INDEX

 INTRODUCTION TO PROJECT VENUE – CENTURY RAYON, SHAHAD

 RAYON – HISTORY & UTILITY

 METHOD OF RAYON PRODUCTION

 YARN

 VISCOSE PROCESS OF RAYON YARN PRODUCTION

 EFFLUENT TREATMENT

 TOTAL QUALITY MANAGEMENT IN PRODUCTION

POLLUTION ANALYSIS
PHYSICAL PARAMETER
CHEMICAL PARAMETER
WATER ANALYSIS
PREPARATION OF STANDARD SOLUTIONS
(NaOH, H2SO4, Na2S2O3.5H2O)

 GENERAL

 SAFETY IN LABORATORY

1
CENTURY RAYON is a division of Century Textiles & Industries Limited, which belongs to B. K.
Birla Group of Companies, one of the largest industrial houses in India. The division is situated at
Shahad, about 60 Kms, North of Mumbai, on the bank of Ulhas River.

Rayon division at Shahad commenced its operations in 1956 with an industrial production capacity
of 5.5 Tons of Viscose filament yarn per day. Today, it is the largest producer of viscose filament yarn
in the country, having the capacity of 45 tons per day.

Century Rayon commenced Caustic Soda production for its captive consumption way back in the
year 1964 with 30 TDP mercury cell plant. In the year 1993, the company installed pollution free
membrane cell plant and discontinued mercury cell plant. Today, it produces 55 TDP of Caustic Soda
& allied chemicals. Century Rayon also produces Carbon-disulphide, Sulphuric Acid which are the
basic raw materials for producing viscose filament yarn.

It’s now one of the largest manufacturer & exporter of Viscose Filament Pot Spun Yarn, Continuous
Spun Yarn, & Tyre Yarn. All these plants are accredited with ISO 9001: 2000 Certification. Century
Rayon commands 28% of the Indian Viscose Filament Yarn market. The financial annual turnover
exceeds INR 400 crores (approx US $ 90 Million).

PLANT PRODUCT CAPACITY

Rayon (Estd.1056) Viscose Rayon Filament Yarn 16,000 MT/annum
Tyre Yarn/ Cord (Est. 1963) High Tenacity Tyre Yarn 6,500 MT/annum
CSY (Est. 1998) Continuous Spun Yarn 2.500 MT/annum

Inn 1963, the rayon Division diversified in to production of high tenacity viscose tyre yarn/cord. The
plant was installed in collaboration with Algemene Kuntzidjeunu NV of Holland & Galansztoff AG
of Germany. Today the plant is operating at 18 TPD production capacity.

In the year 1998, the “State of Art” machines for production of Continuous Spinning Yarn were
installed. Continuous Spun Yarn has many advantages over conventional pot spun viscose filament
yarn. The plant was expanded to capacity of 7 TPD in year 2003.
2
 RAYON
Rayon is one of the most peculiar fabrics in commercial use today. Strictly speaking it is not an
artificial fiber, because it is derived from naturally occurring cellulose. It is not, however, a natural
fabric because cellulose requires extensive processing to become RAYON. Rayon is usually
classified as manufactured fiber and considered to be “Regenerated Cellulose”.

Skeins of artificial silk produced by the viscose above shows the first attempt to make colored

Spinning syndicate Silks.

Rayon is the oldest manufactured fiber, having been in production since the 1880’s in France, where
it was originally developed as a cheap alternative to silk. DuPont Chemicals acquired the rights to the
process in the 1920’s and quickly turned rayon into a household world, churning out yards of the
cheap, versatile fabric. Rayon drapes well, is easy to dye, and is highly absorbent, although it tends to
age poorly. Many rayon products yellow with age and pill or form small balls and areas of roughness
where the fabric is most heavily worn.

Rayon is a manufactured regenerated cellulose fiber, because it is produced from naturally occurring
polymers, it is neither a truly synthetic fiber nor a natural fiber; it is a semi-synthetic fiber. Rayon is
known by the names Viscose Rayon and art silk in the textile industry. It usually has a high luster
quality giving it a bright shine. Rayon contains the chemical element carbon, hydrogen, and oxygen.

Cellulose is treated with alkali and carbon disulfide to yield viscose.

3
 RAYON
USES OF RAYON:-
Some major rayon fiber includes apparel (E.g. Blouses, Dresses, Jackets, Lingerie, Linings, Scarves,
Suits, Ties, Hats, and Socks) furnishings (E.g. Bed spreads, Blankets, Window Treatments,
Upholstery, Slipcovers) industrial uses (E.g. Medical surgery products, Non woven products, tire
cord), and other uses (E.g. Yarn, Feminine hygiene products, Diapers)

A sample of rayon from skirt, blouse, shirt with different texture.

4
 RAYON
HISTORY:-

Nitrocellulose
The fact that Nitrocellulose is soluble in organic solvents such as Ether & Acetone, made it possible
for Georges Audemars to develop the first “Artificial Silk” about 1885, but his method was
impractical for commercial use. The commercial production started in 1891, but it was flammable,
and more expensive than acetate or cuprammonium rayon. Because of this, production was stopped
before World War I, for example in Germany. Briefly, it became known as “Mother-in-law silk”.
Nathan Rosenstein invented the spunize process by which he turned rayon from hard fiber to a fabric.
His allowed Rayon to become a popular raw material in textiles.

Acetate method:
Paul Schutzenberger discovered that cellulose can be reacted with acetic anhydride to form
cellulose acetate. The triacetate is only [citation needed] soluble in chloroform making the method
expensive. The discovery that hydrolyzed cellulose acetate is soluble in less polar solvents, like
acetone, made production of cellulose acetate fibers cheap and efficient.

Cuprammonium Method:
The German chemist Eduard Scheweizer discovered that tetraaminecopper dihydroxide could
dissolve cellulose. Max Fremery & Johann Urban developed a method to produce carbon fibers
for use in light bulbs in 1897. Production of Rayon for textiles started in 1899 in the Vereinigte
Galanzstofffariken AG in Oberbrunch. Improvement by J. P. Bamberg AG in 2004 made the
artificial silk a product comparable to real silk.

VISCOSE METHOD

Finally, in 1894, English chemist Charles Frederic Cross, and his collaborators Edward John
Bevan, & Clayton Beadle patented their artificial silk, which they named “VISCOSE”, because the
reaction product of carbon disulphide and cellulose in basic conditions gave a highly viscous solution
of Xanthate. The first commercial viscose rayon was produced by the UK Company Courtaulds
Fibers in 1905. Avtex Fibers Incorporated began selling their formulation in the United States in
1910. The name “RAYON” was adopted in 1924, with “VISCOSE” being used for the viscous
organic liquid used to make both rayon and cellophane. In Europe, though, the fabric itself became
known as “Viscose”, which has been ruled an acceptable alternative term for rayon by the U.S.
Federal Trade
Commission. The method is able to use wood (Cellulose & Lignin) as a source of cellulose while the
other methods need lignin-free cellulose as starting material. This makes it cheaper and therefore it
was used on a larger scale than the other methods.
Contamination of the waste water by carbon disulfide, lignin and the xanthates made this process
detrimental to the environment. Rayon was only produced as a filament fiber until the 1930’s when it
was discovered that broken waste rayon could be used in staple fiber.
The physical properties of rayon were unchanged until the development of high-tenacity rayon in the
1940’s. Further research & development led to the creation of high-wet-modulus rayon (HWM
Rayon) in the 1950’

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 RAYON
MAJOR FIBER PROPERTIES:-
Rayon is a very versatile fiber and has the same comfort properties as natural fibers. It can imitate the
feel and texture of silk, wool, cotton and linen. The fibers are easily dyed in a wide range of colors.
Rayon fabrics are soft, smooth, cool, comfortable, and highly absorbent, but they do not insulate
body heat, making them ideal for use in hot and humid climates.
The durability and appearance retention of regular rayon are low, especially when wet; also, rayon
has the lowest elastic recovery of any fiber. However, HWM rayon is much stronger and exhibits
higher durability and appearance retention. Recommended care for regular is dry-cleaning only.
HWM rayon can be machine washed.

BASIC PRINCIPLESOF RAYON FIBER PRODUCTION:-

In the production of Rayon, purified cellulose is chemically converted in to a soluble compound. A
solution of this compound is passed through the spinneret to form soft filaments that are then
converted or “Regenerated” into almost pure cellulose. Because of the reconversions of the soluble
compound to cellulose, Rayon is referred to as a regenerated cellulose fiber.
There are several types of Rayon fibers in commercial use today, named according to the process by
which the cellulose is converted to the soluble form and then regenerated. Rayon fibers are wet spun,
which means that the filaments emerging from the spinneret pass directly into chemical baths for
sodifying of regeneration.
Viscose rayon is made by converting purified cellulose to Xanthate, dissolving the Xanthate in dilute
caustic soda and then regenerating the cellulose from the product as it emerges from the spinneret.
Most rayon is made by the viscose process.

PRODUCTION OF VISCOSE

Viscose Process:
Most commercial rayon manufacturing today utilizes the viscose process. This process dated to the
early 1900’s, with most of the growth in production occurring between 1925 & 1955. In the early
period, production was mainly textile filament, although the first staple was produced in 1916. High
performance rayons, such as tire cord, did not appear until the late 1930’s with the advent of hot-
stretching and addition of larger amounts of zinc to the spin bath. Invention of modifiers in 1947
brought on super tire cords and marked the beginning of the high-performance rayon fibers.
All of the early viscose production involved batch processing. In more recent times, processes have
been modified to allow some semi-continuous production. For easier understanding, the viscose
process is a batch operation.

6
RAYON

7
 RAYON
Cellulose:
Purified cellulose for rayon production usually comes from specially processed wood pulp. It is
sometimes referred to as “Dissolving Cellulose” or “Dissolving Pulp” to distinguish it from lower
grade pulps used for papermaking and other purposes. Dissolving cellulose is characterized by high
α-cellulose content. I.e. it is composed of long-chain molecules, relatively free from lignin and
hemicelluloses, or other short-chain carbohydrates.

Steeping:
The cellulose sheets are saturated with a solution of caustic soda (or sodium hydroxide) and allowed
to steep for enough time for the caustic solution to penetrate the cellulose and convert some of it into
“Soda cellulose” the sodium salt of cellulose. This is necessary to facilitate controlled oxidation of
the cellulose chains and the ensuing reaction to form cellulose Xanthate.

Pressing:
The soda cellulose is squeezed mechanically to remove excess caustic soda solution.

Shredding:
The soda cellulose is mechanically shredded to increase surface area and make the cellulose easier to
process. This shredded cellulose is often referred to as ‘White crumb”.

8
 RAYON
Ageing:
The white crumb is allowed to stand in contact with the oxygen of the ambient air. Because of the
high alkalinity of white crumb, the cellulose is partially oxidized and degraded to lower molecular
weights. This degradation must be carefully controlled to produce chain lengths and short enough to
give manageable viscosities in the spinning solution, but still long enough to impart good physical
properties to the fiber product.

Xanthation:
The properly aged white crumb is placed into a churn, or other
mixing vessels, and treated with gaseous carbon disulfide. The soda
cellulose reacts with carbon disulfide to form Xanthate ester groups.
The carbon disulfide also reacts with the alkaline medium to form
inorganic impurities which give the cellulose mixture a characteristic
yellow color and this material is referred to as “Yellow crumb”. Because accessibility to the carbon
disulfide is greatly restricted in the crystalline regions of the soda cellulose, the yellow crumb is
essentially a block co-polymer of cellulose and cellulose Xanthate.

Dissolving:
The yellow crumb is dissolved in aqueous caustic solution. The large Xanthate substituents on the
cellulose force the chains apart, reducing the inter chain hydrogen bonds and allowing water
molecules to solvate and separate the chains, leading to solution of the otherwise in soluble cellulose.
Because of the blocks of unxanthated cellulose in the crystalline regions, the yellow crumb is not
completely soluble at this stage. Because the cellulose Xanthate solution (or more accurately,
suspension) has a very high viscosity, it has been termed “Viscose”.

Ripening:
The viscose is allowed to stand for a period of time to “Ripen”. Two important processes occur
during ripening: Redistribution and loss of Xanthate groups. The reversible Xanthation reaction
allows some of the Xanthate groups to revert to cellulosic hydroxyls and free carbon disulfide CS 2 .
This free CS2 can then escape or react with other hydroxyn on other portions of the cellulose chain.
In this way, the ordered, or crystalline, regions are gradually broken down and more complete
solution is achieved. The CS2 i.e. lost reduces the solubility of the cellulose and facilitates
regeneration of the cellulose after form in to a filament.

Filtering:
The viscose is filtered to remove undissolved materials that might disrupt the spinning process or
cause defects in the rayon filament.

Degassing:
Bubbles of air entrapped in the viscose must be removed prior to extrusion or they would cause
voids, or weak spots, in the fine rayon filaments.
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 RAYON

Spinning:
The viscose is forced through a spinneret, a device resembling a shower head with many small holes.
Each hole produces a fine filament of viscose. As the viscose exits the spinneret, it comes in contact
with a solution of sulfuric acid, sodium sulfate and, usually, Zn++ ions. Several processes occur at this
point which cause the cellulose to be regenerated and precipitate from solution. Water diffuses out
from the extruded viscose to increase the concentration in the filament beyond the limit of solubility.
The Xanthate groups form complexes with the Zn++ which draw the cellulose chains together. The
acidic spin bath converts the Xanthate functions into unstable Xantheic acid groups, which
spontaneously lose CS2 and regenerate the free hydroxyls of cellulose. This is similar to the well-
known reaction of carbonate salts with acid to form unstable carbonic acid, which loses CO2. This
results in the formation of fine filaments of cellulose, or rayon.

(JET USED IN SPINNING)

Drawing:
The rayon filaments are stretched while the cellulose chains are still relatively mobile. This causes
the chains to stretch out and orient along the fiber axis. As the chains become more parallel, inter
chain hydrogen bonds form, giving the filaments the properties necessary for use as textile fibers.

Washing:
The freshly regenerated rayon contains many salts and other water soluble impurities which need to
be removed. Several different washing techniques may be used. In cake conditioning room, cakes are
kept in 65% humid atmosphere to retain moisture and become soft and conditioned.

10
 RAYON

Cutting:
If the rayon is to be used as staple (i.e. discreet lengths of fiber), the group of filaments (termed
“TOW”) is passed though a rotary cutters to provide a fiber which can be processed in much the
same way as cotton.

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 YARN
Yarn is a long continuous length of interlocked fibers, suitable for use in the production of textiles,
sewing, crocheting, knitting, weaving, embroidery and rope making.
Thread is type of yarn intended for sewing by hand or machine. Modern manufactured sewing
threads may be finished with wax or other lubricants to with stand the stresses involved in sewing.
Embroidery threads are yarns specifically designed for hand or machine embroidery.

YARN SPOOLS OF THREAD

Structure:
Spun yarn is made by twisting or otherwise bonding staple fibers together to make a cohesive
thread. Twisting fibers in to yarn in the process called spinning can be dated back to the upper
Paleolithic, and yarn spinning was one of the very first processes to be industrialized. Spun yarns
may contain a single type of fiber, or be blend of various types. Combining synthetic fibers (which
have high strength, artificial luster, and fire retardant qualities) with natural fibers (which have good
water absorbance and skin comforting qualities) is very common. The most widely used blends are
cotton-polyester and wool-acrylic fiber blends. Blends of different natural fibers are common too,
especially with more expensive fibers such as Angora and Cashmere.
Yarns are made up of a number of plies, each ply being a single spun yarn. These single plies of yarn
are twisted in the opposite direction (plied) together to make a thicker yarn. Depending on the
direction of this final twist, the yarn will be known as S – TWIST or Z – TWIST. For a single ply,
the direction of the final twist is the same as its original twist.

Filament yarn consists of filament fibers twisted together. Thicker monofilaments are typically used
for industrial purposes rather than fabric production or decoration. Silk is a natural filament, and
synthetic filament yarns are used to produce silk-like effects.

Texturized yarns are made by a process of air texturizing (sometimes referred to as taslanizing),
which combines multiple filaments yarns into a yarn with some of the characteristics of spun yarns.

A SPINNING JENNY, SPINNING MACHINE WHICH INITIATED THE INDUSTRIAL

REVOLUTION & Z AND S TWIST.

12
 YARN
VISCOSE PROCESS OF RAYON YARN PRODUCTION

1. PULPER:-

• Pulp is cellulose and mostly obtained from Eucalyptus plant.

• In pulper, pulp + caustic are mixed properly to form alkali cellulose slurry.

2. HOMOGENISER TANK:-

• It receives alkali cellulose slurry from pulper through pump.

• The homogenizer tank is surrounded by jacket through which hot water is circulated to
maintain temperature of slurry at 470C

3. GRASIM DRUM PRESS:-

• As the name suggests it is made up of 2 drums which rotates in opposite direction so that the
solid particles (alkaline cellulose slurry) can be grabbed by drums to form mat.
• The liquid caustic and dissolved impurities removed from the Grasim drum press can be
reused.

4. SHREDDER:-

• Alkali cellulose mat gets cut here into pieces to form filthy crumbs.

5. AGEING DRUM:-

• Long chain polymers are converted into short chain polymers by air oxidation.
• Time for one rotation is 3 min.
• The alkali cellulose is oxidized for 8 hrs.

6 .HOPPER:-

• It weights up to 2000 kg of alkali cellulose and then dumps it into simplex.

• Hopper balance is calibrated periodically to avoid any error in batch weight.

7 .XANTHATOR:-

• After dumping alkali cellulose in Xanthator, vacuum is created in simplex to avoid

inflammation during addition of CS2 (highly inflammable and toxic).
• Here, alkali cellulose is converted into sodium cellulose Xanthate which is in the form of
sticky balls.
• To dissolve the Xanthate balls chilled NaOH ( 8OC-24GPL) is added to 5500 liters.

8. DISSOLVER:-

• Xanthate slurry from simplex form raw viscose for further purposes.
• The impurities present the slurry mainly contains air bubbles, particles and maturity.

9 .BLENDER:-

13
 YARN
• Viscose is constantly agitated in blender.

10 .GRASIM CONTINOUS FILTER (GCF):-

• This is Іst stage filter.

• Different size particles are separated in this filter.

11. RECEIVING TANK (REACTION TANK):-

• This is Пnd stage filter.

• Waste impurities are allowed to settle down.

12. B – TANK:-

• It is a type of storage tank and has same purpose as reaction tank.

13 .FLASH DEAERATOR:-

• Viscose is passed by feed pump to flash deaerator where air bubbles are removed to avoid
breaking of filament.

14. F.D.BLENDER:-

• This is Шrd stage filter.

• Here fine particles are filtered away.

15. SPINNING VISCOSE TANKS:-

• The viscose is metered by a viscose metering pump for each spinning position.
• The metering pump action ensures constant and regular delivery of viscose to the candle filter
and spinning jet.
• Any change in the speed of pump drive will change the deiner of the yarn. (Denier is wt. in
Gms of 9000m length of a yarn.)

16. SPINNING DEPARTMENT:-

• Viscose is passed in spinning department through pumps.

• In this, spinnerets are submerged in the acid spin bath.
• The acid spin bath contains 3 main acids , H2SO4 , ZnSO4 & Na2SO4 respectively
• H2SO4 (138 gpl) helps neutralize caustic in viscose.
• ZnSO4 (16 gpl) helps to give strength.
• Na2SO4(238 gpl ) helps solidification and regeneration .
• Spinneretes (jets) are made up of an alloy of noble metals like gold, platinum and rhodium. It
has 24 holes having diameter of 250 microns.
• As the viscose sol. Passes through spinnerets into the acid bath it solidifies into filaments.
• Cake formation takes place due to Bakelite spinning pot which rotates at about 7800 rpm.

17 .WASHING:-

14
 YARN
• Washing of cake is done by soft water and by using various chemicals like EDTA, FSS etc.
• Bleaching is also done in order to remove yellowness.

15
 YARN
18 .HYDRO EXTRACTOR:-

• It is used to remove water.

19. DRYING:-

• After washing the yarn contains 200 % moisture.

• In drying process the moisture% is brought down to 0% by maintaing 900c for 68-72 hrs.

20. CAKE CONDITIONING ROOM (C.C.ROOM):-

• In C.C.Room cakes are kept in 65% humid atmosphere to retain moisture and become soft
and conditioned.

21. CONNING:-

• Conning is done to form a uniform bundle of yarn.

• 3 cakes may give 1 cone.

22. INSPECTION:-
• The yarn is thoroughly inspected to check its quality before final packaging.
• Quality and cost of yarn is affected by hairy or broken filament, shade variation, oil stain,
cross ends etc.

23. PACKAGING:-
• This is the final task.
• One carton box contains 50 kg yarn cones.

16
 EFFLUENT TREATMENT

The viscose fiber industry requires huge amount of water of which only a small fraction is
incorporated in the product the remainder fined the ways into the water ways as effluent water.
Principally two types of wastes originate in the viscose Rayon plant-acidic and alkaline.
The acid water also discharged from the industry contains chiefly sulfuric acid, sodium, and
sulphate and zinc sulphate. The alkali wastes contain sodium hydroxide soluble hemi cellulose of
row pulp, residual viscose, sodium polysulphides and sodium thiosulphate.
Effluent flow of 27000m3/day is being neutralized by addition of lime solution on the way of
equalization tank. Hydraulic system has been provided into the tank for equalizing effluent quality
and to keep the solids in suspension.

EXISTING EFFLUENT TREATMENT SYSTEM

There is automatic addition of lime near CS2 plant as the effluent coming is highly acidic.
There is pH meter present to detect the pH of the effluent. There is another automatic lime addition
sensor near ETP inlet were the automatic lime addition is done in order to increase the pH. This
effluent further goes to neutralizer equalization tank

1. NEUTRALISER EQUALISATION TANK (NET) FOR NORMAL EFFLUENT.

Total effluent from acid plant, boiler house rayon plant and tyre cord plant gets collected in
neutralization tank. This effluent contains soda, ash, charcoal, and ash-dust. The normal effluent flow
in equalization tank 22000m3/day.
In order to prevent settlement of (soda, ash, charcoal, ash-dust) the circulatory motion of
water is maintained by used of hydraulic pump. 3 hydraulic pumps are present out of which 2 are 24
hr in working position and 1 pump is in spare. The effluent water from neutralizer equalization tank
(NET) is pumped to flash mixer were coagulant is added for removal of small particles and colloids
and also for reducing BOD and COD to some extent. From flash mixer the effluent water is pumped
to clariflocculator with the help of NEP pump. (Neutralizer equalization pump).
Incoming effluent in (NET) is almost neutralized by inlet auto control value by addition of
lime. In certain times the concentration of effluent is highly acidic which is not neutralized by outlet
inlet control valves. In such condition two additional auto control valves with lime are given in NET
namely New equalization tank stage - 1 and New equalization tank stage - 2 due to use of these
two auto control valves lime almost all effluent is neutralized. There is no treatment present in the
plant to treat alkali effluent.

2. CLARIFLOCULATION FOR NORMAL EFFLUENT

The treated effluent from NET is pumped with help of NEP pump in clarifloculator. In
clarifloculator two chambers are provided. In inner chamber there is sludge present along with
effluent water. The sludge settles down and is transferred to Thickener. The effluent water which is
now sludge free is carried out to outer chamber from the opening present at the bottom of the inner
tank, then it goes to Aeration tank.

3. ZINC REDUCTION PLANT

Zinc rich waste from rayon plant is separated from the rest of the industrial effluent. Then lime
slurry is added to adjust pH of the zinc waste in pH adjustment tank. Lime addition is controlled
by pH controller which is automatic. The overflow from pH adjustments tank is sent to flash
mixing unit where floculant is added to coagulate zinc or zinc hydroxide. From flash mixture the
effluent passes to clarifloculator where large blocks of zinc hydroxide is formed and settled in the
outer zone of the clarifloculator. From clarifloculator which is rich in zinc hydroxide is pumped

17
 to thickener. From thickener sludge is subjected to centrifuge where water and moist sludge are
separated. Sludge goes to Thickener tank and effluent water is transferred to Aerator.

4. REMOVAL OF SLUDGE PRESENT IN CLARIFLOCULATOR

The sludge (solid) acquired from clarifloculators of normal effluent treatment plant and zinc recovery
plant are transferred to gravity thickener where concentration of sludge with supernant takes place.
It’s later pumped to centrifuge for dewatering of solid. The sludge cake having 30% - 40% solid
separated. the liquid or effluent water separated from the sludge is transferred to Aeration tank.

5. AERATION TANK

Four aerators are provided in the aeration tank. They are immersed in water two of the
aerators are in working condition for 24 hr and 2 are in real condition. The aerators are used to
increase the DO (Dissolved O2) before the final discharge.

SUMMARY

The effluent water from equalization tank is pumped by neutralized effluent pump to flash
mixer.
Pumping of effluent water in flash mixer is followed by addition of poly-electrolytes and then
to clariflocculator where flocculation and sending process occur. The clarified water is over flowed to
aeration tank for increasing the dissolved oxygen before final disposal of effluent.
Part of Rayon after treatment and tyrecord spin bath rich in zinc is taken separately in
clariflocculator tank where pH is maintained at pH 9 supernatant liquid is taken back to inlet of
equalization tank.
The settled sludge of both clarifiers are taken into thickener for concentrating the sludge and
then pumped to centrifuge for separation of solid and liquid. Solid sludge is collected in trolley, and
is disposed in an 1100m3 pit made for hazardous water disposal in front of century chemicals. The
liquid or effluent water is Aerated and treated well before the final disposal.

18
 EFFLUENT TREATMENT PLANT
27000 m3 PER DAY

Neutralizer Equalization Tank Neutralizer Equalization Tank

for Zinc Recovery for Normal Effluent

Zink Rich Effluent Normal Effluent

5000m3/Day 22000m3/Day
+ +
Lime Slurry Lime Slurry

FLASH MIXER
FLASH MIXER

CLARIFOCLULATOR

FOR ZINC FOR NORMAL

RECOVERY EFFLUENT

EFFLUENT WATER COAGULATE ZINK SLUDGE EFFLUENT WATER

FORM ZINK OR FROM RAYON
RECOVERY TANK ZINK HYDROXIDE PLANT

GRAVITY THICKENER

SLUDGE EFFLUENT
DISPOSSED CENTRIFUGE WATER
OFF IN PIT

AERATOR

FINAL EFFLUENT OUT

19
 USE OF EFFLUENT WATER

This treated effluent water is used in various purposes.

1. Lime solution preparation for ETP.
2. Sulphuric acid coolers.
3. Gardening is entire factory area.
4. Treated effluent water is used for ash quenching in boiler house.
5. Plan is under study to use treated effluent for floor watering.
6. Gardening in ETP and inCS2 plant.
7. Dimensions of each unit
EQUALISATION DIMENSION [m] CAPACIYY [m3]

Tank for normal effluent 43.75 x 11.12 x 2.43 1200

Clarifier for normal effluent 32 x 3.2 swd 2800

Equalisation Thickener 32 x 3 swd 400

Aerator 30.1 x 7.5 x 2.5 600

Equalisation tank for zinc recovery 12.8 x 12.8 x 2.25 370

Clarifier for zinc recovery 18 x 2.8 swd 730

20
 TOTAL QUALITY MANAGEMENT (TQM)

Among its guiding principles, the company has adopted Total Quality
Management (TQM) concepts as core policy to bring about cultural
changes in the organization, where customer’s delight is Prime Motto.
To achieve appreciation of our products from domestic and international
customers, we shall able to provide products and services of desired quality
at competitive cost.
In this chemical laboratory following things are analyzed:
Pollution analysis
Water analysis
Standardization and preparation of chemicals

21
 POLLUTION ANALSIS

METHOD OF ANALYSIS:

Wastewater characterization studies are conducted to determine the best means of reducing pollutants
concentration.
The analysis used to characterize water ranges from precise quantitative chemical determination. The
result of analysis is are most commonly expressed in physical units such as mg/l it is important to
note that for dilute
System such as industrial waste water. The unit of mg/l are interchangeable with parts per million
(ppm) which is mass to mass ratio.
The following characteristic of the wastewater determined in rayon plant:

1. PHYSICAL PARAMETER:

A) TEMPERATURE:-

The temperature of water or effluent is basically important for its effect on the chemical and
biological reaction of organisms in water. An increase in temperature it speeds up the rate of
chemical reaction in water reduce the solubility of gases and amplifier the taste and odors.
At higher temperature the metabolic activity of organisms increases. They require more oxygen
while at same time the solubility of oxygen is reduced.
In the present study the temperature of effluent before treatment is found to be 390C and effluent after
treatment is found to be 380C.

The standard prescribed by MPCB is 400C for inland surface water disposal purpose, the temperature
of waste water from century rayon under permissible limit of MPCB.

B) pH:-
The ion concentration is an important quality parameter as the suitable range for existing of most
biological life is quite narrow and critical. If the is not altered before discharge it may effect the
concentration. H in the surface water body loading to change in the aquatic system it can be
conveniently measured using pH meter. We have a digital pH meter for accuracy.
Conclusion:-
The pH is defined as the logarithm of hydrogen ion with negative sign the pH is a measure of
relative acidity or alkalinity of water. It does not measure the total acidity; alkalinity depends upon
express H+ or OH- ions over the other and measures in normality or gram equivalent of acid or alkali.
pH is generally measured on log scale and equal to negative log10 of hydrogen ion concentration.
pH = -log10 (H+)
pH of waste water ranges from 6.37 to 7.33 is combined effluent of century rayon plant.
The MPCB limit for pH is 5.5 to 9.0 for disposal into river. The waste water from century plant is
under permissible limit of MPCB.

C) TOTAL SUSPENDED SOLID (TSS):-

These are classified as suspended or filterable solids and can be measured by passing a known
volume of liquid through a suitable filter.
Experimental procedure:-
100ml of sample is filtered through a weighed G4 sintered glass crucible which is previously
weighed using a vacuum pump for suction.
The residue is washed with distilled water and the crucible heated in an oven at 150 0C for 2-
3hrs.
The crucible is cooled in desiccators and weighed.

22
Formula:-
Suppose the difference is ‘X’
100 = X
106 =?
TSS =106 x ‘X’
100
=104 x ‘X’ ppm

Conclusion:-
The total suspended solid is non-filterable residue; they may contain organic or inorganic substances.
Suspended solids are contained in effluents which are not in solution suspended solids are contained
in effluence which are insoluble. Suspended solids comprise settle able floating are not settle able
component.
The total suspended solid contained in century rayon effluent is 27.75 to 70.5 mg/l.
The tolerance limit of industrial effluent discharge into stream allowed by state pollution control
board for TSS is 100mg/l. The TSS in the effluent of century rayon plant is below permissible limit.

D) TOTAL DISSOLVE SOLID (TDS):-

These are solid which is present in dissolved form and can be measured by
keeping a known volume of liquid in evaporating dish.
It contain both suspended and dissolved solid i.e. (TDS + TSS)
Experimental procedure:-
• Take 100ml of sample in aluminum dish which is previously weighed.
• Evaporate on the hot plate.
• Weighed again after cooling.
Formula:-
Suppose the difference is ‘X’
100 = ‘X’
106 =?
TDS = 106 x ‘X’
100
=104 x ‘X’ ppm

[NOTE: - TDS = (TDS + TSS) – TSS

And TDS + TSS = TS (TOTAL SOLID)]

23
 2. CHEMICAL PARAMETER

A) CHLORIDE TEST (NaCl):

Procedure:
• Take 100ml of sample in a beaker.
• Add 1 spoon of CaCO3.
• Add 2ml of 2N HNO3.
• Add 2ml of 5% of K2Cr2O4 (which itself act as a indicator).
• Titrate it against 0.1 N AgNO3 solutions.
• End point will be yellow to brick red.
Formula:-
Suppose the value is ‘Y’
Then,
1000ml of 1N AgNO 3 [solution in burette] = 58.5gms (equivalent wt. of NaCl) [solution in
flask].
1ml of 1N AgNO3 = 58.5
1000
1ml of 0.1 N AgNO3 = 58.5 x 0.1 x ‘Y’ x 106
1000 x volume of sample
= 58.5 x ‘Y’ ppm.

B) SULPHATE:-
Procedure:
• Take 300ml of sample in beaker.
• Add 2 drops of conc. HCL [To settle the dust particle].
• Keep it in a hot plate till its volume reduces to half.
• Add 20ml of 10% BaCl2 when it is warm [white ppt out of BaSO4 forms.
• Filter it through a G4 crucible which is previously weighed.
• Dry it inside oven for 6 hours.
• Again wt. and take the difference.

Formula:-
Suppose the value is 1.4269
Then, 1.4269 = BaSO4
In 300ml the reading is 1.4269
Then, in 100?
So, 100 x 1.4269 = 0.2853 (the amount BaSo4 present in sample)
500
Now, molecular wt. of BaSO4 = 137 + 32 + 64 = 233.
For SO4 = 32 + 64 = 96
i.e. 233  96
0.2853?
So, 0.2853 x 96 = 0.1175 %( amount of SO4 present in BaSO4)
233
In 100 0.1175
Then, in 106 =?
So, 0.1175 x 106 = 1175 ppm. (Amount of SO4 present in per million).
100

24
C) LIME:-

Procedure:
• Take some amount of lime in a crucible and keep in oven for 6 hours to remove
moisture.
• Weighed approximately 1gm of lime in a beaker.
• Add 25ml of conc.HCl in it and keep for 11/2 hour to liberate CO2.
• Make the dilution in 500ml of standard conical flask.
• Pipette out 25ml in a conical flask.
• Add 2ml of buffer pH in it.
• Titrate it against EDTA.
• End point will be purple to blue.
Formula:-
Suppose the value is ‘Y’
Now,
1) Percentage of CaO:
Wt. of lime = 1gm
1000ml of 1N EDTA = 56gm of CaO
1ml of 0.00619N EDTA = 56 x 0.00619 x ‘Y’ x 100 x 20
1000 x 1
= Z%
2) Percentage of Ca(OH)2:-
1000ml of 1N EDTA = 74 gm of Ca(OH)2
1ml of 0.00619N EDTA = 74 x 0.00619 x ‘Y’ x 20 x 100
1000 x 1

D) OIL:

Procedure:-
• Take 100ml of sample in a separating funnel. Add 10ml of 4N H2SO4.
• Add 50ml of Diethyl ether. Mix it well.
• Remove water from the lower side of separating funnel and then Diethyl ether is taken in a
round bottom flask which is previously weighed.
• Distilled out all the Diethyl ether from round bottom flask.
• Keep the flask in the oven for 2 hours.
• Weigh it again. Difference will give you amount of oil.
Formula:-
OIL = Difference x 106
100

25
E) CHEMICAL OXYGEN DEMAND (COD):-

Principle (open reflux method):-

Most types of organic matter are oxidized by a boiling mixture of chromic and sulfuric acids. A
sample is refluxed in strongly acid solution with known excess of potassium dichromate (K2Cr2O7).
After digestion, the remaining unreduced K2Cr2O7 is titrated with ferrous ammonium sulfate to
determine the amount of K2Cr2O7 consumed and the oxidizable matter is calculated in terms of
oxygen equivalent.

The COD test is used to measure the total organic matter content of waste water the oxygen
equivalent to organic mater that can be oxidized is measured by using a strong chemical oxidizing
agent in acidic medium potassium dichromate has been found to be best for the general chemical
reaction can be represented by the following unbalanced reaction:

Organic matter (CHO) + K2Cr2O7 + H+  Cr3+ + CO2 + H2O.

In the process of oxidizing the organic substances found in the water sample, potassium dichromate
is reduced (since in all redox reaction, one reagent is oxidized and the other is reduced), forming
Cr3+. The amount of Cr3+ is determined after oxidization is complete, and is used as an indirect
measure of the organic contents of the water sample.
The determination of chemical oxygen demand (COD) widely used in municipal and industrial
laboratories. In practice, it is usually expressed in milligram O2 per litre. Oxygen demand is
determined by measuring the amount of oxidant consumed using titrimetric methods. The test is not
adversely affected by toxic substances, and test data is available in 1-1/2 to 3 hours, providing faster
quality assessment and process control. A COD test is measures all organic carbon with the exception
of certain aromatics (benzene, toluene, phenol, etc.) which are not completely oxidized in the
reaction. COD is a chemically chellated/thermal oxidation reaction, and therefore, other reduced
substances such as sulphide, sulfites, and ferrous iron will also be oxidized and reported as COD.
The COD of waste is generally higher than the BOD as more compounds can be chemically oxidized
then biological. COD and BOD can be correlated for many types of waste COD measurement can be
used for treatment plant control and operation.

Importance of COD:-
• Many organic substances which are difficult to oxidize biologically can be oxidized
chemically.
• COD test is faster than BOD. COD is usually measured and the test is simple and easy to
perform with right equipment and can be done in 2 hours. BOD usually takes 5 days.
• Since BOD cannot be determined accurately when toxins are present and conditions are
unfavorable for growth of microbes, COD is used.
• This test is used extensively in the analysis of industrial waste.
• It is particularly valuable in surveys designated to determine and control losses of sewer
system.

Experimental procedure:-
• Take 25ml of 0.25 N K2Cr2O7 solutions in conical flask and glass bids are added to avoid
bumping action.
• Pinch of HgSO4 and 5cc conc. H2SO4.
• Add 20ml of sample.
• Add slowly 35cc of conc. H2SO4 thoroughly.
• For the blank test the same procedure is used except that distilled water is used instead of
sample.

26
 • Connect the flask to condenser. Mix the content thoroughly before heating. Improper mixing
result in bumping and the sample may be blown out.
• Reflux for a minimum period of 2 hours. Cool and wash down the condenser with distilled
water.
• Titrate against excess potassium dichromate with 0.1 N ferrous ammonium sulphate
Fe(NH4)SO4 (FAS) using ferrion indicator.
• Sharp colour change from blue green to wine red indicates the end point.
Formula:-
COD mg/l = (blank reading-sample) x 8000 x 0.1
Volume of sample

Where 8000 = milliequivalent weight of oxygen x 1000 ml/l

Conclusion:-
The COD test is very important parameter in management and design of the treatment plant. COD
values are than BOD values for sample of most of the industrial wastes. COD contained in the
century rayon effluent ranges from 60.8 to 135.4 mg/l
The tolerance limit for COD given by MPCB is 250mg/l. Thus the COD in the effluent of century
rayon plant is below permissible limit.

F) BIOLOGICAL OXYGEN DEMAND (BOD):-

Biochemical oxygen demand (BOD) is the amount of oxygen, expressed in mg/l or parts per million
(ppm), that bacteria take from water when they oxidized organic matter or Biochemical oxygen
demand, measures the amount of oxygen consumed by microorganisms in decomposing organic
matter. A test is used to measure the amount of oxygen consumed by these organisms during a
specified period of time. (Usually 5 days at 20oC ). The rate of oxygen consumption in a stream is
affected by number of variables:
temperature, pH, the presence of certain kind of microorganisms, and the type of organic and
inorganic material in water. The carbohydrates (cellulose, starch, sugars), proteins, petroleum
hydrocarbons and other materials that comprise organic matter get into water from natural sources
and from pollution. They may be dissolved, like sugar, or suspended as particulate matter, like solids
in sewage. Because organic matter always contains carbon and hydrogen, oxidation produces carbon
dioxide and water. Bacteria in water live and multiply when organic matter is available for food and
oxygen is available for oxidation. About 1/3rd of the food bacteria consumed becomes the solid
organic cell material of the organisms. The other 2/3rd is oxidized to carbon dioxide and water by the
biochemical action of the bacteria on the oxygen dissolved in the water.

Importance of BOD:-
• Measurement of BOD has long been the basic means for determining the degree of water
pollution.
• BOD test is used to determine size of waste treatment facilities.
• The BOD test is used to measure waste load to treatment plant, determine plant efficiency (in
terms of BOD removal), and control plant processes.
• BOD directly affects the amount of dissolved oxygen in river and streams. The greater the
BOD, the more rapidly oxygen is depleted in the stream.
Major disadvantage:-
The BOD test is the amount of time (5 days) required to obtain the results.

Experimental procedure:-
For estimating BOD of sample 2 special stoppered bottles (approximately 300ml each) are required.
For each sample and an addition pair of the blank test carried out with distilled water.

27
 • Each bottle is filled exactly to 1/10th of its volume of dilution water.
Dilution water is prepared by making a 2% by volume solution of filtered domestic sewage with
distilled water and adjusting its pH to 7.
• Prepare seeding water separately. Seeding water is distilled water in which nutrient CaCL 2,
MgSO4, FeCl3 and phosphate buffer is added. 2ml of each nutrient is added for 1liter of
distilled water.
• Seeding is done in dilution water ml 6.6ml of sample is added to one liter of distilled water.
• Clean the bottles.
• Keep two bottles for blank and three sample dilution bottles in incubator for 3 days, at 20OC.
• After 3 days, at 200C, add 2ml of MnSO4 and 2ml of alkali iodide azide to each bottle, put
stopper and shake the bottle well. Allow the ppt to settle. White ppt indicates absence of
dissolved oxygen.
{When MnSO4 and alkali iodide azide (NaOH + KI + NaN3) is added to sample in which no
dissolved oxygen (DO) is present, white ppt of Mn(OH)2 is formed. If dissolved oxygen is
present, it oxidizes some of Mn2+ ions to Mn4+, forming MnO2 as follows:

Mn2+ + 2OH-  Mn(OH) (under zero condition)

Mn2+ + 2OH- + 1/2O2  MnO2 + H2O (in the presence of DO sample)}

• Add 2ml of conc. H2SO4 and mix well so that ppt will dissolve completely and yellow colour
is obtained in each bottle.
• Transfer 200ml of sample from each bottle to titrate it against 0.1N sodium thiosulphate
solution using starch indicator.
• Titration is continued till colour changes from blue to colourless.
• Find BOD for each sample.

Formula:-

BOD = [Reading of blank – Reading of sample] x 100

Dilution factor

Conclusion:-
The BOD test is widely used to determine the pollution length of sewage and industrial waste in
terms of oxygen that would be required if these waste are discharged into natural water in which
aerobic condition exist.
BOD contained in century rayon effluent ranges from 19.1 to 40.8mg/l
The tolerance limit for BOD is given by MPCB is 100mg/l. Thus the BOD in the effluent of century
rayon plant is below permissible limit.
MPCB limit for discharge of industrial effluent:-

Sr. No. Parameter Concentration

1. Temperature 40
2. pH 5.5 to 9
3. COD 250
4. BOD 100
5. TSS 100
6. OIL & GREASE 10
7. ZINC 5

All values in mg/l except pH.

28
 SUMMARY AND CONCLUSION

Now-a-days pollution is a serious problem on national and international level. As the

industrialization grows the pollution also grows due to that life particularly is threatened so from
these point present study is attempted. It’s broad summary and conclusion is as follows:-
The analysis of treated effluent shows temperature: 370C, pH:6, 45.5, COD:135, BOD: 39.84, Oil
and Grease:6.2, Zinc:4.5mg/l. These values are below limit, prescribed by Maharashtra pollution
control board (MPCB). This clearly indicates that the ETP was working efficiently and the water
would be used for gardening or any other purpose.
As the study period was restricted to 2 weeks. It is difficult to draw a right conclusion on the basis of
the study carried out for a short period of time.
From the present study it appears that environment development conflict can be minimized if not
avoided, though the century rayon is giving adequate treatment. Sometimes lacked of trained
personal or some drawbacks in the existing ETP system creates serious problems thus industry
should take all possible measurements to control pollution.

29
 WATER ANALYSIS

Century Rayon is one of the largest companies in Asia producing Rayon fiber. It is
independent & produces its raw materials & required chemical by itself. It does’ not import
any of its raw materials & have a successfully established & set up plants for required
chemical demand. Going one step ahead it even have set up effluent or waste water treatment
plants by itself. The effluent water is well treated and thoroughly examined before letting out
in environment. Thus environmental care is taken & aquatic life is conserved.
In Century Rayon water from Boilers, Rivers, filter, waste water etc. is analyzed. A
through checking of pH, Alkalinity, Acidity, turbidity, presence of O2 & silica is attempted in
laboratory; even COD & BOD is checked. Hence we found out that Century Rayon have
established laboratory which take care of checking water samples from respective areas.
In the following report represents the water analysis experiments carried out to check
the various parameter before letting out in the aquatic environment.
Waste water characterization studies are conducted to determine the best means of
reducing pollutants concentration. The analysis used to characterize water ranges from
precise quantitative chemical determination. The result of analysis are most commonly
expressed a physical units such as mg/l. it is important to note that for dilute system such as
industrial waste water. The unit of mg/l or g/m3 are interchangeable with parts per million
(ppm) which is mass to mass ratio.

1. pH
2. Turbidity
3. Alkalinity
4. Acidity
5. Sulphite
6. Phosphates
7. Total hardness of water
8. Silica
9. Dissolved O2
10. Dialyser & waste caustic
11. Chloride
12. Total dissolved solid (TDS)

1. pH

• The pH is defined as the negative logarithm of hydrogen ion concentration.

• The pH is a measure of relative acidity or alkalinity of water.
• pH of waste water range from 6.37 to 7.33 in combined effluent of century Rayon plant.
• The MPCB limit for pH is 5.5 to 9.0 for disposal into river.
• The hydrogen concentration is an important quality parameter, as the suitable range for
existence of most biological life is quite narrow & critical.
• If the pH is not altered before the discharge, it many effect the concentration of the water.
• This parameter is measured with the help of a digital pH meter.
• pH can be determined also by taking 50 cc sample & adding universal indicator to it. The
color change can be compared by standard pH paper.
• In Century Rayon, pH of boiler sample River, Filter, Condensate & Deager samples, 45 ton,
Anion, Cation etc are determined.

30
2. TURBIDITY

• Turbidity is a measure of the amount of light scattered and absorbed by water because of the
suspended matter in the water.
• In simple words, turbidity is the lack of clarity or brilliance in water which may be due to
clouding of substance like clay, rock flour, silt, silica, manganese, sulfur or other organic &
industrial wastes.
• In Century Rayon water from River & filter water sample are checked for their turbidity
through Nephlo- Turbidity meter whose unit is NTU (Nephlo Turbidity unit).
• Therefore the potability of water sample can be easily verified & determined whether it is
safe for consumption.

3. ALKALINITY

• Alkalinity refers to the capability of water to neutralize acid.

• Water with a value greater than 7 indicates alkalinity & tends to affect the taste of the water.
• Since hard water contains metal carbonates (mostly CaCO3) it is high in alkalinity.
• In Century Rayon alkalinity of feed water, Boiler, Anion, Condensate is determined.
• The required chemicals are-
• Phenolphthalein indicator
• Methyl orange indicator
• 1N H2SO4 solution

PROCEDURE

• 100cc sample of the given water sample is taken in a conical flask & few drops of
Phenolphthalein indicator is added to it & titrated against 1N H2SO4 unit end point
reaches to pink to colorless.
E.g. Suppose the reading is 1.0 then 1.0 x 100 = 100 (where 100= standard factor)
• To this same colorless solution, few drops of methyl orange indicator is added & continued
titrating against 1N H2SO4 till the end point reaches to yellow to orange.
E.g. suppose the reading is 2.1 then 2.1 x 100 = 210 (where 100 = standard factor)
• By performing the above experiment
Alkalinity can be easily determined.

4. ACIDITY

• Water with a pH value less than 7 indicates acidity & tends to be corrosive. Also low mineral
content in water are common causes of corrosiveness.
• For the above reasons Cation & degraser water samples acidity is regularly checked in
Century Rayon.
• The reagents required for the experiment are
• Methyl red indicator.
• 0.01N NaOH.

PROCEDURE

• 100cc 0f given water sample is taken in a conical flask & few of methyl red indicator are
added to it.
• The solution is then titrated against 0.01N NaOH till end point reaches from yellow to
brick red.

31
• E.g. suppose the reading is 6 then 6x4.9 = 29.4 where 4.9 is a factor.

32
 5. SULPHITE IN BOILER WATER

• Sulfate is a substance that occurs naturally in drinking water but large amount of sulfate
could be hazardous.
• This experiment is attempted in order to find the amount of sulfate in the given water sample
to keep the sulfate level in check.
• The reagents required for the experiment are :
• 1:1 HCL
• Starch indicator
• Standard potassium iodate- iodide sol.
• (0.71gm of KIO3+7gm of KI + 0.5gm NaHCo3 per liter of the solution).

PROCEDURE

• 100cc of given water sample is taken in conical flask & 2cc of 1:1 HCL is added using 1cc
of starch indicator.
• This solution is titrated is against standard KIO3 till a trace of blue color is obtained
throughout the solution. The end point being colorless to blue.
• E.g. Suppose the reading is 3.8 then 3.8x12.5=475
Formula:-
Sulfide as Na2SO3 ppm = Reading of KIO3 x12 (1cc of KIO3 solution = 0.00125gm of Na2So3)

6. PHOSPHATE IN BOILER WATER

• Phosphorous allows plants & animal to grow & function. It is a component of ATP which is
the very basic source of energy for all cellular work.
• Most of the time phosphates added to the soil during forming or other related activities
leaches out to rivers and ocean excess leaching may cause diversions phosphorous cycle &
aquatic environment. Hence it is very important to keep the phosphate level in check through
regular analyzing the water sample.
• In Century Rayon boiler water sample are checked for there phosphate levels before
discharging it in near rivers.
• The reagents required to carry out the test are –
• molybdic acid
• Hydroquinone solution.
• (Na2Co3+Na2So3) solution.

PROCEDURE

• 5ml of given water sample is taken in conical flask & 2cc of molybdic acid, 2cc
hydroquinone solution and 2cc of (Na2CO3+Na2SO3) solution is added.
• During & after each addition the sample is swirled & mixed thoroughly.
• The blue color developed in the solution is compared with the help of lens bond comparator
• The blue color is molybdenum blue & is said to have a composition. (MoO2.4MoO3)2. H3PO4.
Formula: - PO4 ppm = vol. of std. phosphate solution X 20
• E.g suppose the reading is 20 then 20 X 20=400.

33
 7. TOTAL HARDNESS OF WATER
• In Century Rayon Rivers, filter, water sample are checked for their hardness.
• The hardness of this sample is due to presence of CaCO3 & MgCO3.

PROCEDURE

• Taking 100 cc samples in conical flask, 10cc buffer solution is added along with few drops
of mixed indicator.
• The above solution is then titrated against standard EDTA solution.
• The end point being wine red to green.
Formula: - total hardness = reading of std. EDTA x 6.195 solution.
• E.g. suppose the reading is 2 then 2 x 6.195 = 12.39.

8. SILICA

• The following experiment is carried out to trace the presence of silica or amount of sand
particles present in feed, boiler, 4ST, Anion, Cation & condensate water sample in Century
Rayon.
TRACER SILICA

• Chemicals required to carryout the experiment are

1. 1:1 HCL.
2. 5%Ammonium molybdate.
3. 10% oxalic acid.
4. Sulphonic acid.

PROCEDURE

• 50cc sample is taken in conical flask & 1ml of 1:1 HCL is added along with 2ml of
5%Ammonium molybdate, 2cc of 10% oxalic acid & 2ml of Sulphonic acid. It is then
compared with the standards.
1cc in 50ml silica free water = 0.1 ppm.
FOR HIGH PPM SILICA
• Reagent required are
1. 1:1 HCL.
2. 5%Ammonium molybdate.
3. Oxalic acid.

PROCEDURE

• 50cc sample is taken in conical flask & 1ml of 1:1 HCL is added along with 2ml of
5%Ammonium molybdate, 2ml of 10% oxalic acid & 2ml of Sulphonic acid. It is then
compared with the standards.
1cc in 50cc silica free water = 2 ppm.

9 .DISSOLVED OXYGEN

• Oxygen is the main element required for life. Water contains oxygen is dissolved form which
is used by aquatic life for their respiratory processes.
• Variations in oxygen level in aquatic environment can disrupt the aquatic life hence it is very
essential to maintain the optimum oxygen level.

34
• The following experiment is attempted to check the amount of dissolved oxygen in the given
water sample.
• Precautions are taken during sampling such that the bottle does not contain water bubble as
air contain oxygen and it could get mixed and dissolved with the water sample and there may
be error while finding the result.
• The following are the reagents required to carry out the experiment-

1. The manganese sulphate solution (48gms/100ml of D.W).

2. Iodide solution (360gms NaOH and 100gms KI dissolved in 1litre of D.W).
3. Hydrochloric acid 1:1 or H2SO4 (specific gravity 1:4).
4. 0.01N sodium thiosulphate solution.
5. Starch indicator.

PROCEDURE

• In the water sample contend in the bubble free bottle by means of a pipette 2ml of
manganese sulphate solution and iodide solution is added. The bottle is restoped and
shaken thoroughly.
• After the precipitate has settled 2ml of conc. H2SO4 is added and shaked till the precipitate
dissolves completely.
• 100cc of this solution is taken in conical flask and titrated against sodium thiosulphate
solution using starch indicator.

Formula and Reaction

O2 ml/liter= reading of thiosulphate x 0.56
MnSo4+2NaoH → Mn (OH)2+Na2So4.
2Mn (OH)2+O2 → 2MnO(OH)2
MnO (OH)2+2KI+2H2SO4= MnSO4+K2SO4+I2+3H2O+I2+Na2S2O3=Na2S4O6+2NaI.
Calculation based on-
1ml of 1N sodium thiosulphate 0.008gm of O2
(32gms of O2 will occupy 22.4litres)

10. WASTE CAUSTIC SAMPLE (NaOH)

• The waste caustic contains maximum proportion of NaOH.

• The following experiment is attempted in order to check the caustic level.
• The required reagents are-
1. 1.0N H2So4
2. Methyl red indicator.

PROCEDURE

• 5ml of sample is pipetted out in conical flask and few drops of methyl red indicator is
added to it this solution is then titrated against 1.0NH2So4.
• The end point being yellow to light red.
Formula: - NaOH (gpl) =R x 8.
(1ml of 1N H2SO2=0.04gm of NaOH).

11. CHLORIDE

• Through following experiments chlorides in water sample as NaCl is analyzed.

• The chemicals required are as follows.
35
1. Nitric acid (2N)
2. Phenolphthalein indicator.
3. Potassium chromate indicator (5%)
4. 0.1N silver nitrate solution
5. Solid calcium carbonate

PROCEDURE
• 50cc sample is taken in conical flask and neutralized with 2N HNO3 to the same solution
pinch of CaCO3 is added using Potassium chromate indicator.
• This solution is then titrated against 0.1Nsilver nitrate till end point yellow to reddish
brown is attended.
Formula:-
Chloride as NaCl (ppm) =B.R.of 0.1N AgNo3 x 2 x 58.5
(1ml of 1N AgNo3=0.0585gm of NaCl)

12. TOTAL DISSOLVED SOLID (TDS)

• TDS is an expression for the combined content of all inorganic and organic substances
combined in a liquid which are present in a molecular, ionized or micro-granular suspended
form.
• In century rayon TDS of water sample from boilers is obtained to check the amount of
suspended solid particles present in the sample.

PROCEDURE

• 50cc sample is taken in weighed steel dish and kept on water bath till all the water
evaporates.
• The weighed steel dish is then cooled, desiccated and weighed again to obtain the weigh of
the residue.
• Formula:-
TDS (ppm = weigh of the residue x 20,000)
E.g. Suppose 29.893 is the weight of steel plate and 29.899 is the weight of steel plate with
residue then 0.006 is the amount of residue present then 0.006 x 20,000=120 TDS (ppm)

36
 PREPARATION AND STANDARIZATION OF 1N NaOH

REAGENTS:

• 1N H2SO4 SOLUTION
• NaOH PELLATE
• METHYLERED INDICATOR

PROCEDURE:

Equivalent wt of NaOH = 40gm

Therefore, 40gm in 1 Liter = 1N NaOH
I.e. 40g of NaOH pellet weighted and added in 1Liter of distilled water will give us 1N NaOH and
shake well.

To check and standardized the prepared solution of 1N NaOH for normality we titrated it against 1N
H2SO4 using methylered indicator.
This is an acid base titration and End points is yellow to bricked.

Calculation:
N1V1 = N2V2

Where, N1 = 1N H2SO4 ……known

V1 = Burette reading…...known
N2 = Normality of NaOH to be found.
V2 = 25.0ml of NaOH

• If burette reading = 25ml

Therefore, N1V1 = N2V2
N2 = 1.0 x 25/25
= 1.0N
If N2 = 1N we get correct 1.0N NaOH
Case I:
If burette reading = 25.5ml
Then, N1V1 = N2V2
N2 = 1.0 X 25.5/25
= 1.02N
Here, 1.02 > 1.0N
The prepared solution is concentrated.
To dilute it we take N1 = 1.02 and V1 = 1000ml
V2 is the total volume of distilled water which is substrated from V1 (the actual 1000ml) and the
difference is the amount to be added and N2 = 1N NaOH
N1V1 = N2V2
V2 = 1.02 x 1000/1.0
= 1020 ml
Therefore, V2 - V1 = 1020 – 1000
= 20ml
Therefore, if we add 20ml in the prepared concentrated solution we will get perfect 1N NaOH
solution and even the burette reading when titrated against 1N H2SO4 will be 25.
Take one more reading for conformation.

37
Case II:
If the burette reading = 24.8ml
Then, N1V1 = N2V2
N2 = 1.0 x 24.8/25
= 0.992N
Here, 0.992 < 1.0
The prepared solution is diluted so, we use the formula
GPL = Equivalent wt x normality
= 40 x 0.992
= 39.68GPL
• 39.68gpl is to be substrated from 40 (the standard GPL for 1N NaOH)
40 – 39.68 = 0.32 gm

• 0.32 gm is the amount of NaOH pellate to be added in the prepared diluted solution to get
perfect 1N solution. Titrated against 1N H2SO4 and the burette will be 25ml
N1V1 = N2V2
N2 = 1.0 x 25.0/25.0
N2 = 1N
For conformation take one more reading.
Therefore we will get perfect 1N standardized NaOH solution.

38
 PREPARATION & STANDARIZATION OF 1N H2SO4

Reagents:
• 1N NaOH
• Cone H2SO4
• Methyl red indicator

Procedure:

Equivalent wt of H2SO4 = 49g

Therefore 49g in 1000ml = 1N H2SO4
I.e. 49g of H2SO4 weighted and added in 1000ml of distilled water in a standard flask, shake well and
this will give us 1N H2SO4.
If we take it by volume then 27.7ml of H2SO4 in 1000ml of distilled water we will get 1N H2SO4

To check and standardize the prepared solution of 1N H2SO4 for normality we titrate it against
1N NaOH using methyl red indicator.
This is an acid base titration and the end point is pink to Brick red.

Calculation:
N1V1 = N2V2
Where, N1 = NaOH…Known
V1 = Burette reading …known
N2 = Normality of H2SO4 to be found
V2 = 25ml of H2SO4
• If burette reading = 25.2ml
Then, N1V1 = N2V2
N2 =1.0 x 25/25
= 1.0N
If N2 = 1 we get correct 1N H2SO4

Case I:
If burette reading = 25ml
N1V1 = N2V2
N2 = 1.0 x 25.2/25
= 1.008N
Here, 1.008 > 1.0
Therefore, the prepared solution is concentrated.
To dilute it we take N1 = 1.008 and V1 = 1000ml
V2 is the total volume of distilled water which is subtracted from V1 (the actual 1000ml) and the
difference is the amount to be added.
N2 = 1N H2SO4
Therefore, N1V1 = N2V2
V2 = 1.008 x 1000/1.0
= 1008ml

Dilution:
Therefore, V2 – V1 = 1008 – 1000
= 8ml
If we add 8ml in the prepared concentrated solution we will get perfect 1N H2SO4 and even the
burette reading when titrated against 1N NaOH will be 25ml
N1V1 = N2V2
N2 = 1.0 X 25/25.0
= 1.0N
39
Take one more reading for conformation.

Case II:
If the burette reading = 24.8ml
Then, N1V1 = N2V2
N2 = 1 x 24.8/25
= 0.992N
Here, 0.992 < 1
Therefore, the prepared solution is diluted
So, we use the formula
GPL = Equivalent wt x Normality
= 49 x 0.992
= 48.608 g
48.608 gpl is to be subtracted from 49(the standard gpl for 1N H2SO4)
Then, difference in gpl is taken
GPL = 49.0 – 48.608
= 0.392 gm
0.392 gm is the amount of H2SO4 to be added in the prepared diluted solution to get perfect 1N
H2SO4 and even the burette reading when titrated against 1N NaOH will be 25ml.
N1V1 = N2V2
N2 = 1 X 25/25
N2 = 1.0N
For conformation take one more reading.
Note:
As the acid is in liquid form we can take it’s normality by weight as well as by volume also.
If we take it in volume then, we use formula
Volume = Mass/ density
For e.g.
Volume = 0.392/ 1.84
Volume = 0.312 ml
Where, 1.84 is the density of H2SO4

40
 PREPARATION AND STANDARDISATION OF 0.1N H2SO4

Reagents:

• 0.1N NAOH
• CONE H2SO4
• METHYL RED INDICATOR

Procedure:
Equivalent wt of H2SO4 = 49g
I.e. 49g in 1000ml = 1N H2SO4
So, for 0.1N H2SO4 we will take 4.9 gm in 1000ml of distilled water to make 0.1N H2SO4
4.9 gm in 1000ml = 0.1N H2SO4
I.e. 4.9g of H2SO4 weighted and added in 1000ml of distilled water in a standard flask, shake well
and this will give us 0.1N H2SO4.
To check and standardize the prepared solution of 0.1N H2SO4 for normality we titrate it against 0.1N
NaOH using methyl red indicator.
This is an acid base titration and the end point is pink to brick red.

Calculation:
N1V1 = N2V2
Where, N0.1 NaOH…Known
V1 = Burette reading …known
N2 = Normality of H2SO4 to be found
V2 = 25ml of H2SO4
• If burette reading = 25.2ml
Then, N1V1 = N2V2
N2 =0.1 x 25/25
= 0.1N
If N2 = 0.1 we get correct 0.1N H2SO4 solution.

Case I:
If burette reading = 25.5ml
N1V1 = N2V2
N2 = 0.1 x 25.5/25
= 0.102N
Here, 0.102 > 0.1N
Therefore, the prepared solution is concentrated.
To dilute it we take N1 = 0.102 and V1 = 1000ml
V2 is the total volume of distilled water which is subtracted from V1 (the actual 1000ml) and the
difference is the amount to be added.
N2 = 0.1N H2SO4
Therefore, N1V1 = N2V2
V2 = 0.102 x 1000/0.1
= 1020ml
Dilution:
Therefore, V2 – V1 = 1020 – 1000
= 20ml
If we add 20ml in the prepared concentrated solution we will get perfect 0.1N H2SO4 and even the
burette reading when titrated against 0.1N NaOH will be 25ml
N1V1 = N2V2
N2 = 0.1 X 25/25.0
= 0.1N
Take one more reading for conformation.
41
Case II:
If the burette reading = 24.8ml
Then, N1V1 = N2V2
N2 = 0.1 x 24.8/25
= 0.0992N
Here, 0.0992 < 0.1
Therefore, the prepared solution is diluted
So, we use the formula
GPL = Equivalent wt x normality
= 49 x 0.0992
= 3.968 g
3.968 gpl is to be subtracted from 4.9(the standard gpl for 0.1N H2SO4)
Then, difference in gpl is taken
GPL = 4.9 – 3.968
= 0.932 gm
0.932 gm is the amount of H2SO4 to be added in the prepared diluted solution to get perfect 0.1N
H2SO4 and even the burette reading when titrated against 0.1N NaOH will be 25ml.
N1V1 = N2V2
N2 = 0.1 X 25/25
N2 = 0.1N
For conformation take one more reading.

42
 PREPARATION AND STANDARDATISATION OF 0.1 NaOH

REAGENTS:

• 0.1N H2SO4 SOLUTION

• NaOH PELLATE
• METHYLERED INDICATOR

PROCEDURE:

Equivalent wt of NaOH = 40gm

Therefore, 40gm in 1 Liter = 1N NaOH
So for 0.1N NaOH we will take 4.0gm in 1000ml of distilled water to make 0.1N NaOH.
4.0gm in 1000ml = 0.1N NaOH
I.e. 4.0gm of NaOH pellet weighted and added in 1Liter of distilled water will give us 0.1N NaOH
and shake well.
To check and standardized the prepared solution of 0.1N NaOH for normality we titrated it against
0.1N H2SO4 using methylered indicator.
This is an acid base titration and End point is yellow to bricked.

Calculation:
N1V1 = N2V2

Where, N1 = 0.1N H2SO4 ……known

V1 = Burette reading…...known
N2 = Normality of NaOH to be found.
V2 = 25.0ml of NaOH

• If burette reading = 25ml

Therefore N1V1 = N2V2
N2 = 0.1 x 25/25
= 0.1N
If N2 = 0.1N we get correct 0.1N NaOH

Case I:
If burette reading = 25.5ml
Then, N1V1 = N2V2
N2 = 0.1 X 25.5/25
= 0.102N
Here, 0.102 > 0.1N
The prepared solution is concentrated.
To dilute it we take N1 = 0.102 and V1 = 1000ml
V2 is the total volume of distilled water which is substrated from V1 (the actual 1000ml) and the
difference is the amount to be added and N2 = 0.1N NaOH
N1V1 = N2V2
V2 = 0.102 x 1000/0.1
= 1020 ml
Therefore, V2-V1 = 1020 – 1000
= 20ml
Therefore, if we add 20ml in the prepared concentrated solution we will get perfect 0.1N NaOH
solution and even the burette reading when titrated against 0.1N H2SO4 will be 25.
Take one more reading for conformation.

43
Dilution:
V2 – V1 = 1020 – 1000
= 20ml
Therefore, if we add 20ml in the prepared concentrated solution we will get perfect 0.1N NaOH and
even the burette reading when titrated against 0.1N H2SO4, the burette reading will be 25ml.
N1V1 = N2V2
N2 = 0.1 X 25/25
= 0.1N NaOH
Take one more reading for conformation.

Case II:
If the burette reading = 24.8ml
Then, N1V1 =N2V2
N2 = 0.1 x 24.8/25
= 0.0992N
Here, 0.0992 < 0.1
The prepared solution is diluted so, we use the formula
GPL = Equivalent wt x normality
= 40 x 0.0992
= 3.968gpl
• 3.968gpl is to be substrated from 4.0 (the standard gpl for 0.1N NaOH)
GPL = 4.0 – 3.968
= 0.032 gm

• 0.032 gm is the amount of NaOH pellate to be added in the prepared diluted solution to get
perfect 0.1N solution. Titrated against 0.1N H2SO4 and the burette will be 25ml
N1V1 = N2V2
N2 = 0.1 x 25.0/25.0
N2 = 0.1N
For conformation take one more reading.
Therefore we will get perfect 0.1N standardized NaOH solution.

44
 PREPARATION AND STANDARDISATION OF 0.1N SODIUM THIOSULPHATE
(Na2S2O3.5H2O)

Reagents:
• 0.1N Potassium iodate solution (KIO3)
• Solid Potassium iodide (KI)
• 2N acetic acid
• Starch indicator
• Sodium carbonate (Na2CO3) and chloroform (CHCl3) as preservative

Procedure:

Equivalent weight of Na2S2O3.5H2O = 248gm

I.e. 248gm in 1000ml = 1N Na2S2O3
So, for 0.1N Na2S2O3 we will take 24.8gm in 1000ml of soft water to make 0.1N Na2S2O3
24.8gm in 1000ml = 0.1N Na2S2O3
I.e. 24.8gm Na2S2O3 of weighted and added in 1000ml of soft water in a standard flask, shake well.
This will give us 0.1N Na2S2O3. Allow the solution to stand for 5-6 days.
To check and prepare standard solution we titrated 0.1N KIO3 against prepared solution.
Take 25ml 0.1KIO3 in a flask and add 2gm of KI and add 10ml of 2N acetic acid to it.
The colorless solution turns brown as iodine is librated in the solution.
Titrate the librated iodine against the prepared solution and add starch indicator when the solution
turns pale yellow.
End point shows the color change from Blue to colorless

Calculation:
N1V1 = N2V2
Where, N1 = 0.1N KIO3 ……known
V1 = 25ml of KIO3…...known
N2 = Normality of Na2s2O3 to be found.
V2 = Burette reading

• If burette reading = 25ml

Therefore N1V1 = N2V2
N2 = 0.1 x 25/25
= 0.1N
If N2 = 0.1N we get correct 0.1N Na2S2O3 solution.

Case I:
If burette reading = 24.9ml

Then, N1V1 = N2V2

N2 = 0.1 X 25/24.9
= 0.1004N
Here, 0.1004 > 0.1N
The prepared solution is concentrated.
To dilute it we take N1 = 0.1004 and V1 = 1000ml
V2 is the total volume of distilled water which is substrated from V1 (the actual 1000ml) and the
difference is the amount to be added and N2 = 0.1N Na2S2OH3
N1V1 = N2V2
V2 = 0.1004 x 1000/0.1
= 1004 ml

45
Therefore, V2-V1 = 1004 – 1000
= 4ml
Therefore, if we add 4ml in the prepared concentrated solution we will get perfect 0.1N Na2S2O3
solution and even the burette reading when titrated against 0.1N KIO3 will be 25ml.
Take one more reading for conformation.

Dilution:
V2 – V1 = 1004 – 1000
= 4ml
Therefore, if we add 4ml in the prepared concentrated solution we will get perfect 0.1N Na2S2O3 and
even the burette reading when titrated against 0.1N KIO3, the burette reading will be 25ml.
N1V1 = N2V2
N2 = 0.1 X 25/25
= 0.1N Na2S2O3
Take one more reading for conformation.

Case II:
If the burette reading = 25.1ml
Then, N1V1 = N2V2
N2 = 0.1 x 25/25.1
= 0.0996N
Here, 0.0996 < 0.1
The prepared solution is diluted so, we use the formula
GPL = Equivalent wt x normality
= 248 x 0.0996
= 24.7011 gpl
• 24.7011gpl is to be substrated from 24.8 (the standard gpl for 0.1N Na2S2O3)
GPL = 24.8 –24.7011 = 0.1 gm

• 0.1 gm is the amount of Na2S2O3 to be added in the prepared diluted solution to get perfect
0.1N Na2S2O3 and even the burette reading when Titrated against 0.1N KIO3 will be 25ml
N1V1 = N2V2
N2 = 0.1 x 25.0/25.0
N2 = 0.1N
For conformation take one more reading.
Therefore we will get perfect 0.1N standardized Na2S2O3 solution.

Note:
As the prepared solution is degradable so we add preservative to keep constant normality. 0.1gm
of sodium carbonate (Na2CO3) and 0.2ml chloroform (CHCl3) is added in the prepared solution.

46
 PREPARATION OF INDICATORS

Preparation of Methyl red indicator

1gm of methyl red powder is dissolved in 1000ml of alcohol or acetone this will give us 1GPL
solution of methyl red indicator. Keep it for stirring till all the particles of methyl red powder gets
dissolved in alcohol or acetone. In acid it will give Pink color and in base it will give yellow color
and in neutral medium it will give Brick red color.

Preparation of Phenolphthalein indicator

1gm of Phenolphthalein powder is dissolved in 1000ml of alcohol. This will give 1GPL solution of
indicator. Stir it and we will get Phenolphthalein indicator. In acidic and neutral medium it is
colorless and in base it is pink color.

Preparation of Methyl orange indicator

1gm of methyl orange powder in 1000ml of distilled water will give us 1GPL of methyl orange
indicator. In acid it will give red color and in base it will give yellow orange color.

47
 GENERAL
VISCOSITY (BALL & FALL)

 RELATIVE VISCOSITY OF VISCOSE:-

PROCEDURE

1. FILL a viscosity tube with air free viscose. Place it in a constant temperature bath at 200 C +
0.20 C.

2. Drop a polished steel ball (1/8” diameter) in the centre and record the time of fall between the
two marks, which are 20cm apart, with a stopwatch. The time in seconds is of an expression
of relative viscosity of the viscose.

 COAL GCV, MOISTURE, AND ASH

INTRODUCTION

 Bomb calorimeter
It’s used to find the calorific value of steam coal.
Unit = cal/gram
 Calorie:
Amount of heat required to raise the temperature of 1gm of water to 10C
Factors affecting calorific value are moisture and ash.
 Humidifier:
It’s used to absorb inherent moisture for coal sample.
 Moisture in charcoal:

PROCEDURE:

After obtaining a representative sample, crush about 50gms of charcoal in the form of fine powder.
Weight 8-10gms of powder sample in a flat weighting bottle.
Heat in an oven for about 8hrs at 105-1100C to constant weight.
Percentage (%) moisture = loss in weight x 100/ weight of the sample
Or
By halogen moisture weight 2-2.5gm at 1050C

 VOLATILE MATTER IN CHARCOAL:

PROCEDURE:

1. Weight 1.5-2 Gms of the powdered sample in a silica crucible.

2. Cover the crucible with the lid. Keeping a very small opening and heat over the oxidizing
flame of burner for exactly 7mins. (for the first 2mins heat over the low flame & next 5min
over the strong flame)
3. At the end of 7mins remove the flame and cover the crucible completely with the lid.
4. Cool in a dessicator and weight.
Percentage (%) volatile matter + moisture = loss in weight X 100/ weight of sample.
Deduct percentage (%) moisture to get only percentage (%) volatile matter.

48
 PERCENTAGE (%) ASH AND FIXED CABON IN CHARCOAL:

1. After determining the volatile matter, heat the same sample over the strong flame of a burner
(may increase in the temperature gradually to avoid mechanical loss)
2. For about 2hrs to constant weight heating should be done without the lid of the crucible.
3. Cool in a dessicator and weight the ash.
percentage(%) ash = weight of the ash X 100/ weight of the sample
% fixed carbon = 100 – (% moisture + volatile matter + ash)

 FOR CALORIFIC VALUE:

WE use a bomb calorimeter. For that we are taking 0.9960 – 0.9990 dry sample.
FORMULA:
(T2 – T1) X 2457 – 45 / weight of sample=_____________ cal/gm
Where, T2 = final temperature
T1 = initial temperature
2457 = factor calculated using Benzoic acid sample
Heat equivalent of bomb calorimeter for 10C = 2457 cv
45 = calorific value of nichrome wire + thread

Coal is divided in to two parts:

1. Wooden charcoal
Example
Weight of sample Volatile matter moisture %ash
16.3662 16.3662 15.2867
- 15.2618 - 16.2204 -15.2618
1.1044__ 0.1458__ 0.0249__

% moisture = 6.2%
% volatile matter = 7.0%
% ash = 2.3%
% free carbon = 84.5%

2. Steam coal
Example
Weight of sample % ash
18.628 17.135
- 16.693 - 16.693
1.935 0.442
% moisture = 9.2% (halogen moisture)
% ash = 22.8%
Gross Calorific Value (GCV) = 5248 cal/gm

49
  SPECIFIC GRAVITY OF SPINBATH BY HYDROMETER

SULPHURIC ACID IN SPINBATH:

 Reagents:
1. 1.0N sodium hydroxide solution
2. Methyl red indicator

 PROCEDURE:
1. Pipette 10ml of spin bath at 400C in a conical flask.
2. Add 15-20ml of distilled water and 2-3 drops of methyl red indicator.
3. Titrate against 1.0N NaOH.
4. The N point being color change from Red to Light Yellow.
H2SO4 gm/ltr = Reading in ml of 1.0N NaOH x 4.9
therefore, 1ml of 1.0N NaOH = 0.049gm of H2SO4
2NaOH + H2SO4 → Na2SO4 + 2H2O

 AIR ANALYSIS

 INTRODUCTION:
This section mainly deals with the various sources of AIR Pollution in the company and
estimation their concentration. This section also deals with the hazard analysis related to the rupture
of chlorine or carbon disulphide tank. Dispersion modeling by Pasquil Giffords models is done to
estimate the effects of such hazard and predict on how to the gases are going to spread when they
leak.

1. CARBON DISULPHIDE
A solution containing 21ml of rectified spirit, 2.0ml of diethyl amine and 2.0ml of 1gm per
liter of copper acetate was prepared.
Air was passed for specific period of time.
The volume of 25ml was made up with rectified spirit
Transmittance was found at 435nm.

2. HYDROGEN SULPHIDE
15ml of cadmium sulphate was taken and passed through the required amount of air.
A volume of 15ml was made distilled water
1.0ml of 1.1 Sulphonic acid, 0.05ml (1drop) of ferric sulphate (saturated), and 0.6ml of
Diphenyl diamine sulphate was added and the volume 22.0ml was made up using distilled
water
Transmittance at 670nm was found.

3. SULPHUR DIOXIDE
A solution 23ml of sodium tetrachloromerculate and 1.0ml of 0.2% HCHO
(formaldehyde) was prepared and air was passed.
1.0ml of parasosatitine indicator was added.
Transmittance was found at 560nm.

4. NITROGEN DIOXIDE
A solution of 10ml absorbing solution (4gm/ltr NaOH) was taken and air was passed.
Then 1.0ml of H2O2, 10ml of Sulponil amide and 1.5ml NEDA solution was added
Transmittance was found at 540nm.

50
 SAFETY IN LABORATORY

Every person working in a laboratory must be aware of many kinds of hazards. Many of them occur
because of ignorance and carelessness of the worker.

Following are listed few precautions to be taken while working in a laboratory.

1. Wearing an Apron in laboratory is must.

2. One should always wear safety glasses in laboratory for protection of eyes. If any chemical
flashes in ones eye, eyes should be washed with plenty of water and medical help should be
called.
3. Chemicals like concentrated H2SO4 and concentrated HCL are very dangerous as they are
highly dehydrating agents. If they fall on skin they absorb moisture from skin and burn skin
to give a permanent scar.
4. One must use dropper and test tube holder.
5. One must not smell deeply basic chemicals.
6. One must be familiar with the procedure for operating fire extinguisher in laboratory.
7. Work in such a way that you and your neighbor both are safe.
8. Never use open flame near inflammable liquids.
9. never heat graduated glass apparatus over flame
10. One must wear half sleeves and comfortable clothes to avoid accidents.

51