Water Analysis for Pharmaceutical Uses

8/11/2019 Water Analysis for Pharmaceutical Uses

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A

PROJECT REPORTON

WATER ANALYSISFOR

PHARMACEUTICAL USESCarried out at

AKUMS DURGS & PHARMACEUTICAL LTD

PLANT!"# HARIDWAR

$UALTY CONTROL DEPARTMENT

Su%itted i' (artia) *u)*i))e't o* t+eRe,uiree't *or t+e A-ard o* De.ree

O*

MASTER OF SCIENCE

I'

CHEMISTRY

/Coer0ia) Met+od1 o* C+ei0a) A'a)21i13

Su%itted %2

MUNENDRA KUMAR

U'der t+e Su(er4i1io' o*

Dr AK INDRAYAN

Pro*e11or/De(tto* C+ei1tr23

DEPARTMENT OF CHEMISTRY

FACULTY OF SCIENCE

GURUKULA KANGRI UNI5ERSITY

HARIDWAR!678797 /INDIA3


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69::!:6

CERTIFICATE

This is certified that the dissertation entitled ;Water A'a)21i1 *orP+ara0euti0a) U1e1


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CANDIDATE?S DECLARATION

I hereby declare that the work being presented in the project report entitled;Water A'a)21i1 *or P+ara0euti0a) U1e1< is an authentic record of myown work carried out by me during @9:69:6 to @9769:6 at AKUMSDRUGS & PHARMACEUTICALS LTD PLANT!"# HARIDWAR $C

DEPARTMENT< under supervision and guidance of Pro*AK I'dra2a'#and is being submitted in partial fulfillment of the requirement for the awardof degree of Ma1ter o* S0ie'0e i' C+ei1tr2 !ommercial "ethods of!hemical #nalysis$ from Guru=u)a Ka'.ri 5i1+-a4id2a)a2a# Harid-ar

It has not been submitted anywhere else for the award of any other degree%diploma.

&ate ' "unendra (umar$

)lace '


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ACKNOWLEDGEMENT

It is a pleasant duty to acknowledge our deep sense of gratitude to )rofessor AK

I'dra2a'# &epartment of !hemistry* +urukula (angri ,ishwavidyalaya* -aridwar$ forhis invaluable guidance* indefatigable help* unflinching support and constantencouragement without which the present programme of investigation wouldnt haveseen light of the day.

I e/press my grateful thanks to Pro*e11or RD Si'.+# -ead* &epartment of!hemistry*+urukula (angri ,ishwavidalaya* -aridwar who provided me all thenecessary facilities for completion of my dissertation work.

It is a matter of great pleasure to e/press my sincere and heartfelt thanks to MrPardee( Kuar# Senior "anager 0uality !ontrol* #kums &rugs 1 )harmaceuticals

2imited* -aridwar for his never3failing enthusiasm* invaluable encouragement*stimulating discussions and guidance throughout the study to complete my dissertationwork.

I am also grateful to all my teachers and staff of the &epartment of !hemistry of+urukula (angri ,ishwavidyalaya* -aridwar for their help during my study period.

I am greatly thankful to Mr K+o1)a 1ir 4/ecutive Officer 0.!.* Mr 5ia2 1ir#Senior !hemist 0.!.* #kums &rugs 1 )harmaceuticals 2imited* -aridwar for valuablesuggestions and guidance during the course of study.

I am also grateful to Mr Sa'dee( Kuar -5 -ead$ for providing me facilities tocarry out study at #kums &rugs 1 )harmaceuticals 2imited* -aridwar.

I acknowledge with thanks the e/cellent technical support provided by MrA'i)1ir#Sa4ita ada and other staff of #kums &rugs 1 )harmaceuticals 2imited* -aridwarfor the laboratory study.

It would have never been possible to reach the distinction without the silentblessing* affections and encouragement from my especially my father throughout thestudy.

Date > /Mu'e'dra Kuar3


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#kums drugs 1 )harmaceuticals 2T&. -aridwar is the best pharma industryof the sidcul haridwar.#kums drugs is providing its medicine andinjections*eye drops*tablates and other medicines.


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ANTIBIOTICS

"edindia on 3 #ppendicitisThe vermifom appendi/ or appendi/ in short* is a small part of the bowel orintestine. It is situated on the right side of the abdomen at the junction of the

small and large intestines. It is a small narrow sac appro/imately 67 cm longand 6 cm wide. The appendi/ is a vestigial organ* that is* it serves no useful

purpose.

#bdominal )ain#ppendectomy 3 Surgical )rocedure8-O 9rges to 2imit the 9se of #ntibiotics


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#ntibiotic therapy could be a safe and viable alternative to surgery forpatients suffering from acute uncomplicated appendicitis* according toe/perts.

Surgery to remove an inflamed appendi/ appendicectomy$ has been themainstay of treatment for acute appendicitis since 6::; and the generalassumption is that* without surgery* the risk of complications* such as

perforation or infection* is high.

-owever* recent studies have reported fewer problems with antibiotictherapy than surgery in patients with uncomplicated appendicitis* but resultshave been inconclusive.


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TABLATES & CAPSULES


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INDEB

: )5O


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@#N#2=TI!#2 4E)45I"#NT

54S92T

54


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PH METER

It is used to determine the acidity or alkalinity of the solution.

PRINCIPLE >!

The p- of the solution is negative logarithm of hydrogenion concentration. In this all states of acidity and alkalinity b%wthose of the solution containing 6 mole of hydrogen ion and 6 moleof hydrogen ion can be e/pressed by the series of positive no.7 to6A

p-F3log 67G-HThe p- of purified water is B3DThe p- of water is D3;


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FRE$UENCY OF CALIRATION>!

The p- meter will be calibrated before every measurement.

In ease if electrode gets break* new electrode will be

activated by dipping in 7.6N -!2 for p-. !alibration again.

OPERATION PROCEDURE >!

a. Switch on the power.

b. (eep on the instrument for ?7 minutes before use. Thedetermination is carried out the temp of >B ! unlessotherwise specified in the individual monograph.

c. !alibrate the p- meter by p- D.7 buffer solution.

PH MEASUREMENT'3

5emove the electrode from the purified water. 5inse with

purified water and wipe out with tissue paper.

!alibration the p- meter as per the calibration procedure.

@ring the temp of measuring solution to >BHor3 7 ! and

immerse the electrode in the solution.

#fter noting down the p- value of test solution* remove theelectrode from solution. 8ash with purified water and dip inpurified water and press the JST#N& @=K.


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CONDUCTI5ITY METER

INTRODUCTION TO CONDUCTI5ITY>!

DEFINITION>!

!onductivity is the ability of a material to conduct electric current.The principle by which instruments measure conductivity is simple3 two plates are placed in the sample* a potential is applied across

the plates normally a sine wave voltage$* and the current ismeasured. !onductivity !$* the inverse of resistivity 5$ isdetermined from the voltage and current values according to OhmLslaw.

C IR I /a(13 E /4o)t13


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Since the charge on ions in solution facilities the conductance ofelectrical current* the conductivity of a solution is proportional toits ion concentration. In some situations* however* conductivitymay not correlate directly to concentration. The graphs below

illustrate the relationship between conductivity and ionconcentration for two common solutions. Notice that the graph islinear for sodium chloride solution* but not for highly concentratedsulfuric acid. Ionic interactions can alter the linear relationship

between conductivity and concentration in some highlyconcentrated solutions.

UNITS OF MEASUREMENT>!

The basic unit of conductivity is the siemens S$* formerly calledthe mho. Since cell geometry affects conductivity values*standardiMed measurements are e/pressed in specific conductivityunits S%cm$ to compensate for variations in electrode dimensions.Specific conductivity !$ is simply the product of measuredconductivity +$ and the electrode cell constant 2%#$* where 2 isthe length of the column of liquid between the electrode and # isthe area of the electrodes see !

!onductivity measurements are temperature dependent. The degreeto which temperature affects conductivity varies from solution tosolution and can be calculated using the following formula'

Gt Gt0a): /T!T 0a)3


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where' +t F conductivity at any temperature T in !* +tcalFconductivity at calibration temperature Tcalin !*F temperaturecoefficient of solution at Tcalin !.

CONDUCTI5ITY METER CALIRATION AND CELLMAINTENANCE>!

!onductivity meters and cells should be calibrated to a standardsolution before using. 8hen selecting a standard* choose one thathas the appro/imate conductivity of the solution to be measured.The conductivity of some common solutions is shown in the table

below.

So)utio' Co'du0ti4it2

#bsolute pure water 7.7BB S%cm

)ower plant boilerwater

6.7 S%cm

+ood city water B7 S%cm

Ocean water B? mS%cm

# polariMed or fouled electrode must be cleaned to renew the active

surface of the cell. In most situations* hot water with a mild liquiddetergent is an effective cleanser. #cetone easily cleans mostorganic matter* and chlorous solutions will remove algae*

bacteria or molds. To prevent cell damage* abrasives or sharpobjects should not be used to clean an electrode. # cotton budworks well for cleaning but care must be taken not to widen thedistance of cell.

IMPORTANT FEATURES TO CONSIDER>!


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Auto!ra'.i'.>"eter automatically selects the appropriaterange for measurement. There is no need to change the dial*multiply values on the display* or turn the potentiometer.

Te(erature 0o(e'1atio'># cell with built3in

temperature sensor allows the meter to make adjustments tothe conductivity or T&S readings based on changes insolution temperature.

TDS 0o'4er1io' *a0tor>8hen a solution does not have asimilar ionic content to natural water or salt water* then aT&S conversion factor is needed to automatically adjust thereadings.

Adu1ta%)e te(erature 0oe**i0ie't1>The T&S of certain

samples* such as alcohols and pure water* are affected bychanges in temperature. #n adjustable temperaturecoefficient allows the user to compensate for temperaturechanges on the solution being measured.

Adu1ta%)e 0e)) 0o'1ta't>#djusts the reading on the displayto reflect use of a cell with a constant other than kF6.7 cm36.


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TURIDITIMETER

PRINCIPLE'3 Sulfate ion is precipitated in an acetic acid mediumwith barium chloride so as form barium sulfate crystals of uniformsiMe. 2ight absorbance of the @aSOAsuspension is measured by a

photometer and the SOAP P concentration is determined bycomparison of the reading with a standard curve.

PROCEDURE>!


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"easurement of barium sulphate turbidity' after stirring period hasended* poured solution into absorption cell 1 measured turbidity atBQ7.B min.

)reparation of calibration curve' estimated sulphate concentrationby comparing turbidity reading with a calibration curve preparedby carrying out sulphate standards through the entired procedurespace standards through at Bmg%2 increments in the 73A7mg%2range.#bove A7mg%2 accuracy decreases 1 barium sulphate suspensionlose stability.

CALCULATION'3

mg SOAP P%2F mg SOAP PR6777 m2 sample


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TOTAL SUSPENDED SOLIDS

IMPORTANCE>!

8ater having suspended solids are esthetically unsatisfactory thesewaters are unsuitable for bathing etc.

PRINCIPLE>!

# well mi/ed sample is filtered through a standard filter and theresidue retained on the filter is dried at a constant temperature in anoven at 67? to 67B !. Increase in the weight of filter representsthe total suspended solids.

APPARATUS>!

6. "uffle furnace for operation at B77HB7!>. &edicator?. &rying oven for operation at 67? to 67B !

A. #nalytical balanceB. +lass fiber filter disk%what man filter paper no.A>.C. !

6. Select sample volume that yield a residue between 67 to>77mg.

>. Transfer a measured volume of well mi/ed sample onto a filter.?. 8ash filter paper with three successive 67 ml volume of

reagent grade water after filtration.A. &ry filter paper for at least 6 hour in the drying oven 67? to

67B !.B. !ool it in desiccators and weight.


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C. 5epeat cycle of during cooling desiccating until a constantweight is obtained or weight change is less than A of the

previous weight.

CALCULATION>!

"g total suspended solids%2F #3@$ R6777 Sample volume in ml.

8here*#Fweight of dried residue Hfilter in mg@Fweight of filter in mg


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TOTAL DISSOL5ED SOLIDS

IMPORTANCE>!

The total dissolved solids T&S in water comprises of inorganicsalts. The principle ions contributing to T&S are carbonate*

bicarbonates* chlorides* sulfates* nitrates* sodium* potassium andcalcium. Total dissolved solids influence other qualities of drinkingwater such as taste* hardness* corrosion properties and tendency toincrustation.T&S may originate from natural sources* sewage effluentdischarges* urban run off or industrial waste discharges* drinking

water having high T&S is not acceptable to consumers.

PRINCIPLE>!

# well mi/ed sample is filtered through a standard filter andfiltrate is evaporated to dryness in a weighted dish and to aconstant weight in an oven at 6:7!. Increased in the weight ofempty dish represents the total dissolved solids.

PROCEDURE>!


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8here*

#Fweight of dried residue H dish* mg* and @F weight of dish* mg


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FIBED AND 5OLATILE SOLIDS

IMPORTANCE>!

The determination fi/ed and volatile solids provide a rough idea ofthe amount of organic matter present in the solid fraction. This isvery useful in control of waste treatment plant operations.

PRINCIPLE>!

The residue is ignited to constant weight atB77HB7!. Theremaining solids represent fi/ed solids while the loss in weightduring ignition is the volatile solids.

PROCEDURE>!

6. Ignite residue to constant weight in a muffle furnace>. 9sually >73?7 minute ignite is required. -owever for more thanone samples. 2onger ignition is required.

?. !ool dish desiccators in air for partial cooling.A. Transfer it in desiccators for final cooling and weight.B. 5epeat cycle of igniting cooling and desiccating until a constantweight is obtained or weight change is less than A of the previousweight.

CALCULATION>!

mg volatile solids % 2 F #3@$ R677 sample volume in ml


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8here*

#F8eight of residue H dish before ignition*mg @ F8eight of residue H dish or filter after ignition*mg


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HARDNESS

PRINCIPLE >!4thylenediaminetetraacetic acid and its sodiumsalt from a chelated soluble comple/ when added to a solution ofcertain metal cations. If a small amount of a dye such aseriochrome black T or calmagite is added to an aqueous solutioncontaining calcium and magnesium ions at a p- of 67.7Q7.6* thesolution become wine red. If 4&T# is added as a titrant* thecalcium and magnesium will be comple/ed the solution turns fromwine red to blue* marking the end point of the titration.

PROCEDURE>! Take >B ml of sample in a conical flask. #dd 6.7 mlammonia buffer solution to bring its p- 67 to 67.6and ? drops of 4riochrome black T indicator. Titrate with standard7.76N 4&T# solution till color changes from wine red to blue.

!alculation '3

-ardness 4&T#$ as mg !a!O?%2F #R6777

m2 sample

8here* #F m2 of 4&T# used


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ALKALINITY

PRINCIPLE>!

#lkalinity is measured volumetrically by titration withN%B7 ->SOA1 is reported in terms of equivalent !a!O?. while in the second phase the titration is conducted to aboutA.B.

PROCEDURE>!

Take >Bm2 sample in a conical flask. #dd B drops ofmi/ed indicatormethyl red 1 methyl orange$ blue color appear.Titrate 7.7>N ->SOAtill the color change of blue to light red.

CALCULATION>!#lkalinity mg !a!O?%2F #RNRB7777

m2 sample

8here* #F m2 standard acid used and NF normality of standard acid


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CHLORIDE

PRINCIPLE>!

In a neutral or slightly alkaline solution * potassium chromate canindicate the end point of the silver nitrate titration of chloride.Silver chloride is precipitated quantitatively before red silverchrome is formed.

PROCEDURE>!

Take >B ml sample in a conical flask. #dd B drops of potassiumchromate indicator. Titrate with standard 7.76A6N #gNO?solution.8ith the change of color from yellow to brick red.

CALCULATION>!

mg !lP%2 F #RNR?BAB7 m2 sample

8here*A m2 titration for sample

Nnormality of #gNO?


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CHEMICAL OBYGEN DEMAND /COD3

PRINCIPLE>!

"ost type of organic matter are o/idiMed by a boiling mi/ture ofchromic and sulfuric acid. # sample is reflu/ed in strongly acidsolution with a known e/cess of potassium dichromate (>!r>OD$.#fter digestion* the remaining unreduced (>!r>ODis titrated withferrous ammonium sulfate to determine the amount of (>!r>ODconsumed andthe o/idiMable matter is calculated in terms of o/ygen equivalent.

PROCEDURE>!Take >7ml sample in a reflu/ing flask. Then add 6gm -gSOAandadded about 6 ml con. ->SOA 6gm #g>SOAin every DBml acid $slowly to dissolve -gSOA. cool the mi/ture add 67ml * 7.>BN(>!r>ODsolution and again mi/. attach the condenser and start thecooling water .add the remaining acid reagent>;ml$ mi/ andreflu/ed the mi/ture for > hour then cool. &ilute the mi/ture to about 6>7ml an titrate e/cess of (>!r>OD

with standard ferrous ammonium sulphate using ferroin indicator.The color will change from yellow to green blue and finally red.5ecorded ml of titrant used .5eflu/ed in the same manner a blank.

FORMULA>!

!O& mg$F #3@$ RNR:777 ml sample

8here* #F ml


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IOCHEMICAL OBYGEN DEMAND /OD3

PRINCIPLE>!

The @O& test is based on mainly bioassay procedurewhich measured the dissolved o/ygen consumed bymicroorganism while assimilating and o/idiMing the organic matterunder aerobic condition.The standard test condition includes incubating the sample in an airtight bottle in dark at a specified temp. for specific time.

PREPARATION OF DILUTION WATER'3

#erate the required vol. of distilled water in acontainer by bubbling compressed air for : to 6> hours to attaindissolved o/ygen saturated. 2et it stabiliMe for A hours at roomtemp. around >D!$

#t the time of use* add 6ml each of phosphate buffer* magnesiumsulphate* calcium chloride and ferric chloride for each liter of

dilution water. #dd >3B ml of treated sewage per liter of dilutionwater for seeding purpose.

DILUTION OF SAMPLE AND INCUATION

NEUTRALIATION>!

NeutraliMe the sample to p- around p- D.7using alkali or acid of such strength that the quality of reagent doesnot dilution the sample by more than 7.B percentage.

SAMPLE 5OL AND DILUTION TECHNI$UE'3 On the basis of !O& determination e/pected @O& used thefollowing formula for calculating sample volume.Sample vol. in m2%2 dilution F ER6777 4/pected @O&


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dilution take EF>.B and A.A


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8hen diluted water is unseeded@O&* mg%2F &63&>R6777

)

8hen dilution water is seeded @O&* mg%2F&63&>3@63@>$ RfR6777 )8here* &6F initial &O of sample in mg%2

&>F &O of sample after incubation in mg%2@6F &O of seed control before incubation in mg%2

@>F &O of seed control after incubation in mg%2 f F 5atio of seed in diluted sample to seed in control 'seed in diluted sample$' seed in seed control ) F dilution of sample sample vol. in ml%2$


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WATER SAMPLE /KARNAL# WYC3

SMAPLE NO ::999:

SNO PARAMETER RESULT: p- D.:7

6 !onductivity ?BC"s

" -ardness >AAmg%2

7 Turbidity 7.A6>:mg%2

@ #lkalinity 6AAmg%2

!hloride 6>mg%2

!O& >mg%2

@O& 7.Cmg%2

8 TSS ?Cmg%2

:9 T&S >ACmg%2


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DRINKING WATER $UALITY STANDARDSNO Su%1ta'0e

C+ara0teri

Sti01

Re,uiree'tde1ir

a%)e )iit

U'de1ira%)e

e**e0t out1ide

t+e de1ira%)e)iit

: !olour *haMen unit*ma/

B #boveB*consumeracceptancedecreases

6 Odour 9nobjectionable " Taste #greeable 7 Turbidity *

NT9* "a/ B #bove B

consumeracceptancedecreases.

@ p- value C.: to :.B @eyond thisrange the waterwill affect the

mucousmembrane andwater supplysystem.

Totalhardness

?77 4ncrustation inwater supplystructure and

adverse effecton domestic use. Ions mh%2*

ma/7.? @eyond this

limittaste%appearance


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are affected hasadverse effecton domestic

uses and watersupply structureand promotesiron bacteria.

!hlorideas!l$mg%2*ma/

>B7 @eyond thislimit* taste*corrosion andpalatability are

affected.:9 &issolved

solids%2*ma/

B77 @eyond thispolabilitydecreases andmay causegastro intestinalinitation

:: !alciummg%2 *ma/

DB 4ncrustation inwater supplystructure andadverse effectson domestic use.

:6 !opper

mg%2* ma/

7.7B #stringent taste*

discoloration:" "anganesemg%2 ma/

7.6 @eyond thislimittaste%appearanceare affected* hasadverse effect


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on domesticuses and watersupply structure.

:7 Sulphatemg%2 ma/ >77 @eyond thiscause gastrointestinalirritation whenmagnesium orsodium arepresent.

:@ Nitrate

mg%2 ma/

AB @eyond this

methaemoglobiemia takes place.

:


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STANDARD METHOD FOR THE EBAMINATION

OF WATER AND WASTE WATER FROM APHA

/Aeri0a' Pu%)i0 Hea)t+ A11o0iatio'3

SNo Paraeter Mea1uri'.ra'.e

Mi'iudete0tio' )iit

: !olour 6to B77 haMen 6 haMen6 !onductivity 7 to >777 s%cm 7.76 s%cm" p- 7 to6A p- 7.76 )h7 Suspended solid 7.6mg%2 to >77

g%27.6mg%2

@ Suspended volatile

solid

7.6 mg%2 to

>77g%2

7.6mg%2

Settleable solid 7.6 mg%2 to>77g%2

7.6mg%2

Sludge volumeinde/

Total solid 7.6 mg%2 to>77g%2

7.6mg%2

8 Total volatile solid 7.6 mg%2 to

>77g%2

7.6mg%2

:9 Temperature 7 to 667! 7.6 !:: Turbidity 7 to 6777 NT9 7.76 NT9:6 #cidity 7.B to B77mg%2 7.Bmg%2:" #lkalinity 7.B to B77mg%2 7.Bmg%2:7 #mmonical free 7.7> to 7.Cmg%2 7.7>mg%2:@ #mmonical

nitrogen7.7> to 7.Cmg%2 7.7>mg%2

: @O& > to C77mg%2 >mg%2: @romide : !hloride 7.6B to 67 mg%2 7.6Bmg%2:8 !arbon di o/ide

69 !O& 6 to 6777mg%2 6mg%2


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ANALYTICAL EBPERIMANT


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TOTAL KJELDAHL NITROGEN

PRINCIPLE>!

The nitrogen of the organic water is converted intoammonium sulphate when treated with sulphuric acid in the

presence of copper sulphate catalyst. #n e/cess alkali is than addedto liberate ammonia from ammonium sulphate and distilled. Thedistilled is either treated with nesselers reagent or titrated withstandard sulphuric acid after absorbing in boric acid solution.

PROCEDURE>!

Taken 677ml water sample in a conical flask and added6gm salicylic acid followed by 67 ml of conc. Sulphuric acid. Thecontent of flask are shaken thoroughly for >3?min. and allowed tostand for half and hour for complete reaction. To this mi/ture :gmof (>SOAand added 7.Bgm of !uSOA. #fter an interval of aboutBmin the flask is now placed under fuming chamber to first slowheating followed by strong heated. The process of digestion

continues for >3? hour till the solution becomes clears and a tingeof blue3 green colour appear. The mi/ture is cooled is diluted with677 ml of distilled water. This is filtered as usual and washed withconstant jet of water. The filtrate and washing are colleted >B7mlvolumetric flask. The volume is made up to mark will distilledwater. 677ml of this solution is taken in a B77ml conical flask anddistilled with B7ml of A7NaO-.

The librated ammonia is absorbed in a >B7ml conical flaskcontaining B7ml of 7.6N sulphuric acid. The unused acid is titratedagainst 7.6N NaO- using methyl red indicator.


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CALCULATION>!

Total kjeldahl nitrogen* mg%2F S3@$ R N R 6777R6Aml of sample

8here* SFvolume of titrant used against sample m2$ @Fvolume of titrant used against blank m2$ NFnormality of titrant7.6N NaO-$


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NITRATE

PRINCIPLE>!

Nitrate is reduced quantitatively to nitrite NO>P$in the presence of cadmium !d$.This method uses commerciallyavailable !d granules treated with copper sulphate and packed in aglass column.The NO>Pproduced thus is determined by diaMotiMing withsulphanilamide and coupling with N363naphthyl$3ethylenediaminedihydrochloride to form a highly colored aMo dye that is measuredcolorimetricall. # correction can be made for any NO>P present in

the sample by analyMing without the reduction step.The applecablerange of this method is 7.76 to 6.7mg NO?PN%2.The method isrecommended especially for nitrate ion levels below 7.6mg N %28here other methods lack adequate sensitivity.

PROCEDURE>!

PREPARATION OF REDUCTION COLUMN>!Insert a glass wool plug into bottom of

reduction column and fill with water add sufficient !u V !dgranules to prevent entrapment of air wash column with >77mldilute N-A!l34&T# solution. #ctivate column by passing throughit* at Dto67m2%min. at least 677m2 of a solution compose of >B6.7 mg NO?P N%2 and DB N-A!l 34&T# solution.

(H ADJUSTMENT>! #djust p- to between D and ;* asnecessary* using a p- meter and dilute -!l or NaO-. This insuresa p- of :.B after adding N-A!l3 4&T#.Sample reduction' To >B.7m2 sample or a portion diluted to>B.7m2 add DBml N-A!l 34&T# solution and mi/. )oured mi/ed


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sample into column and collect at a rate of D to 67m2%min.&iscardfirst >Bm2.collect the rest in original sample flask. There is noneed to wash columns between samples* but if columns are not to

be reused for several hours or longer* pour B7m2 dilute N-A!l

34&T# solution on to the top and let it pass through the system.Store !u3!d column in this solution and never let it dry.!olour development and measurement' #s soon as possible andnot more than 6Bmin after reduction* add >.7m2 colour reagenttoB7m2 sample and mi/. @etween 67min and >hour afterward."easure absorbance at BA?nm against a distilled water reagent

blank.

Standards'3 using the intermediate NO?P N%N by diluting thefollowing volumes to 677m2 in volumetrically flask7.B*6.7*>.7*B.7*and 67.7 m2. !arry out reduction of standardse/actly as described for sample. !ompare at least on NO>Pstandard to a reduced NO?P standard at the same concentration toverify reduction column efficiency.

CALCULATION'3Obtain a standard curve by plotting absorbance of standards

against NO?P N concentration compute sample concentrationdirectly from standard curve. 5eport as mg o/idiMed nitrogen perliter.


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ATOMIC ASORPTION SPECTROSCOPY

PRINCIPLE>!

Atomic Absorption Spectroscopy (AAS)

In atoi0 a%1or(tio' 1(e0tro10o(2##S$* elements as analyteare transformed into the free atomic state in an atomiMation device

by input of thermal energy. These atoms are able to absorbelement3specific radiation. To this end* an element3specific lampwith a hollow cathode made of the element to be investigated is
http://www.merck-chemicals.com/aas-standards-titrisol-/c_ml.b.s1L61MAAAEW9eAfVhTl?back=truehttp://www.merck-chemicals.com/aas-standards-titrisol-/c_ml.b.s1L61MAAAEW9eAfVhTl?back=true


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introduced into the ray path of an atomic absorption spectrometerwith the atomiMation device and a detector. &epending on theconcentration of the element to be determined in the sample* someof the radiation intensity of the hollow3cathode lamp is absorbed

by the atoms formed. Two photomultipliers measure the intensityof the non3attenuated radiation and the radiation after leaving theatomiMation device during the supply of a sample solution. Theelement concentration in the sample can be calculated from thedifference in the two intensities.&etermination of #l* !d* !r* !u* !

I'1true't O(eratio''3 #s per the instructions given bythe manufacturer of the instrument.

Sta'dardiatio'>!Select at least three concentrations ofstandard metal solutions to breaket the e/pected metal

concentration of sample. #spirate each in turn into theflame. 5ecord absorbance and calibrate.

#nalysis of the sample'3 5inse atomiMer and atomiMe asample and determine its absorbance and determine itsconcentration from the standard calibration graph.

Ca)0u)atio'>! !alculate the concentration of the metal ionin micrograms per liter by referring to appropriatecalibration curve or read the concentration directly frominstrument read out. If sample has been diluted multiply byappropriate dilution factor.


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PHOSPHORUS

PRINCIPLE>3The phosphate react with ammo. molybdate and

form comple/ molybdophosphoric acid *which gets reduced tocomple/ of blue colour in the presence of Sn!l>.the abjorption oflight by this blue colour can be measured at C;7nm to calculate theconcentration of phosphate.)rocedure'3preparation of standard curve'3make various dilutionsat the interval of 7.6mg)%2 from the std.phosphate solution.TakeB7 m2 each of dilution and add Am2 amm. "olybdate and 7.:m2 or 67drops of Sn!l> solution and mi/ thoroughly.

Take the readings after 67 minutes but before 6> minutes at C;7nmand plot a graph between absorbance and concentration .Sample reading'3take B7m2 of filtered clear sample in a cleanconical flask.if the sample contains colour and colloidalimpurities* they can be removed by adding a spoonful of activatedcharcoal and then filtering the sample.#dd Am2 ammo. "olybdate followed by 67 drops of Sn!l>solution.

# blue colour will appear. Take reading after 67 min. but before 6>min. at C;7nm on a spectrophotometer using a distilled water blankwith the same amount of the chemicals.!

mg )%2 F mg ) in B7 m2R6777 m2

m2 of sample


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REFERENCES

#)-# #merican )ublic -ealth #ssociation $.

Sawyer * -einemann * @eebe * !hemical 4/periment for

Instrument "ethod * 8iley .New =ork *6;:A

&.!.-arries quantitative !hemical #nalysis Ath4d* 8.-.

freeman and company* New =ork * 6;:A.

The theory 1 practice of industrial pharmacy by 2ackman

tucker.

4nvironmental chemistry by (udesia.

Instrumental methods of chemical analysis by -. (aur.

8ater 1 8aste 8ater Testing by 5.). "athur.

Documents

Water Analysis for Pharmaceutical Uses