TR 47-03 TR 47-03 - South African National Accreditation System
TR 47-03 TR 47-03 - South African National Accreditation System
TR 47-03 TR 47-03 - South African National Accreditation System
SANAS Page 1 of 11
TR 47-03
CONTENTS:
6. Authorship ........................................................................................................................... 8
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The purpose of this document is to define the specific environmental, general and technical accreditation
criteria with which accredited bodies must comply including accredited calibration laboratories in the
discipline of volume metrology. This document is applicable to accredited bodies in this discipline and as
defined in the Accreditation Act, Act No. 19 of 2006 [12].
This document does not address the requirements for accreditation as a volume verification laboratory,
or the requirements for volume metrology using either dimensional or volume to volume methods.
2.1 References
2.2 Definitions
2.2.3 Diluters
Diluters are used to deliver mixtures of liquids of defined volumetric proportions. [4]
2.2.4 Dispensers
Dispensers are used for the repetitive delivery (dispensing) of a measured volume of
liquid. [4]
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2.2.10 Pycnometer
A standard vessel used to measure and compare the densities of liquids.
2.2.12 Syringes
Syringes used in Laboratories fall into two broad categories, high precision metal and
glass instruments, and general purpose, low precision, disposable plastic syringes. [11]
2.3 Abbreviations
3. Environmental Requirements
3.1 When the calibration of pipettes and laboratory glassware is undertaken, the environmental
temperature must be maintained between 15 and 30 °C provided that the temperature is stable,
and is kept constant within ± 0,5 °C during the period of measurement.
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3.2 When pipettes are calibrated, the relative humidity shall be maintained above 50% rh in order to
minimize the effects of evaporation. [4]. The relative humidity is not as critical when calibrating
laboratory glassware due to the relatively smaller surface area of the liquid exposed to
atmosphere when compared to the volume of the liquid.
3.3 Where necessary the laboratory shall maintain appropriate records to demonstrate and confirm
both the temperature and temperature stability.
3.4 Lighting within the laboratory shall be adequate to facilitate the correct performance of the
calibration work undertaken. Cognisance shall be taken of the minimum levels of lighting as
specified in the environmental regulations of the OHS Act. [1] [2]
3.5 Drafts in the laboratory caused by doors, fans and/or air conditioners should be such that they do
not have an adverse effect on the measurement results, where necessary local isolation in the
form of draft shields should be utilized.
3.6 Measuring instruments used for the measurement and recording of the ambient temperature,
relative humidity and/or barometric pressure in the laboratory shall be calibrated by an accredited
calibration laboratory.
4. General Requirements
4.1 Laboratories shall have a policy and procedure/s that addresses how their own standards and
equipment, and those belonging to customers are to be handled, cleaned and maintained. These
policies and procedures shall also address biological and chemical decontamination.
4.2 Laboratories shall be equipped with appropriate calibrated measurement equipment necessary to
perform calibration by gravimetric means, and shall include:
When performing measurements below 100μℓ the laboratory shall use a balance with a resolution
of at least 10μg.
4.4 The schedule of accreditation shall list the types of volume measuring and dispensing equipment
that the laboratory is competent to calibrate under the parameter ‘Volume metrology’. This list
may include the following:
• Syringes;
• Automated (Glass) Pipettes;
• Piston Pipettes;
• Burettes;
• Flasks;
• Measuring Cylinders;
• Pycnometers;
• Diluters;
• Dispensers;
• Simple measures other than glass;
• Metal Strike measures;
• Other Metal measures.
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5. Technical Requirements
5.1.1 Either distilled or deionised water shall be used to calibrate the pipette, and both the water
and equipment to be calibrated shall have been allowed to stabilize for a period of not
less than 2 hours prior to performing the calibration. [5]
5.1.2 When dispensing volumes of especially less than 50μℓ, errors due to evaporation of the
test liquid during weighing shall be taken into consideration. Where the evaporation has
been determined experimentally and corrected for, the uncertainty associated with the
correction shall be included in the uncertainty budget. [5]
5.1.3 Where dispensing volumes greater than 50 μℓ the uncertainty associated with the
evaporation may still be an influencing factor in the associated uncertainty of
measurement. Where it is considered that the uncertainty associated with the evaporation
is insignificant, the laboratory shall have documented evidence to support this claim.
5.1.4 When calibrating pipettes that deliver a variable selected volume, the pipettes shall be
calibrated at a minimum of 3 different volumes, namely:
5.1.5 When calibrating pipettes using the gravimetic method, a minimum of 6 measurements at
each test volume shall be taken, however laboratories wishing to claim compliance with
ISO 8655 shall ensure that the minimum number of measurements is in compliance with
the relevant sections of the ISO 8655 standard. [5]
5.1.6 Prior to the commencement, and after completion of the calibration of each test volume
the barometric pressure, relative humidity, air temperature and the temperature of the test
liquid shall be recorded. [5]
5.1.7 The laboratory shall have a comprehensive procedure describing the calibration process,
and the procedure shall address as a minimum:
• The identification of the pipette including the supplier (or manufacturers) name, the
type or model number, the serial number (unique or other inventory number),
nominal volume or volume range;
• The reference temperature;
• Identification of the pipette tip (or description);
• The environmental conditions (barometric pressure, relative humidity, and
temperature).
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5.1.9 Where devices are made from composite materials (e.g. piston pipettes) it is difficult to
state a specific value for the thermal coefficient of expansion, and therefore the
calibration should be conducted at a temperature as close to the temperature at which the
pipette is to be used, and this temperature shall be specified on the calibration certificate.
An approximate value should then be used when estimating the uncertainty of
measurement.
See Appendix 2.
5.1.10 The following should be considered as a minimum when calculating the uncertainty of
measurement:
Any deviation from the above shall be technically justified, and supported with
documented evidence. [8]
5.2.1 In addition to the equipment identified in 4.2, the laboratory shall have a stopwatch
necessary for the evaluation of the delivery time.
5.2.2 The standard reference temperature, i.e. the temperature at which the volumetric
glassware is intended to contain or deliver its nominal volume is 20⁰C. [3]. Should the
laboratory calibrate the glassware at a reference temperature other that 20°C, this shall
be clearly stated on the Calibration certificate or report.
5.2.3 Prior to calibration, the glassware shall be visually inspected to determine if there are any
visible defects, graduation lines shall be clean, permanent and of uniform thickness, and
shall lie in planes at right angles to the longitudinal axis of the glassware. There shall be
no irregularity in the spacing of graduation lines. [6] If any defect in the glass or
graduation lines is observed this shall be reported on the calibration certificate or report.
5.2.4 The measurements shall be performed with distilled or deionized water suitable for
general laboratory use. [3]
5.2.5 The temperature of the liquid shall be measured and corrections in temperature from the
reference temperature shall be applied.
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• The identification and description of the glassware, the supplier (or manufacturers)
name, the nominal volume or capacity, the serial number, (or other unique
identification);
• The reference temperature;
• An indication if the glassware is intended to contain (In) or deliver (Ex) the indicated
volume;
• The environmental conditions (Barometric Pressure, Relative Humidity, and
Temperature);
• The cubic coefficient of expansion used.
5.3.1 In addition to the equipment identified in 4.2 the laboratory shall have a stand capable of
supporting the pipette in a vertical position.
5.3.2 Automatic pipettes are normally used for the calibration of volumetric instruments –
including volumetric standards of a lower order. [7]
6. Authorship
This Technical Requirement document was originally prepared by a working group / committee
consisting of the following members:
SANAS appreciates the contribution made by the committee members in the preparation of this
document. Later amendements have been undertaken by the SANAS STC for Mass and Volume
Metrology.
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SCHEDULE OF ACCREDITATION
VOLUME METROLOGY
Postal Address:
P O BOX 32222
Johannesburg
2000
Issue No. : 03
Tel: (011) 499-8778 Date of Issue : August 2003
Fax: (011) 499-8879 Expiry Date : July 2005
CALIBRATION AND
MEASURED QUANTITY MEASUREMENT
RANGE OF MEASURED FREQUENCY,
ITEM OR TYPE OF GAUGE OR CAPABILITY
QUANTITY STANDARD, ETC.
INSTRUMENT EXPRESSED AS AN
UNCERTAINTY (±)
3 Volume
3.1 Piston Pipettes
3.1.1 Piston Pipettes 5 μℓ to 100 µℓ ISO 8655-5 ± 0,2 µℓ
100 μℓ to 200 µℓ ± 0,6 µℓ
200 μℓ to 1 000 µℓ ± 4,0 µℓ
1 000 μℓ to 10 000 µℓ ± 50 µℓ
3.2 Laboratory Glassware
3.2.1 Automated pipettes 1 mℓ to 5 mℓ ± 0,5 %
Volume dispensers 5 mℓ to 20 mℓ ± 0,7 %
3.2.2 Pipettes 20 mℓ to 100 mℓ ± 0,25 %
Burettes 100 mℓ to 1 000 mℓ ± 0,1 %
3.2.3 Measuring Cylinders 1 000 mℓ to 20 000 mℓ ISO - 4788 ± 0,5 %
Pycnometers
Flasks
3.2.4 Syringes
3.3 Simple measures other than glass
3.3.1 Flasks 10 mℓ to 20 mℓ ± 0,6 %
Measuring cylinders 20 mℓ to 100 mℓ ± 0,3 %
100 mℓ to 1 000 mℓ ± 0,2 %
1000 mℓ to 20 000 mℓ ± 0,5 %
3.4 Metal measures
3.4.1 Metal Strike Measures 10 mℓ to 1 000 mℓ ± 0,5 %
3.4.2 other Metal volume 1 000 mℓ to 1 000 ℓ ± 0,1%
measures
On-site calibration of items 3.1 and 3.4
Original date of accreditation:1994 Page 1 of 1
The CMC, expressed as an expanded uncertainty of measurement, is stated as the standard uncertainty of
measurement multiplied by a coverage factor k = 2, corresponding to a confidence level of approximately 95%
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Cubic coefficients of expansion of various materials used in the manufacture of volume measuring and
dispensing devices
* The cubic coefficient of expansion of ‘plastic’ materials can vary greatly due to their actual composition.
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AM 1 Align purpose and scope with the accreditation Act, Act 19 of 2006
2,1 Add Accreditation Act as a reference
2.2 Add definitions for Accreditation Criteria and Accredited Boby
5.1.2 Amend section to align with ISO 8655
5.1.3 Add clause dealing with evaporation where the dispensed volume exceeds
100 μℓ
5.1.9 Added requirements for uncertainty of measurement calculations in line with
ISO/TR 20461.
WG Members 1 Revised wording for Purpose and Scope
2.2.1 Revised working for accreditation criteria
2.2.9 Added ‘Aspirate’ to definition
3.2 Added ‘…..when compared to the volume of the liquid’
3.6 Added ‘….by an accredited calibration laboratory.’
4.1 Added’…. and those….’
5.1.5 Clause added requiring repeated measurements at each test volume
5.1.10 Clause amended and additional requirements added
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