Saif Instruments

C-H-N ANALYZER
FT-IR SPECTROMETER
GAS CHROMATOGRAPH – MASS SPECTROMETER
ICP ATOMIC EMISSION SPECTROMETER
THERMAL ANALYSIS DTA/TGA
THERMAL ANALYSIS DSC
UV-Vis-NIR SPECTROPHOTOMETER
SCANNING ELECTRON MICROSCOPE - ENERGY DISPERSIVE SPECTROMETER
ULTRA PURE WATER SYSTEM
X-RAY POWDER DIFFRACTOMETER
FT NMR SPECTROMETER
SINGLE-CRYSTAL X-RAY DIFFRACTOMETER
MERCURY ANALYSER




C-H-N Analyzer

The percentage of elements C, H, N, S and O in an organic compound can be individually or simultaneously analyzed over a wide range of sample matrices and concentrations with this instrument
Make/Model Elementar Vario EL III
Operation Modes CHNS, CHN, CNS, CN, N, S and O
Detection Ranges* C :0.004 – 30 mg abs (or 100%)
H :0.002 – 3 mg abs (or 100%)
N :0.001 – 10 mg abs (or 100%)
S :0.005 – 6 mg abs (or 100%)
O :0.005 – 2 mg abs (or 100%)
*Depending on samples :
Standard deviation :0.1% abs
Sample weight :0.02 mg up to approx. 1 gm
Digestion temperatures :950 – 1200°C
This instrument is ideally suited for research, quality control and quality assurance applications. Wide range of applications such as analysis of chemicals, pharmaceuticals, synthetic materials, coals, oils and derivatives, geological substances, agricultural products, environmental products etc are met with this instrument.
Samples must be non-fluorinated, non explosive, about 10-30mg for solid sample or 25 ml for liquid sample (depending on the components)


Fourier Transform Infra Red spectrometer (FTIR)

Atoms or atomic groups in molecules are in continuous motion with respect to one another. They vibrate about some mean position. IR spectrum of a compound is the superposition of absorption bands of specific functional groups. The subtle interactions with the surrounding atoms or molecules impose the stamp of individuality of the spectrum of each compound. IR absorption has numerous applications in qualitative and quantitative analysis.
Make/Model :Thermo Nicolet, Avatar 370
Spectral range :4000-400 cm -1
Resolution :4 cm –1
KBr beam splitter
DTGS Detector
HATR Assembly for convenience of measurement.
Database for identification of unknown compounds
Solid / liquid samples about 2 mg. Solvent should be specified for measurement in solution phases


GAS CHROMATOGRAPH – MASS SPECTROMETER

Make / Model :Varian 1200 L Single Quadrupole
Mass Range :10-800 u
Scan mode :Centroid
Carrier gas :Helium
Resolution :Unit mass over entire range
Library :NIST Library
Column Specifications :Column type – WCOT fused silica Stationary phase – VF – 5MS Column length – 30m
Maximum temp :325°C
The applications of this instrument include Qualitative and quantitative determination of molecular species in organic and biological samples, concentration of elements in inorganic samples, separation and identification of unknown compounds, trace analysis and determination of isotopic contents, analysis of herbicides, pesticides, nitro compounds, structural information about molecules etc.



Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES)

The atomic spectrum emitted by a sample is used to determine its elemental composition in this instrument. The wavelength at which emission occurs identifies the element, while the intensity of the emitted radiation quantifies its concentration.
Make/Model :Thermo Electron IRIS INTREPID II XSP DUO
Flexible axial and radial view instrument, with high concentration capabilities.
Spectral range :165 to >1000nm
Resolution :0.005nm at 200nm
Detection limit :ppb level
CID Detector
Microwave Digestor (Milestone) available for sample digestion.
The applications of this instrument are in elemental level analysis of environmental samples, pharmaceuticals, research samples, soil and fertilizers, etc.
5 - 10 ml of aqueous solution required for analysis. Elements to be determined are to be clearly specified


Thermal analysis system - TG/DTA

Thermogravimetric Analysis (TG) determines the weight changes of a sample, whereas Differential Thermal Analysis (DTA) measures changes in temperature between a sample and a reference, as a function of temperature or time.
Make/Model :Perkin Elmer, Diamond TG/DTA
Flexible axial and radial view instrument, with high concentration capabilities.
:Ambient – 1200°C :165 to >1000nm
TG Measurement Range :200 mg
TG Sensitivity :0.2 mg
DTA measurement Range :±1000mV
DTA Sensitivity :0.06mV
Programmable rate :0.01 – 100°C / min
Sample pan volume :45ml or 90ml
Atmosphere :Air, inert gas, Oxygen
Pure gas flow rate :0-1000 ml/min
Make /Model :Perkin Elmer STA 6000
Furnace design :Vertical
Balance design :Top loading, single beam
Temperature range : 15 ˚C to 900 ˚C
Temperature accuracy :< ±0.5 ˚C
Thermocouples :PT-PT/Rh (Type R)
Applications of the TG/DTA instrument are compositional analysis, decomposition temperature, oil volatility measurements, flammability studies, heat of transition, thermal stability analysis, oxidative stability analysis, transition temperature detection etc.
Non-explosive, non-corrosive samples about 20mg are required for analysis. Please avoid samples containing Halides and Nitrates.


Thermal analysis system –DSC

DSC (Differential Scanning Calorimetry) measures the amount of heat energy absorbed or released by a sample, as it is heated, cooled or held at a constant temperature
Make/Model :Mettler Toledo DSC 822e
Temperature Range :-130 °C to max. 450°C
Measurement range :± 350 mW at RT
Measurement resolution :0.04 mW at RT
Temperature Accuracy :± 0.2°C
Temperature reproducibility :± 0.1°C
Heating rate :RT to 700°C in 7 min
Cooling rate :+ 100°C to - 100°C in 15 min
Sampling rate :Max 10 values / sec
Pure gas flow rate :0-1000 ml/min
The applications of DSC are numerous, either for routine quality control measurements or in research, where high sensitivity and flexibility are important aspects. Investigations can be carried out on samples like polymers, pharmaceuticals, chemicals, liquid crystals, food samples, glasses etc.
Applications include study of melting behavior, glass transition, specific heat anomaly, oxidation stability, chemical kinetics etc.
Non-explosive, non-corrosive samples, about 10-20 mg. are required for analysis.

UV-Vis-NIR Spectrophotometer

The optical absorption by samples in the ultraviolet, visible and near infrared regions are measured with this instrument. Near IR spectroscopy is a valuable tool for analyzing aromatic mixtures. This region finds wide acceptance in food and grain industry for the determination of protein, fat, moisture, sugar, etc. Absorption measurements in the UV and visible regions provide information about electronic transitions in a sample
Make/Model :Varian, Cary 5000
Spectral range :175 – 3300 nm
Wavelength accuracy :±0.1nm (UV-Vis), ±0.4nm (NIR)
Wavelength reproducibility :0.025nm
Limiting resolution :0.05nm(UV-Vis), 0.2nm(NIR)

DRS Facility available

The applications of this instrument include overtone analysis of X-H containing molecules (X=C, O, N, Si), determination of hydrogen bonds, energy gap measurements in solids, study of molecular structure, concentration measurements etc.

Solid/liquid samples up to 100mg/ml. are required for analysis. Thin film samples on glass or quartz substrate required. Solvents should be specified for solid sample analysis in the NIR region. 60mg-1gm of sample required for DRS Measurement

Scanning Electron Microscope –Energy Dispersive Spectrometer

Scanning electron microscopy (SEM) is a method for high resolution surface imaging. The SEM uses an electron beam for surface imaging. The advantages of SEM over light microscopy are greater magnification and much larger depth of field. Different elements and surface topographies emit different quantity of electrons, due to which the contrast in a SEM micrograph (picture) is representative of the surface topography and distribution of elemental composition on the surface.

Qualitative elemental analysis, standard less quantitative analysis, X-ray line scans and mapping can be performed with SEM-EDS combination.

The SEM-EDS installed in SAIF, STIC have the following technical specifications.
SEM Make :JEOL Model JSM - 6390LV
EDS Make :JEOL Model JED - 2300
Resolution :3 nm (Acc V 30 KV, WD 8 mm, SEI)
:8 nm(Acc V 3.0 KV, WD 6 mm, SEI)
:15 nm(Acc V 1.0 KV, WD 6 mm, SEI)
Magnification :5 × to 300, 000 × (Both in High and Low Vacuum Modes)
Image Modes SEI, BEI
Probe Current : 1 pA to 1mA
High vacuum resolution 3 nm
Low vacuum resolution 4 nm
Specimen Stage 4 nm
Specimen Stage
Type Eucentric
Tilt +90º
Specimen holder 10 mm dia
Maximum loadable specimen size :150 mm dia

Milli-Q Gradient Ultrapure Water

This is for the information of all concerned that Milli-Q Gradient Ultrapure water purification system is now installed in STIC. This Milli-Q Gradient Ulrapure water has the following specifications:
Resistivity at 25°C 18.2 Mohm-cm
TOC Level 1-5 ppb
Bacteria <1cfu/ml
Particulates > .22 µm : <1p/ml
UV absorbance .0001 AU
Those who are interested can get this water from STIC on payment basis. The prices will be as follows :
1 Users from CUSAT and other academic institutions : Rs. 250/lit
2 Other users : Rs. 500/lit
Users who come to collect water should bring their own ultra clean vessel for the same.
Users are urged to confirm availability of water before coming to collect the same.

FT NMR Spectrometer

Nuclear Magnetic Resonance spectroscopy is a powerful and theoretically complex analytical tool Nuclear magnetic resonance (NMR) is a property that magnetic nuclei have in a magnetic field and applied electromagnetic pulse , which cause the nuclei to absorb energy from the EM pulse and radiate this energy back out.
Make/Model :Bruker Avance III, 400MHz
Magnet :9.4 Tesla super-conducting Magnet
Probe :BBO 400MHz , with Z-gradient , 2H lock; for observation of nuclei like 1H, 13C, 31P, 15N etc with 1H decoupling,Any of these nuclei can be fully automatically selected and optimally tuned and matched (ATM).
Operation Temperature Range :360°
RF Console :Stable lock compatible with pulsed field gradients, gradient shimming with low heat dissipation. Automatic gradient shimming, Deuterium lock.
Samples requirements
Solid Samples, ~ 1 gm, are required for analysis. Sensitivity to moisture, air etc are to be specific

Samples requirements :5mg for 1H and 15mg for 13C and other nuclei. Solvent must be specified. Samples must be free of paramagnetic impurities.

X-ray Powder Diffractometer.

X-Ray Powder Diffractometry is one of the most powerful and established technique for material structural analysis, capable of providing information about the structure of a material at the atomic level. Low and High temperature measurement facilities are available

The Temperature attachment enables analysis from -170 Deg C to +450 Deg C under vacuum. Change in unit cell dimensions, structural changes at phase transitions etc, as a function of temperature can be determined.
Make/Model : Bruker AXS D8 Advance
Configuration :Vertical, Theta/2 Theta geometry
Measuring circle diameter :435, 500, and 600 mm predefined
Angle range :360°
Max. Usable angular range: :3° to 135°
X-ray source :Cu, Wavelength 1.5406 A°
Detector :Si(Li) PSD
Temperature attachment
Make /Model :Anton Paar, TTK 450
Temperature Range :-170 °C to +450 °C
The D8 Advance X-ray Diffractometer can be used for all X-ray powder diffraction applications such as structural analysis of crystalline solids, determination of unit-cell parameters, determination of crystal morphology etc.

Solid Samples, ~ 1 gm, are required for analysis. Sensitivity to moisture, air etc are to be specific

Single-Crystal X-ray Diffractometer

Single-crystal X-ray Diffraction is a non-destructive analytical technique which provides detailed information about the internal lattice of crystalline substances, including unit cell dimensions, bond-lengths, bond-angles, and details of site-ordering. Directly related is single-crystal refinement, where the data generated from the X-ray analysis is interpreted and refined to obtain the crystal structure.
Make/Model: Bruker Kappa Apex II
Temperature measurements available
Structure Solution Software: X Shell

Mercury Analyzer

Mercury analyzer   measures mercury in solid and semi-solid sample matrices directly without any acid digestion (sample preparation). The system employs the technique of sample combustion (thermal decomposition), mercury concentration via gold amalgamation and detection by cold vapor atomic absorption
 

Liquid Nitrogen Generator

1 STIC has procured a "LIQUID NITROGEN GENERATOR" as a support facility for instruments in SAIF. Some of the instruments procured in SAIF need liquid nitrogen for their operation. Excess liquid nitrogen produced by the generator are supplied to external users on payment basis.
2 Make/Model : Iwatani Model NL 50 Capacity : 15 Litres per day
3 System consist of a nitrogen gas generator (Model GN – 10A) a nitrogen liquifier and a built in storage tank of capacity 40 Litres. This is a water cooled system.
4 Liquid Nitrogen has a wide range of applications as coolant for thermal analysis instruments, biomedical instruments, storage of specimen, cryostats etc.
 

Procedure for using the chemical / Material Analysis Facility (SAIF)

1 Samples for analysis, along with duly filled work order and Demand Draft may be sent to The Director, STIC, Cochin University of Science & Technology Cochin 682 022. The payment should be made by a crossed DD drawn in favour of The Director, STIC , Cochin 682 022 payable at Ernakulam. Payments can also be made by cash in the office of STIC. The results will be sent to the user only after receiving payments.
2 Samples should be submitted separately for each analysis (except thin films). Samples should be packed well in airtight vials.
 

For efficient use of the facility, users are requested to comply with the following.

1 Be specific with respect to the nature of measurements/ analysis to be made, indicating solvents, temperature range and other details, if any.
2 For measurements in person, inform us well in advance and start the trip only after getting appointment
3 Complaints regarding the measurements should be brought to the notice of Director, STIC immediately after the receipt so that corrective action can be taken.
4 Acknowledge the services rendered by SAIF in all your publications and thesis to expose the facilities to other users.
5 Send us a copy of your reprints (involving measurements done at the SAIF) and such documents as thesis (only acknowledgement section), reports etc for reference to other users.
6 Write to us about the requirements of a new facility, which will have sufficient utility for workers in this region of the country. User suggestions are discussed at the FMC meeting for recommendation to DST for funding.
7 Expose your colleagues and friends in other institutions about the facilities available in SAIF, Cochin so as to enlarge our user – base.
8 Any special help, other than routine analysis, will be treated as constancy service for which charges will be extra.