ICP Presentation

Presentation of ICP Instrumentation at IICT Hyderabad

1. CRCL Group A Officer’s Training at IICT Welcome Distinguished Faculty Members of IICT & Officers of Revenue Laboratories.

2. CRCL Group A Officer’s Training at IICT Topic: ICP-OES Spectroscopy Group-III Team Members: T.R Suresh A.J Aleyamma Ajay Kumar Singh H S Bhandarkar K Thambidurai

3. CRCL Group A Officer’s Training at IICT Topic to be Covered 1. Introduction 2. Basic Principle of I nductively C oupled P lasma O ptical E mission S pectroscopy 3. Instrumentation 4. General Applications 5 . Application in CRCL Samples

4. CRCL Group A Officer’s Training at IICT Introduction: Interaction of an atom in the gas phase with electromagnetic radiation (EMR). Samples are solids, liquids and gases. ICP OES is a Inductively Coupled Plasma – Optical Emission Spectroscopy and it is also called ICP AES.

5. Comparison: AAS & ICP-OES • AAS : Absorption Spectroscopy, Single element, ppm /ppb range, – Cheap, simple – Small dynamic range – GFAAS about 100 times more sensitive than FAAS, but also more challenging • ICP-OES: Emission Spectroscopy, Multi-element, ppb range – Limited spectral interferences, good stability, low matrix effects

6. CRCL Group A Officer’s Training at IICT Basic Principle: M + e* → M* M* → M + Energy The energy emitted is directly proportional to the concentration of analyte present the solution.

7. Inductively coupled plasma optical emission spectrometry (ICP-OES) - is a type of emission spectroscopy that uses the inductively coupled plasma to produce excited atoms and ions that emit electromagnetic radiation at wavelengths characteristic of a particular element. Sample solution containing elements Formation of liquid droplets atomization excitation Emission of Radiation at a Specific Wave Length Measure the intensity of emitted radiation

8. 3 Instrumentation Schematic Diagram of ICP-OES

9. Sample Introduction Plasma Detector 3 Instrumentation

10. Sample Introduction: liquid samples    Often the largest source of noise Sample is carried into flame or plasma as aerosol, vapour or fine powder Liquid samples introduced using nebuliser

11. PUMPS: Peristaltic pumps are almost exclusively the pumps of choice for ICP-AES. • The pumps utilize a series of rollers that push the sample solution through the tubing using a process known as peristalsis. • With a pumped solution, the flow rate of the solution into the nebulizer is fixed and is not as dependent on solution parameters such as viscosity and surface tension.

12. SPRAY CHAMBER:   Aspray chamber is placed between the nebulizer & the torch. The primary function of the spray chamber is to remove large droplets from the aerosol.   The secondary purpose is to smooth out pulses that occur during nebulization due to pumping of the solution. It is designed to allow droplets with diameters of about 10 micrometre or smaller to pass to the plasma.

13. What is a Plasma? • Plasma source provides atomization • Plasma: ―a gas-like phase of matter that consists of charged particles‖ • ICP-AES plasma source is from the carrier Gas typically argon is used Emission Source: Plasma

14. Plasma Gas (15~16 L/min) ICP torch schematic Auxiliary Gas (1L/min) Carrier Gas (1.2L/min) + Sample Blend Gas (0.6L/min) Plasma Generation In ICP, the plasma is generated from radio frequency magnetic fields induced by a copper coil which is wound around the top of a quartz torch.

15. ICP temperatures The Temperature of ICP flame is about 6000 K and up to 10000 K at its hottest point.

16. Excitation/ionization of atoms in Plasma Achieved by three mechanisms: 1. Collisional transfer of excitation energy e* + M → M* + e M* → M + + e 2. Through meta stable states of argon atoms/ions (Penning ionization) Ar* + M → Ar + M* M* → M + + e 3. Charge transfer between argon ions and the analyte atoms Ar + + M → Ar + M +

17. Radial or axial configuration Axial Sometimes called a “Horizontal Plasma” ■ Useful analysis in many different sample matrices ■ Excellent Detection Limits ■ Has certain limitations ■ Matrix Interferences ■ Na and K can have problems ■ The solution complicates sample preparation Radial: Original ICP View ■ Sometimes called “Vertical” or “Side-On” Plasma ■ Accommodates all ICP matrices ■ Detection Limits similar to Flame AA ■ Better for Refractory Si, Ti, B, W, Mo ■ Can analyze S, P and Halogens

18. PMT is to convert optical rotation(photons) into an electrical signal(electrons).The vaccum tube devices are very sensitive&cover a large wavelength range. It consists of a vaccum photocell with an anode, photocathode and a number of dynodes which have an increasingly positive potential with respect to the photocathode.

19. ICP-OES wavelengths

20. Comparison: Detection limits and working ranges http://pubs.acs.org/hotartcl/tcaw/99/oct/element.html

21. 4      ClinicalAnalysis: metals in biological fluids (blood, urine). Environmental Analysis: trace metals and other elements in waters, soils, plants, composts and sludges. Pharmaceuticals: traces of catalysts used; traces of poison metals (Cd, Pb etc). Industry: trace metal analysis in raw materials; noble metals determination. Forensic science: gunshot powder residue analysis, toxicological examination ( e.g., thallium (Tl) determination. 4.General Applications of ICP -OES

22. 1. Estimation of elements Metals and Alloys. Estimation of Heavy metals in Vegetable, Mineral Oil and Waste Oils. Analysis of trace elements in Ores & Minerals Applications in CRCL Laboratories 5.Applications of ICP –OES in CRCL

23. 1. From 1000 ppm Multiple STD Stock solution prepare 1 ppb, 5 ppb and 10 ppb etc. Digest the suitable quantity of sample using Microwave Digestion and made up to 100ml SMF. Analyse both STD and sample in ICP-OES in a following manner. Preparation of Standards and Sample Solution Applications of ICP –OES in CRCL Analysis of Tin, Zinc and Manganese in Metal samples

24. 32 Microwave digestion Supplied with dedicated vessels (e.g. PTFE) Closed vessel digestion minimises sample contamination Faster, more reproducible, and safer than conventional methods Rotor

25. Calculation: C alculation (ppb) Concentration of unknown sample = Sample conc (ppb) - Blank conc (ppb ) × Volume (mL) Sample weight in gram

26. CRCL Group A Officer’s Training at IICT T H A N K Y O U