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Calibration 1

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13 views

Calibration 1

Uploaded by

sevdaaslanturk2003
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PPT, PDF, TXT or read online on Scribd
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CALIBRATION of an Analytical Volumetric-glassware

What is volumetric-glassware?
When do we use volumetric-glassware?

• For quantitative measurements where high degree of precision is required


you should use volumetric glasswares such as buret, pipet and volumetric-
flask.

• For measurements where precision is not important you can use regular
glasswares such as gratuated cylinders, beakers, erlenmeyer flasks etc.

• All glass vessels can expand and contract slightly with temperature.
Therefore the true capacity of the glassware can be known after it is
calibrated properly at the temperature it is going to be used.
Calibration:

General directions:
• All volumetric ware should be cleaned before being calibrated.
• The water used for calibration should be in thermal equilibrium with its
surroundings. This condition is best attained by drawing the water in
advance, noting its temperature at frequent intervals, and waiting until no
further changes occur.
• An analytical balance is used for calibration, weighing bottles serve as
receivers for the calibration liquid.
• Calibration of a Volumetric Pipet
• 1) Determine the mass of the empty stoppered weighing bottle to the ±0.1 mg.
• 2) Transfer a portion of temperature-equilibrated water to the weighing bottle with the
pipet, weigh the bottle and its contents to ±0.1 mg.
• 3) Calculate the mass of water delivered from the differences in these masses.
• 4) Pour water, rinse the weighing bottle w ith acetone, dry in oven for 10 minutes( be
sure its dry).Cool in desicator for 10 minutes.
• 5) Repeat the above steps 5 more times.

• Calibration of a Buret
• 1) Fill the buret with temperature-equilibrated water and make sure that no air
bubbles are trapped in the tip. Lower the liquid level to bring the bottom of the
meniscus to the 0.0-ml mark. Wipe the tip of the buret with a paper tissue to remove
any adhering drop.
• 2) Weigh a 125-ml erlenmeyer flask fitted with a stopper to ±0.1 mg.
• 3) Transfer 5,10,15,20,25 ml of water to the flask, touch the tip of the buret to the wall
of the flask. Record the volume that was apparently delivered, and refill the buret.
• 4) Weigh the flask and its contents to ±0.1 mg; the difference between this mass and
the initial value gives the mass of water delivered.
• 5) Repeat the above steps 5 more times.
Calculation
• Pipet
1) Calculate mass of water delievered.
mass of water = [ Weight of weighing bootle+water ] – [ weight of weighing bootle]
2) Apply Q test for the most deviated data.
What is Q- test ?
the questionable result : Xq
the nearest result to Xq: Xn Q exp = I Xq-Xn I / I Xq – Xf I
the furhest result to Xq: Xf
if Qexp > Qcri  deviant data should be rejected
if Qcri > Qexp  deviant data should be retained
You can find Qcri values in table

3) Calculate the volume delivered at temperature T (oC) with the aid of Table 28-3
(Skoog West & Holler, 6th edition)
4) Calculate the mean of volume delievered at T (oC) .
5) Calculate the standard deviation at T (oC) .

Sample value Mean value


•Buret
1) Calculate mass of water delievered.
mass of water = [ Weight of weighing bootle+water ] – [ weight of weighing bootle]
2) Apply Q test for the most deviated data.
What is Q- test ?
the questionable result : Xq
the nearest result to Xq: Xn Q exp = I Xq-Xn I / I Xq – Xf I
the furhest result to Xq: Xf
if Qexp > Qcri  deviant data should be rejected
if Qcri > Qexp  deviant data should be retained
You can find Qcri values in table

3) Calculate the volume delivered at temperature T (oC) with the aid of Table 28-3
(Skoog West & Holler, 6th edition)
4) Calculate the correction factor (deviation from true value)
correction factor = true volume – apparent volume
5) Calculate mean correction factor.
6) Plot mean correction factor versus volume graph.
mean correction factor versus apparent volume

0,8

0,6

0,4 1st reading – 3 mL


0,2

0 2nd reading – 18 mL
0 5 10 15 20 25
-0,2
18-3 = 15 ml is delivered (expected)
-0,4

-0,6

-0,8
However
1st reading – (3 -0,3)mL = 2.7 mL
2nd reading – (18 + 0,5)mL = 18.5 mL
Then 18.5 – 2.7 = 15.8 mL delievered.

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