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CALIBRATION
OF GLASSWARE
• Submitted by :- Surendra Puniya
• Class :- B.Tech (Dairy technology) Part 3rd Sem. 1st
• Submitted to :- Dr. Rekha Rani
CALIBRATION
• It is the act of marking units of measurement on
an instrument so that it can be used for measuring
something accurately
GROUPS OF
GLASSWARE
• Glassware can be divided into two main groups :-
1. Volumetric Glassware
2. Non-volumetric Glassware
VOLUMETRIC
GLASSWARE:
• Burettes
• Pipettes
• Volumetric flasks
• Graduated cylinders
• Thermometer
• Syringe
• Beakers
COMMONLY
USED
GLASSWARES
FOR ANALYSIS
OF MILK IN A
DAIRY
INDUSTRY
1. Milk Butyrometer
2. Pipette
3. Lactometer
4. Thermometer
5. Burette
MILK
BUTYROMETER
Comparison method :- In this the accuracy of newly
purchased butyrometers is compared by estimating fat by
Gerber method in a one milk sample, along with the
butyrometers of the previous batch, well calibrated and
known to be accurate. If the readings of the fat values of
new butyrometers are the same as of old ones, then the
new butyrometers are accepted otherwise rejected.
Limitation of this method is that the previous
butyrometers may not be accurate or their internal volume
may have been changed due to acid corrosion.
• (ii) BIS Method :- In this method a specially designed mercury pipette is used to calibrate the butyrometers.
• The method is based on the principle that the internal volume of the graduated tube of the milk butyrometer is
0.125 ml corresponding to each 1% fat range. In other words, the full scale of graduated tube from 0 to 10% fat
marks, has the internal volume of 1.25 ml.
• Accordingly an automatic mercury pipette has been designed to dispense exactly 0.3125 ml mercury which fills
the tube corresponding to 2.5% fat graduation limits.
• To calibrate the full scale from 0 to 10% fat marks, the bulb of the butyrometer is first filled upto 10% graduation
mark as the base point.
• Then the mercury is added in the butyrometer from the mercury pipette four times, each time dispensing exactly
0.3125 ml of mercury corresponding to 2.5% fat graduation limit on the butyrometer column.
• If the graduated column of the butyrometers are exactly filled from 0 to 10% fat marks in four deliveries of the
mercury pipette, then the butyrometers are accepted, otherwise rejected.
PIPETTES
(i) Comparison method :-
• In this the accuracy of newly purchased pipettes is compared by estimating fat by
Gerber method in a one milk sample, along with the pipettes of the previous batch,
well calibrated and known to be accurate.
• If the readings of the fat values of new pipettes are the same as of old ones, then
the new pipettes are accepted otherwise rejected.
Limitation - The previous pipettes may not be accurate or their internal volume may have been
changed due to breakage of their tips.
(ii) BIS method :-
• According to BIS the milk pipette is defined as to dispense 10.75 +_ 0.03 ml of
distilled water at 270C when held for 15 s.
• For calibrating the milk pipettes, the water dispensed by the pipette is taken in a
previously weighed beaker and its mass is recorded.
• Knowing the density of the water at 270C i.e. 0.99654, the volume of the water
dispensed is calculated as
Volume of water = (Mass of water dispensed)/(0.99654) If the calculated volume of
water dispensed by the pipette is equal to 10.75+_ 0.03 ml, then the pipette is accepted,
otherwise rejected
(III) MATHEMATICAL
METHOD OF
CALIBRATION AND
GRADUATION
• For checking the marks/points corresponding to
10.75 ml capacity of milk pipettes, the following
procedure can be applied:
• As the stem of the pipette is of uniform cross-
section, therefore, internal volume per unit length
of stem at any point is constant. Fill the pipette
with distilled water to a temporarily marked point
A on the upper stem of the pipette and dispense
in a tarred` beaker and weigh. Knowing density of
water, calculate the volume of pipette up to the
mark A. Similarly again fill up the pipette with the
water up to another point B (above A) and find the
volume of water dispensed.
• Let volume of water up to point A = Va ml
• And volume of water up to point B = Vb ml
• Therefore, volume between A and B = (Vb – Va) ml
• Now note the distance between A and B points, let it is = d cm
• Therefore, stem of the pipette has volume = (Vb – Va)/d ml per cm length.
• Now, let Va is less than 10.75 ml
• Therefore, difference of volume = (10.75 – Va) ml
• Now as we know that volume (Vb – Va)/d mloccupies length = 1 cm
• And (10.75 – Va) ml occupies length = d x (10.75 – Va)/(Vb – Va) cm
• Therefore, mark a point above A at a distance = d x (10.75 – Va)/(Vb – Va) cm, which will correspond to
10.75 ml mark.
CALIBRATION
OF
LACTOMETERS
(i) Comparison method :-
In this method each lactometer is calibrated before
use by floating side by side in a liquid, against a
standard lactometer. If the lactometer readings of
newly purchased lactometers resemble with that of
standard lactometer, then the new lactometers
should be accepted otherwise rejected.
(II) BIS METHOD OF TESTING ACCURACY OF BIS
LACTOMETER
• Dissolve appropriate mass of
anhydrous sodium carbonate
given below in 300 ml of distilled
water. Add 50 ml 92% ethanol to
the solution so obtained and
make up the total volume of 500
ml with distilled water. Compare
the accuracy of each and every
lactometer in all the solutions.
• Specific gravity and lactometer
reading of pure Sodium
carbonate Solution
Sl. No. Wt. of
anhydrous
Na2CO3
(gm/500ml)
Specific
gravity at
270C
(gm/ml)
Lactometer
Reading (LR)
1 19.2 1.025 25
2 21.6 1.030 30
3 24.0 1.034 34
(III) BIS METHOD OF TESTING ACCURACY OF
QUEVENNE LACTOMETER
• This can be conveniently done by
taking the specific gravity of
suitable salt solutions at 15.50C.
The solutions used are given
below.
Specific gravity of pure Sodium
Chloride Solution
Sl. No. Pure
sodium
chloride
solution
Specific
gravity at
15.50C
(gm/ml)
Lactometer
Reading (LR)
1 3.863 % 1.026 26
2 4.415 % 1.032 32
CALIBRATION
OF
THERMOMETERS
(i) Comparison method :- Though it is not very accurate
method, however, usually it is mostly used. In this
thermometers are compared with one or more thermometers
which are known to be accurate. At least two different
temperature marks (preferably nearer to lower and upper
limits) are compared.
(ii) Physical method :- In this method the zero point is located
by dipping the mercury bulb of the thermometer in the
melting ice kept in a wide funnel. Where the temperature
becomes stationary, mark that 0 C point. The 100 C point
is located by keeping the mercury bulb of the thermometer in
steam at normal pressure. If the pressure is not 760 mm then
appropriate correction is applied. In general at the natural
atmospheric pressure 0.038 C is added or deducted from the
observed boiling point per mm pressure of mercury lower or
higher than 760 mm, respectively.
CALIBRATION OF
FREEZING POINT
DEPRESSION
THERMOMETER
• Before calibration of these thermometers, the
definitions of two types of solutions are to be
understood
Molar solution
It is defined as a solution prepared by dissolving one
gm molecule of any substance in solvent so as to
make 1000 ml solution.
Molal solution
It is defined as a solution prepared by dissolving one
gm ion (in case of ionized molecules) or molecule (in
case of non-ionized molecules) in 1000 gm of
solvent.
The soluble ions or molecules play very important role in depressing the freezing point of solvent such as water. Milk is
a solution in which water is the solvent and mainly lactose and minerals are solutes, which depress its freezing
point. The one molal solution of any ion or unionized molecule depresses the freezing point of water by 1.860C.
• It means one molal solutions of non-ionized substances like sugar (360g in 1000g of water), glucose (180 g in 1000 g
of water) etc. depress the freezing point by 1.860C.
• However, one molal solution of ionized molecules depresses the freezing point by (1.86 x numbers of ions per
molecules)0C.
• For example, one molal solution of sodium chloride (Na+Cl-) will depress the freezing point by 1.86 x 2 = 3.720C.
• Now, 1.860C is depressed by a solution = 1 molal
• 10C is depressed by a solution = 1/1.86 = 0.538 molal
• 0.50C is depressed by a solution = 0.269 molal
• Therefore, -0.50C and -10C points on the freezing point depression thermometer are checked by using the 0.269 and
0.538 molal solutions, respectively. For pure milk –0.540C = 0.29 molal or –0.550C = 0.3 molal.
CALIBRATION OF
BURETTE
• Burette is checked at various
intervals say 5, 10, 25 or 50 ml for
determining the accuracy of its
scale and the capacity of the
burette. The volume actually
delivered for each interval is
obtained as per the procedure
outlined for milk pipette.
Capacity (ml) Burettes
Class A Class B
1 0.006 0.01
2 0.01 0.02
5 0.01 0.02
10 0.02 0.05
25 0.05 0.1
50 0.05 0.1
100 0.1 0.2
Tolerance for burette
THANK YOU

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Calibration of Glassware in laboratory

  • 1. CALIBRATION OF GLASSWARE • Submitted by :- Surendra Puniya • Class :- B.Tech (Dairy technology) Part 3rd Sem. 1st • Submitted to :- Dr. Rekha Rani
  • 2. CALIBRATION • It is the act of marking units of measurement on an instrument so that it can be used for measuring something accurately
  • 3.
  • 4. GROUPS OF GLASSWARE • Glassware can be divided into two main groups :- 1. Volumetric Glassware 2. Non-volumetric Glassware
  • 5. VOLUMETRIC GLASSWARE: • Burettes • Pipettes • Volumetric flasks • Graduated cylinders • Thermometer • Syringe • Beakers
  • 6. COMMONLY USED GLASSWARES FOR ANALYSIS OF MILK IN A DAIRY INDUSTRY 1. Milk Butyrometer 2. Pipette 3. Lactometer 4. Thermometer 5. Burette
  • 7. MILK BUTYROMETER Comparison method :- In this the accuracy of newly purchased butyrometers is compared by estimating fat by Gerber method in a one milk sample, along with the butyrometers of the previous batch, well calibrated and known to be accurate. If the readings of the fat values of new butyrometers are the same as of old ones, then the new butyrometers are accepted otherwise rejected. Limitation of this method is that the previous butyrometers may not be accurate or their internal volume may have been changed due to acid corrosion.
  • 8. • (ii) BIS Method :- In this method a specially designed mercury pipette is used to calibrate the butyrometers. • The method is based on the principle that the internal volume of the graduated tube of the milk butyrometer is 0.125 ml corresponding to each 1% fat range. In other words, the full scale of graduated tube from 0 to 10% fat marks, has the internal volume of 1.25 ml. • Accordingly an automatic mercury pipette has been designed to dispense exactly 0.3125 ml mercury which fills the tube corresponding to 2.5% fat graduation limits. • To calibrate the full scale from 0 to 10% fat marks, the bulb of the butyrometer is first filled upto 10% graduation mark as the base point. • Then the mercury is added in the butyrometer from the mercury pipette four times, each time dispensing exactly 0.3125 ml of mercury corresponding to 2.5% fat graduation limit on the butyrometer column. • If the graduated column of the butyrometers are exactly filled from 0 to 10% fat marks in four deliveries of the mercury pipette, then the butyrometers are accepted, otherwise rejected.
  • 9.
  • 10. PIPETTES (i) Comparison method :- • In this the accuracy of newly purchased pipettes is compared by estimating fat by Gerber method in a one milk sample, along with the pipettes of the previous batch, well calibrated and known to be accurate. • If the readings of the fat values of new pipettes are the same as of old ones, then the new pipettes are accepted otherwise rejected. Limitation - The previous pipettes may not be accurate or their internal volume may have been changed due to breakage of their tips.
  • 11. (ii) BIS method :- • According to BIS the milk pipette is defined as to dispense 10.75 +_ 0.03 ml of distilled water at 270C when held for 15 s. • For calibrating the milk pipettes, the water dispensed by the pipette is taken in a previously weighed beaker and its mass is recorded. • Knowing the density of the water at 270C i.e. 0.99654, the volume of the water dispensed is calculated as Volume of water = (Mass of water dispensed)/(0.99654) If the calculated volume of water dispensed by the pipette is equal to 10.75+_ 0.03 ml, then the pipette is accepted, otherwise rejected
  • 12. (III) MATHEMATICAL METHOD OF CALIBRATION AND GRADUATION • For checking the marks/points corresponding to 10.75 ml capacity of milk pipettes, the following procedure can be applied: • As the stem of the pipette is of uniform cross- section, therefore, internal volume per unit length of stem at any point is constant. Fill the pipette with distilled water to a temporarily marked point A on the upper stem of the pipette and dispense in a tarred` beaker and weigh. Knowing density of water, calculate the volume of pipette up to the mark A. Similarly again fill up the pipette with the water up to another point B (above A) and find the volume of water dispensed.
  • 13. • Let volume of water up to point A = Va ml • And volume of water up to point B = Vb ml • Therefore, volume between A and B = (Vb – Va) ml • Now note the distance between A and B points, let it is = d cm • Therefore, stem of the pipette has volume = (Vb – Va)/d ml per cm length. • Now, let Va is less than 10.75 ml • Therefore, difference of volume = (10.75 – Va) ml • Now as we know that volume (Vb – Va)/d mloccupies length = 1 cm • And (10.75 – Va) ml occupies length = d x (10.75 – Va)/(Vb – Va) cm • Therefore, mark a point above A at a distance = d x (10.75 – Va)/(Vb – Va) cm, which will correspond to 10.75 ml mark.
  • 14.
  • 15. CALIBRATION OF LACTOMETERS (i) Comparison method :- In this method each lactometer is calibrated before use by floating side by side in a liquid, against a standard lactometer. If the lactometer readings of newly purchased lactometers resemble with that of standard lactometer, then the new lactometers should be accepted otherwise rejected.
  • 16. (II) BIS METHOD OF TESTING ACCURACY OF BIS LACTOMETER • Dissolve appropriate mass of anhydrous sodium carbonate given below in 300 ml of distilled water. Add 50 ml 92% ethanol to the solution so obtained and make up the total volume of 500 ml with distilled water. Compare the accuracy of each and every lactometer in all the solutions. • Specific gravity and lactometer reading of pure Sodium carbonate Solution Sl. No. Wt. of anhydrous Na2CO3 (gm/500ml) Specific gravity at 270C (gm/ml) Lactometer Reading (LR) 1 19.2 1.025 25 2 21.6 1.030 30 3 24.0 1.034 34
  • 17. (III) BIS METHOD OF TESTING ACCURACY OF QUEVENNE LACTOMETER • This can be conveniently done by taking the specific gravity of suitable salt solutions at 15.50C. The solutions used are given below. Specific gravity of pure Sodium Chloride Solution Sl. No. Pure sodium chloride solution Specific gravity at 15.50C (gm/ml) Lactometer Reading (LR) 1 3.863 % 1.026 26 2 4.415 % 1.032 32
  • 18.
  • 19. CALIBRATION OF THERMOMETERS (i) Comparison method :- Though it is not very accurate method, however, usually it is mostly used. In this thermometers are compared with one or more thermometers which are known to be accurate. At least two different temperature marks (preferably nearer to lower and upper limits) are compared. (ii) Physical method :- In this method the zero point is located by dipping the mercury bulb of the thermometer in the melting ice kept in a wide funnel. Where the temperature becomes stationary, mark that 0 C point. The 100 C point is located by keeping the mercury bulb of the thermometer in steam at normal pressure. If the pressure is not 760 mm then appropriate correction is applied. In general at the natural atmospheric pressure 0.038 C is added or deducted from the observed boiling point per mm pressure of mercury lower or higher than 760 mm, respectively.
  • 20. CALIBRATION OF FREEZING POINT DEPRESSION THERMOMETER • Before calibration of these thermometers, the definitions of two types of solutions are to be understood Molar solution It is defined as a solution prepared by dissolving one gm molecule of any substance in solvent so as to make 1000 ml solution. Molal solution It is defined as a solution prepared by dissolving one gm ion (in case of ionized molecules) or molecule (in case of non-ionized molecules) in 1000 gm of solvent.
  • 21. The soluble ions or molecules play very important role in depressing the freezing point of solvent such as water. Milk is a solution in which water is the solvent and mainly lactose and minerals are solutes, which depress its freezing point. The one molal solution of any ion or unionized molecule depresses the freezing point of water by 1.860C. • It means one molal solutions of non-ionized substances like sugar (360g in 1000g of water), glucose (180 g in 1000 g of water) etc. depress the freezing point by 1.860C. • However, one molal solution of ionized molecules depresses the freezing point by (1.86 x numbers of ions per molecules)0C. • For example, one molal solution of sodium chloride (Na+Cl-) will depress the freezing point by 1.86 x 2 = 3.720C. • Now, 1.860C is depressed by a solution = 1 molal • 10C is depressed by a solution = 1/1.86 = 0.538 molal • 0.50C is depressed by a solution = 0.269 molal • Therefore, -0.50C and -10C points on the freezing point depression thermometer are checked by using the 0.269 and 0.538 molal solutions, respectively. For pure milk –0.540C = 0.29 molal or –0.550C = 0.3 molal.
  • 22.
  • 23. CALIBRATION OF BURETTE • Burette is checked at various intervals say 5, 10, 25 or 50 ml for determining the accuracy of its scale and the capacity of the burette. The volume actually delivered for each interval is obtained as per the procedure outlined for milk pipette. Capacity (ml) Burettes Class A Class B 1 0.006 0.01 2 0.01 0.02 5 0.01 0.02 10 0.02 0.05 25 0.05 0.1 50 0.05 0.1 100 0.1 0.2 Tolerance for burette
  • 24.