ABCT 3631 Metrology and Calibration

(5 Sep 2022)
Volumetric Instruments
Calibration
2

What is Calibration?
• For
Definition

“Operation that, under specified conditions,

in a first step, between the
# with provided by
AND
with associated * and,
in a second step, uses this information to a
for obtaining a from an
.”
____________________________________________
# e.g. rod length, body mass, sample temperature, …
* of the calibrated instrument or secondary standard
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3

Calibration
• when a result is from a , it
is to that value
to references allows
between

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4

Calibration
• a calibration may be expressed by
a , calibration , calibration
, calibration , or calibration
• may consist of or
of the with associated

• should be confused with of a

measurement nor with of

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Calibration
• set of that establish, under
, the between
indicated by a
or , OR
represented by a or
,
AND
the corresponding

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 Volumetric instruments
calibration methods
– The volume of the (distilled water
normally) dispensed from the volumetric glassware is
by of the water at
specific temperature
method
– The volume of tap water dispensed from the
volumetric glassware is calibrated by other graduated
glassware previously calibrated by gravimetric method
• For accurate calibration, gravimetric method is
preferred
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 Gravimetric method
• The volume of the pure water (distilled water normally)
dispensed from the volumetric glassware is calibrated by
measuring the mass of the water at specific temperature
𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀 𝑚𝑚
= ; ( 𝜌𝜌 = )
𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉 𝑉𝑉

= ;( )
is chosen is because is easy to be obtained and
the density is well characterized with different temperature
range
• Gravimetric calibration is a as it
builds to the base quantities (mass and
temperature)
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Terminology
• Conventional mass -
Conventional value of the result of weighing in air in
accordance with OIML D 28 - “Conventional value of the
result of weighing in air”
The unit of the quantity “conventional mass” is the
The value of a body is equal to the
that balances this body under
conventionally chosen conditions
The conventionally chosen conditions are:
reference temperature density of air as a reference
value equal to ; reference density of the
standard, i.e.
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of volume calibration at HK SCL

The measurement values of the SCL working

standard weight set are to the
as
illustrated in the traceability chart for mass
measurement.

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 Volumetric glassware

• Single-volume

• One-mark

• Graduated © BRAND GMBH + CO KG

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Factors affecting the accuracy of
volumetric instruments

of glass surface
of used volumetric
and

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 Parameters for volumetric apparatus
Parameters Description
Nominal Volume Cubic centimeter:
Ref. temperature
Apparatus is calibrated to
accurately transfer the
stated volume to another
container.
Apparatus is calibrated to
an accurate measure of
the volume contained
Class

© BRAND GMBH + CO KG

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 Classes of volumetric glassware
• Classes of accuracy - Classes /
– Class A and AS stand for higher grade
– ' stands for
(pipettes and burettes)
with wide neck are marked
with class (normally ) © BRAND GMBH + CO KG

: The long at
least of the tube perimeter or are present as ring
markings
Delivery time for bulb pipette
( )
Delivery time +
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 Classes of volumetric glassware
• Class
– stands for the in accuracy
– Generally of class
A/AS
– Graduation: The long
extend of the tube
perimeter © BRAND GMBH + CO KG

– Delivery time ( )
for 25 ml bulb pipette

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 Apparatus required for calibration

(De-ionized)
• Pipette sucker

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Precision of apparatus required
Selected Volume Balance Standard Linearity
under test Resolution Deviation*
V mg mg mg
< V <
1000 mL < V < 2000 mL 10
V > 2000 mL 100
*repeatability

Apparatus / Liquid Maximum Uncertainty

Thermometer
Hygrometer
Barometer
Calibration Liquid / De-ionized
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 Examples for volumetric errors
Parameter Parametric Volumetric error
tolerance relative to the
volume*
Water temperature ±0.5 ℃ ±10-4
Air pressure ±0.8 kPa ±10-5
Air temperature ±2.5 ℃ ±10-5
Relative humidity ±10 % ±10-6
Density of weights ±0.6 g/mL ±10-5
* a relative volumetric error of ±10-4 ( ) to the measured volume of
100 mL would be 0.01 mL [i.e. 100 mL x 0.5 ℃ x 2 x 10⁻⁴ ⁻℃]
* atmospheric pressure: ~101.325 kPa

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 Environmental requirement

– Maintained at and during calibration

– Maintained in range of ,
preferable to maintain at

– Volumetric instruments and test water

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 Cleaning of volumetric glassware
of volumetric glassware should be
carefully cleaned
• hydrophobic stain should be removed by suitable

in the cleaning solution for at

room temperature, then with ,
and finally with
and with a cloth or sponge
soaked in cleaning solution (no abrasive agents)
• be sure that vessel before commencing
calibration

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 Reading Meniscus level

must be
level
(
)

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© BRAND GMBH + CO KG
 Calibration Procedure
• Keep the involved at
• During the calibration
in the laboratory should
• Make sure the glassware is by the
calibration
• Make sure the used is well
the of the used
• Record the , and in
the test place

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 Calibration Procedure –
& Cylinders (to )
1. Measure and record the weight of empty testing flask
2. Fill distilled water up to the required mark of predefined
volume
3. Measure the weight of the testing flask with water in
4. Measure the using the
thermometer.
the above step 2 to 4 and record the
readings
6. Repeat the above step 2 to 5 for flask

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 Calibration Procedure –
(to )
1. Weigh a empty container and record the value
2. Fill pipette with distilled water up to the index mark
3. Any water on the outside of the tip is removed with filter
paper after the filling is completed
4. Transfer the distilled water to empty vessel weighed in step (1)
5. Weigh the vessel with distilled water
6. Measure of distilled water using the thermometer
the above steps

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Calibration Procedure –
(to )

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© BRAND GMBH + CO KG
 Calibration Procedure –
(to )
1. Weigh empty container and record the value
2. Fill burettes with distilled water up to the index mark
on the is with filter paper after the
filling is completed
4. Transfer the distilled water to empty vessel weighed in step (1)
5. Weigh the vessel with distilled water
6. Measure of distilled water using the thermometer.
the above steps and record in the data recording form
the above steps 1 to 7 for burettes at least

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 Correction of volumetric calibrations
1
𝑉𝑉𝟐𝟐𝟐𝟐 = − × 1 − × 1 − − 20
−

𝑉𝑉𝟐𝟐𝟐𝟐 volume at the reference temperature of

- balance reading of (reference liquid) in g
- balance reading of in g
- in g/mL

- when weighing in air as though the is

- at in g/mL
- of the material of which the
item of under tested is made of, in reciprocal °C
- of the used in the testing in °C
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Density of air at various temperature and pressure

1 atm = 1 013.25 hPa

© ISO 4787-2010 27
of &

© ISO 4787-2010

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 Simplified version
To calculate the instrument’s volume 𝑉𝑉20 at a reference
temperature of 20 ℃ from the apparent mass obtained by
using a balance, a factor Z can be introduced as follows:
𝑉𝑉20 = ×
- is the balance reading of vessel with water reference
liquid in g
- is the balance reading of empty vessel in g
• Using values given in * for different types of
glass at various &
B6 (borosilicate glass 3.3),
B7 (borosilicate glass 5.0) and
B8 (soda-lime glass) *ISO 4787:2011

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requirement of

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requirement of

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requirement of

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 Maximum permissible errors for
( )

Maximum permissible error*

Nominal Capacity
(mL)
Class A (mL) Class B (mL)

50 ± 0.060 ± 0.12

100 ± 0.100 ± 0.200

250 ± 0.150 (0.06%) ± 0.300

*extreme value of measurement error, with respect to a known reference quantity

value, permitted by specifications or regulations for a given measurement,
measuring instrument, or measuring system

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 Maximum permissible errors for
( )
Nominal Capacity Subdivision Maximum permissible error
(mL) (mL) Class A and AS (mL) Class B (mL)
1 0.01 ± 0.006 ± 0.01
2 0.01 ± 0.01 ± 0.02
5 0.01 ± 0.01 ± 0.02
5 0.02 ± 0.01 ± 0.02
10 0.02 ± 0.02 ± 0.05
10 0.05 ± 0.03 ± 0.05
25 0.05 ± 0.03 ± 0.05
25 0.10 ± 0.05 ± 0.10
50 0.10 ± 0.05 (0.1%) ± 0.10
100 0.20 ± 0.10 ± 0.20

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 Maximum permissible errors for
( )
Nominal Capacity Maximum permissible error
(mL) Class A and AS (mL) Class B (mL)
0.5 ± 0.005 ± 0.010
1 ± 0.008 ± 0.015
2 ± 0.010 ± 0.02
5 ± 0.015 ± 0.03
10 ± 0.02 ± 0.04
20 ± 0.03 ± 0.06
25 ± 0.03 (0.12%) ± 0.06
50 ± 0.05 ± 0.10
100 ± 0.08 ± 0.15

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 Maximum permissible errors for ( )
Nominal Capacity Subdivision Maximum permissible error
(mL) (mL) Class A and AS (mL) Class B (mL)
0.1 0.01 ± 0.006 ± 0.01
0.2 0.01 ± 0.006 ± 0.01
0.5 0.01 ± 0.006 ± 0.01
1 0.01 ± 0.007 ± 0.01
1 0.10 ± 0.007 (0.7%) ± 0.01 9 (1%)
2 0.02 ± 0.010 ± 0.02
2 0.10 ± 0.010 ± 0.02
5 0.05 ± 0.030 ± 0.05
5 0.10 ± 0.030 ± 0.05
10 0.1 ± 0.05 (0.5%) ± 0.1 (1%)
20 0.1 ± 0.1 ± 0.1
25* 0.1 ± 0.1 ± 0.1
25 0.1 ± 0.1 ± 0.1
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*length 450mm
Suggested operating temperature limits
for Class A glassware
Volume / cm3 Temperature limits / ℃
10 < 31
50 10 - 26
100 13 - 25
250 16 - 23
1000 17 - 22
• For example, an aqueous volumetric solution occupying
100 cm3 at 20 ℃ will have volume of
99.9 cm3 at 13 ℃ [i.e. 100 mL x 7 ℃ x 2 x 10⁻⁴ ⁻℃] or
100.1 cm3 at 25 ℃ [i.e. 100 mL x 5 ℃ x 2 x 10⁻⁴ ⁻℃]
i.e. 0.1% of 100 mL
• At temperatures below 13 ℃ or above 25 ℃ the volume will exceed the
Class A tolerance (100 cm3 ± 0.1%)

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EN ISO 8655−2:2002

7.2 Fixed-volume piston pipettes of types A and D1

Table 1 — Maximum permissible errors for types A and D1

Nominal volume Maximum permissible systematic error Maximum permissible random error
µl ±% ± µl a ± %b ± µl c
1 5,0 0,05 5,0 0,05
2 4,0 0,08 2,0 0,04
5 2,5 0,125 1,5 0,075
10 1,2 0,12 0,8 0,08
20 1,0 0,2 0,5 0,1
50 1,0 0,5 0,4 0,2
100 0,8 0,8 0,3d 0,3d
200 0,8 1,6 0,3d 0,6d
500 0,8 4,0 0,3 1,5
1 000 0,8 8,0 0,3 3,0
2 000 0,8 16 0,3 6,0
5 000 0,8 40 0,3 15,0
10 000 0,6 60 0,3 30,0
a Expressed as the deviation of the mean of a tenfold measurement from the nominal or selected volume (see ISO 8655-6:2002, 8.4).
b Expressed as the coefficient of variation of a tenfold measurement (see ISO 8655-6:2002, 8.5).
c Expressed as the repeatability standard deviation of a tenfold measurement (see ISO 8655-6:2002, 8.5).
d For piston pipettes of type D1 the maximum permissible errors may be ± 0,4 %.

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EN ISO 8655−2:202

7.4 Variable-volume piston pipettes

Table 2 — Maximum permissible errors for type D2

Nominal volume Maximum permissible systematic error Maximum permissible random error
µl ±% ± µl a ± %b ± µl c
5 2,5 0,13 1,5 0,08
10 2,0 0,2 1,0 0,1
20 2,0 0,4 0,8 0,16
50 1,4 0,7 0,6 0,3
100 1,5 1,5 0,6 0,6
200 1,5 3,0 0,4 0,8
500 1,2 6,0 0,4 2,0
1 000 1,2 12,0 0,4 4,0
a Expressed as the deviation of the mean of a tenfold measurement from the nominal or selected volume (see ISO 8655-6:2002, 8.4).
b Expressed as the coefficient of variation of a tenfold measurement (see ISO 8655-6:2002, 8.5).
c Expressed as the repeatability standard deviation of a tenfold measurement (see ISO 8655-6:2002, 8.5).

Repetitive piston pipettes with a continuously selectable volume shall be considered as variable-volume piston
pipettes of type D2 and the maximum permissible errors of Table 2 shall apply.

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 Auto pipette
• Air displacement type of
pipette
• Use partial vacuum to
draw liquid up
• Mainly for aqueous
sample

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1. Preparation 2. Aspiration
Hold the instrument in a Immerse the pipette tip in the
nearly vertical position. liquid*. Allow the plunger to
Depress the plunger smoothly move up smoothly to the rest
to the first stop position. position. Wait so
that all the liquid has time to
move up into the tip.

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3. Distribution
Place the pipette tip at an
angle ( °)
of the receiving
vessel. Depress the plunger
to the first stop
position.
4. Purge 5. Home
Wait , then depress Allow the plunger to move up
the plunger to the second stop to the rest position.
position. This “ ” stroke
removes any remaining sample
from the tip. Remove pipette tip
end from sidewall by sliding it up
the wall.
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 References
• ISO 385:2005 Laboratory glassware –
• ISO 648:2008 Laboratory glassware - Single-volume

• ISO 835:2007 Laboratory glassware - Graduated

• ISO 1042:1998 Laboratory glassware - One-mark

• ISO 4787:2021 Laboratory glassware - Volumetric

instruments – for testing of capacity and for
use

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Thank You

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