INTRODUCTIONUnited Ghee industry is situated Nashtabad Kashmir road.It is reputed and leading name in vegetable ghee,cooking oil and soap products comprised upon following processes with in existing premises:-

1. Vegetable ghee2. Cooking oil3. Tin packaging and printing4. Laundry soap

United Ghee Mills(Pvt) Limited having production capacity of vegetable ghee as 24000 M/Ton,cooking oil 20000 M/Ton and laundry soap 24000 M/Ton per annum.Its products are registered with defence forces,utility stores corporation and canteen stores department of defence forces.Where its supplies are successfully being supplied and many contracts of vegetable ghee,cooking oil and laundary soaps have already been successfully completed and few in pipelines.The unit is registered with Pakistan Vanaspati Ghee Manufacturing Association, Chamber of Commerce and industry,Sales Tax Department Government of Pakistan,Pakistan Army,Navy,Trade Marks Government of Pakistan.Technical staff United Ghee Mills(Pvt) limited is highly experienced and well educated in this field.The unit comprised upon 74 Kanal 04 Marla’s and 165 sq.ft of land,which is equipped with unique type of latest machinery and plant installed in its attractive building.The beautiful roadside Mosque,Fruity garden on the front side of the office block creates extra ordinary beauty.Private energy source,Gas connection and sewerage line linked with disposal drain are in existence within premises of the mills.The people who are dealing in vegetable ghee,cooking oil and laundary soap they know well the name of United ghee mills renowned products,which are in the market with the name and style of “Kashmir banaspati,Kashmir cooking oil and laundry soap.

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BRANDS: Kashmir cooking oil Kashmir canola oil Kashmir premium gold Kashmir banaspatti

Oil refinery Neutralizers Bleachers Deodorizers Autoclaves Filter press Coolers

Hydrogenation plant Quality assurance lab Steam boiler unit Soap preparation plant Filling unit Work shop Tin printing unit Bleaching earth preparation unit Raw oil storage tank Water storage tank Caustic soda tank Centrifugal pumps

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POLICIES OF UNITED GHEE INDUSTRY’S (Pvt) LIMITED

Quality and consumer safety policyUnited ghee industry take care to ensure that their customers & consumers are provided with the best quality products that are safe in use.To meet the customer’s expection and needs United ghee industry is committed to develop and ensure consistent supply of affordable,convenient,safe and high quality products.As a service company we take care to ensure that our customers are provided with the best quality services to fulfill all customers needs.In order to achieve these goals United ghee industry will:

Agree quality and consumer safety objectives along with implementation plans on annual basis and maintain follow up by reporting process.

Design operate & maintain processes and plants to establish and maintain standards and procedures for the control and monitoring of all operations that prevent potential product safety hazards.

Will ensure the compliance with applicable legislation and set standards, Introduce appropriate product quality management system & maintain HACCAP as a

management tool at all their operating sides. Help their suppliers to develop their quality process & standard so as to get consistent

quality suppliers and develop supply chain to improve overall quality performance audits.

Responsibility to implement this policy lies with general manager & the same is filtered to the functional heads and respectives manager in their areas of responsibility.

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Environmental Policy United ghee industry are committed to meet the needs for customers and society in an

environment sound and sustainable manner. Work in co-operation with members of industry,government bodies and public interest

groups,scientists,environmentalists,technical department and customers to promote achievements of high standards of environmental care.

Continuously strive to reduce the wastage,conserve energy,examine reuse & recyle throughout operation being carried out at United ghee industry.

Ensure all the employees are the aware of the company environmental policy and are motivated to apply it.

Ensure the safety of our product manufacture at our side & will continue monitor and report all progress & notify environmental incident on regular basis.

Glass Policy

Glass contamination in products must be regarded as a major problem in product safety. Glass jars/bottles must be of adequate design and specification. Glass containers must always be coated to minimize the risk of breakage and

improve line handling characteristics. On incoming pallets,if broken glass is detected they should be rejected. In-line inspection must be adequate at the appropriate steps in the manufacturing

and filling process. Adequate separation between the filling area and glass cleaning,rinsing and blowing

area. Heating and cooling operation must be design to prevent thermal shock. No glass container is used for the sampling from production lines. All the persons using glass spectacles must use protective string while working in

production areas. All handling ,conveying and filling steps must be design to prevent unacceptable

mechanical shock. Lights and wall clocks in production area must be covered with plastic covering.

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STEPS GENERAL PROCESSING OF OIL PREPARATION

Oil seed

Cleaning

Steeping

Germ separation

Germ Drying

Expeller

Crude oil

Neutralization

Bleaching

Filtration

Deodourization

Cooling

Filtration Vitamins addition Packaging Storage

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REFINING PROCESS

1. Neutralization2. Bleaching3. Filteration4. Deodourization5. cooling6. Filteration7. Packaging

- At every step FFA determined to check whether process is working properly- Fresh crude oil contain less FFA.- During storage it increase gradually- Factors that enhane FFA are

a) Moistureb) Enzyme

Main objective of all the steps is - least possible damage to glycerides- minimize the oil losses

1. Neutralization :

Objective;To reduce FFA- Load the neutralizer with oil- Add caustic soda (have strength 50 Bomee dilute to 16 Bomee),depend upon amount of

FFA present if FFA is less than add less caustic soda,if higher amount of FFA present it will take more amount of caustic soda.

- Agitate by air- Temperature 45-50 0C.Temperature should not exceed 50 0C otherwise maximum oil

losses will occurs.- Provide heat by steam coil in neutralizer- Apply water that contain salt for half an hour- Remain at rest for 3 hours- Soap contents settle down than remove it- Take different washings to remove all soap contents at temperature 90 0C- During this take saop test to sure that all soap remove

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2. Bleaching:

Objective;To remove color bodies

- At this step some FFA increase due to activated bleaching earth.- Chemical bleaching earth is used under vaccum it adsorb the pigments- Its physical reaction not chemical- Temperature 110 0C- It cut the color,if more color more bleaching is required.- After bleaching noted FFA %age of corn oil

- FFA = mL of NaOH used × 2.82 / Wt. of sample= 0.8 × 28.2 × 0.1 / 15= 0.15 %

- At this stage determined the moisture %age of corn oil. - Moisture %age = Wt. of beaker + sample – Wt. after drying × 100

Wt. of original sample = 103.16 – 103.14 × 100 15 = 0.13 %

3. Filteration:

Objective;To remove impurities

- Oil pass through filter that contain different parallel filters- Bleaching earth remain in the filters - Also impurities remain in the filters- After that oil goes to deodourizer

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4. Deodourization:

Objective;To remove odourous compounds - Contain vessels in which steam is provide to raise temperature- Treat under high vaccum for 5-6 hours at 200 0C- Time depend on quality if good quality is required more time otherwise less time e.g 3-4

hours - Volatile compounds evaporate to deodourizer roof that is bend shape from which it

remove from outlet pipe- Add small amount of citric acid to increase the shelf life as well as quality.Citric acid act

as chelating & antioxidant agent.- After that noted FFA %age- FFA = ml of NaOH used × 28.2 × N / Wt. of sample

= 0.7 × 28.2 × 0.1 / 30= 0.06 %

- Moisture %age = 110.5 – 110.5 × 100 20

= 0%5. Cooling:

- Oil is cool at 35 0C in cooling tank- Cooling is provide by cool water- Cooling tank contain vessels in which cool water circulate - Add vitamins 44.5g per tonn in cooling tank- At this stage vitamins conc. is less so add the vitamins - Vitamin E (tocopherol) is natural anti-oxidant already present in oil

6. Filteration:

- After cooling again filteration is done- Cooling result in better filterate the oil- At this stage noted FFA %age- FFA %age of corn oil = 0.7 × 28.2 × 0.1 / 30 = 0.06 %- FFA %age for cotton oil = 1 × 28.2 × 0.1 / 40 = 0.08 %

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7. Packaging:

- At this stage FFA contents varies from 0.1-0.08 %- Fill the oil in different capactiy tin cans (2L,4L, by automatic plant and 9&17 liters

manually)- Before lidding add nitrogen gas for preservative but rare in Pakistan.

RECEIPT OF RAW AND PACKAGING MATERIAL

Arrival ofRaw material

in vehicle

Visual inspection of vehiclematerial by QA.

Vitamins and Packing material Bleaching earth & Caustic soda 50 Bepreservatives to the packing chemical to in caustic soda tank

material storage chemical storage

NO Sampling/Analysis by QC Inform to Raw Material store

YES

Pasting of red tag with Accepted Yes/No status REJECT

Transferred to RMS Pasting of red tagwith status

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Paste green tag (Status QA released)RECEIPT OF RAW OIL

Arrival of oil tankerat factory gate

Sampling & analysis by QA

Gross weight on weigh bridge

Connect pipelines & adjust valves for decantation & pumping

Decentation & pumping to storage tank

Mopping

Tare weight after decantation and mopping

W/B operator given acknowledgement

Tanker leaves factory

W/B Operator given acknowledgement

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Tanker leaves factory

NEUTRALIZATION / BLEACHING

Oil Storage Tanks

Oil charging through pump to Caustic soda neutralizers heating through storage tank closed steam coils

Neutralization Intermediate Caustic tank 18 Be

Settling/draining Hot water tank

QA Hopper for

bleaching earth

Washing

Heating/Drying bleaching under vaccum

Filtration

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Storage in B.O. Tank

DEODOURIZATION

Bleached Oil Tanks

Deodorization Stage 1Heating through closed steam Open steam

coils temp. 150 0C Vac. 26” – 28”.

Deodorization Stage IITemperature 150-195 0C

Ejector Vac 28” – 30”

Deodorization Stage IIICooling by water in closed Ctric acid dosing

coils to140 0C Vac. 28” – 30”

Mix Vitamins/PreservativeTemperature 35 0C

Refined oil to Filtration storage tank

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CAN FILLING

RBD oil instorage tanks

Churn

Filling Machine

Tin from storage

Lid placing and Seaming

Coding

Complete Cleaning Trays & wrappingreel from storage

Filled tins are shrink-wrapped

Warehousing & Despatch

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EXPLANATION FOR CRUDE & REFINED OIL TESTS

FFA TEST

Both for crude & refined.For corn crude oil FFA should not exceed 6% and for other edibles oil 0.39%.According to PSI standard FFA for refined oil should not more than 0.24%.

PRINCIPLE:The fat is dissolved in appropriate solvent,after which the solution is tritrate with NaOH solution.

REAGENTS:- Ethyl alcohol- 0.1 N NaOH- Phenolphthalene

EQUIPMENT:-Conical flask-Electric balance-Burette

PROCEDURE:- Take 50 mL spirit in 250 mL conical flask- Add few drops of indicator than neutralize with 0.1N NaOH till light pink olor attain- Add sample 5g for crude oil and 30g for refined oil- Than heat it upto 40 0C- Again add few drops of indiator- Now tritate with 0.1 N NaOH till light red color attain- Note the mL of NaOH used

Corn crude oilCalculation:FFA %age = mL of NaOH used × 28.2 × 0.1 / Wt. of sample = 10.3 × 28.2 × 0.1 / 5 = 5.06 %

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Corn refined oil

FFA %age = 0.7 × 28.2 × 0.1 / 20= 0.08%

COLOR TEST

Both for crude & refined oil.

NSTRUMENT:TintometerThis method describe the colour by comparison with a trichromatic system of yellow,red and blue filters.In practice,mainly red & yellow filters are used.

GLASSES FOR INSTRUMENT:Red0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.91 2 3 4 5 6 7 8 910 20 30 40 50Yellow1 2 3 4 5 6 7 8 910 20 30 40 50 60 70Blue0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.91 2 3 4 5 6 7 8 9

For crude oil;- Check that windows of the measuring cell and filters are clean and not covered with film

of oil.- Use one inch cell- Place the sample in cell and put in Tintometer- Adjust the red & yellow color in ratio 1:10 respectivily.- Adjust the yellow color reading at 45 scale,should not exceed 50.- Red color reading should not exceed 5.If greater it will reject- Observed reading for corn crude oil is 4.2 red.

For refined oil;- Use 5.25 inches cell- Place the sample in it- Adjust the yellow color reading at 35 scale- Red color reading should not exceed 5.

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- Observed reading for corn crude is 3.5 red.

MOISTURE DETERMINATION

Both for crude & refined oil.For crude moisture limit should not be more than 0.2%.For refined it should be 0%. Two methods a) Oven method b) Sand-bath method

a) OVEN METHOD:

PROCEDURE:- Take empty beaker and weight it.- Than 20g sample in it and weight- Now place it in an ovan for 1-2 hours at 110 0C- After that remove and place in desicator to retain temperature at 40 0C - Weight it again- Calculate the moisture by following formula- Moisture %age = Difference in weight / Wt. of original sample × 100

b) SAND-BATH METHOD:

PROCEDURE:-Weight 20g prepared sample to the nearest 0.01g into dish containing thermometer.-Heat on sand-bath upto 90 0C stirring constantly with thermometer-Than reduce the rate of heating,nothing the rate at which bubbles rise from the bottom of the dish:donot allow the temperature to exceed 105 0C.-Continue to stir the liquid,scraping the bottom of the dish until all evolution of bubbles of steam has ceased.-Allow to cool to 95 0C & reheat to 105 0C-Cool the dish and contents to room temperature weight.

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MINERAL OIL TEST

For crude oil

REAGENTS:- Alcoholic caustic potash solution 0.5 N- Distilled water

EQUIPMENT:-Conical flask-Condenser-Water bath-Hot plate-Weight balance

PROCEDURE:- Take 2g oil sample in 150mL conical flask which has been previously dried thoroughly to ensure absence of water.- Add 25mL of alcoholic potash solution in conical flask.- Saponify the oil by keeping the flask fitted with glass-bulb air condenser on a water bath for 45 minutes.- Care should be taken to ensure that saponification is completed and also that there is no loss of alcohol during saponification.- Cool the flask and add 120mL distill water.- The development of turbidity indicates the presence of mineral oil.

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RANCIDITY TEST

For refined oil

REAGENTS:Conc. HClFloroglucinol + ether solution

EQUIPMENT:-Cylinder

PROCEDURE: - Take 10 mL of sample in cylinder and 10 mL of sample in the same cylinder- Shake well- Than add 10 mL ether solution in it and shake well- If sample is rancid it will give red color the test is positive otherwise negative.

SOAP TEST

For refined oil

REAGENTS:-Distill water-Phenolphthalene indicator

EQUIPMENT:-Beaker-Hot plate

PROCEDURE:- Take a beaker.- Add distill water plus phenolphthalene.

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- Heat it than add sample in it.- Oil will goes to top and water at the bottom.- If bottom is pink than it means soap is present and if white than it means the soap is not present.

PEROXIDE TEST / POV

For refined oilThis test is performed to check the oxidation.

PRINCIPLE:Treatment of test portion,solved in a mixture of acetic acid and dichloromethane with an aqueous solution of KI.Tritrate liberated iodide with standardized solution of sodium thiosulphate solution.

REAGENTS:-Acetic + Chloroform solution-KI (saturated)-Distill water-Starch indicator-Na-thiosulphate

EQUIPMENT:-Conical flask-Cylinder-Burette

PROCEDURE:- Take 10g of sample in flask and add 60mL acetic solution + chloroform solution (60% +

40%). - Than add 1mL of potassium iodide solution (saturated solution).- After shaking it well put this flask in dark place for 1 minutes - Now add 60mL of distill water and shake it well- Now add few drops of starch (indicator solution).- If the color of sample does not change POV consider to be nill.- If the color changes to dark than tritrate it against 0.1 N solution of Na-thiosulphate- End point white color - Blank tritration is also performed- Standard POV value is 1.5 – 2.

Calculation;

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mL of Na-thiosulphate used × N × 1000 wt. of sample

VITAMINS TEST

For refined oil

REAGENTS:-Antimony trichloride

EQUIPMENT:-Test tube-Test tube holder

PROCEDURE:- Take the sample after refining in beaker- Add Antimony trichloride in it - If it settle down with blue color it means vitamins are present in the oil- If settle down with no color or other colour than blue it means vitamins are absent.

REFRACTIVE INDEX

INSTRUMENT:Refractometer

PRINCIPLE:The refractive index of liquid fat & oil sample is measured by means of suitable refractometer at costant temperature and using monochromatic light source,emitting monochromatic light by means of sodium vapour lamp.

PROCEDURE:- Circulate water in Abbe’s refractometer and note the temperature.- Place a drop of fat or oil on the glass prism

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- Close and take reading on scale- Make correction with the help of chart provided for correction.

SAPONIFICATION VALUE

For crude oil

PRINCIPLE:Boiling the sample with ethanolic KOH in reflux condenser.Tritrating the excess KOH with standard solution of HCl.

REAGENTS:-Alcoholic potash-0.5N HCl-Phenolphthalene indicator

EQUIPMENT:-Conical flask-Burette-Water bath -Hot plate-Condenser

PROCEDURE:- Take 5g of sample in dried conical flask.- Add 50mL of 0.5 N alcoholic potash.- Sponify it for 1 hours under condenser.- Cool it and tritrate it against 0.5 N HCl using phenolphthalene indiator.- Also perform blank tritration- Calculate by using the formula

Wt. of sample = 5gSample reading = 24mLBlank tritration reading = 10mLDifference = 14 mLSp. Value = 56.1 × N of HCl × tritration reading

Wt. of sample

= 56.1 × 0.5 × 145

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= 78.54

IODINE VALUE

For crude and refined oil

PRINCIPLE:The product to be investigated is treated with an iodide monochloride solution.After addition of halogen has taken place,the excess of iodine monochloride is determined by tritration with Na-thiosulphate.REAGENTS:-KI solution-Carbon tetrachloride-Iodine monochloride-N/10 Na-thiosulphate-Starch indicator

PROCEDURE:- Take 0.25g sample in a flask. - Add 10mL carbon tetrachloride and 20mL iodine monochloride solutions.- Cover the flask with stopper moistened with 10% KI solution.- Allow the flask to stand in dark place.- After a period of 30 min. add 15ml of 10% KI solution,washing the stopper and sides of

flask with 100mL distilled water.- Tritrate the contents with N/10 Na2S2O3 using starch indiator- Note the volume of Na2S2O3

- Also perform blank tritrationCaculation:

Iodine value = (b-a) 0.01269 ×100 Wt. of sample

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WATER ANALYSIS

HARDNESS

REAGENTS:-Erichrome black T (indicator)-0.01N EDTA or tritriplex-Buffer solution (Ammonia)

EQUIPMENT:-Beaker-Burette-Pipitte filler

PROCEDURE:- Take 100mL water in a beaker- Add 3mL buffer solution to maintain the pH of water- Now add few drops of Erichrome black T- If the color will purple it means no hardness in water- If color will other than purple it means hardness is present- Than tritate it against 0.01N EDTA till purple color obtain

Calculate the hardness as; mL of EDTA used × 10 = (hardness) ppm

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SOLUTION PREPARATION

PREPARATION OF STARCH INDICATOR SOLUTION

PRINCIPLE

Starch solution is prepared by dissolving the starch in distilled water

SCOPE

This procedure is applicable for preparation of 1% starch indicator solution.

EQUIPMENTS

Balance analyticalSuitable means of mechanical agitation.Beaker, 250 mL.Flask volumetric ,100 mL capacityFunnel

REAGENTS

Starch Distilled water

PROCEDURE-Weigh 1g starch and transfer in a 250 mL beaker.-Dissolve the starch (solution) from beaker to 100 mL volumetric flask.-Transfer the dissolved starch (solution) from beaker to 100 mL volumetric flask.-Rinse the beaker thoroughly with distilled water and transfer in to volumetric flask.-Make-up the volume with distilled water up to 100 mL mark.Cover and manually shake the flask to mix the solution thoroughly.-Transfer the solution to an appropriately labeled reagent bottle.

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PREPARATION OF SATURATED POTASSIUM IODIDE SOLUTION

PRINCIPLE

Potassium Iodide solution is prepared by dissolving the potassium iodide crystals in distilled water up to saturation point.

SCOPE

This procedure is applicable for the preparation of saturated Potassium iodide solution.

EQUIPMENTSBalanceSuitable means of mechanical agitation.Beaker, 250 mL.

REAGENTSPotassium iodide crystals.Distilled water.

PROCEDURE-Weigh 100 g of Potassium iodide crystals and transfer in a 250 mL beaker containing 100 mL of distilled water.-Dissolve the potassium iodide crystals in distilled water by using the magnetic stirrer.-If no sedimentation is observed at bottom of the beaker, add more potassium iodide crystals.-Stir the solution constantly and make sure that about half inch layer of potassium iodide crystals have been deposited at the bottom of beaker. It indicates the saturation of solution.-Transfer the solution to an appropriately labeled reagent bottle.

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PREPARATION OF PHENOLPTHALEIN INDICATOR SOLUTION

FORMULA

C20H14O4

PRINCIPLE

Phenolphthalein solution is prepared by dissolving the phenolphthalein in ethanol.

SCOPE

This procedure is applicable for the preparation of 2% phenolphthalein indicator solution.

EQUIPMENTSBalance analyticalSuitable means of mechanical agitationSpatulaBeaker, 250mLFlask volumetric,1000 mL capacityFunnel

REAGENTSPhenolphthaleinEthanol

PROCEDURE-Weigh 20 g of Phenolphthalein and transfer in a 250 mL beaker.-Dissolve the phenolphthalein in ethanol by using the magnetic

stirrer.-Transfer the dissolved phenolphthalein (solution) from beaker to 1000 mL volumetric flask.

-Rinse the beaker thoroughly with ethanol and transfer in to volumetric flask.

-Make-up the Volume with Ethanol up to 1000 mL mark. Cover and manually shake the flask to mix the solution thoroughly.

-Transfer the solution to an appropriately labeled amber reagent bottle

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PREPARATION OF ACETIC-CHLOROFORM SOLUTION

PRINCIPLE

Acetic acid-chloroform solution is prepared by mixing glacial acetic acid and chloroform.

SCOPE

This procedure is applicable for the preparation of 60:40 acetic acid-chloroform solution.

EQUIPMENTS

Graduated cylinder,1000mL.

REAGENTS

Glacial acetic acid

Chloroform

PROCEDURE

-Accurately measure 400mL of chloroform by a graduated cylinder and transfer to amber reagent bottle-Then accurately measure 600 mL of glacial acetic acid by a graduated cylinder and transfer reagentbottle already containing choloroform.-Mix the contents of bottle well.

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PREPARATION & STANDARDIZATION OF SODIUM HYDROXIDE

PRINCIPLE

Sodium hydroxide solution is prepared by dissolving the sodium hydroxide in distilled water and standardized by titrating it against 0.1N potassium hydrogen phthalate solution to the pink color end point

SCOPE

This procedure is applicable for the preparation and standardization of 0.1N solution of sodium hydroxide.

EQUIPMENTSBalance analyticalDissecatorSuitable means of mechanical agitationSpatulaBeaker, 250 mL, 1000 mL capacityBuette, 50 mLFlask volumetric, 1000 mL capacityFunnelCyinder, 100 mLPipette, 25 mL

REAGENTSSodium-hydroxide (NaOH) pelletsPotassium hydrogen phthalate solution, 0.1NPhenolphthalein (2.0%) Indicator solution.Distilled water

PROCEDURE-Weigh 4.3 g of sodium hydroxide pellets and transfer in a beaker.-Dissolve the sodium hydroxide pellets with distilled water by using the magnetic stirrer.-Transfer the dissolved pellets (solution) from beaker to 1000 mL volumetric flask.-Rinse the beaker thoroughly with distilled water and transfer into volumetric flask.-Make-up the volume with distilled water up to 1000 mL mark.Cover and manually shake the flask to mix the solution thoroughly.-Transfer the solution to an appropriately labeled reagent bottle.-Filter and standardized the clean solution.

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STANDARDIZATION

-Take 25 mL of 0.1N potassium hydrogen phthalate solution with the 25mL pipette in a 250 mL beaker.-Add 100 mL distilled water and Stir it manually or with magnetic stirrer.-Add approximately 1.0 mL of phenolphthalein indicator.-Titrate with sodium hydroxide solution with constant stirring to light pink end point.-Record the “mL” used of sodium hydroxide solution.

CALCULATION

Normality (N) = Normality of KHP x mL used of KHP mL used of NaOH

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PREPARATION & STANDARDIZATION OF SODIUMTHIOSULPHATE

PRINCIPLE

Sodium thiosulphate solution is prepared by dissolving Sodium Thiosulphate & Sodium carbonate in distilled water and standardized by titrating it against 0.1N potassium dicheomate solution to the colorless end point.

SCOPE

This procedure is applicable to prepare and standardize 0.1N Sodium Thiosulphate solution.

EQUIPMENTSBalanceDissectorSuitable means of mechanical agitationSpatulaBeaker, 250mL,1000 mL capacityBurette, 5-mlFlask volumetric,1000 mL capacityFunnelCuliner, 100 mLPippette, 25mL

REAGENTSSodium thiosulphateSodium carbonatePotassium dichromateHydrochloric Acid, ConcentratedPotassium Iodide solution, SaturatedStarch indicator solutionDistilled water

PROCEDURE-Weigh 25.5 g of Na2 S2 O3. 5H2O and 0.17 g Na2 CO3 and transfer in a beaker. -Dissolve it with distilled water by using the magnetic strirer.-Transfer the dissolved pellets (solution) from beaker to 1000 mL volumetric flask.-Rinse the beaker thoroughly with distilled water and transfer in to volumetric flask. -Make-up the volume with distilled water up to 1000 mL mark. - Cover and manually shake the flask to mix the solution thoroughly. -Transfer the solution to an appropriately labeled amber reagent bottle.-Standardized the solution.

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STANDARDIZATION

-Take 25mL of Potassium dichromate solution (0.1N) with the 25mL pipette in a 250 mL beaker.-Add 5 mL of concentrated Hydrochloric acid solution and stir it manually or with magnetic stirrer.-Add 2 mL of saturated Potassium iodide solution.-Titrate it against 0.1N Sodium thiosulphate solution till pale yellow color.-Add approximately 1.0 mL of starch indicator solution as an indicator and continue titration till colorless end point.-Record the “mL” used of Sodium thiosulphate solution.

CALCULATION

Normality (N) = mL taken of Potassium dichromate1000xmL used of Sodium thiosulphate x0.04

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PREPARATION OF POTASSIUM HYDROGEN PHTHALATEFORMULA

C8H5KO4

PRINCIPLE

Potassium hydrogen phthalate solution is prepared by dissolving the dried potassium hydrogen phthalate in distilled hot water (60 0C) and cooling it to room temperature.

SCOPE

This procedure is applicable for the preparation of potassium hydrogen phthalate solution.EQUIPMENTS

Oven Balance, analyticalDessicatorSuitable means of mechanical agitationBeaker, 250 mL, 1000 mL capacityFlask volumetic, 1000 mL capacityFunnelSpatulaCylinder, 100 mL

REAGENTSPotassium hydrogen phthalate (KHP)Distilled water

PROCEDURE-Dry the potassium hydrogen phthalate (KHP) at 120 0C in oven for 2 hours.-Cool it in the dessicator for 30 minutes.

-Accurately weigh 20.422 g of Potassium hydrogen phthalate and transfer to 1000 ml volumetric flask.-Add 600 mL hot (60 C) distilled water in the flask containing KHP and shake it well.-When it dissolved properly, allow to cool at room temperature.-Make-up the volume with distilled water up to 1000 mL mark. -Cover and manually shake the flask to mix the solution thoroughly.-Transfer the solution to an appropriately labeled amber reagent bottle

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