1.0
Objective:
To provide the
procedure for calibration of Volumetric Glassware.
2.0 Scope:
This SOP covers all the volumetric glasswares received in the
laboratory, which includes volumetric
flasks, burettes, and volumetric pipettes.
3.0
Responsibility:
Jr.
Research Officer /Research Officer
Calibrate the glassware and record the observation of calibration.
QA Officer/QA Manager: Review the records and
governing the document.
4.0 Procedure:
4.1 Pharmacopoeial assay and tests involving
volumetric measurements require the use of accurately calibrated glassware.
4.2 All the volumetric glassware shall be
calibrated at 27° C.
4.3 Calibration
procedure for 5 ml to 100 ml volumetric flask:
4.3.1 Weigh the empty volumetric flask on a
precision analytical balance and record the weight (E).
4.3.2 Fill the volumetric flask up to mark with
purified water maintained at 27° C and wipe the outer surface with a tissue
paper.
4.3.3 Again weigh the flask and record the weight
(F).
4.3.4 Subtract weight ‘E’ from weight ‘F’. The resulting
weight should be within the limits as given in the Table - 1.
4.3.5
Simultaneously calibrate one
class A flask and compare the results along with the
certificate received for the same. Record the observation of class A
glassware calibration
in the format as given in Annexure - 2. Continue the calibration of
class B glassware if
class A glassware calibration is
found to acceptable.
4.4 CALIBRATION
PROCEDURE FOR VOLUMETRIC FLASKS 200 ml
TO 1000 ml
4.4.1 Tare one 100 ml beaker on a precision
analytical balance.
4.4.2 Fill the beaker with water and record the
weight.
4.4.3 Quantitatively transfer water from the
beaker to the volumetric flask under calibration.
4.4.4 Record the weight of water transferred to
the flask, each time.
4.4.5 The sum of the weights of water transferred
to the flask up to the mark gives the total weight of water in the flask.
4.4.6 Record the
observations. The weight shall be within the limits as given in Table - 1. (Annexure - 1)
4.5 CALIBRATION PROCEDURE
FOR BURETTES:
4.5.1 Fill the burette with
water up to zero of the burette.
4.5.2 Collect the water from
the burette in a tarred beaker, weigh and record the weight.
4.5.3 For
10 ml burette record the weight of water at each ml up to 10 ml. For a 25 ml
burette record the weight of water at the interval of 5ml. (i.e. 5ml, 10ml,
15ml, 20ml and 25 ml)
4.5.4 For
a 50 ml burette, record the weight of water at the interval of 10 ml. (i.e. 10
ml, 20 ml, 30 ml, 40 ml and 50 ml).
4.5.5 The
weights observed shall be within the limits as given in Table - 2.
(Annexure-1).
4.6 CALIBRATION
PROCEDURE FOR PIPETTES:
4.6.1 Fill
the pipette with water up to mark of the pipette.
4.6.2 Collect
the water from the pipette in a tarred beaker, weigh and record the weight.
4.6.3 The
weights observed shall be within the limits as given in Table - 3.
(Annexure-1).
4.7 Record
the observation in the log book as given in Annexure - 2.
4.8
All the calibrated volumetric flask shall be numbered using a permanent
glass marker as follows: Department Name
/ Glassware Name/Glassware strength - 001
Where’
Department Name (H for HPLC, W
for Wet chemistry, M for microbiology, G for GC and A for AAS).
Glassware
name (F for volumetric flask, B for burette, P for pipette and GP for Graduated
pipette.
Glassware strength (1 for 1ml, 5 for 5 ml, 25 for 25 ml, 100 for 100 ml
etc.)
001
is serial No.
4.9 At 27° C, 1 ml of water is equivalent to 0.99549 g.
4.10 The calibration record shall be checked by QA Officer.
4.11 If the volumetric glassware is not within the limits of
calibration discard the glassware.
5.0 Precautions:
5.1 Use clean and dried volumetric glassware at the time of
calibration.
5.2 Ensure that the glassware is maintained at 27° C at the time
of calibration.
5.3 Use lower meniscus for calibration.
6.0 Documentation:
6.1 Annexure – 1 -Tables.
6.2 Annexure – 2 -Glassware calibration record format with
uncertainty: XXX/FRM/000-007.0 History of Revision:
Revision No.
|
Effective
Date
|
Revision
details
|
Reason for
revision
|
01
|
DD/MM/YEAR
|
---------
|
-----
|
Annexure - 1
|
||||||||||||||||||||||||||||||
Table - 1 (Volumetric
flasks)
|
||||||||||||||||||||||||||||||
Nominal
Capacity, ml
|
5
|
10
|
20
|
25
|
50
|
100
|
200
|
250
|
500
|
1000
|
||||||||||||||||||||
Tolerance
Class A
|
± ml
|
0.02
|
0.02
|
0.03
|
0.04
|
0.06
|
0.1
|
0.15
|
0.2
|
|||||||||||||||||||||
+ in g
|
||||||||||||||||||||||||||||||
- in g
|
||||||||||||||||||||||||||||||
Tolerance
Class B
|
± ml
|
0.04
|
0.04
|
0.04
|
0.06
|
0.08
|
0.15
|
0.15
|
0.20
|
0.30
|
0.80
|
|||||||||||||||||||
+ in g
|
||||||||||||||||||||||||||||||
- in g
|
||||||||||||||||||||||||||||||
Table
– 2 (Burettes)
|
||||||||||||||||||||||||||||||
Nominal Capacity, ml
|
10
|
25
|
50
|
100
|
||||||||||||||||||||||||||
Tolerance,
Class A
|
±
ml
|
0.01
|
0.03
|
0.05
|
0.1
|
|||||||||||||||||||||||||
+
in gm
|
||||||||||||||||||||||||||||||
- in gm
|
||||||||||||||||||||||||||||||
Tolerance,
Class B
|
±
ml
|
0.02
|
0.06
|
0.1
|
0.2
|
|||||||||||||||||||||||||
+
in gm
|
||||||||||||||||||||||||||||||
-
in gm
|
||||||||||||||||||||||||||||||
Table
– 3 (Pipettes)
|
||||||||||||||||||||||||||||||
Nominal
Capacity, ml
|
1
|
2
|
3
|
4
|
5
|
10
|
15
|
20
|
25
|
50
|
||||||||||||||||||||
Tolerance
class A
|
± ml
|
0.01
| 0.01 | 0.01 | 0.01 | 0.02 | 0.02 | 0.02 | 0.03 | 0.03 | 0.04 | |||||||||||||||||||
+ in g
|
||||||||||||||||||||||||||||||
- in g
|
||||||||||||||||||||||||||||||
Tolerance
class B
|
± ml
|
0.02
|
0.02
|
0.02
|
0.02
|
0.03
|
0.04
|
0.04
|
0.05
|
0.06
|
0.08
|
|||||||||||||||||||
+ in g
|
||||||||||||||||||||||||||||||
- in g
|
||||||||||||||||||||||||||||||
Table
– 3 (Graduated Pipettes)
|
||||||||||||||||||||||||||||||
Nominal Capacity, ml
|
1
|
2
|
5
|
10
|
25
|
|||||||||||||||||||||||||
Subdivision, ml
|
0.01
|
0.02
|
0.05
|
0.10
|
0.20
|
|||||||||||||||||||||||||
Tolerance
class A
|
±
ml
|
0.006
|
0.01
|
0.03
|
0.05
|
0.10
|
||||||||||||||||||||||||
+ in g
|
||||||||||||||||||||||||||||||
-
in g
|
||||||||||||||||||||||||||||||
Tolerance
class B
|
±
ml
|
0.02
|
0.06
|
0.10
|
0.15
|
0.15
|
||||||||||||||||||||||||
+ in g
|
||||||||||||||||||||||||||||||
-
in g
|
||||||||||||||||||||||||||||||
SOP
No. : XXX/SOP/000-00
|
||||||||||||||||||||||||||||||
Annexure - 2
|
|||||
Glassware Calibration Record
|
Page No. : 01 of 02
|
||||
Name of Glassware
|
:
|
||||
Glassware ID No.
|
:
|
||||
Date of
Calibration
|
:
|
||||
Balance ID No.
|
:
|
||||
Temperature of Water used for calibration
|
:
|
||||
Correction Factor of Temperature
|
:
|
||||
Sr. No.
|
Weight of Empty Flask / beaker in gm
|
Weight of Empty Flask / beaker + water in gm
|
Weight of water in gm
|
||
1
|
|||||
2
|
|||||
3
|
|||||
4
|
|||||
5
|
|||||
Average =
|
|||||
Capacity of
Glassware in ml
|
Weight of Water in gm +
Correction Factor of Temperature
|
||||
= ml
|
|||||
Tolerance
|
Capacity of
Glassware in ml – Nominal capacity
|
=
Limit :
|
|||
Calibrated
by :
Checked by :
|
|||||
SOP No. : XXX/SOP/000-00 Format No. : XXX/FRM/000-00
|
|||||
Annexure – 2
|
|||||
Uncertainty Measurement of Glassware
|
Page No. : 02 of 02
|
||||
Name of Glassware
|
:
|
||||
Glassware ID No.
|
:
|
Sr. No.
|
Weight of water in gm
|
||
Date of Calibration
|
:
|
1
|
|||
Balance ID No.
|
:
|
2
|
|||
Uncertainty of
Balance for gm
|
:
|
3
|
|||
Co-efficient of Volume Expansion of water
|
:
|
4
|
|||
Temperature Variation in Laboratory
|
:
|
5
|
|||
Degree of
Freedom (V1) = n -1
Where n = number of Observation
|
:
|
Mean
|
|||
SD
|
|||||
TYPE A UNCERTAINTY (U1)
:
Uncertainty
due to repeat Observations (U1) = SD = = g/ml
V-n-
TYPE
B UNCERTAINTY :
Due to Balance(U2) :
For g (below) is ± mg for 95 % normal distribution
U2 = = mg = g = ml
Due
to Temperature Coefficient (U3) :
U3 = Coefficient of volume Expansion of water
X Nominal of Glassware X Temperature Variation
Distribution Factor
U3 =
COMBINE UNCERTAINTY (Uc) = [(U1)2 + (U2)2 + (U3)2 ]1/2
(Uc) =
Effective
Degrees = (Combine Uncertainty) 1/2 =
of
Freedom (U1)n-1 + (U2)n-1 + (U3)n-1
n-1 n-1 n-1
VEFF =
_____________________ hence K
Value is __________@ 95 % Confidence
Level
Expanded
Uncertainty is UE = Combine Uncertainty X Coverage Factor
|
|||||
SOP No. : XXX/SOP/000-00 Format No. : XXX/FRM/000-00
|
|||||
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