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CHM 421

Analytical Chemistry
EXPERIMENT 1
TITLE: Calibration of a Volumetric Flask
NAME:

NIK HARITH BIN NIK ABD HALIM

STUDENT ID:

2014 88 7616

GROUP :

ED 260 5A

PROGRAMME :

ED 260

DATE OF
EXPERIMENT :

11TH OCTOBER 2016

DATE REPORT
SUBMITTED :

18TH OCTOBER 2016

LECTURER :

DR NOR SUHAILA MOHAMAD HANAPI

ABSTRACT

In this experiment, the purpose of this experiment is to calibrate a used volumetric flask and
determine the new calibration mark of the volumetric flask. In the beginning of the experiment,
the volumetric flask should be clean and dry before used. The volumetric flask should be
handled with care and all the precautions were being taken during the experiment was held.
This was to ensure to avoid any errors such as parallax error especially while reading water
meniscus. This experiment must be repeated three times or more and take the average reading
to get more accurate data. Although the instrument may measure a given sample, the value
might need to be altered due to various conditions and errors.
OBJECTIVES
1. To calibrate a used volumetric flask
2. To determine the new calibration mark of the volumetric flask.
INTRODUCTION
Reading error for a 100mL of volumetric flask is +- 0.1ml. Any 100ml volumetric flasks with
volume exceeding this tolerance needs to be calibrated. Calibration is an important process
because it ensures apparatus to contain or deliver good, accurate volume. In this experiment,
the same procedure can be applied to other volumetric glassware.
Volumetric flask is calibrated by measuring the mass of a liquid of known density and
temperature that is contained in the volumetric flask. The weight obtained must be corrected for
buoyancy since the density of water is quite different from that of the standard weights of the
analytical balance.

The calculations for the calibration are quite involved. First, the weighing data are corrected for
buoyancy. Next, this data is converted to the volume of the apparatus at the temperature of

calibration by dividing the density of the liquid at the temperature. Finally, this volume is
corrected to the standard temperature of 20C.
Use the table provided in your calculation for calibration. This table has already incorporated the
buoyancy error for stainless steel or brass weights and for the volume change of water and
glass containers.
METHODOLOGY

Equilibrating was started


using 200mL of distilled
water. It was placed into
a clean beaker let it
stand for 15 minutes.

The flask was filled with


equilibrated distilled
water up to the mark and
the flask was weighed
again accurately.

100mL of volumetric flask


was dried and cleaned.
2cm sticker was pasted
onto the 100mL mark of
the flask.

2 temperature was the


same and proceed to the
next step.

The mark of the flask


was let at the center of
the sticker. The weight of
the volumetric flask was
determined accurately.

After 15 minutes, the


temperature of the room
was measured and the
water was equilibrated.

RESULT

A new mark on the


sticker was made 5m
above or below the
present mark when the
volume was less or more
than 100ml and
adjustment was done.

Water was reduced or


added up to the new
mark that has been
made. The volumetric
flask was weighed again
and the new volume was
calculated.

The exact distance for


the new mark was
determined using the
ratio of volume and
distance.

Weight of empty volumetric flask, W1 = 55.3074g


Weight of volumetric flask + water, W2 = 154.3706g
Weight of water, W3, W2 - W1 = 152.6533g - 53.3362g = 99.0002g
Since the room temperature is 28C, from Table 1 in laboratory manual, the volume of 1.0g of
water is 1.0046g.
Volume of water, V1 = W3 x 1.0046ml = 99.3171g x 1.0046ml = 99.4556ml
Since V1 is less than 100ml, water was added up to 5mm above the original calibration mark
done.
The difference in volume from 100ml, V2 = (100 - V1) ml =100ml - 99.7740ml = 0.226ml
Weight of flask + 5mm above, W4 = 153.4126g
Weight of water + 5mm above mark, W5, W4 W1 = 153.4126g 53.3362g = 100.0764g
Volume of water + 5mm above mark, V3 = W5 x 1.0046ml = 100.5368ml
Volume if water in 5mm, V4 = V3 - V1 = 100.5368ml 99.7740ml = 0.7628ml
To calculate the exact 100ml mark using the distance/volume ratio:

V4mL = 5mL , then 5mm/V4 = xmm/V2


5mm/0.792 = 6.3083 (0.5444) = xmm = 3.4342mm

DISCUSSION

The purpose of the experiment of calibration of volumetric flask is to calibrate certain


measurement by using volumetric flask. The calibration was done by measuring the mass of
water contained in or delivered by the flask. The density of water at a particular temperature
which is measured is used to convert mass into volume.
In this experiment, we were exposed to a variety of important concepts related to quantitative
experimentation. The weight of empty volumetric flask and weight of water with volumetric flask
was required to calculate the weight of water used in this experiment. From the calculation, the
weight of water used which is W3 is said to have 99.0002g. This value was then needed to be
multiplied with the amount of volume for 1.00g of water at room temperature.
During the experiment, the room temperatures have been measure using thermometer which is
28C. It was important to measure the temperature of surrounding as density of water changes
variously according to the temperature. However, since the volume of water at specific
temperature was 99.4556ml which is less than 100ml with the difference of 0.5444ml, therefore
water was added up to the 5mm above of calibration mark. The new volume of water was
calculated which is 100.2482ml while the amount of water added to reach the new calibration
mark was 0.7926ml.
From the values that have been calculated, the distance between the original calibrations to the
new mark can be determined by using the ratio of volume and distance which is to get
0.7926mm.
Precaution steep need to be taken in order handling glassware. First, the apparatus that used
need to be clean in order to avoid any contamination that could make the reading error. The
proper handling technique need to measure correctly in terms of volume to reduce the error.

ERROR

When conduction the experiment, there are some error that occur which effect the result of the
experiment. The result obtained show that the reading is precise but not accurate
i)
ii)

The 2cm sticker that mark on the 100mL flask need to be aligned correctly
The 2cm sticker that mark on the 100mL flask weighed may be the cause of the error
reading

SUGGESTION

When conducting the experiment, there is some factor that affected the result. The results are
precise but not accurate.
i)

Each part in the experiment must be repeat at least trice for a better result.

CONCLUSION:
A used volumetric flask has been calibrated and the new calibration mark of the volumetric flask
was determined to be 0.7926mm above from the original calibration mark.

REFERENCES:

Raymond Chang. (2010). Chemistry Tenth Edition, New York: McGraw-Hill Publishing.

Martin S. Silberberg. (2013). Calibration of a Volumetric Flask, New York: McGraw-Hill


Publishing.

David N. Blauch. (2012). Analysis Of Unknown Sample. Retrieved on 15 October 2015 from
http://www.chm.davidson.edu/vce/Kinetics/ReactionRates.html

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