CHN/S analysis
CHNS analyser is an elemental analyser that’s used for the rapid determination of Carbon, Hydrogen, Nitrogen and Sulphur content in material. The analyser can operate in either CHN mode or CHNS mode.
Available instrument: Perkin Elmer 2400 Series II CHNS Analyser
Sample acceptance and analysis
Explosive/poisonous samples and samples giving rise to toxic/obnoxious gasses/fumes on heating will not be accepted for analysis.
The maximum combustion temperature for a sample is limited to 950 °C.
At least 10 mg of sample is required for analysis.
The sample should be homogeneous, finely ground and between 50 – 100 µm sized.
Sample preparation can be done by the laboratory as well.
X-Ray Fluorescence Spectroscopy (XRF)
X-Ray Fluorescence (XRF) has the capability of detecting elements from 11Na to 92U. However, this technique produces low detection sensitivity for lighter elements.
Furthermore, the elemental percentages generated by the instrument are given as a percentage of the total detected elements and not the actual elemental composition.
Therefore, the total detected elements percentage values are added up to 100 %.
The overlapping of characteristic spectral lines of two or more elemental constituents of a sample is another drawback in x-ray fluorescence analysis (ED-XRF).
The following energy overlaps affect the quantification if they are present in the sample.
Ex: S with Mo, Fe with F, Cr with Mn, Mn with Fe
Available instrument: : HORIBA Scientific XGT- 5200 X-ray Analytical Microscope
Sample acceptance and analysis
At least 50 mg of sample will be required as a powder, solid, semisolid etc.
For each sample, six different 100 µm x 100 µm areas will be analysed and reported.
Based on the customer request, results are reported as elemental percentages and/or their oxide %.
Instrument measures the elemental % only and not the oxidation state of the element.
Thus the oxide forms of the results do not represent the actual compound.
TEM-EDX
Transmission Electron Microscopy (TEM) is a microscopy technique in which a beam of electrons is transmitted through a specimen to form an image.
Available instrument: JEOL – JEM – 2100 High Resolution Transmission Electron Microscope and EDAX Ametek Energy Dispersive Spectroscopy with TEAM EDX software.
Sample acceptance and analysis
Particle size should be < 50 nm for high resolution imaging.
Samples containing Fe won’t be accepted.
| Sample Type | Sample Quantity Required |
|---|---|
Dispersion |
1 – 2 mL |
Powder |
0.1 – 0.5 g sample and
20 mL of the solvent used to make the dispersion. |
Since further dilutions may be required, 5-10 ml of the pure solvent used to make the dispersion will also be required with the sample.
TEM Imaging – Only 10 images will be provided.
TEM/EDX – 10 images and 2 EDX maps will be provided.
Inductively Coupled Plasma- Mass Spectrometry (ICP-MS)
Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is a type of mass spectrometry that uses an inductively coupled plasma to ionize the sample. It atomizes the sample and creates atomic and small polyatomic ions, which are then detected.
Available instrument: Agilent Technologies 7900 ICP-MS with ASX-500 Series ICP-MS autosampler.
Analytical Elements: Na, K, Ca, Ag, Al, As, Ba, Be, Cd, Co, Cr, Cs, Cu, Fe, Ga, K, Li, Mg, Mn, Ni, Pb, Rb, Se, Sr, Tl, U, V, Zn, Hg, B, Ge, Mo, Nb, P, Re, Si, Ta, Ti, W, Zr
Analytical Range: Please contact the laboratory for more information.
Sample acceptance and analysis
We accept undigested and digested samples.
The digested sample should comply with the following requirements.
i. Digestion should be carried out using only Nitric acid or HNO3/H2O2 mixture. Please do not use acids such as HF, HCl and H2SO4.
ii. Digested samples should be pale Yellow or colorless with no particulate matter.
iii. For the analysis of volatile elements such as Hg, As, Pb, Cd, Zn etc. microwave digestion is recommended.
iv. At least 10 – 12 mL of properly digested and filtered samples placed in 15 mL falcon tubes shall be submitted for analysis.
v. Acidity of the digested sample should be less than 10%.
vi. Total dissolved solids (TDS) level should be less than 2000 ppm.
vii. Sample should be filtered with 0.45 µm syringe filters.
viii. Final make up volume, sample weight used and acid content in the final solution should be clearly mentioned in Test Item Submission Form.
X-Ray Photoelectron Spectroscopy (XPS)
Elemental composition and the chemical and electronic state of all elements from Li and above can be analysed.
Available instruments: Thermo ScientificTM ESCALAB Xi+ X-ray Photoelectron Spectrometer (XPS)
Sample acceptance and analysis
| Sample Type | Sample Quantity Required |
|---|---|
Film |
1 cm x 1 cm Piece |
Powder |
The powdered material should be made in to a pellet. |
Dispersions |
0.5 mL of concentrated solution |
Samples containing Sulphur and Iodine will not be accepted.
For each sample, either the XPS survey and the narrow scan of three selected elements will be provided or six survey scans will be provided.
SEM-EDX
A Scanning Electron Microscope (SEM) is a type of electron microscope that produces images of a sample by scanning the surface with a focused beam of electrons
Available instrument: Hitachi SU6600 FE-SEM (Field Emission Scanning Electron Microscope) and Oxford instruments EDX with AZtec software.
Sample acceptance and analysis
| Sample Type | Sample Quantity Required |
|---|---|
Thin Film |
Maximum 1x1cm |
Powder |
About 50 mg |
Solid sample |
Maximum 0.5 x1x1 cm |
Dispersion |
0.5 mL concentrated dipersion |
Since further dilutions may be required for dispersion or if dispersion needs to be prepared from the powder sample, 5-10 ml of the pure solvent used to make the dispersion will also be required with the sample.
Samples should be free from moisture (except dispersions) and shouldn’t show magnetic properties (should not contain high quantities of Fe)
EDX – Suitable for qualitative analyses.
This technique produces low detection sensitivity for the elements below Sodium (Na) in the periodic table and is not sensitive to elements present in ppb/ ppm level.
SEM imaging – Only 6 images will be provided.
SEM/EDX – 6 images and 2 EDX maps will be provided.
