Icp MS
Icp MS
Icp MS
“SHRUTHI D”
103CH20054
Department of Chemical Engineering
“ROOPASHREE”
103CH21704
Department of Chemical ngineering
1 Synopsis
2 Introduction
3 Sample Preparation
5 Applications
6 About AP-89
7 Results
Serial Table of Content Page
No. No.
1 Synopsis
2 Introduction
3 Sample Preparation
5 Applications
6 About IS9833
7 Results
Inductively Coupled Plasma – Mass
Spectroscopy:
Synopsis:
Introduction:
Sample Preparation:
Sample preparation for ICP-MS is relatively simple; biological
samples are usually diluted or thermally digested before analysis.
Common diluents include dilute acids (e.g. nitric acid, hydrochloric
acid) or alkali (e.g. ammonium hydroxide, tetramethylammonium
hydroxide). Deionised water has been used as a diluent, however
some elements are unstable in pure water, therefore acidic or alkaline
diluents are preferred in most cases. The isoelectric point of many
proteins is approximately 5–6, therefore the addition of an acidic
diluent to a highly proteinaceous sample such as blood may cause
protein precipitation, which may co-precipitate certain analytes or
cause an obstruction in the nebuliser. Proteins tend to be more tolerant
of dilute alkali, however not all elements are soluble at alkaline pH,
therefore a chelating agent such as EDTA is often incorporated into
alkaline diluents. Surfactants such as Triton-X100 are also commonly
added to help solubilise and disperse lipid and membrane proteins in
the sample.
Instrumentation and working of ICP MS
Nebuliser:
A number of different nebulisers are commercially available,
including pneumatic, ultrasonic and desolvating types. Pneumatic
nebulisers which use gas flow to generate the aerosol are the most
common type for routine clinical applications. There are several
different types of pneumatic nebulisers, including concentric, cross-
flow, Babington and v-groove (a variant of the Babington). Each has
its own advantages and disadvantages; the choice is application
dependent. Concentric nebulisers are ideal for low matrix (low TDS)
samples, whereas cross-flow and v-groove nebulisers are more
rugged, tolerating high matrix samples. In contrast to the pneumatic
design, an ultrasonic nebuliser utilises sound energy (from a
piezoelectric transducer) to generate the aerosol. These nebulisers
improve analytical sensitivity by an order of magnitude compared to
pneumatic nebulisers, however they are significantly more
expensive. Desolvating nebuliser systems use a heated spray chamber
to desolvate the sample before it reaches the plasma. In addition to
increasing sensitivity, desolvating nebulisers also decrease the
formation of oxide species in the plasma which can interfere with the
measurement of certain analytes (discussed in Interference section).
Spray Chamber:
After being aerosolised by the nebuliser, the sample enters the spray
chamber. The spray chamber has a simple design but serves a few
important purposes: it selectively filters out the larger aerosol droplets
that are generated by the nebuliser and acts to smooth out nebulisation
‘pulses’ produced by the peristaltic pump. This is important because
the plasma is inefficient at dissociating large droplets (>10 μm
diameter). In a double-pass spray chamber, aerosol droplets emerge
from the nebuliser and travel down a central tube in the spray
chamber. At the end of the tube, larger aerosol droplets exit the spray
chamber under the influence of gravity and are drained to waste while
smaller droplets, roughly <10 μm diameter, are transferred to the
plasma. Cyclonic spray chambers have a different design but operate
in a similar manner. In contrast to techniques such as graphite furnace
atomic absorption, the sample introduction process in ICP-MS is quite
inefficient. Normally only 1–2% of the sample reaches the plasma;
the remainder is drained to waste. Therefore factors which influence
the efficiency of sample introduction even slightly can have marked
effects on instrument response. One such factor is the spray chamber
temperature, which is normally maintained at around 2°C using a
thermoelectric cooling device or water jacket. Operating the spray
chamber at this temperature minimises the formation of oxides, and
prevents overloading the plasma with solvent.
Detector:
The most common detector used for ICP-MS is an electron multiplier
(EM). Positively-charged analyte ions strike the first dynode of the
detector which is held at a high negative voltage. The impact of the
ion on the detector causes the emission of several electrons from the
surface, which, in turn, strike the next dynode releasing more
electrons. This process (called secondary emission) continues,
generating an amplification cascade that culminates in a signal large
enough to be measured reliably as an ion ‘count’. In this way, an EM
can generate a measurable signal pulse from the impact of a single ion
on the detector, conferring very high analytical sensitivity. In fact,
detection limits in ICP-MS are far superior to flame atomic
absorption, and are comparable (or superior) to graphite furnace
atomic absorption. Typical limits of detection in ICP-MS are in the
nmol/L range for most elements; the exact value being dependent on
the element, the type of biological matrix, the dilution factor
employed during sample preparation, the design of the sample
introduction system, instrument operating conditions (including
plasma temperature) and background signals (reagent purity etc.).
Most detectors are able to operate in both a pulse (digital) and
analogue mode. These so-called dual detectors automatically switch
from pulse to analogue mode when the signal intensity exceeds a
certain threshold, allowing the linear dynamic range of the detector to
be extended to approximately 8–12 orders of magnitude. These two
detector modes require cross-calibration to ensure optimum linear
response across this range.
Having regard to the fact the colourants are used to impart a colour to
plastic material coming into contact with food.
Considering that plastic materials coming into contact with food may
by reason of their colouration, pose a risk to human health if not used
under normal conditions or if the colourants used to do not meet
purity criteria based on good manufacturing practice.
Taking the view that each member state faced with the need to
introduce regulations governing this matter would find it beneficial to
harmonise such regulations at European level.
Test Procedure
Approximately 10 gm of sample taken in glass beaker and added
150ml of 0.1M HCl
Kept the beaker with sample in mechanical agitator for 15
minutes.
Allowed it to stand for 15mins.
After 15 minutes filtered the solution.
Then analysed the same in ICP-MS
Impurities Limit(ppm)
Antimony(Sb) 500ppm
Arsenic(As) 100ppm
Barium(Ba) 100ppm
Cadmium(Cd) 100ppm
Chromium(Cr) 1000ppm
Selenium(Se) 100ppm