NOIDA INSTITUTE OF ENGINEERING & TECHNOLOGY,

GREATER NOIDA
(Affiliated by Dr. APJ Abdul Kalam Technical University)

DEPARTMENT OF CHEMICAL ENGINEERING

REPORT ON
“INDUSTRIAL TRAINING AT INTERTEK”

Submitted to : Dr. Meghna Kapoor

Submitted by : Lovely Choudhary
Roll number : 1901330510008
Course : Bachelor of Technology
Branch : Chemical engineering
Semester : Seventh
Session : 2021-22
 INDEX
Page no.
Acknowledgement …………………………………...3
List of figures……………………………………………….4
Abstract…………………………………………………......5
Certificate…………………………………………………...6

CHAPTERS –
1. About Company….....………………………………..
1.1 History of company……………………………….
1.1.1 What we do….………………………………
1.1.2 Purpose, Mission, Vision and Values……………..

2. Industrial Terminologies……………………………..
2.1 Quality…………………………………………….
2.1.1 Quality control…………………………….........
2.1.2 Quality Assurance………………………………
2.2 Quality Assessment………………………………...
2.2.1Accreditation…………………………………
2.2.1.1 Accreditation Bodies…………………….
2.2.1.2 Accreditation Process………………………
2.2.2Audits…………………………………………..
2.2.3Inter-comparison……………………………….

3. Method of Analysis…………………………………......
 3.1 Standards……………………………………………
3.2 Analysis and determination…………………….......
3.3 Resources…………………………………………….
4. Organic Department…………………………………….
4.1 Chromatography and its types……………………….
4.2 Gas chromatography Mass spectrometryMass
Spectrometry………...
4.3 Liquid Chromatography with Mass Spectrometry
4.3.1 Liquid Chromatography…………………..
4.3.2 About LC-MS/MS…………………………………..
4.3.3 How does LC-MS works……………………………
4.3.4 Tests Performed on LC-MS…………………………
5. Inorganic Department…………………………………...
5.1 Milli-Q Equipment…………………………………..
5.2 Inductively Coupled Plasma Optical Emission
Spectrometry…………………………………………
5.3 Inductively Coupled Plasma Mass Spectrometry….
5.4 pH Meter ……………………………………………..

My Role and Responsibility……………………………………………

Conclusion………………………………………………………………
ACKNOWLEDGEMENT
I would like to express my special thanks of gratitude to Mr.
Anurag Gupta (Deputy Manager) for trusting me with the new
role and Mohd. Sabir khan (Assistant Supervisor) for providing
me with all the support that I needed. Also would like to thank
you to Head of department (Dr. Ankita Sharma) who gave me
this opportunity to do this wonderful training. By attaining
practical knowledge will eventually develop my professional
skills.

In addition to this, I would also like to express my gratitude to

my parents for supporting me emotionally and mentally .

LOVELY CHOUDHARY
LIST OF FIGURES Page no.
Figure 2.1. Hierarchy of Quality Department 16
Figure -2.2.1 Shows the importance of Accrediation 18
Figure 4.2: Systematic Diagram of GC 24
FIGURE 4.2.1: Chromatogram output from GC. Image courtesy: 25
Anthias Consulting.
Figure 4.3.3 : Example schematic diagram of an LC-MS setup. Credit: Cwszot 30
, Dagui1929, CasJu, and YassineMrabet, reproduced under the
Creative Commons CC0 1.0 Universal Public Domain Dedication license.
Figure 4.3.3.1: Example output plot from LC-MS analysis. Credit: Daniel 31
Norena-Caro, reproduced under the
Creative Commons CC0 1.0 Universal Public Domain Dedication license.
Figure 5.1 Above figure shows the Milli-Q Equipment 33
Figure 5.3 The main components of an ICP-MS instrument. 38
Figure 5.3.1 Main components of a single quadrupole ICP-MS instrument. 39
Figure 5.3.2Main components of a triple quadrupole ICP-MS (ICP-QQQ) instrument. 40
Figure 5.3.3 A nebulizer turns the liquid sample into an aerosol. 40
Figure 5.3.4 The aerosol passes through a spray chamber where the larger 41
droplets are removed.
Figure 5.3.5 The plasma is formed from argon gas flowing in a quartz tube. 41
Figure 5.3.6 The argon gas is ionized by a radio frequency generator. 42
The sample aerosol is carried through the center of the plasma.
Figure 5.3.7 Processes to convert aerosol droplets to ions in the plasma. 42
Plot 5.3 showing degree of ionization (% of atoms converted to ions) 43
plotted against first ionization potential for all elements.
Figure 5.3.8 Layout of an ICP-MS system showing vacuum interface 44
between the plasma and mass spectrometer.
Figure5.3.9 An ICP-MS interface includes a sampling cone (left) 44
and skimmer cone (right).
Figure 5.3.10 Cutaway showing position and operation of the ion lens. 45
Figure 5.3.11 Cutaway showing position of the collision/reaction cell
between the ion lens and mass filter of a single quadrupole ICP-MS.
The cell can be pressurized with a collision or reaction gas to resolve interfering ions. 46
Figure 5.3.12 Reaction mode operation with single quadrupole ICP-MS configuration 47
Figure 5.3.13 Reaction mode operation with triple quadrupole ICP-MS configuration 47
Figure 5.3.14 Quadrupole mass filter used in most ICP-MS instruments.
RF and DC voltages filter the ions by mass to charge ratio (m/z), allowing only
1 m/z at a time to pass through to the detector. 48
Figure 5.3.15 shows pH Meter 48.
CERTIFICATE
 1. ABOUT COMPANY
 For more than 130 years, companies around the world have depended on
Intertek to help ensure the quality and safety of their products, processes and
systems.
 Intertek provides Assurance, Testing, Inspection and Certification services to
customers.
 They provide a systemic approach to support customers’ Quality Assurance
efforts in each of the areas of their operations including R&D, raw materials
sourcing, components suppliers, manufacturing, transportation, distribution and
retail channels, and consumer management.
 Intertek is an industry leader with more than 44,000 employees in 1,000
locations in over 100 countries delivers innovative and bespoke Assurance,
Testing, Inspection and Certification solutions for our customers’ operations
and supply chains.

1.1 History of company:

 The Intertek story starts at the inception of the modern testing industry. The
history of Intertek goes back over 130 years, and evolves from the combined
growth of a number of innovative companies.

1940-1980:
 A diverse international group at the time enters the testing industry by
establishing 'Labtest' Hong Kong to serve the internal needs of the Dodwell
companies, a multinational corporation acquired by Inchcape (1973).
 Labtest began with just three people – Raymond Kong, Alfred Yung and
Thomas Chan.
 Labtest originally focuses on textile testing, and later broadens across other
consumer goods. It is the first commercial consumer goods testing facility
in Hong Kong.
  Labtest expands internationally, extending its business in the United States
(1975) and establishing labs in the Philippines (1979), Taiwan (1982), New
York city (1983), Singapore (1984), Thailand (1985) and the UK (1987)
and China (1989).

 Inchcape acquires multiple testing and inspection companies, ranging from

petroleum, petrochemical, textiles, to electronics and minerals testing
(1975- 1980)

1980-2000:
 Inchcape reorganises. It forms a specific testing business stream, 'Inchcape Testing
Services' (1987), including Labtest and its other acquisitions in the testing,
inspection and certification area.
 Inchcape acquires the Caleb Brett group of companies, and the government trade
and inspection services businesses in the UK ('Foreign Trade Standards') and the
US (Intertek Testing Services and Intertek Services International) (1984-87).
 Labtest acquires the product safety consulting business RAM (Risk Analysis &
Management™). RAM supports clients such as McDonalds and their toy safety
programme (1988).
 Inchcape acquires ETL Testing Laboratories (1988).
 Inchcape continues its acquisitive path, buying Warnock Hersey in North America
(1992) and SEMKO in Sweden (1994), and other testing companies. It amasses a
range of accreditations and registrations needed to provide certification, inspection
and testing services across various industries including automotive, aerospace,
electronic and consumer goods.
 Inchcape's Testing Services division is bought as part of a management buy-out by
Charterhouse Development Capital, a global investment company (1996).
 The company is renamed 'Intertek Testing Services,' forming the present-day
Intertek. Richard Nelson, the existing CEO of Inchcape Testing Services, becomes
CEO of Intertek.

2000 – Present:
Intertek lists on the London Stock Exchange on 29 May 2002, becoming Intertek
Group plc.

o It lists with a share price of £4, market capitalisation of £614m, and joining
the FTSE 250 in the Support Services sector
o Intertek's stock symbol is ITRK.
 o Upon listing, Intertek had around 10,500 employees and around 750
laboratories and offices worldwide

and generated around £450m revenue per annum.

Intertek continues to expand by acquiring complementary companies in the

testing, inspection and certification arena, with the wider focus on providing
quality and safety services across a wide range of industries (2000 to present).

o Intertek expands its own services and operations in growing areas such as
supply-chain management and ethical sourcing services, industrial asset
inspection, food, pharmaceutical renewable energies and bio-fuels, solar
and wind-powered product services.
o It commences major laboratory outsourcing contracts with companies,
including BP, Kodak, DSM, Unilever, ICI, Sabic, Volkswagen and Lilly.
 Richard Nelson, CEO of 20 years, retires. Dr. Wolfhart Hauser is appointed CEO
in 2005.
 Intertek internal business units were aligned around customers' industries into four
core divisions in 2006.
 In January 2011, we reorganised our operational structure to further improve the
alignment of our business lines with those of our customers, and renamed certain
divisions to better describe their core activities.

o Oil, Chemical & Agri is renamed Commodities, and incorporates Minerals;

Analytical Services is renamed Chemicals & Pharmaceuticals, and
incorporates Health & Environmental; Industrial Services is renamed
Industry & Assurance, and incorporates Food, Agri, and Upstream
Services.
 Intertek's share price on the London Stock Exchange exceeds the £10-mark for the
first time in June 2007; and 2011 marked the first time that the share price
exceeded the £20-mark.
 Intertek's annual revenue exceeds £GBP 1 billion in 2008, reporting total revenue
of £1,003.5k for the full year.
 Intertek enters the FTSE 100 for the first time in 2009.
 In February 2011, Intertek expanded its brand identity to Intertek: Valued Quality,
Delivered, underlining the company’s global mission of partnering with its
customers to provide quality services that add value to their organizations.
 In May 2011, Intertek completed its acquisition of Moody International for £450
million. As a result, the number of Intertek employees reaches 30,000.
 May 2015: Wolfhart Hauser, CEO retires from Intertek after 10 years of service
and is succeeded by André Lacroix.
 Intertek completes four acquisitions in 2015 including PSI for $330m in the US –
a provider of testing and assurance services to commercial and civil construction
 markets – with 2,400 people across 87 locations. At the end of 2015, the number
of Intertek employees totals 41,400.
 In 2016, Intertek acquired the Italian food quality assurance business FIT-Italia,
the Canadian cyber security assurance business EWA-Canada, and entered a joint
venture with the environmental quality assurance business ABC Analitic in
Mexico.
 In 2016, Intertek established the world’s first Qi Extended/Basic Power Wireless
Charging Test Centre in Hong Kong.
 2017: Intertek unveils its brand reinvention, with the Customer
Promise: "Intertek Total Quality Assurance expertise, delivered consistently
with precision, pace and passion, enabling our customers to power ahead
safely."
 2017: Intertek acquires leading provider of automotive engineering and testing
services, KJ Tech in Germany and Acumen Security, a leading provider of
Security Certification Solutions for products in the US.
 2017: Intertek recognized by investors worldwide as one of the best performing
FTSE 100 stocks of 2017.
 2018: ‘Intertek Caleb Brett’, the new name for our Cargo and Analytical
Assessment business is launched.
 2018: Intertek acquires cargo inspection specialist, Aldo Abela Surveys (AAS)
Ltd. and announces its intention to acquire Proasem, a leading provider of fuel
testing, inspection, metrology and training services to the Oil & Gas sector, based
in Colombia.
 2018: In July Intertek built its presence in the UK Cyber Security and Network
Assurance market with the acquisition of NTA Monitor and in August expanded
its global Assurance business with the acquisition of Alchemy, a leading provider
of SaaS-based People Assurance solutions.

1.1.1 What we do?

We provide certain service like:

A.

 Enabling you to identify and mitigate the intrinsic risk in your operations,
supply chains and quality management systems.
 B.

 Validating the specifications, value and safety of your raw materials,

products and assets.

C.

 Evaluating how your products and services meet and exceed quality, safety,
sustainability and performance standards

D.

 Formally confirming that your products and services meet all trusted
external and internal standards.
1.1.2 Purpose, Mission, Vision and Values:
2. INDUSTRIAL TERMINOLOGIES
2.1 Quality
 Quality is totally a characteristic of an entity that bear on its ability to satisfy
stated and implied needs.
 Good Quality does not mean necessarily high quality.
 Quality (In market Demand)
a) High standard of level
b) Degree of excellence
c) Special feature
d) Faculty skills accomplishment
e) Satisfaction of customer
f) Invisible when good, impossible to ignore when its bad .
 Quality is classified into 2 parts:
Quality

Quality Control Quality Assurance

2.1.1 Quality Control

Quality control refers to measure that must be included during each assay run to verify that
the test is working properly.

2.1.2 Quality Assurance

Quality Assurance is defined as the overall program that ensures that final result reported
by laboratory are correct.
QA is concerned with much more that the right test is carried out on the right specimen and
that the right result, right interpretation is delivered to right person at right time .

Quality Management
System (QMS)

Quality Assurance
(QA)

Quality Control (QC)

Figure 2.1. Hierarchy of Quality Department

2.2 Quality Assessment

2.2.1 Accreditation:
Accreditation is given by government body like National Accreditation Board for testing
and Calibration Laboratories (NABL) .
Accreditation pushes institutions to meet and maintain their high standards, in turn increasing
trust and confidence in them among the public and boosting accountability.

Figure -2.2.1 Shows the importance of Accrediation

2.2.1.1 Accreditation Bodies
a) ILAC : International Laboratory Accreditation Corporation . It consist of all
types of accreditation authority.
b) EA : European Co-operation for Accreditation.

c) APLAC: Asia Pacific Laboratory Accreditation Co-operation .

d) IAAC : Inter American Accreditation Co-ordination.

3. Method of Analysis
3.1 Standards
Standard methods which is used for conducting the various tests

a) CEN (EN): European Committee for Standardization . It will only in

European countries.
b) BS Standard : British Standard . this will only use in British countries.
c) ASTM Standard : American society for testing materials . This standard can
only use in American countries .
d) IS : Indian Standard , this standard is mainly use in India .
e) DIN Standard : Deutsches institute furnormung . This standard is used at
German.
f) ISO: International Standard Organization, ISO is an independent , non-
governmental international organization with a membership of 167 national
standards bodies. Through its members, it brings together experts to share
knowledge and develop voluntary, consensus-based, market relevant International
Standards that support innovation and provide solutions to global challenges.
There headquarter is at Geneva, Switzerland.

3.2 Analysis And Determination

Chemical Analysis:
 Analysis used for the sample determination used in sample.
 Trace analysis is an application of analytical chemistry with very small analyte .
 Many analyst apply to below PPM level other applying to analyte to low enough
to cause difficult in obtaining reliable result based on spectrometry and
chromatography analysis.
 These development in instrument analysis enable the analyst to routinely lower
concentration of analytes.
 PPT<PPB<PPM (PPT- Parts per Trillion
PPB- Parts per Billion
PPM – Parts per Million)
3.3 Resources for chemical Analysis:
 Laboratory
 Qualified Experienced Staff
 Instrumentation or other Equipment
 Consumable Supplies
 4. ORGANIC DEPARTMENT
4.1 Chromatography and its types
 Chromatography is the technique for the separation, purification, and testing of
compounds.

Principles of Chromatography
Chromatography is a separation method where the analyte is combined within a liquid or
gaseous mobile phase., which is pumped through a stationary phase. Usually one phase is
hydrophilic and the other is lipophilic. The components of the analyte interact differently
with these two phases. Depending on their polarity they spend more or less time
interacting with the stationary phase and are thus retarded to a greater or lesser extent.
This leads to the separation of the different components present in the sample. Each
sample component elutes from the stationary phase at a specific time called as retention
time. As the components pass through the detector their signal is recorded and plotted in
the form of a chromatogram.

4.2 GAS CHROMATOGRAPHY MASS SPECTROMETRY

Gas chromatography Mass spectrometry or Gas Liquid Chromatography is a technique
applied for separation, identification and quantification of components of a mixture of
organic compounds by selective partitioning between the stationary phase and mobile
phase inside a column followed by sequential elution of separated components. The
technique is suitable for separation of compounds having following characteristics :

 High volatility
 Thermal stability
 Low molecular weights

Purpose of gas chromatography

The main purpose of the Gas chromatography Mass spectrometry technique is to separate
the compounds that possess:

 High volatility
 Low molecular weights
 Thermal stability
How does Gas chromatography Mass spectrometry work?

For having a hold on how does chromatography works, we need to be aware of the
individual components of a GC chromatogram or GC Chromatograph.

The main components are:

Mobile phase
In gas chromatography, usually, three types of gases are employed namely –

1. Carrier gas – This is needed for the transfer of the injected sample to the
separation column. They are also responsible for the subsequent transfer of
separated components to the detector. Common examples: Nitrogen, helium, or
hydrogen
2. Fuel gas – They support the flame in Flame ionization detector (FID) detector
such as Hydrogen.
3. Zero air – These are the purified air that plays the role of oxidant to support
the combustion of flame in the detector. Before being led to the gas
chromatographic system, the above three are intermixed in the desired proportion.

Sample injector
The injector is a heated block where the sample is injected. Through the carrier gas
stream, the sample is spontaneously vaporized and led to the column.

With the help of a gas-tight syringe, the liquid sample mixtures are injected whereas, with
the help of automated injection valves, the gaseous mixtures are injected.

Column
This is filled with the stationary phase or its walls are covered with a liquid adsorbent.
This is done for selective absorbance and retention of the sample components.

Commonly used: Packed columns and Capillary columns (More popular)

Component of a Column – Oven
The column is enclosed by a column oven which is responsible for maintaining a constant
temperature during isothermal operation. This temperature when temperature
programming is needed can be increased in a controlled way for acquiring effective
separation of mixture components possessing different volatilities.

Detector
This is employed for the identification and quantification of components.
Here, the regions of individual peaks created relate to their concentrations and their
retention times are representative of their identity.

Common examples: Flame ionization detector, Thermal conductivity detector (TCD), and
Electron capture detector (ECD).

Data system
It is a set of dedicated software that provides control over many important operational
parameters like injection sequence, wash cycles, over-temperature control, the flow rate
of gases, detector wavelength, etc. Simultaneously, the data station calculates and
displays the parameters.

Figure 4.2: Systematic Diagram of GC

Gas chromatographic analysis

The X-axis – Retention time of peak (Rt)

This is calculated from the time the sample was injected into the column (t0) till it
reaches the detector. Every analyte peak has a retention time that is measured from the
apex of the peak, just like tR.

The Y-axis – Detector response

This shows the measured response of the analyte peak within the detector.

The baseline here represents the signal received from the detector where no analyte is
eluting from the column or is beneath the detection limit. It is considered as an indication
of a problem or indication to check the maintenance, in situations where the baseline is
found higher than usual.

Measurements such as width at the baseline, width at half height, area, and total height
can be withdrawn from the peak. For better sensitivity and better resolution, narrower,
sharper peaks are desired.

The accuracy of measurements is influenced by the total number of data points present
across a peak.

FIGURE 4.2.1: Chromatogram output from GC. Image courtesy: Anthias

Consulting.
Types
Majorly, there are two Gas chromatography Mass spectrometry types into which it is
classified – GLC or gas-liquid chromatography and GSC or gas-solid chromatography.

Both the methods use either liquid or solid as a stationary phase while using gas as the
mobile phase. In Gas-solid chromatography, the retention of analytes is due to physical
adsorption. On the other hand, gas-liquid chromatography separates the ions or molecules
that are dissolved in a solvent.

The underlying principle is – as the sample solution makes contact with the second solid
or liquid phase, the solutes will start interacting with the other phases. Due to different
adsorption rates, ion-exchanges, partitioning or sizes, the interaction will vary, and that’s
what will enable the separation of the mixed components from each other. These
differences will make the sample mixture pass at different rates through the column, and
the compounds can be separated.

A Gas Chromatograph like any other analytical instrument has evolved from one with
several knobs and dials to one having a simple microprocessor-based keypad to control
the operational parameters.

The simplification has resulted in ease of operation and time-saving. An understanding of

the main component parts will help in maximum utilization of system capabilities.

Gas chromatography Mass spectrometry applications

Since the discovery of the gas chromatographic system, the areas of Gas chromatography
Mass spectrometry applications is ever-increasing which includes:

 Pharmaceutical industry
 Research
 Medical and Forensic
 Environmental monitoring (both inside laboratories, and natural water bodies)
 Petroleum refining and petrochemicals
 Edible oils
 Flavors, beverages, and the food industry
 Fragrance industry (Cosmetics)
 Polymers and plastics
 Pesticides
Tests performed on GC-MS :
 PCP (Pentachlorophenol) Test
 SCCP (Short chain chlorinated paraffin) Test
 Azo Dyes Test
 PAHS(Polyaromatic hydrocarbons)Test
 COC(Chlorinated aromatic hydrocarbons) Test
 OTC(Organotin compound) Test
 Phthalate Test
 DMFU(Dimethyl fumarate) Test
 Pesticides
 PBDE (Polybrominated diphenyl ethers)
 Bis-Phenol A

4.3 Liquid Chromatography with Mass Spectrometry

4.3.1 Liquid Chromatography
Liquid chromatography is a technique used to separate a sample into its individual parts.
This separation occurs based on the interactions of the sample with the mobile and
stationary phases. Because there are many stationary/mobile phase combinations that can
be employed when separating a mixture, there are several different types of
chromatography that are classified based on the physical states of those phases. Liquid-
solid column chromatography, the most popular chromatography technique and the one
discussed here, features a liquid mobile phase which slowly filters down through the solid
stationary phase, bringing the separated components with it.

4.3.2 About LC-MS/MS

LC-MS is an analytical technique that involves physical separation of target compounds
(or analytes) followed by their mass-based detection. Although relatively new, its
sensitivity, selectivity and accuracy have made it a technique of choice for detecting
microgram or even nanogram quantities of a variety of analytes ranging from drug
metabolites, pesticides and food adulterants, to natural product extracts.

From pharmaceuticals and food to bodily fluids and soil, the analytical lab has seen an
increasing need for accurate measurement of microgram and sub-microgram quantities of
targets, sometimes in complex matrices. While this is no mean task in itself, the potential
need to analyze hundreds of samples as quickly as possible while ensuring data quality
adds additional challenges.
Coupling of liquid chromatography (LC) with mass spectrometry (MS) has provided
analytical scientists with a powerful tool to meet these stringent demands. Due to their
versatility and efficiency, liquid chromatography-mass spectrometry (LC-MS)
instruments have become desirable in many modern analytical laboratories.

The LC-MS technology involves use of an HPLC, wherein the individual components in
a mixture are first separated followed by ionization and separation of the ions on the basis
of their mass/charge ratio.

4.3.3 How Does LC-MS Works?

LC separation

LC brings about a physical separation of the analytes in a liquid sample or a solution of a

solid sample. A few microliters of sample solution are injected into a flowing stream of a
solvent, called the mobile phase. While the optimal injection volume is dependent on the
experimental conditions, it is possible to inject as little as 0.1 µL up to as much as 100 µL
of the sample accurately using an autosampler.1 The mobile phase is continuously
pumped through a column (a stainless-steel tube) usually filled with silica particles
coated with another liquid, the stationary phase. When the sample solution-mobile phase
mix reaches the column, its components will differentially interact with the stationary
phase (which remains in the column) depending upon their chemical composition or
physical properties. Based on the mechanism of interaction between the analyte and the
stationary phase, LC separations have been classified into different modes, such as:

- Partition chromatography –Based on the differing solubility and

hydrophobicity of the analytes in the stationary phase as compared to the mobile phase.

- Ion-exchange chromatography – Separates the analytes on the basis of

their ionic charges.

- Size-exclusion chromatography – Exploits the differences in the sizes

of the analyte molecules to separate them.

- Affinity chromatography –Separates the analytes based on their ability to

bond with the stationary phase.
Some analytes will interact more strongly with the stationary phase than others, resulting
in their separation as they pass through the column. The analytes that have the least
interaction with the stationary phase emerge from the column first. As the mobile phase
continues to flow through the column, the remaining analytes are flushed out
sequentially, those with the strongest interactions emerging last. The time a specific
analyte spends in the column is characteristic of that analyte and is called its
retention time (RT).

LC detection
The mobile phase flowing out of the column (the eluent) passes through a detector that
“responds” to a certain physical or chemical property, such as refractive index or light
absorption, of the analytes within it. This response is captured as a signal or a “peak”
whose intensity (peak area or peak height) corresponds to the amount of the component
present in the sample. The time at which the detector “sees” the analyte is its RT. The
identity of a compound in a sample can be confirmed by comparing its RT with the RT of
a known compound. While this is not an accurate method of compound identification, it
helps when some information about the sample is known a priori.

Using MS for LC detection

Although a wide variety of detectors of differing technologies and sensitivities have been
coupled with LC for analyzing different sample types, the mass spectrometer has
emerged as a selective, sensitive and universal detector.
Unlike other detectors, the LC eluent carrying the separated analytes is not allowed to
flow into the mass spectrometer. While the LC system is operated at ambient pressures,
the mass spectrometer is operated under vacuum and the two are coupled through an
interface. As the column eluent flows into the interface, the solvent is evaporated by
applying heat and the analyte molecules are vaporized and ionized. This is a crucial step
as the mass spectrometer is only capable of detecting and measuring the gas phase
ions.
As the analyte ions are generated at atmospheric pressure in the interface, the process is
called atmospheric pressure ionization (API) and the interface is known as the API
source. Electrospray ionization (ESI) and atmospheric pressure chemical ionization
(APCI) are the most commonly used sources in LC-MS analysis.

The analyte ions are drawn into the mass spectrometer where they are subjected to
electric fields and/or magnetic fields. The flight paths of the ions are altered by
varying the applied fields which ensures their separation from one another on the
basis of their mass-to-charge (m/z) values. Post-separation, the ions can be collected
and detected by a variety of mass detectors,2 of which the most common one is the
electron-multiplier. When the separated ions strike the surface of the electron-
multiplier (a dynode), secondary electrons are released. These secondary electrons
are multiplied by cascading them through a series of dynodes. The amplified
current generated by the flow of the secondary electrons is measured and correlated
to the ion concentrations in the mass spectrometer at any given instant in time
(Figure 4.3.3).

Figure 4.3.3 : Example schematic diagram of an LC-MS setup. Credit: Cwszot, Dagui1929,
CasJu, and YassineMrabet, reproduced under the Creative Commons CC0 1.0 Universal Public
Domain Dedication license.

Plotting LC-MS data

The abundances of the ions measured during the analysis of a sample by LC-MS are
plotted as a total ion chromatogram (TIC). This plot displays the peak intensities of the
analyte ions versus their RT. Further, each point in the chromatogram is associated with a
mass spectrum. The mass spectrum depicts the ion abundances versus the measured m/z
values (Figure 4.3.3.1).
Figure 4.3.3.1: Example output plot from LC-MS analysis. Credit: Daniel Norena-Caro,
reproduced under the Creative Commons CC0 1.0 Universal Public Domain
Dedication license.

The mass spectrum of a compound not only provides information about the mass of the
parent compound (from the m/z value of its ion), but also helps to elucidate the structure
of the compound from the relative abundances of isotopic mass peaks. The area of the
analyte peak is used for its quantification.

The mass spectrometer can be operated in two modes, a) scan and b) selected ion
monitoring (SIM). In the scan mode, it is set to detect all the ions from low m/z to high
m/z values within a specified time period. This mode is used when analyzing unknown
samples or when there is no available information about the ions present in a sample.
When operating in SIM mode, the mass spectrometer is set to measure specific m/z
values. This is the preferred mode of operation for accurate quantification of known
compounds in a sample.

Combining liquid chromatography with tandem mass

spectrometry (LC-MS/MS)

Further improvements in sample identification and accurate quantification can be

achieved by coupling two mass analyzers that are operated in series. Triple quadrupole
mass spectrometers (QQQ or TQMS) and quadrupole time-of-flight (QTOF) are the most
commonly used tandem mass spectrometers. These configurations offer several
possibilities for sample analysis.

LC-MS analysis
LC-MS has been extensively applied for the analysis of both small molecules and large
protein molecules in diverse matrices. Some examples of the applications of this
technology are:
- quantification of genotoxic impurities in active pharmaceutical ingredients
- detection of twelve model compounds that represent specific classes of doping agents,
such as anabolic agents and simulants, in exhaled breath
- quantification of drug metabolites in biological fluids
- detection of adulterants in food materials and dietary supplements
- determination of alkylphenol ethoxylates (APEOs) in tannery sediments
- quantification of personal care products in swimming pool and river water samples
- quantification of nucleotides and their derivatives in bacterial cells
- quantification of the proteome
- as a rapid assay for the detection of SARS-CoV-2

The technique has also been used in the analysis of drinking

water, petrochemicals, soil, biopharmaceuticals, food and wine, and to detect per- and
polyfluoroalkyl substances (PFAS) and pesticide residues.

4.3.4 Tests Performed LC-MS/MS:

• AP/APEO(Alkyl phenol / Alkyl phenol ethoxylates) Test
• Dispersed and Carsogenic dyes/ Blue colorant / quinolone Test
• Bis-phenol A
• PFC( Poly Flurosubstances compound) Test
• Flame retardant Test
• Phenol Test
• PET Analysis
• Vegan Test
 5.INORGANIC DEPARTMENT
• Inorganic department, They are dealing with those tests which consist of
inorganic element such as Lead , Carsogenic , cobalt, cadmium , Mercury ,
Nickel and other heavy metals.
• Different equipment used by inorganic department to get the result with high
accuracy.
• Inorganic chemistry labs play an important role in modern industry. They
are used to study and develop reaction catalysts, polymers, fuels, surfactants,
new materials, superconductors, highly technical ceramic components, and
pharmaceuticals.

5.1 Milli-Q Equipment

• This equipment is used for the purification of water.
• It exclude all the impurity that is less conductivity.
• Milli-Q water is produced by reverse osmosis that normally can even
remove bigger ion.
• To obtain Milli-Q water quality, purified water passes through a long-life
dual wavelength UV lamp, which ensures organic molecule degradation by
photooxidation. The Quantum® polishing cartridge then removes the
remaining ionic and organic contaminants below trace levels.

Figure 5.1 Above figure shows the Milli-Q Equipment

 5.2 Inductively Coupled Plasma Optical
Emission Spectrometry
ICP-OES (Inductively coupled plasma - optical emission spectrometry) is a technique
in which the composition of elements in (mostly water-dissolved) samples can be
determined using plasma and a spectrometer.
• The ICP-OES principle uses the fact that atoms and ions can absorb energy to
move electrons from the ground state to an excited state. In ICP-OES, the
source of that energy is heat from an argon plasma that operates at 10,000 kelvin.
• One of the primary applications of optical emission spectroscopy based on
inductively coupled plasmas (ICP OES) is to analyze elements in very low
concentrations. If you consider metals such as mercury or metalloids like arsenic,
then the reason for these analyses is not hard to understand. Soil sample
investigations, foodstuff testing and drinking water analyses are all carried out for
the health of people and the environment, but the environmental sector is just one
of many important applications for ICP OES. Today, ICP OES plays a crucial role
in other fields as well. Trace elements in fuels can cause premature wear on
engines. The slightest impurities in metals can compromise the most important
properties of those materials. High-frequency tests with low detection limits have
therefore become the standard in many fields.
• ICP OES takes on this role, superseding other methods of elemental analysis.
Short analysis times, multi-element detection and exceptional device sensitivity
are hallmarks of this method. The latest generation of ICP OES devices makes
elemental analysis even more user-friendly, economical, and flexible.
• Atomic spectroscopy basics
Atoms absorb light of the same wavelengths that they themselves emit when
luminescing. Because atoms can only absorb energy in specific quanta, the light
they emit consists of different frequencies. Consequently, by looking at the
spectrum of the absorbed or emitted light, it is possible to distinguish atoms
clearly – two points of departure for elemental analysis.

The principle of operation behind ICP OES

The essential characteristic is in the name itself: ICP OES uses an inductively coupled
plasma to excite the atoms in the sample. A generator supplies argon gas with enough
energy for it to jump to the next physical state. With a high particle density, the plasma
reaches temperatures of 5,000 to 10,000 K. The measurement solution is then injected
into the plasma. It takes a fraction of a second for the sample to dry out, melt and finally
to vaporize. The gas molecules, which are now also being excited, are then atomized and
ionized. They emit the electromagnetic radiation that is used for the actual analysis.
Transfer optics direct the radiation to another optical component that can separate out the
various wavelengths. After the waves are split, a detector registers the intensity of each
wavelength, which is proportional to the concentration of the respective analyte. As the
analysis depends on the correlation between the light intensity and the element
concentration, calibration standards come into play. These calibration standards help to
derive a mathematical function which relates radiation to concentration.

Structure of an ICP OES device

Generate the plasma, insert the sample to excite the atoms, then split and measure the
resulting radiation: Those are the most important steps for ICP OES in a nutshell. The
following overview translates these steps to the technical components of an ICP OES
device.

 Plasma torch: This component is responsible for maintaining the plasma.

The torch also has an injector which introduces the previously atomized sample
into the plasma from the upstream sample insertion system.
 High-frequency generator: The plasma is coupled to a high-
frequency generator responsible for feeding energy to the plasma. It operates at
frequencies of 27 or 40 MHz, which are reserved internationally for this purpose.
 Sample insertion system: Many components come together here. A
peristaltic pump delivers the measurement solution to the atomizer. There, a gas
stream disintegrates the fluid into droplets. The downstream spray chamber serves
to remove larger droplets from the resulting aerosol. The injector in the torch is
connected to this component.
 Transfer optics: The transfer optics are not responsible for separating the
wavelengths. They only serve to transmit the radiation to the dispersing optics.
 Monochromator/ polychromator: Separation into the component
wavelengths can be accomplished in two ways: either sequentially
(monochromator) or simultaneously (polychromator). With ICP OES it is critical
that the optics can distinguish adjacent lines that are extremely close to each other.
 Detector: A CID or CCD sensor is used to detect the signals. The incident
light on the sensor induces a change in charge which is processed as a signal.

Applications of ICP OES

Detection requirements for trace elements are continually increasing. Low detection
limits and short analysis times, and all at low operational expenses: Many laboratories
face the challenge of reconciling these divergent requirements. Its wide range of
applications demonstrates that ICP OES is employed in practically every sector:

 Oil and gas: Political regulations greatly impact fuels and their use. For
example, gasoline is subject to ever-stricter limits on harmful elements like lead
and advanced engine technologies are also pushing up requirements on the quality
of fuel. Elements like vanadium, iron and nickel can damage components through
corrosion processes. Volatile organic compounds like gasoline are therefore one of
the toughest sample matrices for elemental analysis. Soot formation, commonly
observed here, is one of the core challenges for ICP OES. However, state-of-the-
art ICP OES devices with a high plasma power can handle the analyses of these
matrices with high sensitivity and excellent long-term stability.
 Food and agriculture: Cooking oils and fats are important in the food
sector, and also play an important role in the cosmetics industry. Care is required
in the manufacturing process: Secondary processing steps come after the seed oils
are pressed. These are used to adjust desired properties in terms of odor, taste or
shelf life, for example. Chemical changes in the product occur during the process,
which makes it important for analytical testing to follow the product through the
manufacturing process. It ensures that the content of undesired trace elements is
within acceptance criteria. For example, iron and copper stemming from the
manufacturing process can reduce the shelf life of oil. The same goes for beverage
manufacturing: In breweries, one use for ICP OES is to monitor copper impurities
from the brewing kettle. The resulting metallic aftertaste is not exactly a customer
favorite.
 Power plants and energy: In Europe, there is no getting around the
shift to renewable energy. It is steadily becoming a larger proportion of the energy
mix. Cogeneration plants enjoy flexibility in their choice of fuel, but when using
alternative renewable fuels, the limits on the concentrations of potassium or
sodium impurities have to be observed. Otherwise, these alkali metals can cause
severe corrosion on the blades of the gas turbines. Scientists use ICP OES to help
exploit renewable energy sources in sustainably sourced energy generation.
 Geology, mining and metallurgy: The elements in the group of rare
earth metals are indispensable materials in technology products in every field.
Batteries and electric motors are among the most prominent applications. But
increasing demand is threatening a stable supply, making it necessary to extract
even difficult-to-reach deposits. The challenge begins before extraction even
starts, however, as detecting the desired elements in the first place is very difficult.
Matrix-rich rock samples have to be analyzed reliably. Two characteristics of
modern ICP OES instruments are especially in demand here: Stable plasma and a
high-resolution optical system. Stringent requirements also apply to application in
metal production, where even the slightest amount of trace elements can
 significantly alter the performance of high-tech materials. High-resolution ICP
OES devices are a must-have here as well, guaranteeing reliable measurement of
impurities.
 Chemistry and materials science: Urea is a breakdown product
from metabolism; a synthetic form of it is used in cosmetics. Urea is also used to
scrub exhaust gases from combustion. Using selective catalytic reduction, it is
possible to target the reduction of nitrogen oxides. For the treatment of exhaust
gases from diesel motors using urea, standards define upper limits for the content
of iron, copper or zinc to the order of one-tenth of a milligram per kilogram. Other
applications go even further in their purity requirements. Their quality control
requirements are putting more pressure on contract laboratories to detect these
trace amounts continuously and precisely. For ICP OES devices, this means that
they must combine high sensitivity with high long-term stability.
Tests Performed on ICP-OES:
• Lead and cadmium Test
• Nickel test
• Chromium Test

5.3 Inductively Coupled Plasma Mass Spectrometry

Everything around us is made of different combinations of elements. When analysts need
to identify which elements something is made of, they will often use a technique
called inductively coupled plasma mass spectrometry (ICP-MS, or ICP Mass Spec). ICP-
MS is an elemental analysis technique, meaning it is used to measure elements, rather
than the molecules and compounds that are measured by LC/MS and GC/MS.

ICP-MS uses an argon (Ar) plasma – the ICP – to convert the sample into ions that are
then measured using a mass spectrometer – the MS. ICP-MS is similar to inductively
coupled plasma optical emission spectroscopy (ICP-OES), but ICP-OES uses an optical
spectrometer to measure the light emitted from elements as they pass through the plasma,
whereas ICP-MS measures the elements (ions) directly. Both techniques provide fast
analysis of multiple elements in a sample, but ICP-MS provides much lower detection
limits than ICP-OES, so it’s a better choice for trace element analysis.

An ICP-MS instrument consists of the ion source (the ICP), a mass spectrometer (MS) –
usually a scanning quadrupole mass filter, and a detector. The ICP is at atmospheric
pressure, while the MS and detector operate in a vacuum chamber, so an ICP-MS also
requires a vacuum pump, a vacuum interface, and some electrostatic ion “lenses” to focus
the ions through the system. Modern ICP-MS systems also typically contain some device
or mechanism to resolve spectral interferences.
Figure 5.3 The main components of an ICP-MS instrument.

ICP-MS is typically used to analyze samples that are liquids (such as water) or that can
be dissolved, or acid digested, to give a liquid. But ICP-MS is very versatile and can
easily measure organic solvents, detect extremely small (nano)particles, or be connected
to accessories that allow direct analysis of solid materials or gases. ICP-MS can also be
coupled to a chromatographic separation device, such as an HPLC, IC, GC, CE, or Field
Flow Fractionation (FFF), to provide information on the different chemical forms or
“species” of each element in a sample. And, as a mass spectrometric technique, ICP-MS
can also separate and measure the individual isotopes of an element, so it can be used for
applications where isotopic abundances or isotope ratios are of interest.

ICP-MS analysis is used in practically every industry from routine environmental

monitoring, consumer product testing, food and pharmaceutical safety applications,
through life science and clinical research, mining and metals analysis, geochemistry,
nuclear, and petrochemicals, to measuring trace metal contaminants in high purity
chemicals and materials used in semiconductor manufacturing.

ICP-MS can measure virtually every naturally occurring element plus many non-natural
“radiogenic” isotopes such as technetium, neptunium, plutonium, and americium. The
only elements that ICP-MS can’t measure are H and He (which are below the mass range
of the mass spectrometer), Ar, N, and O (which are present at high level from the plasma
and air), and F and Ne (which can’t be ionized in an argon plasma). Of these
“impossible” elements, even F can be analyzed indirectly using a triple quadrupole ICP-
MS.

One of the reasons ICP-MS is so widely used is that it provides extremely low detection
limits for nearly all the elements it can measure. ICP-MS can detect many elements at
levels below 0.1 part per trillion (ppt) – equivalent to one drop of water (50 uL) in 200
Olympic-sized swimming pools (500 million liters). But ICP-MS can also measure
elements at concentrations up to 100s or even 1000s of parts per million (ppm). One
thousand ppm is 0.1%, and the concentration range from 0.1 ppt to 0.1% covers 10 orders
of magnitude. No other technique has such broad elemental coverage, low detection
limits, and wide measurement range.
ICP-MS is a fast and sensitive elemental analysis technique that can measure almost all
the naturally occurring elements and many non-natural, radiogenic elements as well.

How does an ICP-MS work?

An ICP-MS instrument uses a plasma (ICP) to ionize the elements in a sample and
then measures the ions using a mass spectrometer (MS).
The main components of a single quadrupole ICP-MS instrument are:

1. Sample introduction system to form a fine aerosol mist from the liquid sample
2. Plasma (ICP) to convert the elements in the sample aerosol to ions
3. Interface to extract the ions into the vacuum system
4. Ion lens to focus the ions and separate them from background signals
5. Collision/reaction cell (CRC) to resolve the analyte ions from interfering ions
6. Mass spectrometer (MS) to filter the analyte ions by mass
7. The electron multiplier detector
8. Data processing

Figure 5.3.1 Main components of a single quadrupole ICP-MS instrument.

A triple quadrupole ICP-MS (ICP-QQQ, sometimes also referred to as a “TQ”)

includes all these components but with the addition of another quadrupole mass
filter between the ion lens (4) and the CRC (5). The additional mass filter (Q1) of
a QQQ filters the ion beam before the ions reach the CRC, so only a single mass
enters the cell at any given time. This tandem ICP-MS configuration (ICP-
MS/MS) means that reactive cell gases can be reliably used to resolve
interferences, leading to lower detection limits and better accuracy for some
difficult analytes.

Figure 5.3.2Main components of a triple quadrupole ICP-MS (ICP-QQQ) instrument.

Let’s look in a little more detail at the most important components of an ICP-MS
instrument.

1. The sample introduction

ICP-MS is usually used to measure liquid samples. The sample solution is pumped
into a nebulizer, where the liquid is converted into a fine spray or aerosol mist
using a jet of argon gas. The aerosol mist passes through a spray chamber, where
the larger droplets are removed. The fine droplets are carried by the argon gas
flow to the ICP plasma torch.

Figure 5.3.3 A nebulizer turns the liquid sample into an aerosol.

Figure 5.3.4 The aerosol passes through a spray chamber where the larger
droplets are removed.

The sample introduction components are selected and optimized to work in

combination with the ICP. This means that the nebulizer and spray chamber are
designed to produce an aerosol that can be effectively processed by the plasma.
The overall solution load, the aerosol density (number of droplets), and the droplet
size are key factor that affect the ability of the plasma to dry and decompose the
sample material carried in the droplets. The plasma is most effective at producing
ions if the aerosol contains small droplets of uniform size, dispersed across the
central channel of the plasma.
2.The ICP (plasma) ion source
The term “plasma”, which refers to a substantially ionized gas, can apply to things
as diverse as a fluorescent light bulb and the sun. In the plasma used in ICP-MS,
the ionized gas is argon, which flows through a quartz tube. The energy is
provided by a radio frequency (RF) generator operating at about 1.5 KW – around
half the power of a typical domestic kettle. The RF energy is transferred to the
argon gas flow by inductive coupling from a load coil wrapped around the outside
of the quartz tube. The RF field causes free electrons in the argon gas flow to
oscillate; causing them to collide with argon atoms with enough energy to remove
an electron, ionizing the argon atoms. The new argon ions and electrons also
oscillate in the RF field, leading to further collisions and further ionization in a
process that distributes energy through the gas stream to form the plasma. The
energy density in the ionized argon gas is very high, so the ICP reaches a
temperature of 10,000 degrees Celsius – hotter than the surface of the sun!

Figure 5.3.5 The plasma is formed from argon gas flowing in a quartz tube.
 Figure 5.3.6The argon gas is ionized by a radio frequency generator. The sample aerosol is carried
through the center of the plasma.

The argon gas passing through the outer quartz tube flows at a rate of around 15
liters per minute. This “plasma gas” forms the plasma and cools the quartz tube to
prevent it from melting. Two additional, smaller quartz tubes are positioned
concentrically inside the outer tube, together making up the plasma “torch”. The
middle quartz tube carries an auxiliary gas flow which pushes the base of the
plasma away from the inner quartz tubes to prevent them from melting. The
smallest tube – known as the “injector” – carries the aerosol droplets from the
spray chamber to the plasma at a flow rate of around 1 liter per minute. The
injector tube typically has an internal diameter (ID) of around 2 mm or more, so
the carrier gas travels at high speed, punching a hole through the plasma to form
an elongated “torus” or donut shape. The aerosol droplets are carried through the
center of the plasma, where the droplets are dried and the sample material is
decomposed and dissociated into individual atoms, which are then ionized.

Figure 5.3.7 Processes to convert aerosol droplets to ions in the plasma.

Some ICP-MS applications use different torch designs. Options include a demountable
torch with a platinum or sapphire injector tube for use with samples prepared in highly
corrosive acids like HF. Torches with a narrow injector are also available and are
typically used for analysis of volatile solvents and other specialized applications.
The degree of ionization of each element in the plasma depends on the element’s
ionization energy (or ionization potential, IP) and the plasma temperature. The IP is the
amount of energy input that causes one electron to be removed from a neutral atom to
create an ion. Argon is an ideal support gas for ICP-MS because it has a first IP that is
above the first IP of most other elements, but below their second IP (the energy input
required to remove two electrons). This property of argon means that most elements that
pass through the ICP-MS plasma are converted efficiently to singly charged positive ions
(M+), with only a small percentage of doubly charged ions (M2+) being formed. Under
typical plasma conditions, most naturally occurring elements are at least 75% ionized,
which is one of the main reasons for the very high sensitivity of ICP-MS. A few
important elements are less well ionized, however, notably As, Cd, and Hg. Good plasma
optimization is important to achieve high sensitivity and low detection limits for these
elements.

Plot 5.3 showing degree of ionization (% of atoms converted to ions) plotted against first
ionization potential for all elements.

3. The vacuum interface

The plasma ion source and the quadrupole mass spectrometer are separated by a vacuum
interface, which transfers ions from the plasma (at atmospheric pressure) to the mass
spectrometer (in a vacuum chamber). The interface consists of a series of cooled metal
plates or “cones” with small holes in them to allow the ions to pass through. The typical
arrangement uses a sampling cone to extract ions from the plasma, followed by a
skimmer cone to sample the central portion of the ion beam to pass to the high vacuum
region.
Figure 5.3.8 Layout of an ICP-MS system showing vacuum interface between the plasma and
mass spectrometer.

Small cone apertures – around 0.5 to 1.0 mm – are preferred as they provide optimum
vacuum conditions for operation of the quadrupole mass filter and detector. Lower
vacuum pressure (less residual gas) leads to higher ion transmission, less peak
broadening due to scattering, and lower background. But small aperture cones are more
difficult to manufacture precisely and lead to fewer ions being extracted from the plasma
and passed through the interface. Smaller cone apertures would also be more susceptible
to clogging if the sample matrix was not completely dissociated in the plasma. These
considerations mean that the performance benefits of using small cone apertures can only
be realized if the ICP-MS system has a very robust, high temperature plasma and a high
transmission ion lens system.

Figure5.3.9 An ICP-MS interface includes a sampling cone (left) and skimmer cone (right).

4. Ion focusing and separation

After the ions pass through the interface cones, they are focused into a narrow beam
using an ion “lens”. The lens is composed of several metal plates with adjustable voltages
applied to them. A plate with a positive voltage repels the positively charged ions while a
plate with a negative voltage attracts the ions. A combination of lens plates with different
voltages is used to steer and focus the ions.
As well as focusing the ions to maximize transmission and therefore sensitivity, the ion
lens also separates the ions from the neutral particles and photons extracted from the
plasma. These uncharged particles would cause a high background signal, so they must
be prevented from passing through the vacuum system and reaching the detector. This is
usually achieved by deflecting the ions off axis, while the photons and neutrals, being
uncharged, continue in a straight line and so are removed from the ion beam. Several
different ion lens designs are used in ICP-MS, but all have the same goal of providing
high transmission for ions of all masses, while minimizing background signals due to
photons and neutral particles.

Figure 5.3.10 Cutaway showing position and operation of the ion lens.

5. Collision/reaction cell
Since the early 2000s, nearly all new ICP-MS systems have included a collision/reaction
cell (CRC) to resolve spectral overlaps caused by unwanted ions that appear at the same
mass as the analyte ions being measured. By far the most significant spectral overlaps in
ICP-MS are caused by molecular (or “polyatomic”) ions. A polyatomic ion overlap
occurs when a combination of atoms forms an ion at the same mass as an analyte of
interest. For example, 40Ar can combine with 16O to create an ArO+ polyatomic ion at
mass 56, overlapping the major isotope of iron (56Fe). Similarly, 40Ar can combine
with 35Cl to form an ArCl+ polyatomic ion at mass 75, overlapping the only isotope of
arsenic (75As). Polyatomic ion overlaps have been a longstanding problem in ICP-MS, so
the development of CRCs to address these overlaps was a major factor in improving data
accuracy and increasing adoption of ICP-MS across many routine industries.
A CRC consists of an ion guide – usually an octopole or quadrupole – positioned in an
enclosed chamber (or “cell”), that can be pressurized with a gas. Small entrance and exit
apertures maintain the cell pressure while allowing the ions to enter and exit the cell. The
process used to remove the interferences depend on the gas (or gases) added to the cell
and can be broadly divided into collision and reaction modes.
Figure 5.3.11 Cutaway showing position of the collision/reaction cell between the ion lens and
mass filter of a single quadrupole ICP-MS. The cell can be pressurized with a collision or
reaction gas to resolve interfering ions.

Collision mode
In collision mode, the CRC is pressurized with a nonreactive gas – usually helium (He).
Ions passing through the CRC collide with the He atoms, losing a small amount of kinetic
energy with each collision. Polyatomic ions always have a larger ionic cross section than
analyte ions of the same mass, so polyatomic ions collide more often than the analyte
ions do. The different collision rates mean the polyatomic ions emerge from the cell exit
with lower residual energy than the analyte ions. The low energy ions are rejected from
the ion beam by a positive bias voltage “step” using a process called kinetic energy
discrimination (KED).
Collision mode requires that all the ions enter the cell with a narrow ion energy spread.
Also, the ion guide must minimize scattering losses to provide high ion transmission at
the high cell gas pressures and high collision rates required for effective KED.
He KED can be considered as a universal CRC mode, as the same cell conditions can be
used to resolve multiple polyatomic ion overlaps on multiple analyte masses in multiple
different sample types.

Reaction mode
Reaction mode uses the same CRC hardware as collision mode, but the cell is pressurized
with a reaction gas such as H2, O2, NH3, CH4, N2O, or CH3F, rather than He. Reaction
mode can be extremely efficient, as a reaction between the ion and the cell gas molecule
often occurs within the first few collisions, whereas He KED requires multiple collisions
and therefore higher cell gas pressure. Reaction gas methods are also more specific than
He KED, because the gas must be selected based on its different reaction chemistry with
the interfering ion and the analyte isotope. Analysts must therefore know which
interfering ions they are trying to resolve before they select the reaction gas.
Reactive cell gases differ from He KED in that they can be used to resolve interferences
other than polyatomic ions. These other spectral overlaps – such as isobaric overlaps,
doubly charged ion overlaps, and adjacent mass peak-tail overlaps – are less common
than polyatomic interferences but can still be significant.
Figure 5.3.12 Reaction mode operation with single quadrupole ICP-MS configuration

Figure 5.3.13 Reaction mode operation with triple quadrupole ICP-MS configuration.

Reactive cell gas methods combined with ICP-MS/MS have allowed analysts to perform
completely new applications that have been impossible to address with conventional
single quadrupole ICP-MS. New users may be overwhelmed by the range of reaction gas
modes and analysis possibilities available with ICP-QQQ. But the technique is well
established, the reaction chemistry is well understood, and there are software tools and
published methods available to support users in setting up many typical analyses.

6. The mass spectrometer (MS)

Most ICP-MS instruments use a quadrupole (or “quad”) mass spectrometer to filter ions
by mass, or, more accurately, by mass to charge ratio (m/z). Since most ions produced by
the ICP are singly charged, ICP-MS can usually be considered to produce a “mass
spectrum”.
A quadrupole mass filter consists of two pairs of rods; opposite pairs of rods are
connected to separate electrical supplies. An out of phase RF voltage and a positive or
negative DC voltage is applied to the two pairs of rods (RF/+DC on the y-axis rods and
RF/-DC on the x-axis rods). The electric field that is set up in the space between the rods
determines the “set mass” of ions that can travel stably along the quadrupole axis and
pass through the mass filter. The alternating electric fields destabilize the trajectories of
all ions above and below the set mass, so ions at any mass other than the set mass are
rejected from the ion beam.

Figure 5.3.14 Quadrupole mass filter used in most ICP-MS instruments. RF and DC voltages
filter the ions by mass to charge ratio (m/z), allowing only 1 m/z at a time to pass through to
the detector.

The quadrupole set mass is controlled by the applied rod voltages, which can be changed
very rapidly. This means the quadrupole can scan very rapidly across the mass range, for
example from Li (mass 7) to U (mass 238) more than 10 times per second. With each
quadrupole scan, the ions present at each mass are passed to the detector and counted.
In normal quantitative “spectrum” and isotope ratio analysis, the mass spectrum is built
up from multiple scans across the selected masses. Other measurement modes include
time resolved analysis (TRA), where the ion counts collected in each quadrupole scan are
saved on a time-based scale. Single mass monitoring is also available and is typically
used for measurements such as single nanoparticle analysis.

5.4 pH Meter

pH meter, electric device used to measure hydrogen-ion activity (acidity or alkalinity) in

solution. Fundamentally, a pH meter consists of a voltmeter attached to a pH-
responsive electrode and a reference (unvarying) electrode. The pH-responsive electrode
is usually glass, and the reference is usually a silver–silver chloride electrode, although
a mercury–mercurous chloride (calomel) electrode is sometimes used. When the two
electrodes are immersed in a solution, they act as a battery. The glass electrode develops
an electric potential (charge) that is directly related to the hydrogen-ion activity in the
solution (59.2 millivolts per pH unit at 25 °C [77 °F]), and the voltmeter measures the
potential difference between the glass and reference electrodes.

Fig 5.3.15 shows pH Meter

MY ROLE AND RESPONSIBILITY
 Performed and coordinated multiple quality control
activities , knowing about all policies and procedures to
conduct tests followed by the various standards such as
ISO, EN, IS, BS, DIN.
 Worked on several instruments like GC-MS, HPLC, LC-
MS, ICP-MS, ICP-OES, PH Meter, UV Spectrometer.
 Learn new techniques and perform multiple task
simultaneously.
 Good understanding and keep accurate records of testing
methodologies which comply with company policies.
 Prepare reports of different test through analysis of
different formulation as per the SOP.