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cement

Physical Test

Setting Time
Compressive Strength
Specific Gravity
Fineness of Cement (By Dry Sieving)
Blains Fineness

Chemical Test

LOI (Loss on Ignition)
Silica
Combind Ferric Oxide & Alumina
Ferric Oxide Fe₂O₃ (Pottasium Permegnate Method)
Magnesium Oxide (EDTA Method)
Sulphor Tri-Oxide
Insoluble Residue
Sodium Oxide & Pottasium Oxide

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NORMAL CONSISTENCY & INITIAL / FINAL SETTING TIME

OBSERVATION:
To Determine the Normal consistency & Initial / Final Setting time of the cement.
APPARATUS REQUIRED:

Vicat apparatus as per IS –5513 – 1976 1No.
Digital Balance accurate to 1gm. 1No.
Measuring Cylinder 150 & 100ml s 1No
Vicat Mould (Height 40mm) & top dia 70mm, 1No.
Stopwatch 1No.
Room thermometer 1No.
Gauging trowel 1No.
Humidity Chamber 1No.

APPARATUS OPERATING PROCEDURE:
As per Apparatus Operating Manual (File No.: B22)

ACCESSORIES:

G.I Tray (Size: 300cm X 250cm X 56cm)                  1No
Gauging Trowel                                                        2No.
Normal Tray                                                             2No.

STANDARDS USED:
IS – 4031 (Part 5) – 1988

other reference STANDARDS:
IS – 3535 – 1986, IS – 5513-1976

EQUIPMENTS REQUIRING CALIBRATION:

Vicat mould
Digital Balance
Measuring Cylinder
Stop Watch
Room Thermometer

MINIMUM Quentity OF SAMPLE REQUIRED:
At least 10kg.

ENVIRONMENTAL CONDITIONS REQUIRED FOR TESTING:
Room Temperature should maintain at 27oC+-2 oC & Relative Humidity 65+-5% at the time of mixing & storing of cement & water. Moist room or chamber should maintain at 27oC+-2 oC & Relative Humidity 90% for Initial & Final setting time.

METHOD OF TEST:
Normal Consistency

Take 400gm of cement sample & add suitable amount of water and mix it very well in the tray. The time of gauging should not be less then 3 minutes & preparation of sample within 5 minutes.
Fill the sample up to the top level of the Vicat mould. And put it on the vicat apparatus.
Now check its normal consistency with the help of Vicat Needle. Note down the reading.
Repeat the test until & unless you get reading 5 to 7 from bottom or 35 to 33 from top.
Calculate the Normal consistency by using following formula.

Initial & Final Setting Time

Prepare a cement paste by gauging the cement with 0.85 time of the Normal consistency.
The time of mixing cement should not be less then 3minutes & 5min for preparation of test specimen. Fill the cement paste in Vicat mould resting on non-porous plate. Vibrate the mould by hand to remove air bubbles from cement paste & level the top surface by using gauging trowel.
Now check its initial setting time with the help of initial setting time needle and check final setting time with the help of final setting time needle at every 10-to15 min.

SPECIAL CARE TO BE TAKEN:
Clean apparatus shall use for every test.
Needle should be straight while testing.
All the apparatus shall free from vibration during test.
DO’S & DON’TS:
Do not vibrate the mould in mean time of the test.
Air bubbles shall remove before actual testing starting.
Time start at the time of water adding in the cement
OBSERVATION:
Observations should recorded in observation format QMS/QFT/QCL/203/00
CALCULATION:
The Normal Consistency in % = (Total weight of water / Total weight of cement) X100
Time of the initial setting is that the reading measuring 5 to 7 from bottom & Final setting is that the needle makes an impression on the surface of the test specimen while the attachment fails to do so.
Associated Software For Calculation & Report:
Calculator
Computer QC1, QC2, QC3.
REPORT:
Normal Consistency of the cement shall be reported to the nearest two points.
Initial & Final setting time shall be reported to the nearest five minutes.

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COMPRESSIVE STRENGTH

OBSERVATION:
To determine the compressive strength of cement.

APPARATUS REQUIRED:

Vibration Machine 1No.
Poking rod 1No.
Cube mould (7.06X7.06cm) 9 Nos
Gauging trowel 2Nos.
Digital balance 1200gm 1Nos.
Graduated glass cylinder 1Nos.
Standard Sand grade I, II & III 1800 gm each
Stop Watch 1No
Room Thermometer 1No

APPARATUS OPERATING PROCEDURE:
As per Apparatus Operating Manual (File No.: 22)

ACCESSORIES:

Mixing tray 1Nos.

STANDARDS USED:
IS – 4031 (Part 6) – 1988

OTHER REFERENCE STANDARDS:

EQUIPMENTS REQUIRING CALIBRATION:

Vibration Machine
Digital balance 1200gm
Graduated glass cylinder
Stop Watch
Room Thermometer

MINIMUM SIZE OF SAMPLE REQUIRED:
At least 10 kg (shall be packed in airtight container)

ENVIRONMENTAL CONDITIONS REQUIRED FOR TESTING:
27 ± 2 º C & RH 65 ± 5 % for molding room and 27 ± 2 º C & RH 90% for moist closet or moist room.

METHOD OF TEST:
MIX PROPORTION of test specimen:
Clean appliances shall be used for mixing and the temperature of water and that of the test room at the time when the above operations are being performed shall be 27± 2ºC.
Distilled water shall be used in preparing the cubes.
The material for each cube shall be mixed separately and the quantity of cement, standard sand and water shall be as follows:
Cement = 200gm.
Standard sand = 600gram (200 gm each)
The quantity of water = (P /4 + 3) X 8 ml
Where: P is the Normal Consistency of cement.

MOULDING SPECIMEN:

Place on a nonporous plate, a mixture of cement and standard sand. Mix it dry with a trowel for one minute and then with water until the mixture is of uniform Colour.
The time of mixing shall in any event be not less than 3min.
Place the assembled mould on the table of the vibration machine and hold it firmly in position by means of a suitable size and securely at the top of the mould to facilitate filling and this hopper shall not be removed until the completion of the vibration period at least 2 minutes.
The period of vibration shall be two minutes at the specified speed of 12000 ± 400 vibrations per minute.
At the end of vibration, remove the mould together with the base plate from the machine and finish the top surface of the cube in the mould by smoothing the surface with the blade of trowel.
Keep the filled moulds in moist closet or moist room for 24hour after completion of vibration.
Open the cube mould after 24 hours and immersed in curing tank.
At the end of that period keep it on the curing tank for 3days, 7days and 28 days.
Check the dimension and weight of each cube before test
Test the specimen for compressive strength on the machine, which comply to specification.

SPECIAL CARE TO BE TAKEN:
Check the vibrating machine for proper electric supply, earthling etc.
Room temperature and humidity shall be maintained during the process.

DO’S & DON’TS:
Use rubber globs while mixing.
Care shall be taken that no mix should spill out during process.

OBSERVATION:
Observation shall be record in observation format no. QMS/QFT/QCL/0203/00

CALCULATION:
Maximum load (kgf)
Compressive strength (kgf / cm2) =
Surface area of Specimen (cm2)

Associated Software For Calculation & Report:
Calculator
Computer QC1, QC2, QC3.

REPORT:
Report the result of average of three cubes to round of the numerical value.

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SPECIFIC GRAVITY TEST

OBJECTIVE:
TO DETERMINE THE DENSITY OF THE HYDRAULIC CEMENT.

APPARATUS REQUIRED:

Le-Chatelier Flask 1No.
Digital Balance capable of weighing up to 10 gm with 10mg accuracy. 1No.
Constant Temperature Bath 1No.

APPARATUS OPERATING PROCEDURE:
As per Apparatus Operating Manual (File No.: B22)

ACCESSORIES:
Kerosene fee from water 1Lit Approx.

STANDARDS USED:
IS – 4031 (Part- 11) – 1996

other reference STANDARDS:
IS – 460-1985

EQUIPMENTS REQUIRING CALIBRATION:
Digital Balance
Le-chatelier Flask
Constant Bath

MINIMUM SIZE OF SAMPLE REQUIRED:
At least 100gm.of cement sample.

ENVIRONMENTAL CONDITIONS REQUIRED FOR TESTING:
Room Temperature should maintain at 27oC+-2 oC & Relative Humidity 65+-5%.

METHOD OF TEST:
Filled the flask with water free kerosene or naphtha between 0 and 1 mark and place the flask in constant water bath for settlement the level.
Weigh about 64 gm Portland cement introduced in the flask by thin steel rod.
In the mean time flask should be shake to prevent the cement sticking to the neck.
The flask should be rolled in an inclined position or gently whirled in horizontal circle to free the cement from air until no further air bubble rise to the surface
Stopper the flask after introducing whole cent in the flask.
After adding the proper amount cement the level of liquid will be in final position at some point of upper graduation.
Immersed the flask in water bath for sufficient time at room temperature till the temperature of flask is equal to water in the bath.
Record the reading on upper graduation.

DO’S & DON’TS:

OBSERVATION:
Observations should recorded in observation format QMS/QFT/QCL/203/00

CALCULATION:
The difference between the first and final reading represents the volume of liquid displaced by mass of cement used in the test.

Density = Mass of cement in gms
Displaced volume in cm2

Associated Software For Calculation & Report:
Calculator
Computer QC1, QC2, QC3.

REPORT:
Density of cement sample shall be reported to the nearest two decimal points.

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(OPC, SLAG, PPC) & Pozzalanic Material FINENESS

OBJECTIVE:
To determine the fineness of the cement by dry sieving.

APPARATUS REQUIRED:

Test sieve 90 microns with lid and pan 1No.
Digital Balance capable of weighing up to 10 gm with 10mg accuracy. 1No.
Nylon brush 1No.

APPARATUS OPERATING PROCEDURE:
As per Apparatus Operating Manual (File No.: B22)

ACCESSORIES:
Enamel Tray 1No.

STANDARDS USED:
IS – 4031 (Part 1) – 1996

other reference STANDARDS:
IS – 460-1985

EQUIPMENTS REQUIRING CALIBRATION:
Digital Balance
IS Sieve

MINIMUM SIZE OF SAMPLE REQUIRED:
At least 500gm.for minimum three test.

ENVIRONMENTAL CONDITIONS REQUIRED FOR TESTING:
Room Temperature should maintain at 27oC+-2 oC & Relative Humidity 65+-5%.

METHOD OF TEST:
Take 100gm of cement sample in a stoppered jar or bottle to disperse agglomerates for 2 minute, wait for 2 minutes & stir the resulting powder gently using a clean dry glass rod in order to distribute the fines through out the cement.
Weigh about 100 gm of specimen to nearest .01 gm R1
Transfer the above sample in IS Sieve No-9 and sieve using lid and pan until no further particle pass through it.
Transfer the fraction retain in the tray and weigh to nearest .01 gm. R2
Take another 100 gm from the same sample and repeat the procedure described as above.
The mean of the two reading is expressed as % fineness nearest to 0.1 %
If the result differs by more than 1 percent repeat the test for third specimen as same procedures.
The mean of the three reading is expressed as % fineness nearest to 0.1 %

DO’S & DON’TS:
Check sieves after every 100 sieving.
Do not use wire brush for cleaning the sieves.
Do not use wet jar, bottle and glass rod for dispersing the sample.

OBSERVATION:
Observations should recorded in observation format QMS/QFT/QCL/0

CALCULATION:
Fineness by 90-Microns = (r1-R2)/(r2) X100

Associated Software For Calculation & Report:
Calculator
Computer QC1, QC2, QC3.

REPORT:
Report the value of fineness nearest to 0.1 %, as the residue on the 90-micron sieve for the cement tested.

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FINENESS BY BLAIN AIR PERMEABILITY

OBJECTIVE:
TO DETERMINE THE FINENESS OF THE CEMENT BY BLAIN AIR PERMEABILITY METHOD.

APPARATUS REQUIRED:

Blain Air Permeability apparatus with Permeability cell 1No.
Digital Balance capable of weighing up to 3 gm with 1mg accuracy. 1No.
Le- Chatelier flask 1No.
Stop Watch capable to read 0.2 second 1No.
Wet and Dry Bulb Thermometer 1No. Each

APPARATUS OPERATING PROCEDURE:
As per Apparatus Operating Manual (File No.: B22)

ACCESSORIES:
Mercury
Reference Cement
Filter Paper

STANDARDS USED:
IS – 4031 (Part 2) – 1999

other reference STANDARDS:
IS – 5516

EQUIPMENTS REQUIRING CALIBRATION:

Blain Air Permeability apparatus with Permeability cell
Digital Balance capable of weighing up to 3 gm with 1mg accuracy.
Le- Chatelier flask
Stop Watch capable to read 0.2 second
Wet and Dry Bulb Thermometer

MINIMUM quentity of SAMPLE REQUIRED:
At least 100gm.of cement sample.

ENVIRONMENTAL CONDITIONS REQUIRED FOR TESTING:
Room Temperature should maintain at 27oC+-2 oC & Relative Humidity 65+-5%.

METHOD OF TEST:
Take 2.8 gm of standard cement of known specific surface as describe in IS 1727-1967 t the accuracy of 1 mg.
Place the perforated disc on the ledge at the bottom of the cell and place on it a new filtered paper ensuring that the perforated plate is fully covered by it and flat by pressing with clean dry rod.
Tap the cell to level the cement, place the second filtered paper on the leveled cement.
Insert the plunger to make contact with the filter paper disc.
Press the plunger gently but firmly until the lower face of the cap is in contact with the cell.
Slowly withdraw the plunger about 5mm, rotate it through 90º and press the bed once again until the plunger cap is in contact with the cell. Lowly withdraw the plunger.
Insert the conical surface of the cell into the socket of the manometer using a little light grease to ensure an airtight contact. Care shall be taken that it should not disturb the bed.
Open the stopcock and raise the level of liquid in manometer by gentle aspiration to the highest etched line.
Close the stopcock and observed that the level of liquid in manometer is constant.
In case leak remake the cell manometer joint and check the stopcock.
Close the stopcock the level of manometer liquid will begin to flow, Start the timer as the liquid reaches second etch line and stop it when it reach the third etched line.
Record the time, repeat the procedure on the same bed and record the reading.
Record the temperature and humidity.
Take the average of two reading as the time taken.
Take 100gm of cement (OPC) sample to be tested for fineness in a stoppered jar or bottle to disperse agglomerates for 2 minute, wait 2 minutes stir the resulting powder gently using a clean dry glass rod in order to distribute the fines through out the cement.
Weigh 2.80 gm to the accuracy of 1 mg and repeat the procedure.

TO DETERMINE THE SPECIFIC SURFACE OF SLAG CEMENT, PPC & POZZOLANIC MATERIAL (EXCEPT SILICA FUME), WHO’S DENSITY IS LOWER THAN THE OPC CEMENT AS BELOW:

Determine the density of cement using Le-chatelier device using non-reactive liquid as describe in MECH-CEM-004.
Determine the Volume of bed using 2.80 gm of standard cement.
Determine the mass of cement for making cement bed, m=  V (1-e) where e is the porosity and considered 0.500.
Volume can be determine calibrating with mercury as follows:
Make the cement bed as mentioned above, place two fresh filtered paper disc in contact of the bed. Fill with mercury taking care that there shall not be any air void.
Remove the mercury above the cement bed and weigh to nearest 10 mg. M3
Remove the cement bed, place the perforated plate on cell with two fresh filter paper disc taking care that the base of the cell shall be covered fully whilst lying flat by placing with a rod.
Fill the cell fully with mercury remove any air bubbles with the clear dry rod. Ensure that the same is full by placing the glass plate in the mercury surface until it flushes with the cell top.
Empty the cell; weight the mercury to nearest 10 mg. M2.

DO’S & DON’TS:
Care shall be taken that the mercury shall not come in contact with the skin and eyes of the operator..
Do not use wet jar, bottle and glass rod for dispersing the sample.

OBSERVATION:
Observations should recorded in observation format QMS/QFT/QCL/0203/00

CALCULATION:
Specific Surface at 27  2 C
Constant factor = Specific Surface of Reference Cement /  t
Specific Surface of unknown sample = Constant factor x  t
Or

S = (521.08K  t)

Apparatus constant K can be determine from the density and specific surface and time taken of reference cement.

Where:

S = Specific Surface
K = is the apparatus constant
T = Time in seconds
 = Density of cement

Associated Software For Calculation & Report:
Calculator
Computer QC1, QC2, QC3.

REPORT:
Report the value of fineness of cement rounding of the numerical value M2/Kg

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Chemical Analysis of Cement:

OBJECTIVE:
Determination Of Chemical analysis of Hydrolic Cement.

APPARATUS REQUIRED:
APPARATUS QUANTITY
Analytical Balance
Drying Oven
Hot Plate
Flame Photometer
Fuming Chamber
Platinum Crucible
Silica Crucible
Burette- 50ml 2Nos.
Pipette-25ml 2Nos.
Beaker’s-500ml 2Nos.
Beaker’s-400ml 4Nos.
Beaker’s-250ml 4Nos.
Beaker’s-100ml 4Nos.
Volumetric Flask-250ml 2Nos.
Volumetric Flask-100ml 4Nos.
Conical Flask-250ml 4Nos.
Watch Glass
Evaporating Dish
Glass Rods
Finnel-100mm Dia 4Nos.
Funnel Stand 4Nos.
Filter Paper – 40No. 41No. 42 Nos.

Reagents
Hydrochloric Acid –Conc.
Nitric Acid – Conc.
Sulphuric Acid- Conc.
Orthophosphoric Acid- Conc.
Hydrofluoric Acid – 40%
Ammonium Hydroxide
Acetic Acid-Glacial
Diethyl amine – Liquid
Hydrochloric Acid – 1:1,1:3,1:10 and 1:99 (By Volume)
Nitric Acid – 1:4, 1:33 (By Volume)
Sulphuric Acid – 1:3 (By Volume)
Phosphoric Acid- 1:3(By Volume)
Sodium Hydroxide Solution- 4N- dissolves 80gm of sodium hydroxide in 500ml volumetric flask.
Glycerol – 1:21
Ammonium Acetate – 50%
Stannous Chloride- 5% - Dissolve 5gm of Sncl2 in 2.5ml hydrochloric acid and dilute to 100ml
Mercuric Chloride solutions – 5.6%- prepare a 5.6gm of mercuric chloride in 100ml-distilled water.
Manganese Sulphate Solution – Dissolve 35gm of manganese sulphate (MnSo4 7H2O) in 250ml of water. Add 70ml orthophosphate acid and 65ml Sulphuric acid. Dilute to 500ml
Standard Potassium Permanganate solution- 0.05N- dissolves about1.5kg of potassium permanganate (KmNo4) in one Litre of distilled water and standardizing with sodium oxalate.
Barium Chloride Solution-10% - dissolve 100gm barium chloride (Bacl2 2H2O) in one Litre distilled water.
Methyl Red- Indicator
Buffer Solution- Ph10- dissolve 70gm of ammonium chloride in 570ml of ammonium hydroxide and make up to one liter with distilled water.
Standard Zinc Solution - 0.01M – Dissolve 0.6537gm of zinc in dilute hydrochloric acid (1:1) make up 1litre to the mark with distilled water.
Standard EDTA Solution – 0.01M, dissolved 3.7224 gm of EDTA in 400ml hot water and make up to the volume in one Litre. Take 10ml of standard zinc solution add 20ml buffer solution of Ph 10 and warm up to 50 to 60C. Add 50mg Erichrome black T indicator and titrate with EDTA till the Colour changes from wine red to clear blue and calculate the morality of EDTA solution.
Erichrome Black T Indicator
Patton –Readers Indicators
Thymol Blue Indicator
Ammonium Nitrate Indicator

Interference

APPARATUS OPERATING PROCEDURE:
As per Apparatus Operating Manual (File No.: )

ACCESSORIES:

STANDARDS USED:
IS – 4032- 1985

OTHER REFERENCE STANDARDS:

EQUIPMENTS REQUIRING CALIBRATION

MINIMUM SIZE OF SAMPLE REQUIRED:
100gram
SAMPLING
The representative sample of the cement thoroughly mixed before using.

environmental conditions required for testing:
METHOD OF TEst
Loss on Ignition-
Take empty crucible weight.
Take 1gm of cement sample in silica crucible (W1)
The crucible place in muffle furnace at temperature 900C to 1000C for 1 hour.
After one hour remove the crucible and cool in Dessicator.
Weigh the crucible and note down the difference of initial weight to final weight (W2).
% Loss of Ignition = W1 – W2 X 100
Or % Loss of Ignition= Loss in Weight X 100

Silica –
Take 0.5gm of cement sample in evaporating dish, add 5-10ml conc. Hcl, Digest the sample of gentle heat and completely dissolved. Dissolved with light pressure flat glass rod.
Evaporate the solution to dryness on hot plate. Add 10-20ml of (1:1) hydrochloric acid and warm heat on hot plate for 10minutes.
Dilute the solution 10-20ml of hot distilled water.
Filter the solution through Whatman No 41 and wash the spectral silica with hot distilled water.
Reserve the filtrates for the determination of combined Alumina and ferric oxide.
Transfer the silica residue in weighed platinum crucible, dry and ignite the paper in low heat temperature until the carbon of filter paper completely burn without inflaming.
Keep the crucible in muffle furnace at 1100C to 1150C for 35-45minutes.
Remove the crucible and cool in Dessicator and weighed residue.
The silica residue contain small amount of impurities. Add 1-2ml D.W. 1-2ml of hydrofluoric acid and 2drops of Sulphuric acid and evaporate to dryness.
After dryness transfer the crucible in muffle furnace at 1050C - 1100C for 1-5minutes. Cool and weigh.

Silica (Sio2) % = 200 (W1 – W2)
W1= Weight of Silica Residue
W2= Weight of Impurities
Combined Ferric Oxide And Alumina –

To the reserved filterate (Volume 200ml) , add 5-10 drops of methyl red indicator and heat to boiling.
Add few drops bromine water or conc. Nitric acid and add ammonium hydroxide (1:1) drop by drop until the Colour of solution becomes yellow and smells of ammonia.
In boiling time appear the precipitates of Aluminum and ferric hydroxides.
Allow the precipitates to settle (not take more than 5-Minutes)
Filter the solution through Whatman No 41 and wash with 2% ammonium Nitrate solution and reserve the filtrate for CaO and MgO. Wash the residue up to removes complete impurities.
Transfer the precipitates in a weighed platinum crucible, slowly and charred the filter paper and Keep the furnace at 1050C to 1100C for 35 – 45 minutes.
Remove the crucible, cool in Dessicator and weigh as combined alumina and ferric oxide.
R2 O3 % = Weight of residue X 200
Al2 O3 % = R2 O3 % - Fe2 O3 %

If silica is suspected in the residue, add 1-2ml hydrofluoric acid and one drop of Sulphuric acid evaporate up to dryness.
Heat the crucible at 1050C - 1100C for 1-5minutes, Cool and weigh.
The difference between this weight and the weight previously obtained represent the amount of residual silica. Subtract this amount from the weight of ferric oxide and Alumina found.

Ferric Oxide (Fe2O3) Potassium Permanganate Method

Take one gm cement sample in 250ml beaker; add 40ml D.W and mixture stirred vigorously add 15ml of conc. Hydrochloric acid.
Heat the solution and grind the cement with flattened end of a glass rod.
Heat the solution to boiling, add drop bu drop starmous chloride until the solution is decolorized add a few drop of stannous chloride solution in excess and cool to room temperature.
Add 15ml mercuric chloride solution and 25ml manganese sulphate solution and titrate with standard potassium permanganate solution up to appear pink Colour.
Calculation – Fe2O3 = B.R x Number of KMNo4

Calcium Oxide (CaO) (EDTA Method)

Take 10ml from reserved solution in conical flask.
Add 10ml of 4N Sodium hydroxide solution and adjust pH 12or more, add 50ml-distilled water, add pinch paten – reddish solid indicator.
Titrate against 0.01M EDTA solutions to a sharp change in Colour from wine red to clear blue.
Calculation: - Calculate the percentage of CaO as below:
1ml of 0.01M EDTA = 0.5608 x mg of CaO

Calcium Oxide (CaO%) 0.5608 X 25 X BR / Volume of Sample

Magnesium Oxide: EDTA Method: 

Take 10ml from reserved solution in conical flask.
Add 20ml of buffer solution to Ph 10, add 50ml D.W. Erichrome black T indicator (Pintch) solid and shake well
Titrate against 0.01M EDTA until until the Colour changes from blue to clear pink.
Calculation: - Calculate the percentage of MgO as below.
Magnesium Oxide (MgO %) = 0.04032 X 25 X (V1-V) / Volume of sample
Where V1= Volume of EDTA used in this titration ml.
V = Volume of EDTA used in CaO determination in ml.

Sulphur Tri Oxide (So3) 
Take 1gm cement sample in 250ml beakers, add 25-30ml distilled water shake vigorously, add 5ml conc. Hcl
Grind the cement sample with flattened end of glass rod.
Digest the sample for 15-20 minutes.
Filter the solution thorough Whatman No 40 or 41 and wash the residue with hot water.
Dilute the filtrate about 250ml heat & boiling, add drop-by-drop hot barium chloride until the precipitate is formed.
Digest the solution for 4hour.
Filter the precipitate thoroughly Whatman No 42 and wash the filter paper up to remove complete impurities.
Transfer the residue in weighed crucible and slowly heat the paper without inflaming.
Ignite the residue to 800C to 900C for 30minutes. Remove the crucible, cool in Dessicator and weigh the barium sulphate obtained.
Calculation- calculate the percentage of So3 as follows-
Sulphurtrioxide (% So3 ) = W X 34.3

W= Weight of residue (BaSo4) in gm
34.3 = molecular ration of So3 to BaSo4 (0.343) multiplied by 100.
Insoluble residue: -

Digest the filter paper containing the residue from So3 add 25-30 ml hot water and 30ml of 2N sodium carbonate solution
The solution heat for 10minutes.
Filter the solution through Whatman No 40 and wash the residue with dilute Hcl and hot water till the residue is from chlorides
Transfer the residue in weighed crucible and ignite the residue 900 to 1000C for 30 minutes.
Remove the crucible cool in Dessicator and weigh the crucible.
Calculation –
% Insoluble residue = Residue weight X 100
Sodium Oxide and Potassium Oxide – ( By Flame photometer Method)

Preparation of Stock Solution – Sodium chloride and potassium chloride stock solution – dissolve 1.8858 gm of sodium chloride and 1.583 gm of potassium chloride (both dried at 105 to 110C ) in meter. Dilute to one litre in a volumetric flask. This solution equivalent of 1000 ppm (0.10%) each of sodium oxide and potassium oxide.
Standard Solution – Prepared the standard solution as out requirement

Table – Standard Solution
Standard solution number Concentration of Alkali as Na2o or K2o in standard solution
Ppm Volume of stock solution used
Nacl –Kcl
ml Final Volume of Solution
ml
1 100 200 2000
2 75 75 1000
3 50 50 1000
4 35 25 1000
5 10 10 1000
6 0 0 1000
7 100 100 1000

SPECIAL CARE TO BE TAKEN:
Procedure
Take 1.0gm of the cement sample in 250ml beaker, add 20ml-30ml of water with shaking add 5.0ml hydrochloric acid, dilute to 50ml with water.
Break up lumps of cement with glass rod, digest on the hot plate for 15minutes,
Filter the solution through Whatman Bo 41 in volumetric flask 100ml make the volume 100ml mix and cool the solution to room temperature
Determine the sodium oxide and potassium oxide value from flame photometer reading.
Calculate the % of Alkali expressed as Na2 O to the as below.
Total Alkali = A + E
A= B / W X 10
C= D/ WX 10
E=CX 0.658

Where A = % of sodium oxide
W= Weight of cement sample in gm
B= ppm of Na2O in the solution in the 100ml flask.
C= % of potassium oxide
D= ppm of K2O in the 100ml flask
E= % Na2O equivalent of the K2O
0.658= molecular ration of Na2O to K2O

TEST PROCEDURES

NORMAL CONSISTENCY & INITIAL / FINAL SETTING TIME

OBSERVATION:
To Determine the Normal consistency & Initial / Final Setting time of the cement.
APPARATUS REQUIRED:

1. Vicat apparatus as per IS –5513 – 1976	1No.
2. Digital Balance accurate to 1gm.	1No.
3. Measuring Cylinder 150 & 100ml	1No.
4. Vicat Mould (Height 40mm) & top dia 70mm,	1No.
5. Stopwatch	1No.
6. Room thermometer	1No.
7. Gauging trowel	1No.
8. Humidity Chamber	1No.

APPARATUS OPERATING PROCEDURE:
As per Apparatus Operating Manual (File No.: B22)
ACCESSORIES

G.I Tray (Size: 300cm X 250cm X 56cm)                    1No
Gauging Trowel                                                      2No.
Normal Tray                                                           2No.

STANDARDS USED:
IS – 4031 (Part 5) – 1988
other reference STANDARDS:
IS – 3535 – 1986, IS – 5513-1976
EQUIPMENTS REQUIRING CALIBRATION:

Vicat mould
Digital Balance
Measuring Cylinder
Stop Watch
Room Thermometer

MINIMUM Quentity OF SAMPLE REQUIRED:
At least 10kg.
ENVIRONMENTAL CONDITIONS REQUIRED FOR TESTING:
Room Temperature should maintain at 27oC+-2 oC & Relative Humidity 65+-5% at the time of mixing & storing of cement & water. Moist room or chamber should maintain at 27oC+-2 oC & Relative Humidity 90% for Initial & Final setting time.
METHOD OF TEST:
Normal Consistency

Take 400gm of cement sample & add suitable amount of water and mix it very well in the tray. The time of gauging should not be less then 3 minutes & preparation of sample within 5 minutes.
Fill the sample up to the top level of the Vicat mould. And put it on the vicat apparatus.
Now check its normal consistency with the help of Vicat Needle. Note down the reading.
Repeat the test until & unless you get reading 5 to 7 from bottom or 35 to 33 from top.
Calculate the Normal consistency by using following formula.

Initial & Final Setting Time

Prepare a cement paste by gauging the cement with 0.85 time of the Normal consistency.
The time of mixing cement should not be less then 3minutes & 5min for preparation of test specimen. Fill the cement paste in Vicat mould resting on non-porous plate. Vibrate the mould by hand to remove air bubbles from cement paste & level the top surface by using gauging trowel.
Now check its initial setting time with the help of initial setting time needle and check final setting time with the help of final setting time needle at every 10-to15 min.

SPECIAL CARE TO BE TAKEN:
Clean apparatus shall use for every test.
Needle should be straight while testing.
All the apparatus shall free from vibration during test.
DO’S & DON’TS:
Do not vibrate the mould in mean time of the test.
Air bubbles shall remove before actual testing starting.
Time start at the time of water adding in the cement
OBSERVATION:
Observations should recorded in observation format QMS/QFT/QCL/203/00
CALCULATION:
The Normal Consistency in % = (Total weight of water / Total weight of cement) X100
Time of the initial setting is that the reading measuring 5 to 7 from bottom & Final setting is that the needle makes an impression on the surface of the test specimen while the attachment fails to do so.
Associated Software For Calculation & Report:
Calculator
Computer QC1, QC2, QC3.
REPORT:
Normal Consistency of the cement shall be reported to the nearest two points.
Initial & Final setting time shall be reported to the nearest five minutes.

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COMPRESSIVE STRENGTH

OBSERVATION:
To determine the compressive strength of cement.

APPARATUS REQUIRED:

Vibration Machine	1No.
Poking rod	1No.
Cube mould (7.06X7.06cm	9No.
Gauging trowel	2No.
Digital balance 1200gm	1No.
Graduated glass cylinder	1No.
Standard Sand grade I, II & III	1800 gm each
Stop Watch	1No.
Room Thermometer	1No.

APPARATUS OPERATING PROCEDURE:
As per Apparatus Operating Manual (File No.: 22)
ACCESSORIES:

Mixing tray 1Nos.

STANDARDS USED:
IS – 4031 (Part 6) – 1988

OTHER REFERENCE STANDARDS:

EQUIPMENTS REQUIRING CALIBRATION:

Vibration Machine
Digital balance 1200gm
Graduated glass cylinder
Stop Watch
Room Thermometer

MINIMUM SIZE OF SAMPLE REQUIRED:
At least 10 kg (shall be packed in airtight container)
ENVIRONMENTAL CONDITIONS REQUIRED FOR TESTING:
27 ± 2 º C & RH 65 ± 5 % for molding room and 27 ± 2 º C & RH 90% for moist closet or moist room.
METHOD OF TEST:

Clean appliances shall be used for mixing and the temperature of water and that of the test room at the time when the above operations are being performed shall be 27± 2ºC.
Distilled water shall be used in preparing the cubes.
The material for each cube shall be mixed separately and the quantity of cement, standard sand and water shall be as follows:
Cement = 200gm.
Standard sand = 600gram (200 gm each)
The quantity of water = (P /4 + 3) X 8 ml
Where: P is the Normal Consistency of cement.

MIX PROPORTION of test specimen:

MOULDING SPECIMEN:

Place on a nonporous plate, a mixture of cement and standard sand. Mix it dry with a trowel for one minute and then with water until the mixture is of uniform Colour.
The time of mixing shall in any event be not less than 3min.
Place the assembled mould on the table of the vibration machine and hold it firmly in position by means of a suitable size and securely at the top of the mould to facilitate filling and this hopper shall not be removed until the completion of the vibration period at least 2 minutes.
The period of vibration shall be two minutes at the specified speed of 12000 ± 400 vibrations per minute.
At the end of vibration, remove the mould together with the base plate from the machine and finish the top surface of the cube in the mould by smoothing the surface with the blade of trowel.
Keep the filled moulds in moist closet or moist room for 24hour after completion of vibration.
Open the cube mould after 24 hours and immersed in curing tank.
At the end of that period keep it on the curing tank for 3days, 7days and 28 days.
Check the dimension and weight of each cube before test
Test the specimen for compressive strength on the machine, which comply to specification.

SPECIAL CARE TO BE TAKEN:
Check the vibrating machine for proper electric supply, earthling etc.
Room temperature and humidity shall be maintained during the process.
DO’S & DON’TS:
Use rubber globs while mixing.
Care shall be taken that no mix should spill out during process.
OBSERVATION:
Observation shall be record in observation format no. QMS/QFT/QCL/0203/00
CALCULATION:
Maximum load (kgf)
Compressive strength (kgf / cm2) =
Surface area of Specimen (cm2)
Associated Software For Calculation & Report:

Calculator
Computer QC1, QC2, QC3.

REPORT:
Report the result of average of three cubes to round of the numerical value.

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SPECIFIC GRAVITY TEST

OBJECTIVE:
TO DETERMINE THE DENSITY OF THE HYDRAULIC CEMENT.
APPARATUS REQUIRED:

Le-Chatelier Flask 1No.
Digital Balance capable of weighing up to 10 gm with 10mg accuracy. 1No.
Constant Temperature Bath 1No.

APPARATUS OPERATING PROCEDURE:
As per Apparatus Operating Manual (File No.: B22)
ACCESSORIES:
Kerosene fee from water 1Lit Approx.
STANDARDS USED:
IS – 4031 (Part- 11) – 1996
other reference STANDARDS:
IS – 460-1985
EQUIPMENTS REQUIRING CALIBRATION:
Digital Balance
Le-chatelier Flask
Constant Bath
MINIMUM SIZE OF SAMPLE REQUIRED:
At least 100gm.of cement sample.
ENVIRONMENTAL CONDITIONS REQUIRED FOR TESTING:
Room Temperature should maintain at 27oC+-2 oC & Relative Humidity 65+-5%.

METHOD OF TEST:

Filled the flask with water free kerosene or naphtha between 0 and 1 mark and place the flask in constant water bath for settlement the level.
Weigh about 64 gm Portland cement introduced in the flask by thin steel rod.
In the mean time flask should be shake to prevent the cement sticking to the neck.
The flask should be rolled in an inclined position or gently whirled in horizontal circle to free the cement from air until no further air bubble rise to the surface
Stopper the flask after introducing whole cent in the flask.
After adding the proper amount cement the level of liquid will be in final position at some point of upper graduation.
Immersed the flask in water bath for sufficient time at room temperature till the temperature of flask is equal to water in the bath.
Record the reading on upper graduation.

DO’S & DON’TS:
OBSERVATION:
Observations should recorded in observation format QMS/QFT/QCL/203/00
CALCULATION:
The difference between the first and final reading represents the volume of liquid displaced by mass of cement used in the test.

Density = Mass of cement in gms
Displaced volume in cm2

Associated Software For Calculation & Report:
3. Calculator
4. Computer QC1, QC2, QC3.
REPORT:
Density of cement sample shall be reported to the nearest two decimal points.

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(OPC, SLAG, PPC) & Pozzalanic Material FINENESS

OBJECTIVE:
To determine the fineness of the cement by dry sieving.
APPARATUS REQUIRED:

Test sieve 90 microns with lid and pan 1No.
Digital Balance capable of weighing up to 10 gm with 10mg accuracy. 1No.
Nylon brush 1No.

APPARATUS OPERATING PROCEDURE:
As per Apparatus Operating Manual (File No.: B22)
ACCESSORIES:
Enamel Tray 1No.
STANDARDS USED:
IS – 4031 (Part 1) – 1996
other reference STANDARDS:
IS – 460-1985
EQUIPMENTS REQUIRING CALIBRATION:
1. Digital Balance
2. IS Sieve
MINIMUM SIZE OF SAMPLE REQUIRED:
At least 500gm.for minimum three test.
ENVIRONMENTAL CONDITIONS REQUIRED FOR TESTING:
Room Temperature should maintain at 27oC+-2 oC & Relative Humidity 65+-5%.
METHOD OF TEST:

Take 100gm of cement sample in a stoppered jar or bottle to disperse agglomerates for 2 minute, wait for 2 minutes & stir the resulting powder gently using a clean dry glass rod in order to distribute the fines through out the cement.
Weigh about 100 gm of specimen to nearest .01 gm R1
Transfer the above sample in IS Sieve No-9 and sieve using lid and pan until no further particle pass through it.
Transfer the fraction retain in the tray and weigh to nearest .01 gm. R2
Take another 100 gm from the same sample and repeat the procedure described as above.
The mean of the two reading is expressed as % fineness nearest to 0.1 %
If the result differs by more than 1 percent repeat the test for third specimen as same procedures.
The mean of the three reading is expressed as % fineness nearest to 0.1 %

DO’S & DON’TS:
Check sieves after every 100 sieving.
Do not use wire brush for cleaning the sieves.
Do not use wet jar, bottle and glass rod for dispersing the sample.
OBSERVATION:
Observations should recorded in observation format QMS/QFT/QCL/0
CALCULATION:
Fineness by 90-Microns = (r1-R2)/(r2) X100
Associated Software For Calculation & Report:
Calculator
Computer QC1, QC2, QC3.
REPORT:
Report the value of fineness nearest to 0.1 %, as the residue on the 90-micron sieve for the cement tested.

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FINENESS BY BLAIN AIR PERMEABILITY

OBJECTIVE:
TO DETERMINE THE FINENESS OF THE CEMENT BY BLAIN AIR PERMEABILITY METHOD.
APPARATUS REQUIRED:

Blain Air Permeability apparatus with Permeability cell 1No.
Digital Balance capable of weighing up to 3 gm with 1mg accuracy. 1No.
Le- Chatelier flask 1No.
Stop Watch capable to read 0.2 second 1No.
Wet and Dry Bulb Thermometer 1No. Each

APPARATUS OPERATING PROCEDURE:
As per Apparatus Operating Manual (File No.: B22)

ACCESSORIES:

Mercury
Reference Cement
Filter Paper

STANDARDS USED:
IS – 4031 (Part 2) – 1999
other reference STANDARDS:
IS – 5516
EQUIPMENTS REQUIRING CALIBRATION :

Blain Air Permeability apparatus with Permeability cell
Digital Balance capable of weighing up to 3 gm with 1mg accuracy.
Le- Chatelier flask
Stop Watch capable to read 0.2 second
Wet and Dry Bulb Thermometer

MINIMUM quentity of SAMPLE REQUIRED:
At least 100gm.of cement sample.

ENVIRONMENTAL CONDITIONS REQUIRED FOR TESTING:
Room Temperature should maintain at 27oC+-2 oC & Relative Humidity 65+-5%.
METHOD OF TEST:

Take 2.8 gm of standard cement of known specific surface as describe in IS 1727-1967 t the accuracy of 1 mg.
Place the perforated disc on the ledge at the bottom of the cell and place on it a new filtered paper ensuring that the perforated plate is fully covered by it and flat by pressing with clean dry rod.
Tap the cell to level the cement, place the second filtered paper on the leveled cement.
Insert the plunger to make contact with the filter paper disc.
Press the plunger gently but firmly until the lower face of the cap is in contact with the cell.
Slowly withdraw the plunger about 5mm, rotate it through 90º and press the bed once again until the plunger cap is in contact with the cell. Lowly withdraw the plunger.
Insert the conical surface of the cell into the socket of the manometer using a little light grease to ensure an airtight contact. Care shall be taken that it should not disturb the bed.
Open the stopcock and raise the level of liquid in manometer by gentle aspiration to the highest etched line.
Close the stopcock and observed that the level of liquid in manometer is constant.
In case leak remake the cell manometer joint and check the stopcock.
Close the stopcock the level of manometer liquid will begin to flow, Start the timer as the liquid reaches second etch line and stop it when it reach the third etched line.
Record the time, repeat the procedure on the same bed and record the reading.
Record the temperature and humidity.
Take the average of two reading as the time taken.
Take 100gm of cement (OPC) sample to be tested for fineness in a stoppered jar or bottle to disperse agglomerates for 2 minute, wait 2 minutes stir the resulting powder gently using a clean dry glass rod in order to distribute the fines through out the cement.
Weigh 2.80 gm to the accuracy of 1 mg and repeat the procedure.

TO DETERMINE THE SPECIFIC SURFACE OF SLAG CEMENT, PPC & POZZOLANIC MATERIAL (EXCEPT SILICA FUME), WHO’S DENSITY IS LOWER THAN THE OPC CEMENT AS BELOW:

Determine the density of cement using Le-chatelier device using non-reactive liquid as describe in MECH-CEM-004.
Determine the Volume of bed using 2.80 gm of standard cement.
Determine the mass of cement for making cement bed, m=  V (1-e) where e is the porosity and considered 0.500.
Volume can be determine calibrating with mercury as follows:
Make the cement bed as mentioned above, place two fresh filtered paper disc in contact of the bed. Fill with mercury taking care that there shall not be any air void.
Remove the mercury above the cement bed and weigh to nearest 10 mg. M3
Remove the cement bed, place the perforated plate on cell with two fresh filter paper disc taking care that the base of the cell shall be covered fully whilst lying flat by placing with a rod.
Fill the cell fully with mercury remove any air bubbles with the clear dry rod. Ensure that the same is full by placing the glass plate in the mercury surface until it flushes with the cell top.
Empty the cell; weight the mercury to nearest 10 mg. M2.

DO’S & DON’TS:
Care shall be taken that the mercury shall not come in contact with the skin and eyes of the operator..
Do not use wet jar, bottle and glass rod for dispersing the sample.
OBSERVATION:
Observations should recorded in observation format QMS/QFT/QCL/0203/00
CALCULATION:
Specific Surface at 27  2 C
Constant factor = Specific Surface of Reference Cement /  t
Specific Surface of unknown sample = Constant factor x  t
Or

S = (521.08K  t)

Apparatus constant K can be determine from the density and specific surface and time taken of reference cement.

Where:

S = Specific Surface
K = is the apparatus constant
T = Time in seconds
 = Density of cement

Associated Software For Calculation & Report:
Calculator
Computer QC1, QC2, QC3.

REPORT:
Report the value of fineness of cement rounding of the numerical value M2/Kg

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Chemical Analysis of Cement:

OBJECTIVE:
Determination Of Chemical analysis of Hydrolic Cement.

APPARATUS REQUIRED:

Hot Plate Beaker’s-250ml 4Nos.

APPARATUS	QUANTITY
Analytical Balance
Drying Oven
Flame Photometer
Fuming Chamber
Platinum Crucible
Silica Crucible
Burette- 50ml	2Nos.
Pipette-25ml 2Nos.	2Nos.
Beaker’s-500ml
Beaker’s-400ml	4Nos.
Beaker’s-100ml	4Nos.
Volumetric Flask-250ml	2Nos.
Volumetric Flask-100ml 4Nos.
Conical Flask-250ml 4Nos.
Watch Glass
Evaporating Dish
Glass Rods
Finnel-100mm Dia	4Nos.
Funnel Stand	4Nos.
Filter Paper – 40No. 41No. 42 Nos.

Reagents

Hydrochloric Acid –Conc.
Nitric Acid – Conc.
Sulphuric Acid- Conc.
Orthophosphoric Acid- Conc.
Hydrofluoric Acid – 40%
Ammonium Hydroxide
Acetic Acid-Glacial
Diethyl amine – Liquid
Hydrochloric Acid – 1:1,1:3,1:10 and 1:99 (By Volume)
Nitric Acid – 1:4, 1:33 (By Volume)
Sulphuric Acid – 1:3 (By Volume)
Phosphoric Acid- 1:3(By Volume)
Sodium Hydroxide Solution- 4N- dissolves 80gm of sodium hydroxide in 500ml volumetricflask.
Glycerol – 1:21
Ammonium Acetate – 50%
Stannous Chloride- 5% - Dissolve 5gm of Sncl2 in 2.5ml hydrochloric acid and dilute to 100ml
Mercuric Chloride solutions – 5.6%- prepare a 5.6gm of mercuric chloride in 100ml-distilled water.
Manganese Sulphate Solution – Dissolve 35gm of manganese sulphate (MnSo4 7H2O) in 250ml of water. Add 70ml orthophosphate acid and 65ml Sulphuric acid. Dilute to 500ml
Standard Potassium Permanganate solution- 0.05N- dissolves about1.5kg of potassium permanganate (KmNo4) in one Litre of distilled water and standardizing with sodium oxalate.
Barium Chloride Solution-10% - dissolve 100gm barium chloride (Bacl2 2H2O) in one Litre distilled water.
Methyl Red- Indicator
Buffer Solution- Ph10- dissolve 70gm of ammonium chloride in 570ml of ammonium hydroxide and make up to one liter with distilled water.
Standard Zinc Solution - 0.01M – Dissolve 0.6537gm of zinc in dilute hydrochloric acid (1:1) make up 1litre to the mark with distilled water.
Standard EDTA Solution – 0.01M, dissolved 3.7224 gm of EDTA in 400ml hot water and make up to the volume in one Litre. Take 10ml of standard zinc solution add 20ml buffer solution of Ph 10 and warm up to 50 to 60C. Add 50mg Erichrome black T indicator and titrate with EDTA till the Colour changes from wine red to clear blue and calculate the morality of EDTA solution.
Erichrome Black T Indicator
Patton –Readers Indicators
Thymol Blue Indicator
Ammonium Nitrate Indicator

Interference

APPARATUS OPERATING PROCEDURE:
As per Apparatus Operating Manual (File No.: )
ACCESSORIES:

STANDARDS USED:
IS – 4032- 1985

OTHER REFERENCE STANDARDS:

EQUIPMENTS REQUIRING CALIBRATION
MINIMUM SIZE OF SAMPLE REQUIRED:
100gram
SAMPLING
The representative sample of the cement thoroughly mixed before using.
environmental conditions required for testing:
METHOD OF TEst
Loss on Ignition-

Take empty crucible weight.
Take 1gm of cement sample in silica crucible (W1)
The crucible place in muffle furnace at temperature 900C to 1000C for 1 hour.
After one hour remove the crucible and cool in Dessicator.
Weigh the crucible and note down the difference of initial weight to final weight (W2).
% Loss of Ignition = W1 – W2 X 100
Or % Loss of Ignition= Loss in Weight X 100

Silica –

Take 0.5gm of cement sample in evaporating dish, add 5-10ml conc. Hcl, Digest the sample of gentle heat and completely dissolved. Dissolved with light pressure flat glass rod.
Evaporate the solution to dryness on hot plate. Add 10-20ml of (1:1) hydrochloric acid and warm heat on hot plate for 10minutes.
Dilute the solution 10-20ml of hot distilled water.
Filter the solution through Whatman No 41 and wash the spectral silica with hot distilled water.
Reserve the filtrates for the determination of combined Alumina and ferric oxide.
Transfer the silica residue in weighed platinum crucible, dry and ignite the paper in low heat temperature until the carbon of filter paper completely burn without inflaming.
Keep the crucible in muffle furnace at 1100C to 1150C for 35-45minutes.
Remove the crucible and cool in Dessicator and weighed residue.
The silica residue contain small amount of impurities. Add 1-2ml D.W. 1-2ml of hydrofluoric acid and 2drops of Sulphuric acid and evaporate to dryness.
After dryness transfer the crucible in muffle furnace at 1050C - 1100C for 1-5minutes. Cool and weigh.

Silica (Sio2) % = 200 (W1 – W2)
W1= Weight of Silica Residue
W2= Weight of Impurities

Combined Ferric Oxide And Alumina –

To the reserved filterate (Volume 200ml) , add 5-10 drops of methyl red indicator and heat to boiling.
Add few drops bromine water or conc. Nitric acid and add ammonium hydroxide (1:1) drop by drop until the Colour of solution becomes yellow and smells of ammonia.
In boiling time appear the precipitates of Aluminum and ferric hydroxides.
Allow the precipitates to settle (not take more than 5-Minutes)
Filter the solution through Whatman No 41 and wash with 2% ammonium Nitrate solution and reserve the filtrate for CaO and MgO. Wash the residue up to removes complete impurities.
Transfer the precipitates in a weighed platinum crucible, slowly and charred the filter paper and Keep the furnace at 1050C to 1100C for 35 – 45 minutes.
Remove the crucible, cool in Dessicator and weigh as combined alumina and ferric oxide.
R2 O3 % = Weight of residue X 200
Al2 O3 % = R2 O3 % - Fe2 O3 %
If silica is suspected in the residue, add 1-2ml hydrofluoric acid and one drop of Sulphuric acid evaporate up to dryness.
Heat the crucible at 1050C - 1100C for 1-5minutes, Cool and weigh.
The difference between this weight and the weight previously obtained represent the amount of residual silica. Subtract this amount from the weight of ferric oxide and Alumina found.

Ferric Oxide (Fe2O3) Potassium Permanganate Method

Take one gm cement sample in 250ml beaker; add 40ml D.W and mixture stirred vigorously add 15ml of conc. Hydrochloric acid.
Heat the solution and grind the cement with flattened end of a glass rod.
Heat the solution to boiling, add drop bu drop starmous chloride until the solution is decolorized add a few drop of stannous chloride solution in excess and cool to room temperature.
Add 15ml mercuric chloride solution and 25ml manganese sulphate solution and titrate with standard potassium permanganate solution up to appear pink Colour.
Calculation – Fe2O3 = B.R x Number of KMNo4

Calcium Oxide (CaO) (EDTA Method)

Take 10ml from reserved solution in conical flask.
Add 10ml of 4N Sodium hydroxide solution and adjust pH 12or more, add 50ml-distilled water, add pinch paten – reddish solid indicator.
Titrate against 0.01M EDTA solutions to a sharp change in Colour from wine red to clear blue.
Calculation: - Calculate the percentage of CaO as below:
1ml of 0.01M EDTA = 0.5608 x mg of CaO

Calcium Oxide (CaO%) 0.5608 X 25 X BR / Volume of Sample

Magnesium Oxide: EDTA Method: 

Take 10ml from reserved solution in conical flask.
Add 20ml of buffer solution to Ph 10, add 50ml D.W. Erichrome black T indicator (Pintch) solid and shake well
Titrate against 0.01M EDTA until until the Colour changes from blue to clear pink.
Calculation: - Calculate the percentage of MgO as below.
Magnesium Oxide (MgO %) = 0.04032 X 25 X (V1-V) / Volume of sample
Where V1= Volume of EDTA used in this titration ml.
V = Volume of EDTA used in CaO determination in ml.

Sulphur Tri Oxide (So3) 

Take 1gm cement sample in 250ml beakers, add 25-30ml distilled water shake vigorously, add 5ml conc. Hcl
Grind the cement sample with flattened end of glass rod.
Digest the sample for 15-20 minutes.
Filter the solution thorough Whatman No 40 or 41 and wash the residue with hot water.
Dilute the filtrate about 250ml heat & boiling, add drop-by-drop hot barium chloride until the precipitate is formed.
Digest the solution for 4hour.
Filter the precipitate thoroughly Whatman No 42 and wash the filter paper up to remove complete impurities.
Transfer the residue in weighed crucible and slowly heat the paper without inflaming.
Ignite the residue to 800C to 900C for 30minutes. Remove the crucible, cool in Dessicator and weigh the barium sulphate obtained.
Calculation- calculate the percentage of So3 as follows-
Sulphurtrioxide (% So3 ) = W X 34.3

W= Weight of residue (BaSo4) in gm
34.3 = molecular ration of So3 to BaSo4 (0.343) multiplied by 100.
Insoluble residue: -

Digest the filter paper containing the residue from So3 add 25-30 ml hot water and 30ml of 2N sodium carbonate solution
The solution heat for 10minutes.
Filter the solution through Whatman No 40 and wash the residue with dilute Hcl and hot water till the residue is from chlorides
Transfer the residue in weighed crucible and ignite the residue 900 to 1000C for 30 minutes.
Remove the crucible cool in Dessicator and weigh the crucible.
Calculation –
% Insoluble residue = Residue weight X 100

Sodium Oxide and Potassium Oxide – ( By Flame photometer Method)

Preparation of Stock Solution – Sodium chloride and potassium chloride stock solution – dissolve 1.8858 gm of sodium chloride and 1.583 gm of potassium chloride (both dried at 105 to 110C ) in meter. Dilute to one litre in a volumetric flask. This solution equivalent of 1000 ppm (0.10%) each of sodium oxide and potassium oxide.
Standard Solution – Prepared the standard solution as out requirement

Table – Standard Solution

Standard solution number	Concentration of Alkali as Na2o or K2o in standard solution Ppm	Volume of stock solutionused Nacl –Kcl ml	Final Volume of Solution ml
1	100	200	2000
2	75	75	1000
3	50	50	1000
4	35	25	1000
5	10	10	1000
6	0	0	100
7	100	100	1000

SPECIAL CARE TO BE TAKEN:
Procedure

Take 1.0gm of the cement sample in 250ml beaker, add 20ml-30ml of water with shaking add 5.0ml hydrochloric acid, dilute to 50ml with water.
Break up lumps of cement with glass rod, digest on the hot plate for 15minutes,
Filter the solution through Whatman Bo 41 in volumetric flask 100ml make the volume 100ml mix and cool the solution to room temperature
Determine the sodium oxide and potassium oxide value from flame photometer reading.
Calculate the % of Alkali expressed as Na2 O to the as below.
Total Alkali = A + E
A= B / W X 10
C= D/ WX 10
E=CX 0.658