ray Diffractometer (XRD), 400MHz FT-NMR Spectrometer (FT-NMR) etc facilities, which are normally not available at many institutes due to high cost of the instruments. We are happily said that, our USIC_KUD SAIF Centre having such good facilities with well trained technical staff for handling instruments.

Vision: To serve the industry and academic institutes pursuing scientific research for building a better

society by providing total scientific solutions. Mission: To bridge the gap between industries and academic research institutes by spreading awareness of

the importance of Material Analysis.

Major Objectives of the SAIF : To provide instrument facilities to Research institutions, Universities and industries within and outside

Karnataka State. To help and provide consultation/R&D facilities to nearby industries.

2

To establish linkages with various National level and other reputed laboratories so as to collaborate in research projects.

To conduct training programs, workshops etc.

ADMINISTRATION:

The day-to-day functioning of the SAIF is overseen by the Director, USIC or Head, SAIF program, who is a faculty member of the Science (faculty) Department of the University. The Facilities Management Committee (FMC) oversees and guides the activities of the SAIF. The FMC at SAIF Centre, Karnatak University, Dharwad consists of the representatives of DST and experts to be nominated by the University in consultation with DST. The FMC also examines the deployment of staff and equipment from time to time with a view to enhance productivity and efficiency, and to avoid duplication. It scrutinizes the annual budget before it is submitted to DST. It approves and forwards progress report of SAIF to DST. It also approves induction of equipment from other sources that are to be operated under the control of SAIF. Once in a year, a National Steering Committee meets to allocate budgets to the SAIF's and also to discuss the ways and means of improving the services to research and industry. Once in five years, a Review Committee appointed by the DST examines the achievements of each SAIF, and also interviews the user community to assess the effectiveness of these Facilities. It is gratifying that SAIF, USIC_KUD has always been adjudged as one of the best run SAIFs and often looked upon as a pacesetter. SAIF FACILITIES: SAIF at the USIC, KUD is equipped with sophisticated instruments to carry out spectral measurements, structure determination and chemical analysis. Following details about instruments description. 1. Field Emission Gun Nano Nova Scanning Electron Microscope (FEG-SEM) 450 with

EDAX

Model: TEAM EDS Make: EDAX Inc, USA

Resolution: 1.0nm at 15kV

1.4nm at 1kV 3.5nm at 100V

Accelerating Voltage: 20V to 30Kv Beam current: upto 200nA Magnification: X25 to X10,00,000 Sample Navigation:

A 5-axes motorized x-y-z tilt-rotate stage with Eucentric tilt. Tilt +75 degrees to -15 degrees

Field Emission Gun: Ultra-high brightness Schottky emitter

Description: The Nova Nano FEG-SEM 450 is a versatile high resolution low-vacuum Field Emission Gun Scanning Electron microscope capable of producing very high resolution images of the surface of a sample. It has a wide range of applications in biological and materials

3

science in which researchers wish to visualize and analyze the surface of a sample over a wide range of magnifications. It can be used to image over a large surface area of bulk materials as well as thin films.

The FEG SEM has two modes of operation: high vacuum and low vacuum. A major feature is that it does with a single tool, what used to require multiple systems. The resolution achievable under different modes is 1-nanometers. The EDAX (with mapping system) facility provided with the instrument enables the qualitative and quantitative analysis of elements from samples.

Type of samples: Inorganic nanomaterials, low conductive nanomaterials, nanomaterial dispersions, biological samples.

Applications: Three-dimensional details of samples at very high resolution can be obtained. Examples of specimens that will be imaged include three dimensional collagenous scaffolds which are used in tissue engineering, cells adhering to and growing in tissue engineering scaffolds, nanoparticles produced by biomaterials used in hip and knee replacements, nanoparticles in body tissues and in environmental samples, fibrils of proteins that cause disease such as amyloid and prion proteins and proteins that cause muscles to contract, bacteria, virus and ultra structural details of surface of biological samples. Detection and quantification of elements down to boron.

• TEAM EDS Analysis system with octane SDDs deliver on the full promise of SDD technology – high speed analysis with no sacrifice in the quality of the data. • Silicon drift detector (SDD) provides excellent low energy performance • Smart diagnostics and smart acquisition facilitate optimized collection and analysis condition • Quantification for elements starting with Boron (B) • Elemental mapping with supporting phase data. • Maximum energy resolution of 129eV • Measured according to ISO 15632 • This system is useful to academic and leading industries in the semiconductor, metals, geological, pharmaceutical, bio-materials, ceramics, etc. • Quantitative analysis at mapping speeds up to 200,000 cps

2. SCANNING ELECTRON MICROSCOPE (SEM) With EDS Specifications: Electron Optical System: 1. Emission current:0 to 200 μA 2. Accelerating Voltage: 0.2 to 30 kv 3. Resolution: With LaB6 filament 2nm at 30 kv, With W filament 3.5nm at 30 kv

Scanning System: 1. Magnification:10x to 400000x or higher 2. Automatic scaled micron marker

4

Specimen Handling: 1. Eucentric goniometer stage 2. Specimen movement: X=50mm,Y=50mm 3. Rotation: n x 360 degrees 4. Z movement: 25mm internal & external

Electron Detectors: 1. Secondary and back scattered electron detectors

Brief Description: Scanning Electron Microscope XL 30 ESEM with EDAX: Resolution : upto 2; Acc. voltage: 30 kV;

Magnification: upto 2,50,000x A versatile electron microscope that combines high vacuum, low vacuum and Environmental modes

into one instrument Highly flexible Capability of operation at higher gas pressure in the chamber, pure secondary electron detection

and full compatibility with water vapor, to prevent hydrated samples from drying out Important for study of surface topography EDS system is important for chemical analysis at micro level and has better resolution for

qualitative and quantitative analysis.

Applications: ESEM + EDS is useful for R & D work on structural as well chemical studies of various alloys, carbon fibers, semiconductor compounds and 3-D surface study of different biological samples, etc.

Surface and Structural Materials Analysis: Microstructural characterization includes the analysis of materials, polymers, films, coatings, pharmaceuticals, raw materials, metals, plastics, ceramics, glass, food, dust, contaminants and other products. The SEM labs provide elemental analysis of solid samples, impurities, and the identification of physical and chemical defects. The laboratories provide analytical expertise to support research, failure analysis, troubleshooting, quality control and other requirements.

Energy Dispersive X-ray Analysis : SEM/EDAX analysis of small particles by scanning electron microscopy and energy dispersive X-ray analysis (EDAX) is possible without destruction or injury to the sample. SEM/EDAX provides qualitative elemental analysis and element localization on samples being analyzed.

3. Transmission Electron Microscope (Tem) With CCD Camera

Model: Tecnai 20, Make: Philips, Holland

Specifications: • Electron Source:- W emitter and LaB6 • Accelerating Voltage:- 200 kv • Objective lens:- S- TWIN • Point Resolution: 0.27 nm or better • Line Resolution : 2.0 nm or better • Magnification : 25x to 750000x or higher

5

• Single tilt holder with CCD Camera Applications: • Morphology, crystal structure, interface structure, crystal defects can be studied • Study of biological micro organisms. • Particle Size measurement • Liposomes • Single crystal Diffraction • Virus & Bacterial study Transmission Electron Microscope is highly advanced and state-of-the-art instrument. • It uses electron beam optics to achieve very high magnifications of the order of 750,000x • It collects a wide range of signals carrying valuable information. Tecnai 20 has been especially designed to acquire and process these signals efficiently and effectively. • The combination of high-resolution imaging, bright field, dark field, electron diffraction and detailed microanalysis makes the Tecnai 20 a key to material analysis. • Tecnai 20 has S-TWIN objective lens for high resolution, while maintaining high tilts (maximum 40° ) and a Comp Stage for accurate specimen control and exceptional mechanical stability. • The fundamental understanding of a material’s properties starts with a thorough characterization of the material morphology, crystal structure, interface structure, surfaces and defects all have their influence on the properties of material. Transmission Electron Microscope has proven to be a very powerful technique for studying a range of general and advanced materials down to the nm level. 4. X-RAY DIFFRACTOMETER

Model: Xpert MPD, Make: Philips, Holland

Description:

XRD Diffractometer (powder) Philips Xpert MPD Range (2θ): 3º to 136º; X-ray tube: Cu; JCPDF database; 2θ vs intensity plots/X-ray diffractograms; search match facility with JCPDF data for qualitative analysis. X’PERT MPD is specifically designed for powder diffractometery.

X-ray Diffractometers that are commonly referred as XRD are quite useful for study of crystalline nature of materials. X-Ray analysis technique is a non-destructive testing

method Useful instrument for research work and analysis of various types of materials like Powder Analysis,

Texture Analysis, Stress Analysis, High Resolution Analysis.

Specifications:

Source: Cu target X-Ray tube

6

X-Ray Power: 2KW Detector: Xe-filled Counterate or Proportional detector Software: JCPDF database for powder diffractometry Goniometer Operation Modes: Vertical & Horizontal Accuracy: ±0.0025 2º θMeasurement range: 3o to 136º Diffractometer radius: 130 to 230 mm

Applications:

X-ray diffraction is widely used to identify crystalline phases, measure crystallite sizes, lattice parameters, orientation and provide quantitative phase analysis and atomic coordinates. This information is important for relating the production of a material to its structure and hence its properties. As well as being of academic interest, X-ray results are used in patent disputes, forensically and for quality control. Compound Identification areas:

Inorganic Materials Organic Materials Minerals Metal + Alloys Forensic Material Zeolites Explosive Materials Super conducting Material Cement Materials Correction Product Polymer Material Detergent Product Pigments Pharmaceutical Product Ceramic Materials Kidney Stones

5. 400 MHz FT – NMR Spectrometer (Liquid & Solid Multi Nuclei Probe)

Model: 400 MHz FT-NMR Spectrometer,

Make: JNM-ECZ4005, JEOL, Japan

Principle: Nuclei have spin and all nuclei are electrically charged. If an external magnetic field is applied, energy transfer takes place between base energy to higher energy level. The energy transfer takes place at a wavelength that

7

corresponds to radio frequencies. When the spin returns to its base level, energy is emitted at the same frequency. Solid-State NMR Applications: Directly collect spectra by filing the sample in sample tube in solid probe. The extremely fast (25 ns) phase, frequency and amplitude switching characteristics of the AVANCE III are of great benefit for advanced solid state NMR experiments. Modulated decoupling and recoupling sequences are easily programmed and accurately executed with high-precision RF phase and frequency stability.

Applications: The FT- NMR platform for life-science and materials research study. Used for pharmaceutical, biotechnology, chemical sciences, metabolomics, nutritional science and molecular diagnostics research. The technique is useful for structure identification of Organic, Inorganic and Polymer compounds. Description: JNM-ECZ4005 400 Mhz FT-NMR has been installed in SAIF/KUD/M during Feb-2017.

-Observation Nuclei : 1H/19F, 31P to 15N, 39K, 109Ag

-Auto Tuning/matching range : all observation nuclei

-Observation frequency : 1H 400 Mhz, 13C 100 Mhz

-Sensitivity for 1H : 500 or more (0.1% ethyl benzene)

-Sensitivity for 1H: 500 or more (ASTM)

-Variable temperature shim : Digital matrix shim, 21 items controlled

-Room-temperature shim : Digital matrix shim, 21 items controlled

Liquid He holding time : Year Hold magnet

-Liquid N2 holding time : 14 days hold time

Consisting of

NM-6001054L1 ; 400 MHz Narrow Bore Spectrometer

NM-660105w ; ECZ Standard Software

NM-02850ACA ; Air Adaptor Unit SLPO7

NM-03510TH5 ; 400 MHz 5mm FG/TH Auto Tube Probe Multi Nuclear Probe

NM-0459OSCM ; Super conduction Magnet 400/54 year Hold (365 days He Hold Magnet)

Vibration Proof Table

Z400 Workstation English

8

Auto Tuning Unit ; Auto tuning unit 5, 5mm standard NMR tubes with caps

Flow meters, branded hose, Gloves and balloons

Variable temperature Accessory ; Liquid Nitrogen based

10L Dewer

10L Dewar Heater 5

Auto sampler changer 30 sample

SOPHISTICATED ANALYTICAL INSTRUMENT FACILITY (SAIF):

The Head, SAIF

• Sophisticated Analytical Instruments are vital for pursuing research in many areas of modern science and technology. The DST has setup SAIFs in different regions of the country to provide the instruments to research workers to enable them to pursue R&D activities. The SAIFs are equipped with expensive instruments and are accessible to all users irrespective of whether they belong to the host institutes or are from outside the host institutes.

• Sophisticated Analytical Instrument Facility (SAIF) scheme by the DST has been sectioned to Karnatak University. The SAIF is being implemented at USIC and the sanctioned facilities include 400 MHz FT-NMR, Powder X-Ray Diffractometer & Scanning Electron Microscope(SEM) with EDS/WDS and essential sample preparation accessories.

OBJECTIVES OF SAIF :

• To carry out analysis of samples received from the research scholars of the same university and other universities and scientists/ institutes.

• To provide facilities of sophisticated analytical instruments to research scholars, scientists and other users from academic institutes. R&D laboratories and industries to enable them to carry out measurements for R&D works.

9

• To acquire and develop capability for preventive maintenance and repair of sophisticated instruments.

• To organize short term courses/ workshops on the use and application of the instrument and analytical techniques.

• To train technicians for maintenance and operation of sophisticated instruments.

PROGRESS :

• DST has sanctioned Rs.5.5 Crore to setup SAIF vide letter No.SR/RS/DH-1/20132 Dt:15/05/2013

• DST has released Rs.2 Crore during financial year 2014-15 for the procurement of instruments agreed by DST

• Purchase order has been placed on M/s.Jeol India Pte Ltd., Singapore to procure 400 MHz FT-NMR Spectrometer and it will be installed shortly.

SAIF- Advisory Committee Members :

• Vice Chancellor, Karnatak University, Dharwad - Chairman

• Registrar, Karnatak University, Dharwad

• Finance Officer, Karnatak University, Dharwad

• Prof. K.P. Ramesh, Department of Physics, IISc, Bangalore

• Director, P.E.M.B., Karnatak University, Dharwad

• Dean, Faculty of Science, Karnatak University, Dharwad

• Prof. J.R. Tonannavar, Department of Physics, K.U.D.

• Prof. M. V. Kulkarni, Department of Chemistry, K.U.D.

• Prof. H.N. Murthy, Department of Botany, K.U.D.

• Prof. Mrs.K. Pancharatna, Department of Zoology, K.U.D.

• Prof. N. M. Badiger, Director, USIC, Karnatak University, Dharwad

. Prof. N. M. Badiger, The Head, SAIF, Karnatak University, Dharwad, Convener

10

Interested researchers, scientists and engineers from Academic Institutions, Research and Development centres , Universities are invited to get their needs in testing, analysis and measurement of samples etc. The Director/Head, Sophisticated Analytical Instrument Facility (SAIF) Centre, USIC, Karnatak University, Dharwad-580 003. India e-mail: usicofficekud@rediffmail.com phone: +91 836 2215275