CLD 10004 GENERAL CHEMISTRY

EXPERIMENT 1:

CALIBRATION OF VOLUMETRIC GLASSWARE

NAME : NURUL SYAHIRA BINTI MOHMAD SAH

ID NUMBER : 55101212094

SECTION : 1 DIP C

COURSE : DIPLOMA (PROCESS)

DATE : 15th AUGUST 2012

 SUMMARY / ABSTRACT

Calibration is the important part before all measuring instrument can be used in the
experiments. Calibration will help to maintain the accuracy of the instruments because only
instruments with high accuracy can be used in any experiments. In this experiments all
measuring instruments such as pipette, volumetric flask and measuring cylinder were
calibrated by used them to deliver or to contain at specific volumes of liquid. The experiments
were carried out by measure the mass of liquid at room temperature and convert into
volumes by suitable equation. The actual volumes were obtained and the average volumes
were calculated to get the higher accuracy of the measurement. The standard deviations
were calculated. The higher proportion of the data lies near the mean indicates the lower
standard deviation. Lower standard deviation indicates the high accuracy of measurements.
There are error were occurred during the experiments. In the future, the error must be avoid
to produce the good result.

OBJECTIVES

The objectives of this experiment were:

To calibrate a 10 mL volumetric pipette

To calibrate a 25 mL volumetric pipette
To calibrate a 100 mL volumetric flask
To calibrate a 50 mL measuring cylinder

INTRODUCTION

Calibration is the process of maintaining the accuracy and consistency of the

measuring instruments. Accuracy is the closenesss degree of measurement with the actual
value. Consistency or precision is the degree that show the same result when the
measurement is repeated under the constant condition. Calibration requires the comparison
between output value of measuring instruments and authorized standard laboratories as the
acceptable range.

Most of the instruments are labelled with temperature at which the calibration apply,
mark of to contain as TC and to deliver as TD. In this experiments, pipette is calibrated to
delivered the specific volumes while volumetric flask and measuring cylinder as the
container. Only measuring instruments which has reading falls within the value of standard or
tolerance value being used for experiments either in laboratories at school, universities or
gigantic companies all around the world. It is advisable to use only the instruments with
higher accuracy to do any experiments. For example, thermometer in laboratory must be
calibrated to adjust any errors indication from this instrument. After adjusting, this
thermometer will show more accurate value at specific points on the scale. Most of
instruments need to be calibrated at regular scheduled intervals such as quarterly, monthly or
annually to make sure it can be functional and safe to use.

To do the calibration the mass of water for containing or delivering was measured and
the density of water at certain temperature used to convert mass into volume of water. Most
of the procedures for calibration are manage with professional manner. All calibration
operation takes place at particular places that keeping all instruments needed for calibration.
All calibration operation is assign for just one person as the clear responsibility for performing
the procedure. Sometimes a separated room is prefer to control better environmental and
protects against unauthorized usage of the calibration instruments.

Despite of maintaining the accuracy and consistency among the measurements,

other purpose is the instruments which need bias correction. Across the industry, all
measuring instrument reads as the reference standard in the same units. Others instruments
which have different units will be calibrated to eliminate bias and agree with this reference
standard.

A national references standard is use all over the world for this calibration procedure.
Diagram 1 shows a chain-like structure for standardization that is called traceability. When an
instrument calibrate by using standard measurements it will link by this chain of increasing
accuracy back to the primary standard which is national references standard for standard
values and tolerance values. The performance of measuring instruments being compared to
this standard and adjust back to conformance.

National standard organization

(Primary reference standard)

Standards laboratory
(Secondary reference standard)

Company instrument laboratory

(Working standard)

Process instruments

Diagram 1
 For a calibration standard, the 10-to-1 rule or a minimum accuracy of 10 times to the
accuracy of the tested equipment is applied. It is to ensure the equipment calibrated correctly
and no calibration within overlapping tolerance. For example if the tolerance is 0.02mm on a
part, choose an instruments with a resolution 0.002mm.

The standard deviation also can be used as to get the accuracy of measurements.
The high proportion of data lies near the value of mean has lower standard deviation. Lower
standard deviation indicates lower accuracy of the measurements.

If the instruments fail to calibrate correctly, product will be rejected when they are
actually good, lead to troubleshooting, false direction in research and product development. If
it goes on in a long period the result is large losses of money, time and effectiveness. For
example, Chemical Engineer deals with huge amount of chemicals. There are certain
chemicals will explode when it get contacts above certain temperature. If the Chemical
Engineer use non-calibrated thermometer, it will give out inaccurate reading of the
surrounding temperature. The Chemical Engineer might work in danger zone. The chemicals
might be explode and lead to death.

Furthermore, the well-performed of calibration of the instruments lead to maximise the

productivity, optimise resources, the product can be accepting everywhere, keeping the
safety of employees and consumers, reducing cost and time, maintaining the quality and
ensuring the effectiveness of the result of all experiments.

MATERIAL

a) Chemical:

The distilled water

b) Apparatus:

Volumetric pipette, volumetric flask, measuring cylinder, thermometer, transfer pipette,

top loading balance, stopper, small beaker, weighing bottles or small conical flasks
and dropper.

PROCEDURE

a) Calibration of volumetric pipette (10 mL and 25 mL)

1. A clean and dry transfer pipette was obtained.
2. An empty weighing bottle was weighed by using top loading balance and was
recorded.
 3. The distilled water was filled into the small beaker
4. The distilled water from the small beaker was filled until the mark of pipette.
5. The distilled water was drained from pipette into an empty weighing bottle.
6. The temperature of distilled water was measured using thermometer and was
recorded.
7. The weighing bottle with the content was weighed again by using top loading
balance and was recorded.
8. The mass of water was obtained and converted into volume by using the
following equation in Table 1

True (Actual) Volume : (grams of water) x ( volume of 1.0000 grams of water in XC)
TABLE 1
9. Steps 1 until 8 were repeated 2 times for each 10mL pipette and 25mL pipette.
b) Calibration of volumetric flask (100 mL)
1. A clean 100 mL volumetric flask was obtained.
2. The volumetric flask was weighed by using top loading balance and was
recorded.
3. The distilled water was filled into the small beaker.
4. The distilled water in small beaker was poured into volumetric flask until the
mark.
5. The temperature of water in volumetric flask was measured by using
thermometer and was recorded.
6. The volumetric flask with the distilled water was weighed again by using top
loading balance and was recorded.
7. The mass of water was obtained and converted into volume by using the
equation on Table 1.
8. Steps 1 until 7 were repeated 2 times.

c) Calibration of measuring cylinder (50 mL)

1. A clean 50 mL measuring cylinder was obtained
2. The measuring cylinder was weighed by using top loading balance and was
recorded.
3. The distilled water was filled into the small beaker
4. The distilled water in small beaker was poured into measuring cylinder until
the mark of 50 mL.
5. The temperature of water in measuring cylinder was measured by using
thermometer and was recorded.
6. The measuring cylinder with the distilled water was weighed again by using
top loading balance and was recorded.
7. The mass of water was obtained and converted into volume by using the
equation on Table 1.
8. Steps 1 until 7 were repeated 2 times.
 RESULT

A) DATA:
i. 10 mL pipette

Trial 1 Trial 2 Trial 3

Mass of container + 57.54 57.77 57.55
water (g)
Mass of container (g) 47.77 47.85 47.85
Mass of water (g) 9.77 9.92 9.70
Temperature (C) 28 28 28
Actual volume (mL) 9.817 9.968 9.747
Average volume (mL) 9.848
Standard deviation 0.113
Relative standard 0.0115
deviation

ii. 25 mL pipette

Trial 1 Trial 2 Trial 3

Mass of container + 72.29 72.34 72.35
water (g)
Mass of container (g) 47.77 47.84 47.85
Mass of water (g) 24.52 24.50 24.50
Temperature (C) 28 28 28
Actual volume (mL) 24.638 24.618 24.618
Average volume (mL) 24.625
Standard deviation 0.0116
Relative standard 0.000471
deviation
iii. 100 mL volumetric flask

Trial 1 Trial 2 Trial 3

Mass of container + 162.77 162.94 162.95
water (g)
Mass of container (g) 64.01 63.97 64.00
Mass of water (g) 98.76 98.97 98.95
Temperature (C) 28 28 28
Actual volume (mL) 99.234 99.445 99.425
Average volume (mL) 99.368
Standard deviation 0.117
Relative standard 0.00118
deviation

iv. 50 mL measuring cylinder

Trial 1 Trial 2 Trial 3

Mass of container + 117.18 117.39 117.11
water (g)
Mass of container (g) 68.12 68.30 68.38
Mass of water (g) 49.06 49.09 48.73
Temperature (C) 28 28 28
Actual volume (mL) 49.295 49.326 48.964
Average volume (mL) 49.195
Standard deviation 0.201
Relative standard 0.00409
deviation
[4 x15 marks]
 DISCUSSION

In this experiment, all measuring instruments are used to contain or to deliver the
specific volume of water. Only the instruments which have the higher accuracy are advisable
to be used for purpose of doing an experiment. To maintain the accuracy, all measuring
instruments must be calibrated first. All dry measuring instruments must be used to get an
actual mass. Wet measuring instruments would affect the measurements reading. All
measuring instruments contained the distilled water weighed again. The mass of water
[(mass of container + water) (mass of container)] and the actual volumes of water
contained or delivered by these measuring instruments were obtained. Average volumes,
standard deviation and relative standard deviation were calculated. The greater accuracy
also obtained by repeated the experiment.

Standard deviation from this experiment was a series of repetitive measurement to

measure the accuracy of the output reading from measuring instruments. The measurements
from the instruments should be in the tolerance as the reference standard. For example the
tolerance for 10 mL pipette is 0.02 mL so the measurements must be in the range of 9.98
mL to 10.02 mL at certain temperature. If the measurements were too higher or too lower
than tolerance it must be out of calibration and the measurements will have low accuracy.
Relative standard deviation use to compare the uncertainty between different measurements
of standard deviation.

If the value of data is near to the mean indicates low standard deviation and vice
versa. Lower standard deviation indicates higher accuracy of the measurements and vice
versa. The result from experiment shows the standard deviation for 10 mL pipette is 0.11.
The standard deviation for 25 mL of pipette is 0.01. The standard deviation for 100 mL
volumetric flask is 0.12. The standard deviation for 50 mL measuring cylinder is 0.20. All
measurements are not in the range of tolerance. All the data is further away from mean. It
shows high standard deviation that indicates the lower accuracy of the measurements.

From this experiment most of the data are not in the range of tolerance or accepted
values in range available. This happened due to error occurred during the experiment.
Parallax error was occurred due to eyes was above or below the meniscus or scale of
measuring instruments. To avoid this parallax error the eyes must be perpendicular to the
scale of the instruments. Another error is the remaining droplet of water was left in the
measuring instruments after the previous measurements. It was effected the accuracy of
measurements. To avoid this error, the measuring instruments should be dried and cleaned
before being weighed for all trials. Last but not least, the error occurred due to incorrect
technique using the instruments. For example, the remaining water was left in the tip of
pipette due to wrong technique of using this instrument. The recommendation is to conduct
the experiment with the consultant from professional for the right technique.

[10 marks]

CONCLUSION

From this experiment it can be conclude that calibration is vital for the purpose of
maintaining the accuracy of the instruments. Only the instruments with high accuracy must
be used when doing experiments. The accuracy was taken from standard deviation of
measurement. The lower standard deviation indicates the greater accuracy. Most of the value
of instruments measurement in this experiment did not in the range of tolerance. It shows
errors were occurred in this experiment and affect the data taken and the result. In the future,
caution plan must be taken to avoid any error occur during experiment.

[10 marks]

REFERENCES

1. Lab Manual General Chemistry, 17-27 August 2012

2. http://www.coleparmer.com/techinfo/techinfo.asp?
htmlfile=fluke_whycalibrate.htm&ID=296 , 17 August 2012
3. http://infohost.nmt.edu/~jaltig/VolumetricWare.pdf, 18 August 2012

APPENDIX

1. The definition for calibration:

The comparison between values of measuring instrument with values of
applied standard.
The evaluation and adjusting the accuracy and consistency of measuring
instruments.
The process of comparing and maintaining the relationship between the
output of measuring equipment with a standard
The indications of measuring equipment being adjusting to agree with
applied standard.
The process of checking and adjusting the measuring instruments
accuracy by comparing it with standard. [4
marks]
 ATT hhceelemdainsetai5ls0eudmrinwLgaotcfeymrliwnedaaessrufiwrlineagds iwnetoigahed by using top loading bal nce to the nearest
2. The flowchart of procedure for 50 mL measuring cylinder:

TTT hhheee dtmeismetaiplseeudrrainwtugaretceyorlifwnddaiessrtiplwoeiudthrewwdaatientertorwwmaasesamwseuearigisnhugerecddyalibngydaeiunrsbiunyngtuilsitnwgatsop loadin g

cmAsTmyihlliatnehlgdemrbarambswokavaserfnopwdbrtotahceredwuartesswobtesairn ecdoraned converted into vo lum e
Trthheaercmhecodtmuaehltevromaluanmrdketo,hfae5vd0earmat gLew avsolruemcoer,dsetadndard e viation and relative
bbreaypluensaictneegdasfnuodirta2thbteliemdeaqstuawtiaosn recorded
s ta n d a r d e v ia tio n w e r c a lc u la t e d . [10 marks]

3. Volume delivered by this 50 mL pipette at 28C :

= (grams of water) x (volume of 1g of water at 28C)
= (49.960 g) x (1.0048 mL)
= 50.199808 mL
= 50.200 mL
[6 marks]

TOTAL MARKS = 100

Sample of calculations

Note: [All measurements were taken on room temperature at 28C (1.000g of water
weighs in air occupies 1.00048 mL at 28C)]

a) 10 mL pipette
Actual volume for trial 1
= (9.77 g) x (1.0048)
= 9.816896 mL
= 9.817 mL
Actual volume for trial 2
= (9.92 g) x (1.0048)
= 9.967616 mL
= 9.968 mL
Actual volume for trial 3
= (9.70 g) x (1.0048)
= 9.74656 mL
= 9.747 mL
Average volume for all trials
= 9.817 mL + 9.968 mL + 9.747 mL
3
= 9.848 mL
Standard deviation
x ix


2
=
1
N 1

= 1
2
[(9.8179.848)2 +(9.9689.848)2 +( 9.7479.848)2 ]

= 1
2
[ ( 0.000991 )+ ( 0.0144 ) + ( 0.010201 ) ]

= 1
2
(0.025562)

= 0.012781
= 0.113053084
= 0.113
Relative standard deviation
= 0.113
9.848
= 0.115
b) 25 mL pipette
Actual volume for trial 1
= (24.52 g) x (1.0048)
= 24.637696 mL
 = 24.638 mL
Actual volume for trial 2
= (24.50 g) x (1.0048)
= 24.6176 mL
= 24.618 mL
Actual volume for trial 3
= (24.50 g) x (1.0048)
= 24.6176 mL
= 24.618 mL
Average volume for all trials
= 24.638 mL + 24.618 mL + 24.618 mL
3
= 24.624666667 mL
= 24.625 mL
Standard deviation
x ix


2
=
1
N 1

(24.63824.625)2 +(24.61824.625)2+(24.61824.625)2
1
= 2
[]

= 1
2
[ ( 0.000169 )+ ( 0.0000490 ) + ( 0.0000490 ) ]

= 1
2
(0.000267)

= 0.0001335
= 0.01155422
= 0.0116
Relative standard deviation
= 0.0116
24.625
= 0.0004710659898
= 0.000471

c) 100 mL volumetric flask

Actual volume for trial 1
= (98.76 g) x (1.0048)
= 99.234048 mL
= 99.234 mL
Actual volume for trial 2
= (98.97 g) x (1.0048)
= 99.445056 mL
 = 99.445 mL
Actual volume for trial 3
= (98.95 g) x (1.0048)
= 99.42496 mL
= 99.425 mL
Average volume for all trials
= 99.234 mL + 99.445 mL + 99.425 mL
3
= 99.368 mL
Standard deviation
x ix


2
=
1
N 1

(99.23499.368)2 +(99.44599.368)2+(99.42599.368)2
[ ]
= 1
2

= 1
2
[ ( 0.017956 ) + ( 0.005929 ) + ( 0.003249 ) ]

= 1
2
(0.027134)

= 0.013567
= 0.116477465
= 0.116
Relative standard deviation
= 0.116
99.368
= 0.001167377828
= 0.00116
d) 50 mL measuring cylinder
Actual volume for trial 1
= (49.06 g) x (1.0048)
= 49.295488 mL
= 49.295 mL
Actual volume for trial 2
= (49.09 g) x (1.0048)
= 49.325632 mL
= 49.326 mL
Actual volume for trial 3
= (48.73 g) x (1.0048)
= 48.963904 mL
= 48.964 mL
Average volume for all trials
= 49.295 mL + 49.326 mL + 48.964 mL
3
= 49.195 mL
Standard deviation

x ix


2
=
1
N 1


=

1
2
[(49.29549.195)2 +( 49.32649.195)2+(48.96449.195)2]
( 0.01 ) + ( 0.017161 ) +(0.053361)
1
=
2

= 1
2
(0.080522)

= 0.040261
= 0.200651439
= 0.201
Relative standard deviation
= 0.201
49.195
= 0.004085781075
= 0.00409