Analytical Instruments

VIBRATING SAMPLE MAGNETOMETER

Make: Lake Shore: Model: 7404

The magnetic moment measurements of compounds are made with this machine. This is a nondestructive technique. The magnetic susceptibility value is helpful in the determination of the oxidation state of paramagnetic ions.

When a sample is vibrated in a homogenous magnetic field, a moment is induced in the sample. If this sample is made to undergo sinusoidal motion as well, an electrical signal is induced in suitably placed stationary pick up coils.

Essential Specification: Vibration Frequency: 82.5 Hz; Magnet: 4” ( 2” at Pole face); Max. Field : 15 kGauss; Moment range: 1µemu – 56 emu; 80-1400 K temperature.

Sample required: 30-50 mg. For single crystal measurements, the dimensions of the crystal should be less than 2.5 mm.

Applications: The magnetic susceptibility data is used in characterizing magnetic property of materials, catalysis, superconductivity and transition metal chemistry.

UV-VIS-NIR SPECTROPHOTOMETER
Make: Varian Model: 5000

The UV-VIS-NIR spectrum is due to the electronic transitions and vibrational modes of the molecule. This is characteristic of a compound. Qualitative and quantitative estimations of compounds are possible by this non destructive technique.

The absorption (A) of a solution at a particular wavelength is given by Beer-Lambert's law A=ect where c is the concentration of the compound , t is the thickness of the cell and e is the molar extinction coefficient characteristic of the compound at a given wavelength. This principle is used for quantitative measurements.

Essential Features: Wave length Range : 175 nm to 3300nm; Resolution: 0.1 nm, Maximum Absorption: 8(abs).

Attachments: Diffuse Reflectance Accessory; Absolute Reflectance Accessory ; Sample Transport Accessory ; Temperature Controller

Sample required: 50 mg. Solvent must be specified for solution studies.

Applications: Qualitative and quantitative studies of materials and study of molecular structure, reaction kinetics, defect solid state, color centers, etc.

FOURIER TRANSFORM INFRARED SPECTROMETER
Make: Thermo Nicolet Model:6700

The infrared spectrum originates from the vibrational motion of the molecule. The vibrational frequencies are a kind of fingerprint of the compounds. This property is used for characterization of organic, inorganic and biological compounds. The band intensities are proportional to the concentration of the compound and hence qualitative estimations are possible. The IR spectroscopy is also carried out by using Fourier transform technique.

The interference pattern obtained from a two beam interferometer as the path difference between the two beams is altered, when Fourier transformed, gives rise to the spectrum. The transformation of the interferogram into spectrum is carried out mathematically with a dedicated on-line computer.

The spectrometer also works under purged conditions. Solid samples are dispersed in KBr or polyethylene pellets depending on the region of interest. Signal averaging, signal enhancement, base line correction and other spectral manipulations are possible.

Essential Specification: Wave number range: 5000 to 700 cm -1 and 700 to 50 cm -1 (Covering IR & FAR IR); Resolution: 0.1 cm -1.

Sample required:50 mg, solid or liquid.

Applications:Infrared spectrum is useful in identifying the functional groups like -OH, -CN, -CO, -CH, -NH 2, etc. Also quantitative estimation is possible in certain cases for chemicals, pharmaceuticals, petroleum products, etc. Resins from industries, water and rubber samples can be analyzed. Blood and food materials can also be studied. Reaction mechanisms and concentration studies are done.

SPECTROFLUROMETER
Make: Jobin Yvon
Model :FLUOROLOG - FL3-11

Fluorescence is the phenomenon in which absorption of light of a given wavelength by a fluorescent molecule is followed by the emission of light at longer wavelengths. The distribution of wavelength-dependent intensity that causes fluorescence is known as the fluorescence excitation spectrum, and the distribution of wavelength-dependent intensity of emitted energy is known as the fluorescence emission spectrum.

In fluorescent materials, the excited state has the same spin as the ground state. If A * denotes an excited state of a substance A, then fluorescence consists of the emission of a photon:

A *--> A + hν,

where h is Planck's constant and is the frequency of the photon. The quantum yield ø of a fluorescent substance is defined by:

ø= number of photons re-emitted/number of photons absorbed

Usually the absorbed photon is in the ultraviolet, and the emitted light (luminescence) is in the visible range. Fluorescence is named after the mineral fluorspar (calcium fluoride), which exhibits this phenomenon. There are many natural and synthetic compounds that exhibit fluorescence, and they have a number of applications:

The JY Fluorolog-FL3-11 provides optimum performance for highly scattering samples such as proteins, Membranes and Solid samples. Both excitation radiation and emitted radiation can be scanned.

Essential Specifications: Source-Xenon Lamp 450W; Range 180-1550 nm; Detector PMT for UV & Visible (180 to 850 nm) region and Cooled detector for IR region 800-1550 nm; Resolution 0.2 nm (maximum at specific wave lengths); Software DATA MAX / GRAMS/31 Pulsed Nano-LED sources available to excite sample at 295/460/560 nm for life time studies.

Samples required: 5 ml of the sample solution or 5 to 10 mg. of solid sample, dissolved solids Biological samples and thin films etc.

Applications: 1) Fluorescence detection of highly scattering samples; 2) Quantum Yield calculations; 3) Characterizing complex mixtures via Synchronous scanning; 4) Polarization studies.

SCANNING ELECTRON MICROSCOPE
Make: Hitachi, Model: S-3400N

SEM facilitates the observation of very fine details (high resolution) of materials and good focus over a wide range of specimen surface (large depth of field). It also produces clear image of specimen ranging from object visible to the naked eye to a structure spanning few nanometers. Besides its use in studying soils, sedimentary particles, rock materials, synthesized compounds, and biological materials, it also helps to elucidate the architecture and evolution of microfossils. The Energy dispersive X-ray analysis attachment (Thermo SuperDry II) is used to carryout semi quantitative elemental analysis of the samples. A new feature, the Cathedoluminescence detector is installed recently.

Essential Features: Resolution: 3nm@30kV HV mode; 10nm @3 kV HV mode

Detectors: Secondary Electron; Semiconductor BSE (Quad type)*

Magnification: 5x to 300,000x;

Vacuum System: TMP & Rotary to 1.5 x 10 -3 Pa

Specimen Stage: Motorised 5-axis, Eucentric

Specimen height: 80mm at 10mm W.D.

EDX: Peltier cooled X-ray head from Thermo, USA

CLD: Cathedoluminescence detector

WAVE LENGTH DISPERSIVE X-RAY FLUORESCENCE SPECTROMETER (WD-XRF)
Make: Bruker , Model : S4 PIONEER

X-ray fluorescence analysis is a fast, non-destructive and environmentally friendly analysis method with very high accuracy and reproducibility. All elements of the periodic table from Beryllium to Uranium can be measured qualitatively, semiquantitatively and quantitatively in powders, solids and liquids. Rhodium is used as the standard anode material. The tube and generator are designed for a permanent output of 4 kW. The detector is scintillation counter and proportional counter. Besides the standard collimators with aperture angles of 0.15° and 0.46° two additional collimators can be installed to optimize the measurement parameters, depending on the application. A 0.077° collimator is available for high resolution measurements (e.g. with LiF (420). Collimators with a low resolution (e.g.1.5 – 2.0°) are advantageous for light elements such as Be, B and C as the OVO-Multilayer’s angle resolution is limited.

The software is SPECTR Aplus Software Package for X-ray Spectrometers Version 1.6. At present using WD-XRF almost all chemical elements of the periodic system in solids or powders can be analyzed.

400 MHz FOURIER TRANSFORM-NUCLEAR MAGNETIC RESONANCE
Make: Bruker Model : Avance-II

Sophisticated multinuclear FT NMR Spectrometer model Avance-II (Bruker) is the latest acquisition in the Centre. The instrument is equipped with a cryomagnet of field strength 9.4 T. Its 1H frequency is 400 Mhz, while for 13C the frequency is 100 MHz. It is equipped with automatic sample changer.

The instrument is accompanied by TOPSPIN NMR data system and features complete spectrometer control for sophisticated multipurpose applications. Other highlights being, a multicolor displaygradient amplifier accessory, auto shimming auto tuning and homo-hetronuclear de-coupling with 0.005Hz offset result.

A sensitive 5 mm multinuclear probes like BBO and inverse probe allow to study a large number of NMR sensitive nuclei such as 11B, 29Si, 31P, 59CO, 119Sn. Instrument has facility to conduct experiments in the range of -150 to +180 oC.

Following experiments can be carried out on this instrument:

1. 1D 1H and 13C NMR Spectrum.
2. Homonuclear Decoupling (Proton).
3. Solvent suppression experiment.
4. Heteronuclear Gated Decoupling experiment.
5. Heteronuclear Inverse Gated Decoupling experiment
6. 2D COESY and NOESY Experiments
7. DEPT-135, DEPT-90 and DEPT-45 experiments
8. HMQC
9. HMBC

Sample Requirements

1. Samples are accepted in solid or liquid form.
2. Compounds should be highly pure and soluble in commonly available solvents (chloroform, DMSO).

For 1H NMR sample quantity should be 5 to 10 mg and for 13C and other nuclei 40 to 50 mg.

THERMAL SYSTEM (TGA-DTA / DSC)
Make: TA instruments, Model : Q600 SDT and Q20 DSC

Thermal system consists of a group of techniques in which the thermal property of a substance is measured as a function of temperature, while the substance is subjected to a controlled temperature program. These technique include change in weight - Thermogravimetry (TG), temperature difference - Differential Thermal Analysis (DTA) and heat flux difference - Differential Scanning Calorimetry (DSC).

Widely used for development of polymers, metals and alloys, glass and ceramics, building materials, clay and minerals, fossils, quality assurance and control, process optimization, failure analysis and nuclear fuels by determining

Characteristic transition temperatures and enthalpies
Thermal and oxidative stability
Reaction steps and kinetics
TA Instruments Q 600 SDT : Simultaneous Thermal Analyzer
Simultaneous TG-DTA measurements
Temperature range: RT to 1600 0 C (SiC furnace)
TA – Q20 DSC Differential Scanning Calorimeter
Temperature range: - 180 0 C to 725 0 C

Sample Requirements: Sample required is about 10-80 mg for TG/DTA & 10-30 mg for DSC. Samples should be non-explosive and non-corrosive.

GAMMA RAY CHAMBER

Gamma chamber 5000 is a compact, portable, self-shielded type of a Co-60 Gamma Irradiator. Its design conforms to American National Standards ANSI-N433.1, 1977 for safe design and use of self contained Dry Source Storage Gamma Irradiator (category-1) Atomic Energy Regulatory (AERB), India.

Essential Specifications :

Maximum Co-60 source capacity : 518 TBq (14,000 Ci)

Dose rate at maximum capacity : 9.5 kGy/hy (0.95 megarad/hr)

Dose rate uniformity : Radial +25% or better

and axial -25% or better

Irradiation volume : 5000 cc approx

Size of sample chamber : 17.2 cm (dia) 20.5 cm (h)

Shielding material : Lead & Stainless

Minimum irradiation time: : 6 seconds

PLANETARY MONOMILL
Make : Fristch
Model : Pulverisette-7 (Monomill)

Planetary monomill (Widely known as Ball mill) is used to crush and disintegrate sample by the centrifugal forces due to the rotation of the grinding bowl about its own axis and due to the rotating support disc rotating on opposite direction. The resulting frictional effect, the grinding balls running along the inner wall of the grinding bowl, and impact effect, the balls impacting against the opposite wall of the grinding bowl.

The model is applicable for quick dry or wet grinding of inorganic and organic samples for analysis quality control, material testing and mechanical alloying.

Essential Specifications :

Grinding Bowl: Capacity: (12&45 ml)

Material: Silicon Nitride & Tungsten Carbide

Balls:Size:(10mm & 5 mm dia )

Material: Silicon Nitride & Tungsten Carbide

Speed: 100- 800 RPM

High performance Liquid chromatography (HPLC)
Make: Shimadzu
Model: Prominence

In general the analytical HPLC is used to obtain information for the identification, quantification, and resolution of a compound synthesized. Our instrument being a semi preparative model, in addition to the analysis, it can also be used in the process of isolation and purification of compounds with a good degree of solute purity and the throughput. HPLC systems are currently used in a wide variety of fields. Higher reliability in analysis data and higher efficiency in total analysis workflow are required for faster development of new drugs, for better food safety, and for meeting higher standards in environmental regulations.

Essential Specifications:

I Pump: Quarternary Pump
No. of eluents - 4
Composition range - 0-100%
Composition accuracy - ± 0.5% (independent of Back Pressure)

II. Sample Injection System with - For Analytical injector
Dual injector option, for 50/100/200 :l/ 100ps
Analytical & Semi-prep analysis for semi preparative 5ml /100ps

III. Degasser (optional) - In line
Flow rate Analytical - 0.2 - 5.0 ml/min
Semi-prep. analysis - 20-40ml/min

IV. Detectors

1. UV –VIS Detector

2. FID

3. PAD

Broad band Dielectric Spectrometer (BDS)
Make: NOVOCONTROL Technologies GmbH & Co. Germany
Model : Concept 80

The parameters of dielectric constant, permitivity and conductivity are important for material Science and engineering research. BDS can be used for measuring dielectric constant, permittivity and conductivity of liquid, powder and solid samples as a function of frequency or temperature, to understand the relaxation behavior of molecules. It covers wide ranges of frequency and temperatures that may be appropriate for investigation the different scales of molecular motions.

Essential Specifications:

Parameter	Alpha Analyser	Beta Analyser

Frequency	3x10-5 to 2x107 Hz	2 x 106 to 3x109 Hz

Capacity	1fF to 1 F

Impedance	0.01 - 1014 Ω	0.1 - 105 Ω

Loss factor tan(δ)	accuracy < 3·10-5, resolution 10-5	< 3x10-3

Temperature controllers:
Quatro cryo system (for LT measurement) Range : -180 °C to 400 °C.
Novotherm High temperature attachment Range : RT to 1100 °C

Electron Probe Microanalyser
Make: CAMECA, France
Model : SX 100

The principle of an electron microprobe is that if a solid material is bombarded by an accelerated and focused electron beam of sufficient energy it can liberate both matter and energy from the sample. These electron-sample interactions mainly liberate heat, but electrons and x-rays are also generated. Of most common interest in the analysis of materials are secondary and back-scattered electrons, which are useful for imaging a surface or obtaining an average composition of the material. X-ray generation is produced by inelastic collisions of the incident electrons with electrons in the inner shells of atoms in the sample; when an inner-shell electron is ejected from its orbit, leaving a vacancy, a higher-shell electron falls into this vacancy releasing some energy in the form X-rays. These X-rays are characteristic of the element and are quantized to determine the elemental composition. EPMA analysis is considered to be "non-destructive"; that is, X-rays generated by electron interactions do not lead to volume loss of the sample, so it is possible to re-analyze the same materials more than one time.

Essential Specifications:

Number of WDS: 4
Imaging: Optical with Reflected and Transmitted Polarized light
Secondary Electron Imaging
Back Scattered Electron Imaging
Cathode Luminescence Imaging
Number of Crystals: 8 (TAP-2, PET, PC1, PC2, LIF, LLIF, LPET)
Analysis: GEO – Quant, Geo-Chrono

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