Identification:

Procedure for calibration PROC-TC-012

Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

PROC - A

WORK PROCEDURE

FOR

CALIBRATION OF MICRO PIPETTES

Page 1 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

Table of contents

CONTENTS PAGE NO.

1. Purpose 3
2. Scope 3
3. Normative References 3
4. Terms And Definition 3
5. General Requirements 5
6. Weighing Equipment Used 5
7. Operation of Pipette 6
8. Gravimetric Procedure for Calibration 8
9. Calculations 10
10. Calculations for Measurement Uncertainty 11
11. Associated Documents 16
12. APPENDIX A 17

Page 2 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

1.0 Purpose
Purpose of this Lab Calibration Procedure is to provide guideline for the calibration of
volumetric piston pipette.

2.0 Scope

Calibration of automatic pipettes (as per BS EN 8655-2) from 1µl to 10ml:

 with fixed volume
 with adjustable volume

3.0 Normative references

 BS EN 8655-2: Piston pipettes.

 BS EN 8655-6: Gravimetric methods for the determination of measurement error.
 ISO/TR 20461:2000: Determination of uncertainty for volume measurements made using
the gravimetric method
 Operating Manual of Mettler microbalance
 Quality Manual of Calibration Services ISO/IEC 17025.

4.0 Terms and definitions

For the purpose of this Lab Calibration Procedure following definitions shall apply:
4.1 Calibration
The set of operations which establishes under specific conditions the relationship between
value indicated by a measuring instrument or measuring system or values represented by a
material measure and the corresponding known value of the measurand.
4.2 Traceability
The property of a measurement result whereby it can be related to appropriate standards
generally national or international standards through an unbroken chain of comparisons.
4.3 Measurement Standards
A Material measure, measuring instrument or system intended to define, realize, conserve or
reproduce a unit by one or more known value of a quantity, in order to transmit them to other
measuring instruments by comparison.
Note
In this method a measurement standard is the “Unit under Calibration”.
4.4 UUC (Unit under Cal)
Unit under Cal is the instrument, which is being calibrated by this method statement.

4.5 Reference Standard

A standard generally of a highest metrological quality available from which measurements
made at a given location are derived.
Page 3 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

4.6 Uncertainty of Measurement

It is an estimate of the uncertainty of the result of a calibration. The estimate is obtained by
multiplying the combined uncertainty by a coverage factor.
4.7 Internal Uncertainty or Type “A”
The component of uncertainty, which is caused by type “A” errors and is evaluated from the
measurement results using statistical methods.
4.8 External Uncertainty or Type “B”
It is the component of uncertainty, which is caused by Type “B” errors and is evaluated by
non-statistical methods from the external factors having influence on the measurement
4.9 Repeatability
The degree of agreement between results of successive measurements of the same measurand
carried out under identical conditions, with identical methods and over a short period of time.
4.10 Resolution
Smallest difference that can be meaningfully distinguished (e.g. a change of one (1) in the last
place of a digital display)
4.11 Maximum permissible error
Extreme values of error permitted by specification / class
4.12 Adjustment
Altering the pipette so that the dispensed volume is within the specifications.
4.13 Air Displacement Pipettes
These are meant for general use with aqueous solutions. In air displacement pipettes, a certain
volume of air remains between the piston and the liquid.
4.14 Aspirate
To draw up the sample.
4.15 Blow-out
To empty the tip completely.
4.16 Calibration check
Checking the difference between the dispensed volume and the selected volume.
4.17 Dispense
To deliver the sample.
4.18 Positive Displacement Pipettes
These are used for high viscosity and volatile liquids. In positive displacement pipettes, the
piston is in direct contact with the liquid.
4.19 Ambient pressure
The pressure surrounding a device, often equal to the prevailing atmospheric pressure.
Page 4 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

4.20 Fixed Volume pipette

Those which are designed and supplied by the manufacturer to dispense a specific, fixed
volume of liquid (defined as the nominal volume).
4.21 Variable volume pipette
Those in which the user can adjust the volume of liquid to be dispensed over a range
specified by the manufacturer.
5.0 General Requirements
5.1 Laboratory Environment
The Calibration is carried out in controlled environment i.e. Temperature 21 °C ± 5°C and
temperature stability of ± 1 °C during calibration, Relative Humidity 35~65 % rh and
ambient pressure 1014 ± 10 hPa. If the environmental conditions are exceeding specified
limits, calibration will be stopped and measures will be initiated to control the environment
within specified limits. The apparatus and samples should be allowed to stabilize in the
laboratory before any work is carried out. Two hours is normally adequate for this.

5.2 Preliminary Inspection

1. Check the pipette at the beginning of working day for dust and dirt on the outside. If
needed, wipe with 70% ethanol.
2. Check that the tips using, are recommended by the manufacturer. To ensure accuracy, use
only high-quality tips made from contamination- free polypropylene.
3. Tips are designed for single use. They should not be cleaned for reuse, as their metrological
characteristics will no longer be reliable.
4. Pre-rinsing (three to five times) the tip with the liquid to be pipetted improves accuracy.
This is especially important when pipetting volatile compounds since it prevents liquid from
dripping out of the tip.
5. Pipette parallel samples in a similar way.
6. Avoid turning the pipette on its side when there is liquid in the tip. Liquid might get into the
interior of the pipette and contaminate the pipette.
7. Avoid contamination to or from hands by using the tip ejector.
8. Always store pipettes in an upright position when not in use.

6.0 Weighing Equipment Used

 Microbalance

6.1 Requirements of Weighing Equipment

Page 5 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

1. Performance of gravimetric calibration procedure of a pipette requires use of a weighing

instrument with metrological parameters as described in norm ISO 8655-6.
Tested volume (V) Reading Unit Repeatability and Standard Deviation of
d(mg) Linearity measurement
1μl ˂ V ˂ 10μl 0.001 0.002 0.002
10μl ˂ V ˂ 100μl 0.01 0.02 0.02
100μl ˂ V ˂ 1ml 0.1 0.2 0.2
1 ml ˂ V ˂ 10ml 0.1 0.2 0.2
10 ml ˂ V ˂ 200ml 1 2 2

Table.1 Minimal requirements for weighing instruments (according to ISO 8655-6)

In case, where standard deviation of liquid measurement is specified, than it is possible to use
it as acceptance criterion instead of repeatability and linearity parameters of a weighing
instrument. However, it needs to be assumed, that standard uncertainty is not bigger than
twofold or threefold of reading unit d.

In order to maintain measurement re-traceability, a weighing instrument that is utilized for

pipette calibration, should have valid calibration certificate. When analyzing requirements of
the norm with regard to equipment of a workstation and ambient conditions which influence
the result, there have been certain tests performed, which confirm the provisions from the
norm. The results of such tests and conclusions drawn from them are helpful in analyzing
measurement process of pipette checking and calibration.

7.0 Operation of pipette

7.1 General Instruction

1. A pipette is calibrated, and should be held in the vertical position when aspirating the liquid.
The depth to which the tip should be immersed within the liquid varies with the size, type and
make of pipette.

Pipette Volume Immersion Depth

μl (mm)
1-100 2-3
100-1000 2-4
1000-5000 2-5
Table.2 Guide to depth of tip immersion

Note: To improve accuracy, air displacement pipettes are usually pre-wetted by filling them
several times with the liquid being dispensed and expelling it to waste. This reduces the
chance of air bubbles being aspirated, especially with viscous or hydrophobic liquids, and
also allows the humidity of the dead air volume between the piston and liquid to stabilize –
particularly significant when using liquids with a high vapor pressure. However, low volume
air displacement pipettes of less than about 10 µl are usually designed to be used without
pre-wetting. It is not normally necessary or desirable to pre-wet positive displacement pipette

Page 6 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

2. After filling the pipette, any drops adhering to its tip should be carefully removed by
touching it against the side of the vessel containing the liquid. If necessary, any surplus
liquid still adhering to the outside of the tip can be carefully wiped off with a suitable
material taking care to avoid contamination. Check that no further drops are forming at the
orifice. This could be an indication of a poorly fitting tip or instability in the dead air
volume, particularly in the case of a liquid with a high vapor pressure.

3. The procedure for dispensing a liquid is to touch the tip of the pipette against the wall of the
receiving vessel just above the liquid surface at an approximate angle of 30° to 45° and draw
it up for 8 mm – 10 mm after dispensing is complete.

4. The liquid used for testing is pure water conforming to grade 3 of ISO 3696, Water for
Analytical laboratory use – Specification and test methods

Pipettes should be periodically inspected to see that they are functioning correctly, and
whether they have sustained any detrimental wear or damage. Solvents used for cleaning
should be appropriate for removing the liquid the pipette has been used with.

Warning:
If a pipette has been in contact with any substances regarded as hazardous to health as
defined in the current COSHH or Ionizing Radiations regulations, it is the responsibility of
the user to ensure that it is thoroughly decontaminated before it leaves the laboratory. . A
certificate of decontamination should accompany the pipette giving its make, model and
serial number, and listing any hazardous materials that have been used with the device and
any agents used to clean it.

7.2 Operational Procedures

7.2.1 Conventional Method

The usual method of use for a typical hand operated air displacement single channel pipette
with two stop positions is illustrated below. The manufacturer’s instructions should always be
examined to see if any departure from the below method.
1. Attach tip to tip holder taking care to avoid contamination. Hold pipette comfortably in one
hand with thumb resting on plunger
2. Press the plunger down smoothly to the first stop position. At this stage the pipette tip must
not be immersed in the liquid.
3. Immerse the tip of the pipette in liquid to the correct depth (Table 2). Keep the pipette in a
vertical position and release the plunger in a smooth and uniform manner to aspirate the
liquid.
4. Ensure that the plunger extends fully to its upper stop position and wait one or two seconds
before withdrawing the tip of the pipette from the liquid.
5. Touch the pipette against the wall of receiving vessel at an angle of about 30° to 45°. Be
careful to not immerse the tip in any liquid already in the receiving vessel.
6. Expel the contents of the pipette by pressing the plunger down steadily and evenly to first stop
position while keeping the tip in contact with the wall of the vessel. Wipe the tip for 8 mm to
10 mm to remove any remaining liquid.

Page 7 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

7. Push plunger down to second stop. This will force air through the tip to expel any remaining
liquid.
8. Remove tip from the solution and release the plunger

7.2.2 Reverse Pipetting

A variation of the conventional method, termed reverse pipetting, is often useful when dealing
with liquids that have a high vapor pressure or those which are very viscous.
1. Press the plunger down fully, past the first stop position to the second stop position. At this
stage the pipette tip must not be immersed in the liquid.
2. Immerse the tip of the pipette in the liquid to the correct depth. Keep the pipette in a vertical
position and release the plunger in a smooth and uniform manner to draw up the liquid.
3. Ensure that the plunger extends fully to its upper stop position. Check the tip to make sure no
drops are forming at the orifice.
4. Touch tip against wall of receiving vessel and expel the contents of the pipette by pressing the
plunger down steadily and evenly, but only to the first stop position.
5. Touch pipette against wall of delivery vessel at correct angle. Be careful to not immerse tip in
any liquid already in receiving vessel.
6. Note that some liquid will be left in the tip after dispensing. This should be returned to the
original vessel.

8.0 Gravimetric Procedure for calibration

Calibration is an operation to determine the actual volume delivered by a pipette together with
an uncertainty associated with that volume. Variable volume pipettes are designed to deliver
accurate and repeatable volumes over their adjustable range, and should only require periodic
calibration. However, some fixed volume pipettes can be adjusted over a small range to
compensate for minor deviations from their nominal volume which become apparent during
calibration. Similarly, some pipettes are designed to be adjustable so that they can dispense
(after calibration) the correct nominal volume of a liquid other than water. In both cases
details of the adjustment made (and the calibration liquid used, if appropriate) must be clearly
affixed to the pipette itself, recorded on any certificate of conformity and incorporated in the
user’s quality manual.

The basic principal of gravimetric testing is to weigh the amount of pure water delivered in a
single operation of the pipette, and divide the mass obtained by the density of the water, thus
giving its volume.

A physical relationship described by a formula:

V = m/ρ (1)

In practice, a number of repeat measurements are made to which corrections must be applied
to compensate for any variation from standard temperature and atmospheric conditions, and
any significant evaporation of the water during the test period.

Reference with BS EN ISO 8655-6:2002, which describes in detail a gravimetric procedure

for testing piston pipettes as follows,
Page 8 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

1. For most air displacement pipettes, a new tip should be fitted and water from the reservoir
vessel aspirated and expelled to waste five times. This allows the humidity in the dead air
volume to stabilize. For some low volume pipettes and direct displacement pipettes, this pre-
wetting operation is omitted unless specified in the manufacturer’s or supplier’s instructions.
2. Add water to the weighing vessel to a depth of at least 3 mm. immediately before starting a
test run record the temperature of the water, and the ambient air pressure and relative
humidity. Replace the lid (if used) on the weighing vessel. Record the balance reading or null
the balance.
3. Fill the pipette with water from the reservoir vessel and dispense it into the weighing vessel.
The water should be aspirated and dispensed in the same way as conventionally used for
routine work. Use the ‘blow out’ feature if fitted to expel any remaining liquid. Record the
new balance reading. The time taken for a complete cycle should be kept to a minimum
consistent with the smooth and careful transfer of the water – preferably less than 60 seconds.
4. Repeat the operations described in the last paragraph a further nine times. At the end of each
cycle record the balance reading.
5. At the conclusion of the tenth cycle, record the temperature of the liquid in the weighing
vessel and the total elapsed time.
6. If evaporation is likely to be significant, e.g. when testing small volume pipettes, the balance
reading should be recorded once again after leaving the weighing vessel on the balance pan
for a further period equal to the elapsed time of the test run. If a cover has been used on the
weighing vessel this should be left in position. Dividing the mass of water lost in this period
by 10 will give a working approximation of the average mass loss per cycle.
The weighing vessel should be touched only at the edge to avoid heating or residues of hand
sweat. If necessary, gloves are to be used. When smaller volumes are weighed, it is
recommended to use gripping devices (e.g. tweezers) when handling the weighing vessel and
to cover the vessel. The weighing vessel used should go with the weighing instrument, the
dispensed volume and a prefilling possibly made. The prefilling in the weighing vessel leads
to more uniform evaporation effects and thus reduces measurement deviations caused by
evaporation during calibration.

9.0 Calculations

a) Calculate the mass of water delivered for each cycle by subtracting the balance reading
recorded at the end of the previous cycle from the reading recorded at the end of the cycle. If
appropriate, add the mass of water lost by evaporation as determined in the previous
paragraph.
b) To convert each mass value to a volume at 20 °C (the standard reference temperature for the
calibration of pipettes) it must be divided by the density of water corrected to 20 °C. A
correction for air buoyancy, which varies with the air density, must also be applied. Both
these factors are taken into account by multiplying the each mass value by a correction factor
Z. A table specifying the value of Z for a temperatures range of 15 °C and 30 °C and air

Page 9 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

pressure range of 80 kPa to 105 kPa is given as Annex A in BS EN ISO 8655-6:2002. The
correction factor is also given as an equation in ISO/TR 20461:2000.

The volume V is calculated according to the following

V=W .Z.Y (2)

Where net weighed value,

W =W2-W1 (3)

(4)

(5)

(6)
Where,
V = volume in ml
W2 = weighed value of the vessel with calibration liquid in g
W1 = weighed value of the empty vessel in g
ρL = density of the air in g/cm³
ρG = density of the weights in g/cm³ (standardized value for steel weights: 8000 kg/m³
= 8 g/cm³)
ρw = density of the calibration liquid in g/cm³
αc = cubic expansion coefficient in 1/K
td = temperature of the volumetric apparatus in °C (for simplification equated with the
temperature of the calibration liquid)
tb = reference temperature in °C
The water density ρw and the air density ρL can be calculated with the formulas stated in
appendix A

c) Add together each of the 10 volumes calculated in the previous paragraph and divide by 10 to
give the mean volume at 20 °C. This can be expressed in microliters or milliliters.

(7)
9.1 Error characteristics of piston pipettes

ISO 8655-6 describes 2 types of errors for piston pipettes

1. Systematic error is expressed in volumetric units, microliters [ul] and percent [%].It is
marked with es symbol and calculated with a formula:

(8)
Page 10 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

(9)
Where:
Vs – stands for value of tested volume

2. Random error is expressed in volumetric units: microliters [ul] and percent’s [%]. Random
error is marked with CV symbol. The measure of random error is standard deviation
calculated by a formula

(10)

(11)

10.0 Calculation of a Measurement Uncertainty

Determination of uncertainty is calculated according to the Technical Report ISO/TR

20461:2000 – edition 1 together with a correction note ISO/TR 20461:2000/Cor.1:2008

1. A conventional volume of a calibrated pipette in temperature 20 ºC is determined by the

following formula:

V20  mw  mevap  Z  Y (12)

where: mW – mass of distilled water ejected from a pipette

mevap – mass of distilled water evaporated from a pipette
Z – coefficient determined in norm PN-EN ISO 8655-6 expressed by
formula (4)
Y – temperature coefficient related to a pipette determined in ISO/TR
20461 norm expressed by formula (5)

2. General formula of uncertainty of measurement:

2
 F 
u (V20 )   c  u ( x i )  
2 2
i
2
  u 2 ( x i ) (13)
i i  x i 
2
 F 
  
2
ci  (14)
 x i 

where: u2(xi) – particular uncertainties included in the measuring process

Page 11 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

ci 2 – particular coefficients of sensitivity

Uncertainty of measurement formula:

u 2 (V20 )  u 2 (Uw )  u 2 (Lw )  u 2 (Rw 1 )  u 2 (Rw 2 )  u 2 (d w 1 )  u 2 (d w 2 )  u 2 ( m )  u 2 ( mevap )

(15)
 u 2 (V20 )  u 2 (t w )  u 2 (t a )  u 2 ( )  u 2 ( pa )  u 2 ( c )

where Uw – uncertainty of a balance calibration

Lw – a balance linearity
Rw1 – a balance repeatability (for the first indication)
Rw2 – a balance repeatability (for the second indication)
dw1 – a balance resolution (for the first indication)
dw2 – a balance resolution (for the second indication)
m – distilled water mass
mevap – mass of water evaporated during the measuring
V20 – calculated volume value in 20 ºC
tw – water temperature
ta – air temperature
φ – relative air humidity
pa – air pressure
αc – coefficient of material volume expansion of a piston-cylinder kit of the
calibrated piston vessel in 1/°C

2.1 Uncertainty of a balance calibration, Uw -

U
u(Uw )  (16)
3
U – Standard uncertainty of a balance according to chart 1 in norm ISO 8655-6

2.2 A balance linearity Lw :

L
u(Lw )  (17)
3
L – Balance linearity according to chart 1 in norm ISO 8655-6

2.3 A balance repeatability Rw :

R
u(Rw )  (18)
3
R – Balance repeatability according to chart 1 in norm ISO 8655-6

2.4 A balance resolution dw :

d
u (d w )  (19)
2 3
Where: d – a balance interval

Page 12 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

2.5 Distilled water mass m:

d
u ( m)  m (20)
2 3

Note: According to the above formula you need to determine uncertainty of particular
measurements in a series, and then determine standard uncertainty for a series of 10
measurements:

 d  2 
u (m)  10   m   c w 
2
(21)
 2  3  

cw – coefficient of sensitivity related to mass measurement described further in this

procedure in issue 3.1

2.6 Evaporated water mass during calibration process mevap:

mevap
u(mevap )  (22)
3
δmevap – correction for water evaporation – constant 0,02 mg

2.7 Determined volume value in 20 ºC V20:

s
u(V20 )  d (23)
n
sd – standard deviation of n calculation results V = m · Z · Y
n - Number of measurements = 10

2.8 Water temperature tw:

d
u(t w )  tw (24)
3
dtw –Thermometer resolution of water temperature measuring
2.9 Air temperature ta:
d
u(t a )  ta (25)
3
dta –Thermometer resolution of air temperature measuring

2.10 Air relative humidity φ:

d
u( )   (26)
3
dφ – hygrometer resolution

2.11 Air pressure pa:

d
u( pa )  pa (27)
3
dpa – barometer resolution

Page 13 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

2.12 Coefficient of material volume expansion of a-cylinder kit αc:


u( c )  c (28)
3

3. Determine a sensitivity coefficient for every quantity according to chapter 4 of ISO/TR

20461:2000 document.

3.1 Coefficients related to mass measurement (balance):

Uw – balance calibration uncertainty

Lw – balance linearity
Rw1 – balance repeatability (for the first indication)
Rw2 – balance repeatability (for the second indication)
dw1 – balance resolution (for the first indication)
dw2 – balance resolution (for the second indication)
m – distilled water mass
mevap – mass of water evaporated during the measuring

The above coefficients are calculated according to the formula:

F V20
cw  
m m (29)

3.2 A coefficient related to volume determination V20 is calculated in the following formula:

V20
cV 20  1 (30)
V20

3.3 A coefficient related to water temperature determination is calculated in the following formula:

c tw  2,1 10 7  m (31)

3.4 A coefficient related to air temperature determination is calculated in the following formula:

m  ( k 2  t a 0  k 3 )  k1 p a
c ta   (32)
w2 (t a  t a 0 )2

3.5 A coefficient related to relative air humidity determination is calculated in the following
formula:

Page 14 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

m k2  ta  k3
c   (33)
w2 t a  t a0

3.6 A coefficient related to air pressure determination is calculated in the following formula:

m k1
c pa   (34)
w t a  t a0
2

3.7 A coefficient related to αc parameter determination is calculated in the following formula:

cc  10 3  m  (t d  20C ) (35)

td – pipette temperature expressed in [ºC] = ta

4. Determine standard uncertainty according to the below formula:

2 2 2 2 2
u 2 (V20 )  u 2 (Uw )  cw  u 2 (Lw )  cw  u 2 (Rw 1 )  cw  u 2 (Rw 2 )  cw  u 2 (d w 1 )  cw
2 2 2 2 2 2
 u 2 (d w 2 )  cw  u 2 ( m )  cw  u 2 (mevap )  cw  u 2 (V20 )  cv 20  u 2 (t w )  c tw  u 2 (t a )  c ta (36)
2 2 2
 u 2 ( )  c  u 2 ( pa )  c pa  u 2 ( c )  cc

5. Determine expanded uncertainty according to the below formula:

U  k  u(V20 )
(37)

Using an extension coefficient k = 2 which corresponds to the confidence level 95%

The final Uncertainty Budget

Page 15 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

11.0 Associated Documents

 Calibration Data Sheet (…../…../…..)

 Calibration Certificate (…../…../…..)
 Calibration Sticker (…../…../…..)

Page 16 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

APPENDIX A

Page 17 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

The density of pure water is normally provided from formulations given in the literature.
Batista and Paton provide an overview of common formulations used in practice. However it
is generally accepted that the formulation given by Tanaka provides a good basis for
standardization.

g/ml A.1

Where:
t = water temperature, in °C
a1 = -3,983035 ºC
a2 = 301,797 ºC
a3 = 522528,9 (ºC)2
a4 = 69,34881 ºC
a5 = 0,999974950 g/mL

Note: a5 is the density of SMOW water under one atmosphere at this temperature. Many
users of water rely on tap water instead of SMOW. Thus a5 must be changed accordingly to
reflect the density of the water used. The full equation of state for water provided by the
International Association for Properties of the Water Substance (IAPWS) can also be used to
determine the density of the used water and a formulation based on this equation is given in
ref. This provides an alternative to Tanaka and should be used if temperatures above 30 °C
are used.
Where pure water is not available, the relative density of the water may be determined and the
chosen formulation used to determine the temperature expansion factors with insignificant
loss of accuracy.
The air density can be determined according to the formula for the density of moist air -
CIPM-2007

A.2

p =ambient pressure, in Pa
T =thermodynamic temperature = 273,15 + t / ºC, in K
Xv= mole fraction of water vapour
xCO2= mole fraction of carbon dioxide in laboratory air
Z =compressibility factor

If the laboratory ambient conditions are within the limits given then Spieweck’s equation can
be used. The limits are: pressure between 940 hPa and 1080 hPa; temperature between 18 ºC
and 30 ºC; humidity less than 80 %,

A.3
Page 18 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

Where :
tA= ambient temperature, in °C
pA= ambient pressure, in hPa
hr= relative air humidity, in %
k1 = 3,4844 x 10-4 ºC/hPa
k2 = -2,52 x 10-6 g/mL
k3 = 2,0582 x 10-5 ºC

APPENDIX B
PHV-1

PHV-2

Page 19 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

Page 20 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

APPENDIX C
Calibration Certificate

Calibration Certificate
Central Organization for Standardization and Quality Control (COSQC)
Metrology Department - PHYSICS SECTION
P.O. Box13032 Algadria street, Baghdad ,Tel:7785180 - E-Mail : cosqc@yahoo.com
Certificate No.: PHV
Date of issue :

Customer
Name:  
Address:  

Item under calibration

Description:  
Manufacturer:  
Model:  
Serial number (CODE)  
Other identification:  
Date of reception:   Order No.      
Condition of reception:  

Standard(s) used in the calibration

Description:  
Manufacturer:  
Model:  
Serial number:  
Other identification:  

Calibration information
Date of calibration:   Due to:  
Place of calibration: Physics measurement lab
Method(s) of
 
calibration:
Calibrated quantity:  
Results of calibration: Attached a complete result in Annex 1 of this certificate
Measurement There reported expanded uncertainty is based on GUM Standard and the standard
uncertainty: Uncertainty multiplied by coverage factor k=2 to give confidence level of 95%
Metrological The traceability of measurement results to the SI units is assured by the Nationals tandard maintained at
traceability: Central Organization for standardization and Quality Control through calibration at :
Environmental
conditions of Temp. ( C): ±1ºC R. H.( %) ±5% Pressure ( mbar) ±1mbar
calibration:
Observations, opinions
The results and corrections in Annex 1 should be taken into consideration
or recommendations:

Approved by:

Page 21 of 22
 Identification:
Procedure for calibration PROC-TC-012
Central Organization for Standards and
Quality Control Revision: 1

(COSQC)- Metrology Department Valid after:

Calibration Certificate
Central Organization for Standardization and Quality Control (COSQC)
Metrology Department - PHYSICS SECTION
P.O. Box13032 Algadria street, Baghdad ,Tel:7785180 - E-Mail : cosqc@yahoo.com
Certificate No.: PHV
Date of issue :
Annex 1 ( Results )

SIZE Volume Errors

ml ml Uncertainty ± ml
ml
1 1.020 0.020
0.8 0.807 0.007
0.6 0.593 -0.007 0.012
0.4 0.430 0.030
0.2 0.218 0.018

Performed by: Reviese by: Approved by:

Page 22 of 22