Introduction chemistry

Analytical chemistry is the chemistry discipline that studies the chemical composition of
materials and develops the tools used to examine chemical compositions. It involves wet lab
chemistry as well as use of instrumentation. Analytical chemistry is important in science,
engineering, medicine and industry. In another way, we can say analytical chemistry is a
branch of chemistry that deals with the analysis of different substance. It involves the
separation, identification and quantification of matter. Also it involves the use of classical
methods along with modern methods involving the use of scientific instruments.
Types of Analytical methods
Analytical methods are broadly classified into two types
(a) Classical wet chemical methods and
(b) Modern instrumental methods
(a) Classical wet chemical methods
Classical wet chemical methods are classified into Qualitative analysis (what is present) and
quantitative analysis (how much is present).

1. Qualitative analysis
Qualitative analysis deals with the identification of elements, ions and compounds present in
the sample. i,e., it is used to characterizes the identity of a specimen. Techniques used in
qualitative analysis include chemical tests, spectroscopy, spectrometry, microscopy and flame
tests.
2. Quantitative analysis
Quantitative analysis deals with the determination of how much of one or more constituent
present. i,e., it is used to examine mass or concentration of the sample. Quantitative analysis
employs analytical balances, gravimetric analysis, volumetric analysis and separation
technique like filtration, centrifugation and chromatography.

a. Gravimetric analysis
Gravimetric analysis involves determining the amount of material present by weighing the
sample before and/or after some transformation. A common example used in
undergraduateeducation is the determination of the amount of water in a hydrate by heating
the sample to remove the water such that the difference in weight is due to the loss of water.

b. Volumetric analysis
Titration involves the addition of a reactant to a solution being analyzed until some
equivalence point is reached. Often the amount of material in the solution being analyzed
may be determined. Most familiar to those who have taken chemistry during secondary
education is the acid-base titration involving a color-changing indicator. There are many
other types of titrations, for example, potentiometric titrations. These titrations may use
different types of indicators to reach some equivalence point

(b) Modern instrumental methods

Modern instrumental methods used to investigate analytes using scientific instruments.
1. Spectroscopy involves the measurement of the interaction between electromagnetic
radiation and the atoms or molecules belonging to a sample.
2. Mass spectrometry used to measure the ration of the mass of the molecule to its charge
with the help of electric fields and magnetic fields.
3. Electro chemical analysis is a common instrumrntal method used in the field of
analytical chemistry. In this method, the analyte is placed in an electrochemical cell and
the voltage or the current flowing through it is measured.
4. Calorimeter is an instrument used to measure the heat of a chemical reaction.
Applications of Analytical Chemistry
Some important applications of this branch of chemistry are listed below.
● The shelf lives of many medicines are determined with the help of analytical chemistry.
● It is used to check for the presence of adulterants in drugs.
● Soil can be tested to check for appropriate concentrations of minerals and nutrients that are
necessary for plant growth.
● It is employed in the process of chromatography where the blood samples of a person are
classified.
Advantages of Instrumental Methods
● Small samples can be used
● High sensitivity is obtained
● Measurements obtained are reliable
● The determination is very fast
● Even complex samples can be handled easily
Limitations of Instrumental Methods
i) An initial or continuous calibration is required
ii) The sensitivity and accuracy depends on the instrument or wet chemical method
iii) The cost of equipment is large
iv) The concentration range is limited
v) Specialised training is needed
vi) Sizable space is required
Advantages of Chemical Methods
i) Procedure is accurate and simple
ii) The equipment needed is cheap
iii) Methods are based on absolute measurements
iv) Specialised training is usually not required
Limitations of Chemical Methods
i) Chemical environment is critical
ii) There is a lack of versatility
iii) Accuracy decreases with decreasing amounts
iv) Procedure is time consuming
v) There is a lack of specificity

Laboratory Hygiene and Safety

Laboratory is a place that provides facilities and controlled conditions for carrying out
scientific experiments and research
Safety is freedom from danger, injury, or damage.
Being safe -actions by you & by others
always seek to do those things that prevent incidents that might cause injury and harm
To ensure safety we must
✔ Recognize hazards
✔ Assess the risks of hazards
✔ Minimize the risks of hazards
✔ Prepare for emergencies.
Hazard
✔ A potential source of danger or harm
✔ chemicals -inherent hazardous properties
✔ safety - minimizing, managing, or controlling these hazards

Risk
✔ Risk is the probability of suffering harm from being exposed to a hazard or unsafe
situation.
✔ The level of risk depends on many things beyond the inherent hazard of a chemical. For
example, the amount of the chemical, the form it is in (gas, liquid, or solid), and how you
handle the chemical all affect the level of risk
✔ Risk is the probability of suffering harm from being exposed to a hazard or unsafe
situation.
Level of risk
✔ The amount of the chemical
✔ the form it is in (gas, liquid, or solid)
✔ and how you handle the chemical
Three factors contribute to safety: 1. Environmental
2. Person factors
3. Behavioral factors
1. Environmental factors including Facilities, location, equipment, procedures, and
standards
2. Person factors - attitude, beliefs, personality, knowledge, skills, and abilities
3. Behavior factors including safe and risky practices anything out of place- move it back
out of the way.
Safety Rules for Laboratories
1. Follow instructor
2. Wear proper eye protection
3. Wear clothing that protects against exposure and provides protection from spills. -lab coat
✔ Avoid loose cloths
✔ Confine long hair
✔ Avoid wearing dangling jewelery
✔ Do not use personal handkerchief in lab
✔ Do not eat, drink, smoke chew gum, apply cosmetics, or take medications in the
laboratory
✔ Do not use laboratory glassware & equipment to prepare & store food
✔ Keep hands away from eye, nose, mouth, face, hair & open skin wound
✔ Clean all spills immediately & remove broken glassware
✔ Use books & journals only in clean area to prevent contamination
✔ In case of hazardous spill inform instructors
✔ There should be no boisterous conduct, excessive noise (radios, DVD players, iPods), or
practical jokes in the laboratory.
✔ Never taste any laboratory chemical
✔ When smelling a chemical, gently waft the vapors toward your nose.
✔ Do not directly inhale the vapors
✔ If any chemical spills on your skin or in your eyes - flush affected area with water - notify
the instructor
✔ Use test tube holder for heating test tube
✔ Know Location of emergency equipment
✔ If any chemical spills on your skin or in your eyes - flush affected area with water - notify
the instructor
✔ Do not work alone in the laboratory
✔ Do not heat flammable liquids with a Bunsen burner or other open flame 19
✔ Label all containers with chemicals or solutions
✔ Dispose of waste chemicals in the containers provided
Storage & handling of chemicals:
Chemical storage area
1. Located away from process area & occupied building
2. Constructed from fire resistant material
3. must have continuous ventilation
4. Checked periodically for odour
5. Passageways not to be blocked
6. Should not have floor drains to prevent contamination with water
7. Proper posting in front of store room
8. Chemicals to be delivered to storage area for proper maintenance of inventory
9. All containers in good condition & properly closed
10. Tanks & containers properly labeled
11. Secondary containment for all liquid hazardous materials
12. Reserve supply of chemicals kept minimum
13. Expired chemicals marked for disposal
14. Incompatible chemicals separated i) Flammables – oxidizers ii) Strong acid – strong bases
15. Toxic & corrosive chemicals isolated16. Acids stored in acid resistant containers
17. HNO3 , H2SO4 , HCl stored in glass containers HF in plastic or ceresin containers
18. Flammable solvent away from fire hazard, doors
19. Hazardous chemicals not stored above eye level
20. Large bottles stored no more than 2 feet above ground
Inside laboratory
1. Large quantity of chemicals not to be stored in lab
2. Working quantity of routinely used chemicals
3. Minimum quantity of hazardous chemicals
4. Chemicals arranged in compatible families
5. Not arranged alphabetically
6. Shelf with small frontal barriers – prevent sliding
7. Chemicals not to be stored above eye level
8. Chemicals not to be stored on floor
9. Chemicals kept away from heaters & sunlight
10. Clearly & legibly labled
11. Refrigerator used to store chemicals not to store food
12. Chemicals that react vigorously with water kept away from possible contact
13. Toxic, volatile, carcinogenic & reactive chemicals tightly sealed with appropriate
stoppers
14. Potentially explosives flammable chemicals stored only in rated or explosion proof
refrigerators
15. Do not store chemicals in fume cupboard
16. Compressed gas cylinders kept upright, away from heat source without blocking exits
Handling of chemicals
1. Familiar with chemical properties & hazards
2. Read label twice
3. Pour out only required quantity of chemicals –prevent waste
4. Transport chemicals on cart that can contain spills
5. Use non breakable & secured secondary containers for transportation of hazardous waste
6. Do not touch chemicals with hand
7. Do not smell chemicals directly
8. Do not taste chemicals
9. Do not hurry
10. While diluting add acid to water not vice versa
11. Avoid mouth suction of pipette
12. Do not use damaged equipment
13. Ensure ventilation of lab
14. Close containers when not in use
15. Do not use metal spatula to handle peroxides – metals can catalyze their explosive
decomposition, use ceramic, Teflon or wooden spatula

Simple First Aid – Electric shock

1. Switch of source of electricity
2. Check victim for breathing & heartbeat3. If unresponsive or shows abnormal breathing -
CPR (Cardiopulmonary resuscitation
4. Arrange emergency medical aid
Burns : I st degree burns
✔ outer layer of skin damaged
✔ pain low to moderate
✔ no blisters
✔ colour of affected area red
2 nd degree burn
✔ outer & second layer of skin damaged
✔ pain level high
✔ blisters present
✔ colour of area red
3 rd degree burn
✔ outer & second layer of skin & tissue below damaged
✔ pain level high
✔ no pain felt if nerves damaged
✔ burn site white/charred
Initial steps for all burns
1. Put out fire/ stop contact with source of burn
2. If flames on cloth – Stop Drop Roll
3. Burn hot jewelry or burnt clothing that does not stick to skin
4. If sticking to skin do not pull it off
5. Cut or tear aroun
Treatment for 1st & 2nd degree burns
1. Hold under cool running water/immerse in water till pain subsides
2. continue for 15 minutes
3. For large area stay under safety shower for 10-15 minutes
4. Don’t - break blisters apply ice, cream, honey, butter, cream Cover with sterile non
adhesive
bandage Seek medical advice
Treatment for 3rd degree burns
1. Call for emergency medical help
2. Cover burnt area with sterile, nonstick bandage or clean lint free cloth
3. Do not soak in water
4. Do not apply ointment, cream, butter etc.

Cut by glass
Minor Cuts
✔ let it bleed to wash out foreign particles
✔ Wash with antibacterial soap, cold running water
✔ Dry with sterile pad
✔ Apply antiseptic cream
✔ Major cuts Slicing into skin, punctured underlying blood vessel, significant bleeding
If no glass present
✔ Wash with soap & running water
✔ If bleeding does not stop – absorbent pad over wound & apply pressure✔
Hold pressure for 15 minutes
✔ Raise injured area above heart level
✔ Get medical attention
Major cuts Small glass piece in wound
✔ Wash with cool running water
✔ Flush glass out
✔ If glass piece suspected – do not apply pressure
✔ Lightly apply sterile dressing
✔ Get medical attention
Major cuts - Glass/object in wound
✔ Do not i) remove object from wound – increase bleeding ii) Apply pressure above wound
✔ Apply pressure on either side of wound
✔ Apply light dressing to stabilize object
✔ Build up padding around object till higher than object
✔ Bandage over without pressing
✔ Medical attention
Inhalation of poisonous gas
✔ Remove to prevent further inhalation
✔ Take to fresh air
✔ Give CPR
✔ Check MSDS for first aid information
✔ Do not attempt rescue unless safe to do so
Accidents due to acids & alkali
Skin contact
✔ Wash burnt area with large quantity of water
✔ Do not apply neutralizing or buffering agents
✔ Remove contaminated clothing
✔ Check MSDS for first aid
Eye contact
✔ Wash with large amount of running water
✔ Occasionally lift & lower upper lid
✔ Remove contact lens after hurried wash
✔ Medical attention

Disposal of sodium
✔ Add scraps of sodium to 95% ethanol in fume hood
✔ At least 20ml for 1g Na
✔ Solvent should not boil
✔ C2H5ONa formed
✔ When visually reaction is complete, add water with swirling
✔ Allow to stand, dilute & discard
Disposal of broken mercury thermometer
✔ Open all windows for ventilation
✔ Collect large piece of glass – zip bag
✔ Use flash light to check extend of spill✔ Use index card to scoop mercury & small glass
beads to zip bag
✔ Use flash light to locate remaining shiny mercury beads
✔ Use dropper, do not touch with hand
Disposal of broken mercury thermometer
✔ Wrap a piece of scotch tape around gloved index finger with sticky side out & dab
contaminated area
✔ Used index card, dropper, tape, glove into zip bag
✔ Moisten Zn powder rub over contaminated area –leave for a day –solid amalgam formed
✔ 20% solution of Calcium polysulphide –solid mercuric sulphide formed
✔ Use index card to scrap of solid product –zip bag
✔ Zip bag, clothings etc sealed & disposed
CaCl2 & Silica Gel - Dessiccator
✔ Used for absorbing moisture/water
✔ CaCl2 – cheap, high capacity for water absorbtion
✔ Active mechanism - hydration – CaCl2 .6H2O
✔ Water of hydration removed by heating
✔ Hazard – mild skin irritation with dry skin, burns wet skin; Ingestion – irritates mucous
memberane , gastrointestinal problems
Silica Gel
✔ Chemically inert, non toxic
✔ Amorphous, granular & porous form of Silicon dioxide made from sodium silicate
✔ High surface area – best at Room Temp
✔ Active mechanism – adsorbtion, absorbs 40% of mass
✔ Reactivated by heating in a oven
Can irritate eye, skin, respiratory system
Corrosive chemicals

Chemicals which corrode or destroy gradually,skin wood cloth,metal,etc

are called corrosive chemicals
Examples::acids (HCl, HNO3), Chlorine,bromine,phenols

Flammable chemicals
Chemicals which catch fire on exposure to air or on heating over a naked flame
or in a arm surroundings are called flammable chemicals
Examples : ether , benzene,CS2 ,alcohol
Explosive chemicals
Chemicals which explode violently on heating, grinding, or pressing are called
explosive chemicals
Examples: chlorates, nitrates, ethers, peroxides

Toxic chemicals
They are substance related to poison when taken in ,they produce ill effect on
health problems
Examples :benzene, chloroform,CCL4

Carcinogenic chemicals
Chemicals which cause cancer are called carcinogenic chemicals
Examples :methyl iodide (cause blood cancer), aziridine,benzene

Poisonous chemicals
Chemicals which introduced into or absorbed by a living organism cause
death or injury especially one that kills by rabid action ,even in small quantity
are called poisonous chemicals
Examples :benzene,toluene,DDT,CHCl3
 Volumetric Analysis:
Volumetric analysis is a quantitative analysis in which volume of known concentration
solution (standard) required to react with a solution of unknown concentration is determined.
Volumetric reactions are
1. Simple and easy
2. Fast and can be done on site.
3. Less Expensive
4. Estimation of content or Assay of Chemical
5. Precise and accurate-depends on method and specificity.
Apparatus Needed for Volumetric Analysis:

1. Titration:
Titration is the process of determining the volume of the known strength
(concentration) solution required to react with a known volume of unknown
strength solution.
2. Titrant and Titrate:
The solution taken in a burette use in titration is called the titrant and the solution taken in a
conical flask is called titrate.
3. Equivalence Point or Theoretical end point:
The volume at which reaction actually completed by addition of stoichiometric
amount of titrant is known as equivalence point or theoretical end point.
4. Indicator:
A substance which is used for the visual detection of the completion of a
particular reaction to determine the end point of a titration is called as indicator.
5. End Point:
The volume at which the completion of the reaction is observe by using an indicator is called
the end point, the visual observation is colour change or
fluorescence or turbidity formation.
6. Titration error:
In practice, there is difference between equivalence point and end point. This
difference is known as titration error.
Requirements of volumetric Analysis
1. The chemical reaction must be simple and takes place quantitatively to form
known product.
2. The reaction shows some marked changes in some properties at equivalence
point.
3. It should be stoichiometric.
4. It should be free from side reactions
5. It should be specific for the substances to be analysed.
6. The end point should be well defined and shows visible change by the use of indicator,
7. The reaction should be relatively fast.
Advantages of volumetric Analysis
1. These analysis required simple apparatus like burette, pipette, conical flask,
etc.
2. The analysis process does not involve laborious operations.
3. It can be performed quickly and results obtained readily.
4. This method is more precise and accurate.
5. Depending upon the nature of substances to be analysed different types of
titrimetric methods can be used.
Standard Solution:
Volumetric Analysis depends on the use of at least one standard solution. Standard
solution is the solution of known strength. A standard solution is prepared by dissolving an
accurate weighted quantity of a highly puresubstance.

Primary Standard Solution

A highly pure substance which is used to which is used to prepare standard solution by
direct weighting it, is known as primary standard substance. Standard solution is prepared by
dissolving an accurate weighted quantity of a Primary standard substance.
Example :sodium carbonate, ferrous sulphate,potassium dichromate etc
Secondary Standard Solution
Those substances whose solution can not be prepared by direct weighting are not used as a
Primary standard solution. These types of substances are called as Secondary standard
substances
Example : sodium hydroxide,potassium permanganate

Molarity(M)
Number of moles of solute present in one litre (dm3 ) of the solutiom

Molality (m)
Number of moles of solute present in one kilogram (1 kg) of a solvent

Normality

Number of gram equivalent substance present in one litre (dm3 ) of the solutiom
Normality = weight/litre
Equivalent weight
Formality: Formality is the number of formula mass in gram present per litre of a solution

Mole Fraction: The mole fraction of any component of a solution is defined as the ratio
of the number of moles of that component present in the solution to the total number of moles
of all components of the solution.