Nabl 103 PDF

NABL 103
NABL
NATIONAL ACCREDITATION
BOARD FOR TESTING AND
CALIBRATION LABORATORIES
SPECIFIC GUIDELINES
for
CHEMICAL TESTING
LABORATORIES
ISSUE NO : 03
ISSUE DATE: 25.03.2008
AMENDMENT NO : 00
AMENDMENT DATE: --
AMENDMENT SHEET
Sl
Page
No.
Clause
Date of
No. Amendment
Amendment made
Reasons
Signature
QM
Signature
Director
10
National Accreditation Board for Testing and Calibration Laboratories

Doc. No: NABL 103
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Specific Guidelines for Chemical Testing Laboratories

Issue Date: 25.03.2008
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ABBREVIATIONS
AOAC
Association of Official Analytical Chemists
APHA
American Public Health Association
APLAC
Asia Pacific Laboratory Accreditation Cooperation
AS
American Standard
ASTM
American Society for Testing and Materials
BIS
Bureau of Indian Standards
BIPM
Bureau International des Poids et Measure (International Bureau of

Weights and Measures)
BS
British Standard
CRM
Certified Reference Material
ISO
International Organization for Standardization
EA
European Cooperation of Testing Authorities
FTIR
Fourier Transform Infrared
GFAAS
Graphite Furnace Atomic Absorption Spectrometer
e.g.
For Example
GUM
Guide to the Expression of Uncertainty in Measurement
ICPAES
Inductively Coupled Plasma Atomic Emission Spectrometer
ICP-MS
Inductively Coupled Plasma Mass Spectrometer
IEC
International Electrotechnical Committee
ILAC
International Laboratory Accreditation Cooperation
IUPAC
International Union of Pure and Applied Chemists
NABL
NATA
National Association of Testing Authorities
NIST
National Institute of Standards and Technology
NMR
Nuclear Magnetic Resonance
QC
Quality Control
w.r.t.
With Respect To

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CONTENTS
Sl
Title
Page
Amendment Sheet
Abbreviations
ii
Contents
iii
1.
Introduction
2.
References
3.
Terms and Definitions
4.
Scope
5.
Technical Requirements
6.
Groupwise Codification for Chemicals Tests
28
Annexure A
37
Annexure B
40
Annexure C
78

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1.
INTRODUCTION
1.1
The requirements for accreditation are laid down in the International Standard ISO/IEC
17025: 2005 (General requirements for the competence of calibration and testing
laboratories). These requirements apply to all types of objective testing but in certain
instances additional guidance is necessary to take account of the type of testing and the
technologies involved.
1.2
This document has been produced by a TECHNICAL COMMITTEE constituted by NABL

for the purpose. It supplements ISO/ IEC 17025: 2005 standard and provides specific
guidance on the accreditation of chemical laboratories for both assessors and
laboratories preparing for accreditation. It gives detailed guidance for those undertaking
quantitative and qualitative examination of the composition, nature and properties of
materials, products and substances.
1.3
Laboratories conducting tests on food should also consult NABL specific criteria on
biology (NABL 102) and the NABL guidance document on Food (NABL 114).

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2.
REFERENCES
ISO/ IEC 17025: 2005 General Requirements for the Competence of Testing and
Calibration Laboratories
ISO/ IEC 17025 Application Document : 2000 Version 1, NATA, Australia
ISO Guide 30 Terms and Definitions used in connection with reference materials.
UKAS: LAB 27 Accreditation for Chemical Laboratories

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3.
TERMS AND DEFINITIONS
3.1
Selectivity
Selectivity of a method refers to the extent to which it can determine particular analyte(s)
in a complex mixture without interference from the other components in the mixture. A
method which is perfectly selective for an analyte or group of analytes is said to be
specific. The applicability of the method should be studied using various samples,
ranging from pure standards to mixtures with complex matrices. In each case the
recovery of the analyte(s) of interest should be determined and the influences of
suspected interferences duly stated. Any restrictions in the applicability of the technique
should be documented in the method.
3.2
Range
For quantitative analysis the working range for a method is determined by examining
samples with different analyte concentrations and determining the concentration range
for which acceptable accuracy and precision can be achieved. The working range is
generally more extensive than the linear range, which is determined by the analysis of a
number of samples of varying analyte concentrations and calculating the regression from
the results, usually using the method of least squares. The relationship of analyte
response to concentration does not have to be perfectly linear for a method to be
effective. For methods showing good linearity 5 different standards (plus a blank) are
usually sufficient for producing calibration curves. More standards will be required where
linearity is poor. In qualitative analysis, it is commonplace to examine replicate samples
and standards over a range of concentrations to establish at what concentration a
reliable cut-off point can be drawn between detection and non-detection.
3.3
Linearity
Linearity is determined by the analysis of samples with analyte concentrations spanning
the claimed range of the method. The results are used to calculate a regression line
against analyte calculation using the least squares method. It is convenient if a method
is linear over a particular range but it is not an absolute requirement. Where linearity is
unattainable for a particular procedure, a suitable algorithm for calculations should be
determined

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3.4
Sensitivity
Sensitivity is the difference in analyte concentration corresponding to the smallest
difference in the response of the method that can be detected. It is represented by the
slope of the calibration curve and can be determined by a least squares procedure, or
experimentally, using samples containing various concentrations of the analyte.
3.5
Limit of Detection
Limit of detection of an analyte is determined by repeat analysis of a blank test portion
and is the analyte concentration whose response is equivalent to the mean blank
response plus 3 standard deviations. Its value is likely to be different for different types
of sample
3.6
Limit of Quantitation
Limit of quantitation is the lowest concentration of analyte that can be determined with
an acceptable level of accuracy and precision. It should be established using an
appropriate standard or sample, i.e. it is usually the lowest point on the calibration curve
(excluding the blank). It should not be determined by extrapolation
3.7
Ruggedness
Sometimes also called robustness. Where different laboratories use the same method
they inevitably introduce small variations in the procedure, which may or may not have a
significant influence on the performance of the method. The ruggedness of a method is
tested by deliberately introducing small changes to the method and examining the
consequences. A large number of factors may need to be considered, but because most
of these will have a negligible effect, it will normally be possible to vary several at once.
The technique is covered in detail by the AOAC (8). Ruggedness is normally evaluated
by the originating laboratory, before other laboratories collaborate

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3.8
Accuracy
The accuracy of a method is the closeness of the obtained analyte value to the true
value. It can be established by analysing a suitable reference material. Where a suitable
reference material is not available, an estimation of accuracy can be obtained by spiking
test portions with chemical standards. The value of spiking is limited; it can only be used
to determine the accuracy of those stages of the method following the spiking. Accuracy
can also be established by comparison with results obtained by a definitive method or
other alternative procedures and via intercomparison studies
3.9
Precision
Precision of a method is a statement of the closeness of agreement between mutually
independent test results and is usually stated in terms of standard deviation. It is
generally dependent on analyte concentration, and this dependence should be
determined and documented. It may be stated in different ways depending on the
conditions in which it is calculated. Repeatability is a type of precision relating to
measurements made under repeatable conditions, i.e. same method; same material;
same operator; same laboratory; narrow time period. Reproducibility is a concept of
precision relating to measurements made under reproducibility conditions, i.e. same
method; different operator, different laboratories; different equipment; long time period.
3.10
Reference Material
A reference material (RM) is a material or substance one or more properties of which are
sufficiently established to be used for the calibration of an apparatus, the assessment of
a measurement method, or for assigning values to materials.
3.11
Certified Reference Material

A certified reference material (CRM) is a reference material one or more of whose
property values are certified by a technically valid procedure, accompanied by, or
traceable to a certificate or other documentation which is issued by a certifying body.
3.12
Sample
A portion of material selected to represent a larger body of material.

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3.13
Sample handling
This refers to the manipulation to which samples are exposed during the sampling
process, from the selection from the original material through to the disposal of all
samples and test portions.
3.14
Sub-sample
This refers to a portion of the sample obtained by selection or division; an individual unit
of the lot taken as part of the sample or; the final unit of multistage sampling
3.15
Sample preparation
This describes the procedures followed to select the test portion from the sample (or
subsample) and includes: in-laboratory processing; mixing; reducing; coning and
quartering; riffling; and milling and grinding.
3.16
Test portion
This refers to the actual material weighed or measured for the analysis.

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4.
SCOPE
4.1
The Scope of accreditation of a laboratory is the formal statement of the range of

activities for which the laboratory has been accredited; the scope is recorded in detail on
a laboratorys accreditation certificate. A laboratorys scope should be defined as
precisely as possible so that all parties concerned know accurately and unambiguously
the range of tests and/or analyses covered by that particular laboratorys accreditation.
The schedule format should typically define the laboratorys accreditation in terms of:
4.2
(i)
The range of products, materials or sample types tested or analysed;
(ii)
Types of tests or analysis carried out;
(iii)
The specification or method/technique used;
(iv)
The concentration range and accuracy/precision
Where non-routine testing is carried out, it is recognised that a more flexible approach to
scope may be necessary, but the scope must be as specific as is feasible and the quality
assurance system maintained by the laboratory must ensure that the quality of the
results is under control. Frequently, a single measurement technique may be used for
different analytes in a wide variety of samples. This measurement stage may be covered
by a single method. However, the methods used to prepare the samples for subsequent
analysis may vary considerably according to the nature of the analyte and sample
matrix. Thus several methods may be required to cover each different analyte matrix
combination. This is illustrated by gas chromatography, a technique applicable to a wide
variety of analytes. Depending on the matrix, a diverse range of methods may be used
to prepare analytes for gas chromatographic analysis; however, the procedures involved
in the final analytical stage vary little.
4.3
Where a laboratory uses analytical tools such as mass spectrometry, NMR or FTIR, it
may be appropriate to use the terms qualitative and/or quantitative chemical analysis
under the type of test heading. However, the onus will be on the laboratory to
demonstrate to the assessors that in using these techniques, it is meeting all of the
criteria for accreditation. In particular, the experience, expertise and training of the staff
carrying out the tests and those interpreting the data involved will be a major factor in
determining whether or not such analyses can be accredited.

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It is accepted that sometimes it is not practicable for laboratories to use a (fully

documented) standard method in the conventional sense, which specifies each sample
type and determinant. In this case, the laboratory must have its own method or
procedure for the use of the instrument in question, which includes a protocol defining
the approach to be adopted when different sample types are analysed. Full details of the
procedures, including instrument parameters, used must be recorded at the time of each
analysis such as to enable the procedure to be repeated in precisely the same manner
at a later date. Where a particular analysis subsequently becomes routine, a full method
as required by NABL must be written and followed. The statement in the column of the
methods schedule will normally take the form of Documented In-House Methods using
GC-coupled mass spectrometry/NMR/FTIR, ICP-MS, etc. (Refer ISO/IEC 17025: 2005
para 5.4.2, 5.4.3, 5.4.4 and 5.4.5). Whenever there is deviations from standard method
or inadequate clarification in Standard Method, the laboratory needs to develop effective
procedure for ensuring the quality of results.
4.4
The approach to extending or amending the scope of accreditation should be as flexible

as possible. Normally the laboratory will give written notice to NABL of the tests, which it
wishes to add to its scope, quoting Standard method references (where applicable) and
providing copies of documented validated in-house methods before surveillance and reassessment.

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5.
TECHNICAL REQUIREMENTS
5.2
Personnel
5.2.1
The chemical testing laboratory shall be headed by a person preferably having a post
graduate degree in chemistry or equivalent or Bachelor degree in chemical engineering /
technology or equivalent with adequate experience in the relevant area especially in the
analysis of testing of relevant products.
The minimum qualification for the technical staff in a chemical testing laboratory shall be
Graduate in Science with chemistry as one of the subjects or Diploma in chemical
engineering / technology or equivalent or specialization in relevant fields like Textile,
Polymer etc. The staff shall have sufficient training and exposure in analytical chemistry
and in analysis and testing of appropriate products.
The laboratory technicians or equivalent shall have higher secondary certificate in
science / ITI and at least one year experience or training in a relevant laboratory.
5.2.2
The minimum requirement for an Authorized Signatory shall be a Graduate in Science

with chemistry as one of the subjects / Diploma in Chemical engineering / technology or
equivalent from a recognized university with at least 5 years experience in relevant field,
or Post-graduate in chemistry / specialization in relevant subject / Degree in Chemical
engineering / technology or equivalent from a recognized university with at least 2 years
experience in relevant field.
Note: The Assessment team may however recommend Authorized Signatory who does
not meet the above specified minimum experience requirement with specific
recommendations to NABL, after adjudging the competence of the Authorized Signatory
during on-site assessment.
5.2.3
Chemical testing laboratory involved in testing variety of products shall have a group incharge for each area. The group in-charge shall have adequate relevant experience in
addition to the minimum qualification as specified in 5.2.1.

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5.2.4
There shall be a system for imparting periodic, internal and external training to the
laboratory technical staff at different levels wherever required before assigning any
analytical and testing work. Internal Training alone is not considered adequate to make
the staff knowledgeable on the latest status of science and technology. The laboratory
should ensure the availability of necessary infrastructure either internally or access to
external, for training. Evidence of effective training in specific field should be available in
terms of performance in quality checks. All the technical staff working should be
sufficiently trained in all physical, chemical and instrumental methods of analysis of the
particular product under concern.
5.2.5
For meeting the requirement of internal audit, there should be at least one technical
personnel apart from the head with suitable qualification and experience, irrespective of
the size of the laboratory, who has received a formal training on internal audit.
The laboratory shall normally use personnel who are permanently employed by the
laboratory or appointed on long-term contract basis, provided laboratory ensures
availability of technical personnel with adequate experience. A laboratory is not expected
to be operated by trainees. Where additional personnel are required, the laboratory shall
ensure that such personnel are supervised and that their work does not put at risk of the
laboratorys compliance.
5.2.6
Any testing conducted away from the base laboratory (such as in field laboratories, in a
mobile testing laboratory or in the field) must also be under adequate technical control.
This would normally require either the location of Authorized Signatory at each facility or
having an Authorized Signatory visit each facility at appropriate intervals commensurate
with the volume, complexity and range of such tests and the maintenance of a diary
recording the dates and relevant activities of each visit. An authorized signatory must be
involved in the setting up of field or site laboratory.

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5.3 Environment and accommodational condition

5.3.1
Samples, reagents and standards should be stored so as to ensure their integrity. The
laboratory should guard against deterioration, contamination and loss of identity.
5.3.2
The Laboratory shall meet the safety requirements applicable to the test procedure
wherever the published standard specifications mention the requirements.
5.3.3
It may be necessary to restrict access to particular areas of laboratory because of the

nature of the work carried out there. Restrictions might be made because of security,
safety, or sensitivity to contamination. Typical examples might be work involving
explosives, radioactive materials, carcinogens, toxic materials and trace analysis. Where
such restrictions are in force, staff should be aware of:
i.
the intended use of a particular area;
ii. the restrictions imposed on working within such areas;

iii. the reasons for imposing such restrictions
5.3.4
Frequently, it will be necessary to segregate certain types of work which are prone to
interferences from other work, or which present particular problems or hazards.
Examples are trace analysis (where physical separation from high-level is necessary)
and carcinogen analysis. When selecting designated areas for special work, account
must be taken of the previous use of the area. Before use, checks should be made to
ensure that the area is free of contamination. Once in use, access to such areas should
be restricted, and the type of work undertaken there carefully controlled.
5.3.5
The laboratory shall provide appropriate environmental conditions and controls

necessary for particular tests, including temperature, humidity, freedom from vibration,
freedom from airborne and dustborne microbiological contamination, special lighting,
radiation screening. Critical environmental conditions should be monitored.
5.3.6
One key responsibility of the laboratory management is to provide an adequate and safe
working environment. Laboratory facilities should reflect due consideration of space,
design, security, health and safety. It is recognised that laboratories will be required to
comply with Government building and safety legislation. The provisions of such
legislation shall be considered as additional essential requirements.

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5.3.7
Space
Each employee must have adequate work space to accomplish assigned tasks.
Sufficient space must be provided for storage of supplies, equipment and tools.
Analysts/examiners must have space available for writing reports and other official
communications. Where possible, there must be a clear delineation of areas used for the
clerical aspects of laboratory work and the areas used for testing/examinations.
Adequate and appropriate space must be available for records, reference work and
other necessary documents. Sufficient space must be available for each instrument to
facilitate its operation.
Accessories should be preferably stored near each instrument to facilitate its use and
operation. (Labs in which usable space falls below adequate levels may experience
health and safety problems, compromised efficiency, adversely affected morale and
productivity and an increased risk of mishandling and contaminating the evidence. In
designing and planning for additional space or a new facility, future space requirements
should also be projected.
5.3.8
Design
The relative locations of functional areas should facilitate the use of equipment and
instruments. Adequate and proper lighting of minimum 100 lumen must be available for
personnel to carry out assigned tasks. Adequate and proper plumbing and wiring must
be available and accessible. The laboratory must have proper ventilation, adequate
heating, cooling and humidity control as per the requirements. Bench and floor surfaces
must be appropriate for the work being performed. The design should maximise
laboratory functions and activities, safeguard the physical evidence, protect the
confidential nature of the laboratory operations and provide a safe and healthy
environment. (Lack of fiscal resources are not acceptable reasons for unacceptable
laboratory practices).
Where a laboratory exists within a host agency facility, documented procedures may be
required to permit entry during off hours for emergencies.
The laboratory should have a fire detection system wherever applicable. In keeping with
any relevant statutory requirements appropriate fire extinguishing devices must be
available and policies and procedures of laboratory security must be clearly
documented. Laboratory personnel should be trained in fire fighting.

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5.3.9
Health and Safety

Health and safety aspects are to be taken seriously. Details about the same are given in
Annexure A.
5.4
Validation
5.4.1
Laboratory, whenever using non-standard methods or a standard method beyond the

stated limits of operation is required to validate such test methods. The guidance
document on Validation of Test Methods, NABL 212 may be referred. Validation of a
method
establishes,
by
systematic
laboratory
studies,
that
the
performance
characteristics of the method meet the specifications related to the intended use of the
analytical results. The performance characteristics determined include:
-
Selectivity & specificity
Range
Linearity
Sensitivity
Limit of Detection
Limit of Quantitation
Ruggedness
Accuracy
Precision
These parameters should be clearly stated in the documented method so that the user
can assess the suitability of the method for their particular needs.
In theory the development should include consideration of all of the necessary aspects
of validation. However, the responsibility remains firmly with the user to ensure that the
validation documented in the method is sufficiently complete to fully meet his or her
needs. Even if the validation is complete, the user will still need to verify that the
documented performance can be met

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5.4.2
Test and calibration methods and method validation/verification published by BIS,

ASTM, AOAC, etc.
5.4.2.1 A laboratory seeking accreditation for a more open set of terms of accreditation (where
groups of analytes, for example, organochlorine pesticides are specified rather than
individual analytes) must have fully documented procedures covering such elements as:
method selection, method development, method validation or verification, acquisition of
appropriate reference standards or reference materials and staff training. Records of the
application of these procedures will be reviewed as part of each assessment.
5.4.2.2 When standard methods are used, laboratories should verify their own satisfactory
performance against the documented performance characteristics of the method, before
any samples are analysed. Records of the verification must be retained. For published
test methods that do not include precision data, the laboratory must determine its own
precision data based on test data. All methods should include criteria for rejecting
suspect results.
Where a test can be performed by more than one method there must be documented
criteria for method selection. Where relevant the degree of correlation between the
methods should be established and documented.
5.4.2.3 Methods developed in-house must be validated and authorized before use. Where they
are available, certified reference materials should be used to determine any systematic
bias, or where this is not possible results compared with other technique(s), preferably
based on different principles of analysis.
5.4.2.4 All methods shall be fully documented including procedures for quality control, and the
use of reference materials. It is preferable that a common format be adopted for writing
up methods and suitable guidance is given in ISO 78-2:1982, Layout for Standards
part 2: Standards for chemical Analysis.

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5.4.2.5 Developments in methodology and techniques will require methods to be changed from
time to time. Obsolete methods should be withdrawn but must be retained for archive
purposes and clearly labelled as obsolete. The revised method must be fully
documented, and indicate under whose authority the new method was issued (signed
and dated).
Where a change in method involves only minor adjustments, such as sample size,
different reagents, the amended method should be validated and the changes brought to
the attention of NABL at their next visit. Where the proposed change in method involves
a change of scope, such as a significant change in technology or methodology, the
laboratory. Shall inform NABL for appropriate action.
5.4.2.6 Laboratories are required to estimate uncertainty of measurement for the tests being
carried out. This should be on the basis of EURACHEM and GUM where standard
methods include uncertainty factors, laboratories may use them for the estimates.
5.4.3
Use of Computer
5.4.3.1 In chemical testing laboratories, computers have a wide variety of uses including:
control of critical environmental conditions;
monitoring and control of inventories;
calibration and maintenance schedules;
stock control of reagents and standard materials;
design and performance of statistical experiments;
scheduling of samples and monitoring of work throughput;
control chart generation;
monitoring of test procedures;
control of automated instrumentation;
capture, storage, retrieval, processing of data, manually or automatically;
matching of sample and library data;
generation of test reports;
word processing;
communication

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5.4.3.2 The chemical testing environment creates particular hazards for the operation of
computers and storage of computer media. Advice can usually be found in the operating
manuals, however particular care should be taken to avoid damage due to chemical,
microbiological or dust contamination, heat, damp and magnetic fields.
If a testing instrument cannot be isolated from the data processing system, the system
as a whole must be calibrated either statically or dynamically. Each such system will
have to be examined individually.
If the testing instrument can be isolated from the data processing system, the
opportunity is available to calibrate each component of the system separately. The
testing instrument can be calibrated (again, statically or dynamically) in the conventional
manner and a separate verification of the data processing system can be undertaken
incorporating the A/D converters and interfacing systems
5.4.3.3 Computer controlled automated system
Such systems will normally be validated by checking for satisfactory operation (including
performance under extreme circumstances) and establishing the reliability of the system
before it is allowed to run unattended. An assessment should be made of the likely
causes of system malfunction. Where possible the controlling software should be
tailored to identify and highlight any such malfunctions and tag associated data. The use
of quality control samples and standards run at intervals in the sample batches should
then be sufficient to monitor correct performance on a day-to-day basis. Calculation
routines can be checked by testing with known parameter values.
Electronic transfer of data should be checked to ensure that no corruption has occurred
during transmission. This can be achieved on the computer by the use of `verification
files but wherever practical the transmission should be backed up by a hard copy of the
data.

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5.4.3.4 Laboratory information management systems (LIMS)

LIMS systems are increasingly popular as a way of managing laboratory activities using
a computer. A LIMS is a software package allowing the electronic collation, calculation
and dissemination of analytical data, often received directly from other instruments and it
incorporates word-processing, database, spreadsheet and data processing capabilities.
It can perform a variety of functions, typically sample registration and tracking;
processing captured data; quality control; financial control; report generation. Particular
validation requirements include control of access to the various functions and audit trials
to catalogue alterations and file management.
5.5
Equipment
5.5.1
As part of its quality system, a laboratory is required to operate a programme for the
maintenance and calibration of equipment used in the laboratory. Equipment normally
found in the chemical laboratory can be categorised as:
i)
general service equipment not used for making measurements or with minimal
influence on measurements (eg hotplates, stirrers, non-volumetric glassware and
glassware used for rough volume measurements such as measuring cylinders)
and laboratory heating or ventilation systems;
ii)
volumetric equipment (e.g. flasks, pipettes, pyknometers, burettes etc);
iii)
measuring instruments (e.g. hydrometers, U-tube viscometers, thermometers,

timers, spectrometers, chromatographs, electrochemical meters, balances etc);
iv)
5.5.2
physical standards (weights, reference thermometers);
General Service Equipment

5.5.2.1 General service equipment are maintained by appropriate cleaning and checks
for safety as necessary. Calibrations or performance checks will be necessary where the
setting can significantly affect the test or analytical result (eg the temperature of a muffle
furnace or constant temperature bath).

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5.5.3
Volumetric equipment
5.5.3.1 The correct use of volumetric equipment is critical to analytical measurements and it
shall be suitably maintained and calibrated. The correct functioning of some specialist
volumetric (and related) glassware is dependent on particular factors, eg the
performance of pyknometers and U-tube viscometers is dependent on wetting and
surface tension characteristics, which may be affected by cleaning methods etc. Such
apparatus may therefore require more regular calibration, depending on use. For the
highest accuracy, measurements can often be made by mass depending on properly
calibrated weighing mechanism with traceability to accredited calibration laboratories in
INDIA or abroad APLAC/EA Member Countries rather than by volume.
5.5.3.2 Attention should be paid to the possibility of contamination arising from the equipment or
cross-contamination from previous use. The type used (glass, PTFE, etc), cleaning,
storage, and segregation of volumetric equipment is critical, particularly for trace
analyses when leaching and adsorption can be significant.
5.5.4
Measuring instruments/equipments
5.5.4.1 Correct use combined with periodic servicing, cleaning and calibration will not
necessarily ensure an instrument is performing adequately. Where appropriate, periodic
performance checks should be carried out (eg to check the response, stability and
linearity of sources, sensors and detectors, the separating efficiency of chromatographic
systems, the resolution, alignment and wavelength accuracy of spectrometers etc). See
guidelines published by NATA relating to calibration of equipments / instruments
provided at Annexure B as guidance to the laboratories.
5.5.4.2 The frequency of such performance checks will be determined by experience and based
on need, type and previous performance of the equipment. Intervals between checks
should be shorter than the time the equipment has been found to take to drift outside
acceptable limits.
5.5.4.3 It is often possible to build performance checks system suitability checks into test
methods (eg based on the levels of expected detector or sensor response to calibrants,
the resolution of calibrants in separating systems, the spectral characteristics of
calibrants etc). These checks should be satisfactorily completed before the equipment is
used.
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5.5.5
Physical standards
5.5.5.1 Wherever physical parameters are critical to the correct performance of a particular test,
the laboratory shall have or have access to the relevant reference standard, as a means
of calibration.
5.5.5.2 Reference standards and accompanying certificates should be stored and used in a
manner consistent with preserving the calibration status. Particular consideration should
be given to any storage advice given in the documentation supplied with the standard.
5.6
Calibration & Measurement Traceability
5.6.1
The overall programme for the calibration of measuring equipment in the chemical
laboratory shall be designed to ensure that, where the concept is applicable, all
measurements are traceable through certificates held by the laboratory, either to a
national or international standard or to a certified reference material. Where no such
reference standard or certified reference material is available, a material with suitable
properties and stability should be selected or prepared by the laboratory and used as a
laboratory reference. The required properties of this material should be characterised by
repeat testing, preferably by more than one laboratory and using a variety of methods,
see ISO Guide 35, Certification of reference materials General and statistical
principles.
5.6.2
Analytical tests may be sub-divided into three general classes depending on the type of
calibration required:
(i) In general, standards exist for ensuring traceability to international or national
standards for equipment used for the direct measurement of fundamental properties
(e.g., mass, length, temperature and time) or the simpler derived properties (e.g.,
area, volume and pressure). Where these properties have a significant effect on the
results of an analysis, the requirements of ISO/IEC 17025: 2005 shall be met.

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(ii) Where a test is used to measure an empirical property of a sample, such as

flashpoint, equipment is often defined in a national or international standard method
and traceable reference materials should be used for calibration purposes where
available. New or newly acquired equipment should be checked by the laboratory
before use to ensure conformity with specified design, performance and dimension
requirements.
(iii) Instruments such as chromatographs and spectrometers, which require calibration
as part of their normal operation, should be calibrated using chemicals of known and
purity or reference materials of known composition.
-
See Annexure C for calibration of the parameters associated with chemical

analysis. This is taken from ILAC proceedings 1993.
5.6.3
Individual calibration programmes shall be established depending on the specific

requirements of the analysis. Also, it may be necessary to check instrument calibration
after any shutdown, whether deliberate or otherwise, and following service or other
substantial maintenance. The level and frequency of calibration should be at least that
recommended by the manufacturer.
5.6.4
Reference materials and chemical standards

Reference materials and certified reference materials are defined in terms and
definitions.
5.6.4.1 Reference materials provide essential traceability in chemical measurements and are
used to demonstrate the accuracy of results, calibrate equipment and methods, monitor
laboratory performance and validate methods, and enable comparison of methods by
use as transfer standards. Their use is encouraged wherever possible.
5.6.4.2 Where matrix interferences exist, ideally a method should be validated using a matched
matrix reference material certified in a reliable manner. If such a material is not available
it may be acceptable to use a sample spiked with a chemical standard.

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5.6.4.3 It is important that the certified reference material has been produced and characterised
in a technically valid manner. Users of CRMs should be aware that not all materials are
validated to the same standard. Details of homogeneity trials, stability trials, the methods
used in certification, and the uncertainties and variations in the stated analyte values are
usually available from the producer and should be used to judge the pedigree.
5.6.4.4 For many types of analysis, calibration may be carried out using standards prepared
within the laboratory from chemicals of known purity and composition. Some chemicals
may be purchased with manufacturers certificates stating purity. Whatever the source, it
is the users responsibility to verify that quality of such standards is satisfactory.
Normally a new batch of a standard should be checked against the old. All chemical
standards should be subjected to inter/intra laboratory comparisons (amongst referred
laboratories).
Standards for compounds (for example: organic compounds) which are not available
with international traceability, should be procured from reputed manufacturers with
assured quality supported by certificate of analysis from the manufacturer
5.6.4.5 The purity requirements of chemical standards may be considered in relation to the
permitted tolerance of the method. For example, a tolerance of <0.1% of the target value
will require a chemical standard to have a certainty of concentration significantly better
than 99.9%.
5.6.4.6 Reference materials and chemical standards should be clearly labeled so that they are
unambiguously identified and referenced against accompanying certificates or other
documentation. Information should be available indicating shelf-life, storage conditions,
applicability, restrictions of use, etc.
5.6.4.7 Reference materials and standards should be handled in order to safeguard against
contamination or loss of determinant. Training procedures should reflect these
requirements.

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5.7
Sampling and Sample Preparation
5.7.1
Selection of an appropriate sample or samples from a larger amount of material is a very

important stage in chemical analysis. It is rarely straight forward. Ideally, if the final
results produced are to be of any practical value, the sampling stages should be carried
out by, or under the direction of an experienced person, with an understanding of the
overall context of the analysis. Sampling is the operation of selecting part of the
elements of a set, so that it precisely represents the distribution of the properties that we
wish to measure in the total set.
The selection of the elements constituting the sample is determined by means of a
procedure known as the Sample Plan.
The sample plan defines:
5.7.2
The quantity of the sample
The extraction system
The various terms used in sampling are dealt with in detail in recommendations
published by IUPAC. For the purposes of this guidance the definitions of sample, sample
handling, sub-sample, sample preparation and test portion are given in terms and
definitions.
5.7.3
If the test portion is not representative of the original material, it will not be possible to
relate the analytical result measured to that in the original material, no matter how good
the analytical method is nor how carefully the analysis is performed. The final result may
be dependent on the analytical method, it will always be dependent on the sampling
process.
5.7.4
As analytical methodology improves and methods allow or require the use of smaller test
portions the errors associated with sampling become increasingly important. Sampling
errors cannot be controlled by the use of standards or reference materials. Sampling is
always an error generating process and hence demands utmost care.

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5.7.5
Sample packaging and instruments used for sample manipulation should be selected so
that all surfaces in contact with the sample are essentially inert. Particular attention
should be paid to possible contamination of samples by metals or plasticisers leaching
from the container or its stopper into the sample. The packaging should also ensure that
the sample can be handled without causing a chemical or microbiological hazard. The
enclosure of the packaging should be adequate to ensure there is no leakage of sample
from the container and that contamination cannot enter.
5.7.6
The extent to which laboratories become involved in sampling varies. Some laboratories
have no responsibility for sampling, others have partial involvement, while many have
total responsibility for both sampling and testing. It is essential that the laboratory have
available fully documented procedures for sampling. These may take the form of existing
National or International Standards. For in-house procedures, these will be assessed on
the basis of the suitability of the documented procedures for their intended purposes. All
sampling equipments and devices specified in a procedure will need to be available, be
well maintained and fully comply with dimensional and other tolerances specified in the
relevant standard.
Supervisory staff, responsible for the design and documentation of sampling procedures,
must be able to demonstrate the validity of the design of these procedures. The training
and supervision of samplers must be shown to be satisfactory. Sampling procedures will
usually be witnessed as part of on-site assessments of laboratories seeking such
registration.
5.7.7
Sample identification
5.7.7.1 All samples must be uniquely and clearly identified. Identification labels must be secure
and legible. Labelling on caps or lids is considered poor practice as it can lead to
possible mixing of sample identities during testing of like batches.
Containers should be leak-proof and impervious to possible contamination during
transport. Where specified, samples should be maintained within set temperature or
other environmental tolerances during transfer to the laboratory and prior to testing. In
some cases, it may be necessary for sample containers to be pre-tested prior to use to
ensure freedom from contamination.

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5.7.8
Sample registration
5.7.8.1 On receipt, a sample must be registered into the laboratory records. The form of
registration may vary. In most laboratories, a sample register will be used, but in some
cases, the sample details may be written directly on worksheets or into workbooks.
Some sample information is essential and such criteria are covered in the subsequent
section Records System.
5.7.9
Sample retention and storage
5.7.9.1 Sample retention criteria cannot be standardised due to the varying stability and storage
considerations which apply for different materials. Each laboratorys sample retention
and storage practices are, therefore, examined individually in the light of the types of
materials tested, the use-life of the products or materials which the samples represent
and the likely periods within which a recipient of the test results may request a retest.
5.7.9.2 Samples should be stored so that there is no hazard to laboratory staff and the integrity
of the samples is preserved. Storage areas should be kept clean and organised so that
there is no risk of contamination or cross-contamination, nor of packaging and any
related seals being damaged. Extremes of environmental conditions should be avoided,
which might change the composition of the sample, for example, causing loss of analyte
through degradation or adsorption. If necessary environmental monitoring should be
used. An appropriate level of security should be exercised to restrict unauthorised
access to the samples.
5.7.9.3 All staff concerned with administration of the sample handling system should be properly
trained. The laboratory should have a documented policy for the retention and disposal
of samples. The disposal procedure should take into account the guidelines set out
above

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5.7.10 Reagents
The laboratory should purchase reagents only from reliable and reputed manufacturers.
The laboratory should also ensure that the quality of the reagents used is appropriate for
the tests concerned. The grade of reagent used (including water) should be as stated in
the method together with guidance on any specific precautions which should be
observed in its preparation or use. These precautions include toxicity; flammability;
stability to heat, air and light; reactivity to other chemicals; reactivity to particular
containers; and other hazards.
Labelling of reagents should identify substance, strength, solvent (where not water), any
special precautions or hazards, restrictions of use, and date of preparation and/or expiry.
The person responsible for the preparation of the reagent shall be identifiable either from
the label or from records.
Reagents used as primary standards for volumetric and gravimetric methods should
have a traceability to National and International standards. In cases where primary
standards are not available the reagents should be analytical grade (e.g. AR or GR) and
it should have certificate of analysis from the manufacturer along with it.
Acids and alkalies prepared for volumetric analysis should be periodically checked for
their strength and documented properly.
In the case of ultra-trace analysis using different instrumental techniques such as
GFAAS, ICPAES, ICPMS, etc. reagents such as water and acids and other organic
reagents should be purified further using ion exchange resins for water and sub-boiling
distillation for acids and organic reagents and also recrystallization and sublimation
procedures specifically for organic compounds

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5.9.
Assuring the quality of Test Results
5.9.1. Assurance and Quality Control

Analytical performance must be monitored by using quality control procedures
appropriate to the type and frequency of the testing undertaken. The range of quality
control activities available to laboratories include the use of :
reference collections
certified reference materials
internally generated reference materials
independent checks by other analysts/examiners
statistical tables
positive and negative controls
control charts
replicate testing
alternative methods
spiked samples, standard additions and internal standards
correlation of results for different characteristics of an item
retesting of retained items
Depending on the particular test/examination, one or more of these examples may be
appropriate. Quality control procedures must be documented. A record must be retained
to show that appropriate quality control measures have been taken, that quality control
results are acceptable or, if not, that remedial action has been taken. Where appropriate,
quality control data must be recorded in such a way that trends in analysis can be readily
evaluated. It is desirable to participate in proficiency testing for better quality assurance
of test results

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5.9.2. Internal Quality Control

The level adopted should be demonstrably sufficient to ensure the validity of the results.
As a guide, for routine analysis the level of internal QC typically should be not less than
5% of the sample throughout, i.e. 1 in every 20 samples analysed should be a QC
sample. For more complex procedures, 20% is not unusual and on occasions even 50%
may be required. For analyses performed infrequently, a full system validation should be
performed on each occasion. This may typically involve the use of a reference material
containing a certified or known concentration of analyte, followed by replicate analyses
of the sample and spiked sample (a sample to which a known amount of the analyte has
been deliberately added). Those analyses undertaken more frequently should be subject
to systematic QC procedures incorporating the use of control charts and check samples.

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6.
GROUPWISE CODIFICATION FOR CHEMICAL TESTS

This is a guideline for the applicant laboratories to describe the scope of testing w.r.t.
accreditation
6.1.
6.2.
6.3.
Air, Gases & Atmosphere
Ambient air monitoring
Stack emission monitoring
Fugitive emission monitoring
Solid particulate matter
Liquid mists, aerosols
Gaseous pollutants excluding vehicular
Industrial gases
Gases for medical use & diving
Reference gases & mixtures
Liquified/compressed gases
Vehicle emission
Alcohols & Alcohols based Chemical
Industrial alcohols
Alcohols based chemicals
Adhesives
6.4.
Starch based adhesives

Natural gums
Glues
Polymer based adhesives (Synthetic)
Building Materials
Cement & other mortars
Cement concrete
Refractories
Refractory cement
Sand
Clays & soils

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6.5.
6.6.
6.7.
6.8.
Pozzolonic materials
Fly-ash
Limestone, lime gypsum
Waterproofing compounds
Thermal insulation materials
Masonry bricks/blocks, etc.
Ceramics
Glass
Coal, Coke & other Solid Fuel
Coal/coke
Coal carbonization products
Coaltar/bitumen
Charcoal
Briquetted solid fuels
Cosmetics & Essential Oils
Perfumes
Essential oils
Cosmetics and toiletries
Intermediates and miscellaneous chemicals for cosmetics
Herbal-based cosmetics
Dye & Dye Intermediates
Synthetic dyes
Dye intermediates
Natural dyes & colouring materials
Disinfectants
Disinfectants and their formulation

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6.9.
6.10.
6.11.
6.12.
Drugs & Pharmaceuticals
Synthetic drugs
Natural drugs (medicinal plant preparations)
Pharmaceutical formulation
Drug intermediates and raw materials
Veterinary preparations (herbal & synthetic)
Vitamins
Vaccines & sera
Antibiotics
Enzymes
Hormones
Chemicals used in compounding pharmaceuticals
Explosives & Pyrotechnics
Ammunitions
Industrial explosives & associated material
Pyrotechnics
Explosives chemicals and allied materials
Fertilizers
Nitrogeneous fertilizers
Phosphatic fertilizers
Fertilizer mixtures
Potash fertilizers
Micronutrients
Bio-fertilizers
Foods & Agricultural Products
Alcoholic drinks & beverages
Animal feeds
Bakery and confectionery products
Cereals, pulses, and by-products
Coffee, coca and by-products

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6.13.
Milk and dairy products
Tea and tea products
Starch can starchy products
Fish and fishery products
Food additives
Colour, flavour & preservatives
Honey and honey products
Fruits and vegetable products
Infant foods
Meat and meat products
Spices and condiments
Sugar and by-products
Tobacco and by-products
Soft drinks
Nuts & nut products
Oil seeds & by-products
Fruit juices & concentrates
Egg & egg products
Vitamins in foods
Mycotoxins in food & feed
Pesticides residues in food
Polyhalogenated biphenyls
Sensory evaluation-flavour
Oil, fats and related products
Shelf-life
Inks
Printing inks
Writing inks
Duplicating inks

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6.14.
6.15.
6.16.
6.17.
Industrial and Fine Chemicals
Inorganic chemicals
Organic chemicals
Electroplating chemicals
Solvents
Laboratory chemicals
Analytical reagents
Speciality chemicals for:

_ Leather industry
_
Rubber industry
Textiles industry
Electronics industry
Photographic industry
Agricultural chemicals
Firefighting chemicals
Trace elements analysis
Carbon black
Wood and timber treatment chemicals
Lac & Lac Products
Lac
Lac products
Leather
Leather
Synthetic leather
Lubricants
Trace elements
Oils & greases
Solid lubricants
Aviation lubricants
Lubricant additives
Microcrystalline wax

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6.18.
6.19.
Ores & Minerals
Iron ores
Copper ores
Zinc ores
Nickel ores
Manganese ores
Tin ores
Lead ores
Titanium ores
Molybdenum and tungsten ores
Chromium ores
Precious metals ores
Rare metals ores
Radio active metals ores
Bauxite
Limestone & dolomite
Rock phosphate
Gypsum
Silica sands
Mineral sands
Mineral for refractories
Mineral for insulation materials
Other minerals
Minor elements
Gem & semi-precious stones
Geochemical samples for trace elements
Metals and Alloys
Iron, steel and ferro-alloys
Special steel
Copper & its alloys
Aluminium & its alloys
Tin and tin alloys

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6.20.
6.21.
6.22.
Zinc & inc alloys
Lead & lead alloys
Magnesium & magnesium alloys
Nickel, chromium, cobalt & their alloys
Titanium & titanium alloys
Tungsten & its alloys
Other metal alloys
Precious metals
Paints and Surface Coating
Paints and enamels
Vehicles, solvents, thinners
Pigments and extenders
Polishes
Painters materials (gums, driers, paint removers)
Drying oils
Powder coating
Resin coatings
Paper and Pulp
Pulp
Paper, paper board and speciality papers
Newsprint and board packing materials
Composite packing materials
Petroleum
Crude petroleum
Fuels-gaseous, liquid & solid
Aviation fuels
Waxes and jellies
Miscellaneous products, white oil, anti-freeze, solvents insulation oils, feed-stock
Bituminous asphalt, tars and allied products
Pour point depressants (flow improvers)

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6.23.
6.24.
6.25.
6.26.
6.27.
Petrochemical feedstocks
De-icing fluids
Hydraulic fluids
Fuel additives including corrosion preventives
Trace analysis in petroleum products
Plastics and Resins
Resin
Plastics & polymers
Raw materials
Plastic films
Pesticides
Synthetic pesticides & their formulations
Natural pesticides & their formulations
Pheromones, chitin inhibitors
Weedicides
Herbicides
Fungicides
Pollution & Environment
Liquid effluents
Solid wastes
Hazardous solid wastes
Toxic waste
Tests related to work place environment & hazards
Rubber & Synthetic Rubber
Natural rubber
Synthetic rubber
Soap Detergents and Toiletries
Soaps
Synthetic detergents
Wetting and emulsifying agents

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6.28.
6.29.
6.30.
6.31.
Textile & Textile Auxiliaries
Fibre & filaments
Yarns & chords
Fabrics, garments and made-ups
Auxiliaries
Technical textiles (geo-textiles, medical textile, automotive textiles)
Water
Potable and domestic
Irrigation
Industrial/cooling purposes
Steam raising
Medicinal purposes
Distilled demineralized
Waste water
Trace metal elements
Pesticides residues
Bore water
Saline water
Metallic Coatings and Treatment Solutions
Metallic coatings
Conversion coatings
Plating solutions
Anodizing solutions
Metal finishing materials
Corrosion Tests
Salt spray tests
Dezincification tests
Other tests

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Annexure A
Health and Safety
Health and safety are everyones responsibility and require the commitment of each employee
to be effective. Managements commitment is essential for long term success of a health and
safety programme. Such a cooperative relationship will safeguard the employees of the
Laboratory as well as address managements responsibility and liability.
All elements of the laboratorys health and safety programme must be clearly documented in a
manual which is readily available to all staff.
Examples of procedures which must be included, where appropriate, are:
procedure for handling chemical spills,
cleaning and decontamination procedures for radioactive spills,
evaluation procedures including a plan of the facility showing the location of safety
equipments and fire extinguishers,
policy on the use of protective clothing eg. gowns, coats, gloves, goggles etc.
policy on eating, drinking, applying cosmetics etc. in the laboratory,
waste disposal procedures,
routine cleaning and disinfection procedures for work benches, floors, centrifuges,
refrigerators, etc,
accident reporting protocols,
special procedures for handling hazardous substances.
Material safety data sheets must be available in conjunction with the safety manual. Work
related Accident Insurance coverage for all employees shall be provided by the Management.
In large laboratories an officer may be designated as the Health and Safety Manager. Ideally,
the Health and Safety Manager should have received training in occupational health and safety
concepts and in the relevant legislative requirements. The health and safety programme must
be monitored regularly and audited at least annually to ensure that its requirements are being
met.

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Proper equipment and material must be available to handle toxic and carcinogenic and or other
dangerous material spills. Where appropriate, the laboratory should have safety showers and
eye wash equipment of suitable locations and in good working condition. The operation of safety
showers must be checked regularly. If commercial eye wash preparations are used, it must be
ensured that the solutions are within their expiry dates or if distilled water is used the water must
be changed at least once a week.
Sufficient exhaust hoods must be available to maintain a safe work environment. Fume cabinets
must comply with relevant National/International Standards.
Sufficient first aid kits must be available and strategically located. An adequate number of
personnel must be trained in first aid procedures. Appropriate storage must be provided for
volatile, flammable, explosive and other hazardous materials. A flammable liquids storage
cabinet is required for all but small volumes. Acids and solvents should not be stored together. It
may be necessary to store some material in locked cabinets/cupboards and magazines.
Storage on high shelves is discouraged. Suitable carriers must be available to carry large
bottles. The emergency exits from the laboratory must provide safe passage in an emergency.
Evacuation routes must always be kept clear. General cleanliness and good house keeping
must be apparent. Food stuffs must not be kept in laboratory refrigerators/freezers/ ovens. .
There must be a documented waste management programme which includes procedures for
the disposal of:
chemical wastes
sharp and broken glass
uncontaminated waste, for example, paper waste
radioactive waste
A register must be maintained of laboratory accidents, injuries and other incidents and the
follow-up action taken. Suitable protective clothing/equipment must be available at all the times.
The nature of these items will be dependent on the work being undertaken and might include:
laboratory coats/gowns
disposable gloves
rubber gloves

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heat/cold resistant gloves

protective eye wear
face masks
plastic/rubber aprons
foot wear
When radioactive and X-ray work are performed, detectors must be used regularly to monitor
radiation levels and the wearing of film badges by staff may be necessary. Radiation badges are
to be worn by personnel working in X-ray and radiative hazardous areas. Laboratory shall
monitor control and record radiation levels as required by relevant specification methods and
procedures or where they influence the safety of personnel. Staff must be advised of
appropriate precautionary measures. It is recommended that relevant records be kept.
Appropriate hand-washing and hand-drying facilities must be available. Hand-basins should not
be fitted with domestic taps but with a suitable alternative, for example, elbow or foot-activated
devices. The use of communal towels is discouraged. Single use towels or automatic handdrying devices are preferred. A suitable cleaning agent must be available. Gas cylinders must
be secured. Samples/ specimens/exhibits referred to other laboratories must be transported in
accordance with the Indian Post or other relevant requirements.

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ISO/IEC APPLIC APPLICATION TION DOCU DOCUMENT MENT Annexure
-B
EQUIPMENT CALIBRATION INTERVALS (as per NATA Document)
Laboratory equipment calibration and check programs should cover:

a)
commissioning of new equipment (including initial calibration and checks after installation);
b)
operational checking (checking during use with reference standards or reference

materials);
c)
periodic checking (interim but more extensive checking, possibly including partial
calibration);
d)
scheduled maintenance by in-house or specialist contractors;
e)
complete recalibration.
Some items of equipment, such as balances, require rechecking or recalibration if they are
moved or repaired. In general, NATA will accept recalibrations by laboratory staff of items
marked * if the laboratory is suitably equipped, appropriate calibration procedures are
documented (along with the applicable measurement of uncertainty) and the staff has
demonstrated it is competent to perform such recalibrations.
Where calibrations are performed by laboratory staff, full records of these measurements must
be maintained, including details of the numerical results, date of calibration and other relevant
observations.
Note: These are not NABL requirements, but are being provided as a reference guideline
for the benefit of the laboratories and their users.

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CALIBRATION APPENDIX A: CALIBRATION OF COMMON TEST EQUIPMENT

The following requirements for frequency of recalibration and checks on test equipment with
reference to specific calibration and check procedures to be followed. The time intervals
indicated are maximum intervals and are dependent on the accuracy required and the type of
use the instrument is exposed to.
In general, the calibrations are carried out by an external calibrating authority and an endorsed
test report is obtained for this work. If a laboratory wishes to carry out these calibrations inhouse they must demonstrate the capability to do so according to the criteria set out in ISO/IEC
17025: 2005 sub-clause 5.6.2.1.
Checks are normally carried out in-house by the laboratory staff. If however, the checks are
carried out by an external authority then an endorsed test report must be obtained.
ITEM OF EQUIPMENT
Calibration
Interval
(years)
Checking
Interval
(months)
Procedures
and
References
AIR FLOW NOZZLES
Initial
ANEMOMETERS
12
Check throat diameter
AUTOCLAVES
Initial
1
Each Cycle
BALANCES
See also weighing instruments
Temperature profiling of typical loads. NATA

Technical Note 5
Check temperature distribution with no
loading.
Record the temperature, pressure, time and
type of load.
External by NATA accredited calibration
authority or in-house using calibrated
masses refer to Calibration of Balances
Prowse.
12
Service
Repeatability check.
One point check
Each weighing
Zero point check
BAROMETERS
Fortin
Aneroid
Initial
1
60
One point check with transfer instrument.
CALLIPERS (VERNIER)
AS 1984
DIAL GAUGES
AS 2103

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ELECTRICAL INSTRUMENTS
Digital multimeters
Compare with meters of similar resolution.
Analog meters
Compare with meters of similar resolution.
Data loggers
Check at zero and the maximum point.
ENVIRONMENTAL
CONDITIONING CHAMBERS
IEC 600688-2-1,-2,-3,-33,-38,-39
On use
Check at the working temperature
FORCE TESTING MACHINES

Dead weight
AS 2193
Elastic dynamometer
AS 2193
Hydraulic, pneumatic
AS 2193
FURNACES
Initial
12
On use
AS 2853
Check variation within the working zone at
the working temperature
Monitor temperature
HYDROMETERS
Reference
Working - glass
12
Check against reference hydrometer or in

newly prepared solutions of known density.
AS 2026, ASTM-E126
Working - metal
ISO 649.1, .2, ISO 650
Compare
thermometers
at
room
temperature with wick dry. AS 2001.1
Appendix C.
HYGROMETERS
Assmann
and
psychrometers
sling
10
Thermohygrographs
Weekly
Electronic types
Check against a calibrated psychrometer
MANOMETERS
Reference, liquid
10
Working, liquid
36
Check the cleanliness of the fluid
Electronic
36
Check the cleanliness of the fluid
MASSES
Reference
of
integral
stainless
steel
or
nickel
chromium alloy
Working stainless steel,
3 then 6
subsequent
3
nickel chromium alloy

Working other alloy
MICROMETERS
1
5
AS 2102
1
ORIFICE PLATES
Initial
Check zero and one point against gauge

block. Inspect anvils.
BS 1042.1
Visual check for wear and damage.

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PRESSURE EQUIPMENT
Test
gauges
used
for
calibration of industrial gauges
AS 1349
Industrial gauges not subject to

shock loading
Industrial gauges subject to
shock loading
AS 1349
6 months
AS 1349
Pressure transducers
Calibrators
SIEVES
Initial
12
On use
Compliance certificate to AS 1152, BS 410.

Depending on the accuracy required, more
or less frequent checks may be required
against a reference set or a suitable
reference material.
Visual check for wear and binding.
TAPE MEASURES, RULES

Tape measures
Initial
Steel rules
Initial
AS 1290.4, BS 4035
2 to 5
Check at maximum length, depending on

use and accuracy required.
BS 4372
TEMPERATURE
CONTROLLED ENCLOSURES
Ageing
AS 2853
Daily
BOD
On use
Drying
Initial
Monitor temperature
Check the temperature at the start of the
test.
The
maximum
and
minimum
temperature of the laden chamber must be
monitored for the test period.
Temperature variation and evaporation rate
must be checked.
AS 2853, AS 1289 Part 0, BS 2648
24
On use
Vacuum
24
Check temperature variation within the

working zone.
Monitor temperature
Check temperature variation and pressure in
the working space.
AS 2853m VS 3898, BS 3718
TEMPERATURE (DIGITAL)
INDICATING SYSTEM
Hand-held, bench type and
temperature loggers
Calibrate against a reference temperature

measuring system.
Initial
Check efficacy of automatic cold junction

compensation with the temperature sensor
at the ice point.
Check at ice point.

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THERMOMETERS
Reference, platinum resistance
Reference, liquid-in-glass
AC temperature bridge
Working - liquid-in-glass
Working - resistance
Working - digital display
10
CSIRO/NML Temperature
Course Book 2
Before use
Check at ice point
Before use
Check at ice point
Measurement
10
Check linearity and resistance ratio.

Initial
6
Check at ice point or at one point in the

working range against a reference
thermometer.
5
6
Check R at ice point
Check at ice point or at one point in the

working range against a reference
thermometer.
THERMOCOUPLES
K type, sheathed
Initial
K type, wire
For use up to 400C. For use above 400C

to 1100 C the same immersion must always
be used.
Initial (reel
of wire)
T type, wire
For use up to 400C.

Replace if used above 400C.
Initial (reel
of wire)
K and T types
For use up to 350C.

6
Check at ice point.
Test aurally against the Telstra speaking

clock. Two measurements separated by one
hour (ie. a one hour period) must be carried
out.
TIMING DEVICES
Stop watches, clock
WEIGHING INSTRUMENTS
See also balances
Non-automatic weighing instruments.

Uniform Test Procedures, Inspectors
Handbook No 2 for class III and IV
Instruments.

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CALIBRATION
APPENDIX
B:
CALIBRATION
INTERVALS
FOR
CHEMICAL
TESTING EQUIPMENT
The following table sets out the nominal maximum periods between successive calibrations of
general equipment, not listed in the previous table, for laboratories holding accreditation in the
field of Chemical Testing. Subsequent appendices in this section list specific calibration
requirements for special purpose testing. This table also contains information that expands on
the previous table to aid the chemical laboratories.
ITEM OF EQUIPMENT
Maximum
period between
successive
Calibrations or
Checks
BALANCES
BAROMETERS
Procedures
and
Comments
Note 1:
Balances with in-built calibration check

facilities must also have monthly and 6monthly checks carried out.
Note 2:
Electronic balances with more than one range

must have monthly and 6-monthly checks
carried out on all ranges.
For Fortin barometers see NAR Calibration Appendix 1.

Aneroid barometers (mechanical and electronic) should
be checked at least six-monthly. One point is sufficient.
Refer to NATA Technical Note 8 for subsequent
recalibration and checking requirements.
CENTRIFUGES
*1 year (where
operating speed
is specified)
Tachometer (mechanical stroboscope or light cell type).
COMPARATORS
Lovibond
*2 year
Check condition of discs (this check could be done with a

spectrophotometer referenced to standards)
PYKNOMETERS
*1 year
AS 2378; BS 733 App A; IP 190
DENSITY METERS
*Initial; whenever
test temperature
is changed or cell
cleaned
DENSITY BOTTLES,
* Daily
ASTM D4052
With pure substance of known density.
*1 week
Air and double-distilled water.
High flow, ie >1 L/min
*2 years
ASTM D3195
Low flow, ie <1 L/min
*2 years
Soap bubble flow meter.
Rotameters (Working)
*Each time on
use
Soap bubble flow meter.
FLOWMETERS
Rotameters (Reference)

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Orifice plates
Initial
*6 months
BS 1042 Part 1 (calibration by an approved testing

authority)
Visual inspection for damage, wear or contamination.
Wet test meters
*2 years
ASTM D1071
Anemometers
2 years
Calibration by an approved testing authority.
Pitot tubes
*Initial
Check dimensional compliance with BS 1042 Sec 2.1

Annex A.
*On use
Inspect tip for damage, blockage, etc as required by BS

1042 Sec 2.1
FURNACES (FOR USE AT

SPECIFIED
TEMPERATURES)
(In addition to other requirements)
*On use
Monitor temperature with an appropriate sensor
GAS METERS
*2 years
GAUGE BLOCKS
4years
(reference)
*2 years(working)
Calibration by an approved testing authority

Check against reference blocks.
GLASSWARE
(1)
Specialised
calibrated
glassware
water
traps,
sulphonation
flasks,
centrifuge tubes etc
*Initial
AS 2162.1
Piston operated *Initial AS

2162.2 volumetric apparatus
(see below)
Pipetters
*Initial
AS 2162.1
*Initial
Check volume delivered. For adjustable devices check

volume delivered at several settings (refer to AS 2162.2).
(2)
*3 months
Dispensers
*Initial
*3 months
Diluters
Displacement burettes
Check volume delivered at settings in use.

Check volume delivered. For adjustable devices check
volume delivered at several settings (refer to AS 2162.2).
Check volume delivered at settings in use.
*Initial
Check sample and diluent volumes or dilution ratio and

total volume (refer to AS 2162.2).
*6 months
Check sample and diluent volumes or dilution ratio and

total volume (refer to AS 2162.2).
Check volume delivered at maximum and two other
settings.
*Initial
*When
barrel/plunger is
changed
Check volume delivered at maximum and two other

settings.
HYDROMETERS
In addition to other requirements
*On use
Check that scale has not slipped.
*On use
Monitor temperature throughout use, with appropriate

sensor, and record temperature daily.
OVENS
In
addition
requirements
to
other
Ageing
*Daily
Monitor with appropriate sensor and record.
Drying
*On use
Monitor with appropriate sensor and record.

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PENETRATION
NEEDLES
CONES
AND
5 years
Calibration by an approved testing authority. ASTM D217;

IP 50; ASTM D5; ASTM D1321.
*On use
Visually inspect needle tips.
5 years
Calibration by an approved testing authority.
POTENTIOMETERS
Reference
Working
*One year
Check against reference potentiometer.
PRESSURE GAUGE TESTERS

Deadweight
5 years
Manometers
10 years
PYROMETERS
Reference
3 years
Working
*6 months
REFRACTOMETERS
*On use
*6 months
REFRIGERATORS
BS 1041 (Part 5). Calibration by an approved testing

authority
Check against reference pyrometer
Check against distilled water
Check against bromonaphthalene or other reference
compound of known refractive index.
Where critical, the temperature of the working space must
be monitored by an appropriate temperature sensor
throughout use and recorded.
TACHOMETERS
Reference
5 years
BS 3403. Calibration by an approved testing authority
Working
*1 year
Check against reference tachometer
*Initial
Against reference oils. ASTM D2162
VISCOMETERS
U-tube
Reference
*10 years
Working
*Initial
*2 years
Using quality oils against reference tubes or using

reference oils.
ASTM D2162/D445; IP 71
Others
Brookfield
*Initial
*2 years
Against reference oils. ASTM D2556

Against quality (ie. manufacturers) oils
*1 month
Ferranti
*Initial
Against reference oils.
*3 months
Zahn
*Initial
Against reference oils
*1 year
*
commonly done by laboratory staff
IS
Volumetric plasticware is not acceptable because it is prone to irreversible volume changes and deformation.

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CALIBRATION APPENDIX C: PERIODICAL CALIBRATION OF EQUIPMENT FOR

MONITORING STANDARD OPERATING CONDITIONS FOR ASTM METHODS
D2699, D2700 (RON AND MON)
Checks as specified in Calibration Appendices A and B must be carried out on all
thermometers, burettes, viscometers, dial gauges and other items of equipment. Maintenance
and standardisation checks must be done at the intervals specified in ASTM methods D2699
and D2700. Full records of these checks must be kept.
CALIBRATION APPENDIX D: CALIBRATION OF EQUIPMENT FOR TESTS ON COAL AND
COKE
ITEM OF EQUIPMENT
BOMB CALORIMETERS
Pressure, mechanical and

dimensional tests on bombs
Maximum period
between
successive
Calibrations or
Checks
Procedures
*On use
Checks on calorimeter dimensions and for thread

slackness
*3 months
Determination of the water equivalent (bomb factor)

Refer AS1038 Part 5
3 years or 1000
firings depending
on use
Checks as prescribed in AS 1038 (see also BS 4791).

More frequent checks required if calorimeter is
damaged or used repeatedly.
and
Comments
Calibration by an appropriate testing authority.

CRUCIBLE
SWELLING
NUMBER BURNERS
*1 month
Heating profiles of all burners Refer AS 1038 Part 12.1
DENSITY BOTTLES
*3 months
Refer AS 1038 Part 21
DILATOMETER
*6 months
Temperature (absolute and gradient), piston assembly

mass and tube wear. Refer AS 1038 Part 12.3
FROTH FLOTATION CELLS
*12 months
Check cell block and impeller dimensions. Refer AS

4156.2.1
*12 months
Measure and record test zone temperature by the
FURNACES
Ash
use of a certified reference thermocouple, or a working

thermocouple or a calibrated electronic thermometer.
Refer AS 1038 Parts 3,6, 12.2, 15
Gray-King
*12 months
Tube
*12 months
Volatile Matter
*6 months
Ash Fusion
*3 months
GIESELER PLASTOMETER
Bath temperatures
* 6 months
Remove thermocouple and check against reference.

Refer AS 1038.12.4.1
Torque Test
*1 month
Rabble Arms
*Initial
*50 determinations
Check against torque meter.

Check dimensions.
Check for wear.

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HARDGROVE GRINDABILITY
Apparatus
*12 months
Calibrate against four national reference coal samples

with certified grindability indices. Refer AS 1038 Part
20.
Mill revolutions
*12 months
Check number of revolutions per minute.
*12 months
Preferably check side by side against certified reference

hydrometers. If not available check against freshly
prepared solutions of known density. Refer AS 2026.
Laboratory may isolate own reference set of
hydrometers after in-house calibrations.
*On use
Check precision (refer AS 1038 Part 16) against

Standard Method ( AS 1038 Part 6) or against certified
reference materials which cover the full working range.
Prior to each
sample, at fifteen
minute intervals and
at end of sample
measurement
Calibrate using glass or mineral reflectance standards.

Refer AS 2486
HYDROMETERS
Working, for float and sink
testing
INSTRUMENTAL ANALYSERS
For carbon, hydrogen, nitrogen or
sulphur
MICROSCOPE PHOTOMETER
For reflectance measurements
OVENS
Direct gravimetric
*12 months
Check temperature gradient over sample area
Drying
*12 months
Check temperature of working space
Minimum free-space
*12 months
Check temperature
SHALE BREAKDOWN
APPARATUS
Andreasen sizing apparatus
* Initial
Check flask volume, height of stem and pipette volume.

Refer AS 4156.1
Drum tumbler
* 12 months
Check revolution counter on tumbler. Refer AS 4156.1
Check every six months against certified reference thermocouple. (A Gray-King furnace is quite convenient as a
heat source).
NOTES
(I)
The period given between successive calibrations is a maximum period. More frequent calibrations may be
required if the equipment is repaired, moved, is in constant use or a change in operating circumstances
occurs.
(II)
Accredited coal laboratories must maintain adequate quality control in supervision of equipment performance
by the use of appropriate reference materials on a regular basis.
(III)
Whenever possible, unless otherwise stated in the relevant standard, equipment should contain all items of
apparatus specified in the test method when being calibrated.
(IV)
The calibration requirements for other general items of equipment used in coal and coke testing (eg. balances,
thermometers, thermocouples, volumetric glassware, etc) are found in this booklet in Calibration Appendices A
and B.

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CALIBRATION APPENDIX E: PERIODICAL RECALIBRATION OF EQUIPMENT FOR

PHYSICAL TESTS ON PAINTS TO AS 1580
ITEM OF EQUIPMENT
Maximum period
between
successive
Calibrations or
Checks
Procedures and Comments
METHODS 101.1, 101.4, 101.5

Thermohygrograph
*1 month (retain
charts)
Psychrometer
10 years
*6 months
Anemometer
Against calibrated psychrometer

Complete.
Against reference thermometer
2 to 5 years
depending on
use.
Illumination meter
METHOD 101.3
Forced draught oven
Stoving
METHOD 107.3
Reference wheel gauge
Working gauges
*6 months
5 years or *2
years to 5 years
depending on
use.
5 to 10 years
depending on use
2 years
*1 year
Check oven thermometer against reference thermometer.

Temperature variation in working space. (Refer AS 2853)
By approved testing authority. Calibration by laboratory
staff.

Calibration by an approved testing authority, or
Against reference wheel gauge.
METHOD 108.1
Shims
Magnetic instruments
Initial only plus

frequent visual
examination
*On use
Shims bearing ASTM or NIST stamps do not require initial

external calibration.
Against calibrated shims
METHOD 108.2
Paint inspection gauge
METHODS 202.1; 202.2
Pycnometer
* Initial only
*Initial
(at least 50ml capacity)
Graticule and cutting angle of cutting tip

Check capacity.
*6 months
METHOD 204.1
Fineness of grind gauge
block and scraper
Reference
Working
5 to 10 years
depending on
use.
Calibration by approved testing authority.
*1 year plus
frequent visual
examination
Against reference using at least four paints covering the

working range

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METHOD 211.1, 211.2

Settling spatula
METHOD 214.1
Krebs-Stormer Viscometer
*Initial only
Dimensions and mass
*6 months
Re-examine for wear and change
*Initial only
+Masses and paddle dimensions
*Initial, then 1
year
Reference oils
2 years
++Against standard oils stored in sealed container

Replace. Store as directed, well sealed, clean
METHOD 214.2
Flow cup
*Initial only
*Initial, then
*3 months (for
cups in
constant use), or
*1 year (other)
Reference oils
Dimensions
++ Against standard oils stored in sealed container
2 years
As for 214.1
Initial
*On use
2 years
Verification of plate temperature

As for 214.1
* Initial, then 1
year
++Against standard oils stored in sealed container.
METHOD 214.3
Cone and plate viscometer
Reference oils
METHOD 214.4
Roto thinner viscometer
Reference oils
2 years
METHOD 214.5
Brookfield viscometer
* Initial, then 1
year
*1 month
Reference oils
2 years
As for 214.1
Against manufacturers oils
As for 214.1
METHOD 301.1, 301.2

Oven
*6 months
Oven thermometer against reference thermometer
*2 years
Temperature variation in working space.
* Initial
Dimensions and mass of beads delivered
METHOD 401.1
Spoon
METHOD 401.6
Mechanical thumb
METHOD 401.8
Ramp/roller
Roller rubber bands
* Initial only
Dimensions and masses (those that

disassembled must be
checked against one known to conform).
2 years
Hardness of rubber plunger
* Initial
Dimensions and mass
2 years
Hardness.
cannot
be

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METHOD 402.1
Bend
test
mandrels
apparatus
and
* Initial only
Dimensions.
METHOD 403.1
Scratch test apparatus
Initial only
*1 year
Needle dimensions.
Inspect under microscope for wear and damage
METHODS 408.1, 408.3

Adhesion test apparatus
Initial only
Dimensions of cutting tips and points
*1 year
Re-examine under microscope
* Initial
Mass, length and rate of travel
METHOD 459.1
Sponge and holder machine
METHODS 459.1, 461.1,
481.1,481.2, 482.1
Grey scales
Reference
10 years
Working
Replace.
*3 months
Check against reference set.
100 hours
Check lamps, voltage and illumination levels.
METHOD 601.1
Light booth
Colour blindness test
* Initial
Refer Tests for Colour Blindness by S Ishihara
METHODS 601.2, 601.3

Colour master
*On use
Calibration of photometer scale using reference tiles

supplied by manufacturer
Colour eye
METHOD 602.1
Specular gloss
standards
Initial
External certificates (NIST)
5 years
Supplied by manufacturer
METHOD 602.2
Gloss tiles
Primary
Secondary
*6 months
Instrument
*On use
Against primary tiles

Against secondary gloss tiles
Commonly done by laboratory staff
Krebs-Stormer viscometer is considered acceptable as long as it gives a value within 15% of the expected
load for 200 rpm for a given oil and within 5% of the consistency in Krebs units.
If dimensions do not conform, the instrument must be calibrated with two standard viscosity oils to ASTM D562
++ Standard oils need only be replaced every 2 years if correctly stored (in the dark, at the room temperature, in
closed glass or tinned metal containers, free from contaminants).

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NOTES
DETERMINATION OF COLOUR AND VISCOSITY OF RESINS
Accreditation for colour and viscosity of resins using Gardner colour standards and GardnerHoldt viscosity standards (to Federal Test Method. Standard No 141a and ASTM Methods) is
granted on the basis that the applicant can obtain results comparable with laboratories already
accredited for these tests, as an alternative to fundamental calibration of these standards.
QUALITY CONTROL TESTS
NATA Technical Note 1 details requirements for accreditation of quality control testing of paint.

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CALIBRATION APPENDIX F: CALIBRATION OF GAS ANALYSERS

(Except for Motor Vehicle Emission Testing to Australian Design Rules - See Appendix G)
These calibrations should be performed by approved testing authorities using gases of known
concentrations or NATA approved blending techniques appropriate to the gas being measured.
ITEM OF EQUIPMENT
GAS DETECTION INSTRUMENTS

for use in mines, and also for
industrial
and
commercial
applications
Maximum period between

successive Calibrations or
Checks
Procedures
and Comments
Before use Span and zero

check (weekly on field
instruments used for
continuous monitoring)
1 point span check made on 75%-90% of full

scale of range being used. (At approximately
50% for combustible gas detectors with an
output scale of zero to 100% lower explosive
limit).
*6 months complete
recalibration
Six point (and zero) for NDIRS (with

recommended values of 15, 30, 45, 60, 75
and 90% full scale deflection).
Three point (and zero) (see note vi) for other

types including UV, chemiluminescence,
refactive
index,
catalytic,
FID,
electrochemical,
thermal
conductivity,
paramagnetic
and
zirconium
oxide
detectors.
Two point (and zero) (see note vi) for fixed
or stationary instruments (catalytic) and
combustible detectors with an output scale
of zero to 50% lower explosive limit. 1 point
for single point alarm instruments (see note
vii).
2 years
Full calibration, including maintenance and

overhaul to be conducted above ground.
REFERENCE GASES
Non-reactive reference gases at

a concentration greater than
100 ppm
4 years or once the cylinder

pressure drops below
700kPa (100 psi), whichever
comes first.
Non-reactive reference gases at

a concentration of 100ppm or
less whichever comes first.

drops below 700kPa
(100psi)
Reactive reference gases

pressure drops below
700kPa(100psi), whichever
comes first

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NOTES
(i)
Frequency given is MAXIMUM period between calibrations.
(ii)
Instruments must be completely recalibrated after significant maintenance.
(iii)
The calibration history for each instrument must be recorded.
(iv)
The initial calibration must check interferences. The laboratory should be aware of the
contaminants which may create cross-sensitivity.
(v)
Calibrations must be performed more frequently (see Note (ii)) if poisons are likely to be
present for any catalytic sensor.
(vi)
Calibrations using 2 or 3 points (and zero) must adequately cover the range. One point
must be between 75% and 90% of full scale, except for fixed or stationary instruments
used in explosive atmospheres with scales 0 - 100% lower explosive limit, the highest
calibration point approximately 50% lower explosive limit.
(vii)
For single point instrument alarms, a one-point calibration is performed at the level at
which the instrument alarms.
(viii)
Fixed instruments with remote head should be calibrated in-situ, where possible, but if
calibrated in a laboratory suitable leads (same resistance) must be used. Also a polarity
check should be made when the instrument is reassembled.
(ix)
The gas flow rates necessary for optimum response of flame ionisation detectors should
be checked regularly. Zero checks must be made with high purity gases (depending on
precision and accuracy required). Oxygen-quenching effects must be determined on
commissioning only.
(x)
For low level alarms (and semiconductor type detectors) all operating parameters must
be included on the calibration certificate and the instrument must be calibrated with the
gas type which the instrument is to measure.
(xi)
A non-linear instrument, such as non-dispersive infrared analyser, which has a

linearising circuit is not considered to be a linear instrument. A nominally linear
instrument is linear if its response is within 2% of linearity over its range.
(xii)
Wosthoff pumps and gas dividers should be checked annually by an accredited testing
authority.

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METHOD OF REPORTING
Test documents relating to the calibration of gas analysers must meet NATAs general
requirements set out in this booklet. The conditions of tests (temperature, gas mixtures,
laboratory, in-situ, etc.) must be clearly stated and the meaning of the test result must be
unambiguous.
Endorsed test documents must only relate to the calibration of the instrument. Any servicing,
maintenance or opinions on the performance of the instrument must appear on a separate, nonendorsed attachment.
In addition, there must be traceability to the reference gases used for calibration or the method
of generating references (eg. Wosthoff Pump). This must be stated, either on the report or on
the relevant work sheets.

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CALIBRATION APPENDIX G: PERIODIC RECALIBRATION OF EQUIPMENT FOR

VEHICLE EMISSION TESTING LABORATORIES
The following table lists the requirements for periodical calibration of instruments and test
equipment used for motor vehicle emission testing by testing laboratories holding accreditation
in the field of Chemical Testing:
7.90
Motor Vehicles
.01 Vehicle emissions
.02 Fuel consumption tests
It also shows the reference standards for calibration and, where available, the standards
describing detailed procedures for calibration. These are taken from National Standards and
from Australian Design Rules, and also from current emission laboratory testing practice in
Australia. In general, NATA will accept recalibrations carried out by laboratory staff of items
marked *, provided that the laboratory is equipped with the required calibration standards and
the staff is competent to perform such recalibrations.
ITEM OF EQUIPMENT
Maximum period
between successive
Calibrations or Checks
Procedures
and
Comments
CONSTANT VOLUME
SAMPLER
*500 hours of use after

stabilising period or
major maintenance
ADR 37/00 - Appendices 5 (Method), 12
Positive Displacement Pump

Critical Flow Venturi
System verification
Propane
*As indicated by CVS

system verification
Reference Standard; Air Flow Meter (Laminar Flow

Element, Subsonic Venturi or orifice plate).
Calibration traceable to NIST. Accuracy 1 % of air
flow.
*1 week or after
Using CP Propane (C3H8) or Carbon Monoxide or

Carbon Dioxide.
maintenance or
servicing of system
Carbon Monoxide
System accuracy in the order of 2% critical flow

orifice or bomb method
Carbon Dioxide
NOTE: Precautions for use of pure carbon

monoxide
Correlation car
*As required to
supplement other
methods
Approved in-house laboratory methods.

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DYNAMOMETERS
Chassis
Load scale
AS 2193. NML Class B Certified Masses
Knife edge
5 years
Pneumatic/ Hydraulic link
2 years
Electronic
2 years
Bourdon tube
6 months
Roller speed
*3 months
Power absorption
*1 month
Performance check
*1 week
Distance measurement
Digital counter with stop watch
*6 months
Engine
Load scale
AS 2193. NML Class B Certified Masses.
Knife edge
5 years
Pneumatic/ Hydraulic link
2 years
Electronic
2 years
Bourdon tube
6 months
Speed
DYNAMIC
DEVICE
*3 months
GAS
Digital counter with stop watch
BLENDING
Standard gas dividers
*1 year
Using gas analyser and primary gas standards for

each gas type.
*Each use
Single point
*On commissioning or
major overhaul
Anemometer
FANS
Engine cooling

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FLOWMETERS
Air Flow Meter
Laminar Flow Element (LFE)
Orifice Plate
*100 hours of use or

more frequently if drift
occurs
10 years
Venturi Flow Meter
10 years
Anemometers
2 years
Visual inspection
contamination
for
damage,
wear
and
Calibration traceable to NIST

Master within 1%,
ADR 37/00, Appendix 5
Rotameters (see Note below)

Reference
High flow
>1 L/Min
Low flow
*2 years
ASTM D3195
*2 years
Soap bubble flow meter
*On use
Soap bubble flow meter
<1 L/Min
Working
Fuel Flowmeters
*6 months
Gas analyser
For
motor
emissions
vehicle
exhaust
*Span and zero check

before and after each
analysis on each
analyzer
ADR 37/00 Appendices 10, 12, 13
*Complete recalibration
of all analysers at one
month intervals
6 points at 15, 30, 45, 60, 75, 90 % of range, plus

zero for calibration on all instruments.
Using reference gases traceable to national or

international standards.

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Dynamic gas blending devices such as standard

gas divider accurate within 1 % may be used to
generate the points for a calibration.
NOx Convertor efficiency
*1 week
ADR 37/00 Appendix 10
HC Optimisation of
performance
*On first commissioning;

1 year and after major
maintenance
ADR 37/00 Appendix 10
HC oxygen quenching effect

overhaul
SAE J1094a Constant Volume Sampler Systems

for Exhaust.
CO Analyser interference of
CO2, H20
Exhaust
emissions
of
engines at idle NDIR CO,
CO2, HC
Emissions
or
recommendations.
instrument
manufacturers

overhaul
*Electrical check before
each reading
*1 week span and zero

*1 month
Gas check.
Multi-point calibration using standard gases.
SHED
(Sealed housing for evaporative
determinations)
ADR 37 Appendices XI, XII
Background emissions
*1 year
HC retention check
*1 month
HC analyser (FID)
*1 month
Homogeneity test
*On commissioning and

after major service
after major service
after major service
Homogeneity response time

Recovery or validation test
Volume of SHED
Six point calibration not including zero (see gas

analysers)
Time to achieve homogeneity

after major service
REFERENCE GASES
Non
reactive
Reference
gases: at a concentration
greater than 100ppm
Non-reactive gases: at a
concentration of 100ppm or
less
Reactive Reference gases
4 years or once the

cylinder pressure falls
below 700kPa (100psi)
whichever occurs first
2 years or once the
2 years or once the

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NOTE:
In vehicle emission testing (gas analyser and CVS) rotameters are used as
indicators of flow rather than as flow measuring devices.
Non-linear instruments such as NDIR are not considered to be linear when
fitted with linearising circuits.

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CALIBRATION APPENDIX H: CALIBRATION DATA MEASUREMENT FOR A

CONSTANT VOLUME SAMPLER (CVS)
FOR POSITIVE DISPLACEMENT PUMP (PDP) TYPE OR CRITICAL FLOW VENTURI (CFV)
TYPE.
PA
PARAMETER
SYMBOL
TOLERANCE
INSTRUMENT
Atmospheric pressure
PB
0.03 kPa
Barometer
Ambient temperature
TA
0.3C
Thermometer
Air temperature into LFE
ETi
0.15C
Thermometer
Pressure
depression
upstream of LFE
EPl
0.01 kPa
Manometer
Pressure differential across

LFE
EDP
0.001 kPa
Manometer
PDP inlet;
PTi
0.3C
Thermometer
or CFV inlet
Tv
0.3C
Thermometer
PPi
0.01 kPa
Manometer
Pressure at PDP outlet
PPO
0.01 kPa
Manometer
Air temperature at PDP

outlet (optional)
PTO
0.3C
Thermometer
PDP revolutions during test

phase
one
Revolution counter
Elapsed time for test phase
0.1 s
Stopwatch or equivalent
Qs
0.5%
Laminar flow element or subsonic venturi flowmeter
Air temperature at:
Pressure depression at:

PDP inlet; or CFV inlet
Air flow (litres/minute)
RAMETER ARAMETER SYMB SYMBOL OL TOLERANCE INSTRUMENT

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CALIBRATION APPENDIX I: CALIBRATION OF EQUIPMENT FOR ASBESTOS

(FIBRE
COUNTING
AND
IDENTIFICATION)
AND
OTHER
WORKPLACE
ENVIRONMENT MONITORING
ITEM OF EQUIPMENT
Maximum period
between successive
Calibrations or
Checks
MICROSCOPE
* Yearly service
Procedures
and
Comments
Details at end of table
* Regular cleaning
The microscope, lenses and objectives must be kept

clean
HSE/NPL TEST SLIDE
*On use
Used when setting up the microscope prior to

counting each batch of slides. Use to be recorded
WALTON BECKETT
*Measured on
installation then every
12 months and
whenever the
interpupiliary distance,
objective,
intermediate
magnification, or, on
some microscopes,
the eyepieces are
changed.
GRATICULE
NOHSC Guidance Note, 1988
Note: For
microscopes
embodying a
magnification change,
the graticule must be
measured prior to
counting each batch
of slides.
PUMPS
(Where
accreditation
is
held/sought
for
volume
measurement.)
Direct automatic flow control
consecutive tests
Indirect
control
automatic
flow-
*12 months. After 3

consecutive tests (ie.
2 years) showing
results within 5% of
the expected result,
the interval can be
lengthened to 3 years.
Constant flow compensation. Refer to calibration

Appendix J
*6 months. After 3
consecutive tests (ie.
12 months) showing
results within 5% of
the expected result,
the interval can be
lengthened to 12
months
As above

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ALL PUMPS
*On use
Where accreditation for volume measurement is held,

the flow rate must be checked in the field before and
after use
*Regular maintenance
and battery checks
Records must be kept
Small bore, long flow meter,

spherical float
*Monthly for 3 months

then, if measurements
are within 3% of the
expected result, the
interval can be
lengthened to 1 year
Against primary flow meter over the range of use

(including high flow rates where used)
Large bore, short/medium

flow meter, cylindrical float
*As above except, if

the measurements
are within 3% of the
interval can be
lengthened to 2 years
Against primary flow meter over the range of

use(including high flow rates where used)
*Monthly for 3 months

then, if measurements
are within. 3% of the
interval can be
lengthened to 6
months.
Against primary flow meter over the range of use

(including high flow rates where used)
*On commissioning
Check volume using an appropriate measuring

device
ROTAMETERS
ELECTRONIC
SOAP
FILM
FLOW METER (eg. gilibrator,
mini-buck)
MANUAL SOAP FILM FLOW

METER
EFFECTIVE FILTER AREA
*On commissioning
and whenever the
filter, filter holder or
any aspect of the filter
clearing is changed
REFRACTIVE INDEX OILS
*1 year
*3 months
FURNACE
*
* Initial
NOHSC Guidance Note, 1988
High grade proprietary oils

Chemical blends mixed by laboratory
Check using thermocouple or optical pyrometer
SERVICING OF MICROSCOPES
The following servicing must be done on microscopes annually and all defects rectified as
necessary. The service may be carried out either in-house by suitably trained laboratory staff or
externally.

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1. Phase Contrast Microscopes

-
Checking, lubricating (as necessary) and adjusting all mechanical moving parts, such as
condenser rack, stage controls and field diaphragm.
Checking all optical alignments such as oculars, objectives, binocular tube, condenser
and illumination system for surface and mount defects.
Cleaning all optical components as necessary.
Checking for vertical, horizontal and rotational displacement of images in binocular tube
2. Polarising Light Microscopes

-
condenser rack, stage controls and field diaphragm.
Checking all optical alignments such as oculars, objectives, binocular tube, condenser
and illumination system for surface and mount defects.
Checking for vertical, horizontal and rotational displacement of images in binocular tube.
Checking directions of polariser, analyser and accessory plate.
Checking correct operation of iris diaphragm in relation to dispersion staining.
3. Stereo Microscopes
-
focusing rack and zoom controls.
Checking all optical alignments such as oculars, binocular tube, objective and
illumination system for surface and mount defects.
Checking and adjusting for parfocal operation throughout zoom range.
ISO/IEC

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CALIBRATION APPENDIX J: ASBESTOS - PUMP CALIBRATION CHECKS

1.
Indirect Automatic Flow - Control Pumps

Before being placed into service, after three months, and then after a further three months,
the following tests must be done on every indirect automatic flow-control pump used by
the laboratory.
a)
Test each pump at each flow rate that is used. For example, if the pump is used at
1.0, 2.0 and 4.0 litres/ minute, then it must be tested at 1.0, 2.0 and 4.0 litres/
minute.
b)
Set the pump flow rate to the chosen flow rate using a flow meter. No other flow
resistance should be in the circuit.
c)
By inserting an adjustable or specially chosen flow resistance, select the resistance

so that the pressure drop equals or exceeds approximately 2 kPa for each one
litre/minute flow rate. (For example, for 4 litres/minute, the pressure drop must be 8
kPa or greater). This pressure drop can be determined by using devices such as a
simple U tube water manometer or a Magnehelic differential pressure gauge.
d)
Without adjusting the pump, re-measure the flow rate.
e)
If the flow rate changes by more than 5%, the pumps constant flow compensation
must be reset.
f)
Repeat steps a) to e) with the pump set to each relevant flow rate.
g)
If the above tests produce results inside the +/-5% range for tests on three
consecutive occasions, ie. 12 months, then future tests need only be done at twelvemonthly intervals.
h)
If any internal components of the pumps have been serviced or changed, the test
must be repeated before the pump is placed back into service. Pumps that have the
circuit board flow compensation potentiometers accessible must not be used until
the access is blocked so as to prevent accidental adjustment.

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i)
Some manufacturers of indirect automatic flow control pumps specify that flow rates
of 1.0 and 2.5 litres/minute are to be used when electronically adjusting for correct
constant flow compensation. This should not be confused with the mandatory
requirements stated in paragraph (a) above, where pump testing is to be done at
every flow rate used.
2.
Direct Automatic Flow Control Pumps

a)
Before any direct automatic flow control pump is placed into service, and after a
twelve month period, the tests as described in section 1 above (with the exception of
paragraphs g) and i)), must be conducted on every direct automatic flow control
pump used in the laboratory.
b)
If any internal components of the pumps have been serviced or changed, the test
must be repeated before the pump is placed back into service. Pumps that have the
circuit board flow compensation potentiometers accessible must not be used until
the access is blocked so as to prevent accidental adjustment.
c)
If these tests produce results inside the +/-5% range after two consecutive tests (ie.
one year), then future tests need only be done at three yearly intervals.
Note: The tests are based on the flow rate/pressure drop characteristics of 25mm
diameter, 0.8mm pore size and mixed esters of cellulose membrane filters.
Different test conditions may be necessary if other types of filters are used.
3.
Automatic Pump Timers

The above mentioned calibration procedures must be adhered to for automatic pump
timers. In addition to these requirements, the following aspects must also be demonstrated
to check that automatic pump timers:
a)
reliably deliver the correct flow rate immediately after automatic switch-on
i.
set pump at initial nominal flow rate
ii.
program pump to start at least 1 hour later
iii.
measure and record pump flow rate within 5 minutes to auto switch-on
iv.
repeat steps i to iii for each flow rate used
v.
repeat steps i to iv for each pump used
vi.
repeat steps i to v on three separate occasions
vii. accept a pump if any flow rate is within +/-5% of initial nominal reading
viii. reject a pump if any flow rate is more than +/-5% of initial nominal reading
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b)
reliably deliver the correct flow rate immediately before automatic switch-off over the
time cycle chosen
i.
ii.
program pumps to finish at least 1 hour later
iii.
measure and record final pump flow rate within 5 minutes before auto switch-off
iv.
v.
vi.
repeat steps i to v on three separate occasions
vii. accept a pump if any final flow rate is within +/-5% of initial nominal reading
viii. reject a pump if any flow rate is more than +/-5% of initial nominal reading
c)
reliably display the sample duration to +/-1% or better

i.
time in-built pump timer over a typical sampling period and record timers
elapsed time
ii.
repeat step i for each sampling period likely to be used
iii.
repeat steps i to ii for each pump used
iv.
repeat steps i to iii on three separate occasions
v.
accept a pump if pump timer elapsed time is within +/-1% of actual elapsed time
ISO/IEC 1
7025 APPLIC APPLICATION TION DOCU DOCUMENT
d)
reliably switch off automatically in the event of a flow fault such that the final flow rate
is within +/-10% of the initial flow rate
i.
ii.
progressively restrict pump suction so as to cause flow fault condition
iii.
during step ii measure and record pump flow rate just before auto switch-off
iv.
v.
vi.
repeat steps i to v on three consecutive occasions
vii. accept a pump if final flow rate is within +/-10% of initial nominal reading
viii. reject a pump if any final flow rate is more than +/- 10% of initial nominal
reading

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e)
reliably switch off automatically in the event of a low battery such that the final flow
rate is within +/- 10% of the initial flow rate.
i.
ii.
progressively reduce voltage supply to pump so as to cause low battery fault
iii.
during step ii, measure and record pump flow rate just before auto switch-off
iv.
v.
vi.
repeat steps i to v on three consecutive occasions
vii. accept a pump if final flow rate is within +/-10% of initial nominal reading
viii. reject a pump if any final flow rate is more than +/- 10% of initial nominal
reading
Each pump must be tested and records kept of all of the aspects described above.
If the tests described under d) and e) above have not been done, any sample subject to
automatic switch-off due to a flow fault or low battery must be rejected.
A laboratory can submit to NATA for review and approval an alternative series of tests to
those described above, provided that they achieve the same aim. One alternative may be
the measurement of air volumes, actually sucked by a pump during automatic operation.
The test procedures for any alternative would need to be described in detail.

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CALIBRATION
APPENDIX
K:
CALIBRATION
OF
INSTRUMENTATION
(COMPARATIVE TECHNIQUES)
The reference and working equipment listed in previous appendices are calibrated (in most
cases) by reference to fundamental physical standards of measurement and their derivatives.
Other techniques have been included in the previous appendices to be consistent with the
grouping of equipment for specific testing procedures.
This Appendix lists major analytical instrumentation used in the laboratory, that are calibrated
primarily in-house by use of reference materials of known composition.
In the field of Chemical Testing the following general principles apply to the use of analytical
instrumentation.
a)
Sufficient and appropriate reference materials must be used to calibrate instruments over
the full analytical range required to establish the measurement characteristics of the
instrument (linearity, sensitivity, etc).
b)
Stability of measurement must be assessed with reference materials to establish the

required frequency of calibration.
c)
Effects of interfering substances and differing matrices must be assessed.
d)
Limits of detection must be established if the instrument is to be used at concentrations

approaching the limit of detection.
e)
Operating parameters as set in manufacturers instructions and maintenance schedules

must be available and details of critical checks must be recorded.
Where Australian Standards have been published for particular instrumental techniques it is
expected that these will be used in the laboratory. Where this is not the case, relevant ASTM or
other verified procedures must be used. In many cases published procedures for the operation
of analytical instrumentation are unavailable or are specific to a particular application. NATA will
then require a laboratory to document its practice for use of analytical instrumentation. For
example, this may include a description of the operation of the instrument, calibration
procedures, specification of error-boundaries on the nominal values of calibration standards,
frequency of use and nature of quality control samples, the analytical precision at various
concentration levels, and maintenance procedures.

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Specific items of instrumentation are listed below together with some guidelines for their inhouse calibration, operation and maintenance.
Calorimeters
Determine water equivalents using certified benzoic acid at six monthly intervals
Conductivity Meters
Conduct a one-point check on use and check the complete scale each year. Refer ASTM
D1125.
Dissolved Oxygen Meters
Conduct a one-point check on use and compare with a Winkler titration once a month. Refer
APHA 4500-O C.
pH Meters
Check on use with at least 2 standard buffer solutions appropriate to the anticipated pH of the
sample being tested. A record of the checks must be kept. Refer to APHA 4500-H and BS 1647.
The reference electrode junction must also be checked at least weekly, or more frequently if
samples are solid or semi-solid. Refer AS 2300.1.6 and NATA Technical Note 21.
Turbidimeters
Conduct a one-point check appropriate to the anticipated turbidity of the sample being
measured, and a complete calibration each year. Refer APHA 2130B. (Reference standards
may be purchased or made up in the laboratory. Check Hach standards annually against
formazin standards.)
Autoanalysers
Appropriate reference materials must be analysed at regular intervals during each run of the
instrument and records kept of within batch and between batch uncertainties. (The scheduled
use of duplicates and recovery checks by spiking samples is also recommended.) Daily, weekly,
monthly and yearly maintenance and calibration checks must be carried out in accordance with
manufacturers specifications or with practical scientific alternatives derived from experience.
Maintenance and calibration procedures must be established and a log kept of maintenance
carried out and the results of calibration checks.

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A full calibration check must include the photometer or other form of detector, sample and
reagent metering devices and the temperature- controlling device used on the analyser.
Spectrophotometers
A great number of the quantitative analyses performed in a chemical testing laboratory involve
some form of spectrophotometric or colorimetric measurement. It is essential that a laboratory
carry out regular, recorded calibration checks on all spectrophotometers or automated devices
employing spectrophotometers or colorimeters. A new calibration curve must be drawn at least
every month.
Such calibrations must include checks on wavelength accuracy, absorbance, linearity, straylight
and matching of cells. These calibrations must be carried out in accordance with the
manufacturers instructions and/or the codes of practice listed below at intervals appropriate to
the test procedures and the physical environment within which the instrumentation is used (but
at least every three months).
All instruments must be checked on use against appropriate reference materials. A blank and at
least two points on the calibration curve must also be checked. These calibrations should be
compared over time to detect any system deterioration.

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Relevant standards for the checking and use of spectrophotometers include:

a)
Ultraviolet / visible:
AS 3753
Recommended practice for chemical analysis by ultraviolet visible

spectrophotometry.
ASTM E131
Terminology relating to molecular spectroscopy.
ASTM E169
Practices for general techniques of ultraviolet quantitative analysis.
ASTM E275
Practices for describing and measuring performance of ultraviolet, visible

and near infrared spectrophotometers.
ASTM E925
Practice for periodic calibration of narrow bandpass spectrophotometers.
ASTM E958
Practice for measuring practical spectral bandwidth of ultraviolet-visible

spectrophotometers.
b)
Infrared:
ASTM E168
Practices for general techniques of infrared quantitative analysis.
ASTM E275
Practices for describing and measuring performance of ultraviolet, visible

and near infrared spectrophotometers.
ASTM E932
Practices for describing and measuring performance of dispersive

infrared spectrophotometers.
Spectrometers
Instrument performance must be routinely monitored during use with reference materials.
Calibration graphs must be prepared using a blank and three to five solutions of standards
covering the expected concentration range of analyte in the sample. Linearity checks must be
done in the absorbance mode. Spectrometer components and supporting equipment must also
be adequately maintained and checked periodically in accordance with documented procedures
to ensure optimal instrument performance. (This may need to be done by external technicians.)
Relevant standards for the checking and use of spectrometers include:

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a)
Atomic Absorption:
AS 2134
Recommended practice for chemical analysis by atomic absorption

spectrometry.
Part 1 Flame atomic absorption spectrometry
Part 2 Graphite furnace spectrometry
Part 3 Vapour generation atomic absorption spectrometry
AS 2135
Glossary of terms used in flame atomic absorption spectroscopy.
ASTM E663
Practice for flame atomic absorption analysis.
ASTM El184
Practice for electrothermal (graphite furnace) atomic absorption analysis.
APHA 3111
Metals by flame atomic absorption spectrometry.
APHA 3112
Metals by cold-vapour atomic absorption spectrometry.
APHA 3113
Metals by electrothermal atomic absorption spectrometry.
APHA 3114
Arsenic and selenium by hydride generation/ atomic absorption

spectrometry.
(b)
Atomic Emission and X-R ay Fluorescence:

The Association will consider submissions from any laboratory that proposes the use of a
factory calibrated atomic emission (arcspark) spectrometer. Each case will be considered
on its merits.
AS 1502
Glossary of terms used in X-ray spectroscopy.
AS 2563
Wavelength dispersive X-ray fluorescence spectrometers - Determination

of precision.
AS 2883
Analysis of metals - Procedures for the setting up, calibration and

standardization of atomic emission spectrometers using arc/spark
discharge.
AS 3641 .1
Recommended practice for atomic emission spectrometric analysis - Part

1 Principles and techniques.
ASTM E135
Terminology relating to analytical chemistry for metals, ores and related

material.
ASTM E158
Practice
for
fundamental
calculations
to
convert
intensities
into
concentrations in optical emission spectrochemical analysis.

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ASTM E172
Practice for describing and specifying the excitation source in emission

spectrochemical
analysis.
ASTM E305
Practice for establishing and controlling spectrochemical analytical

curves.
ASTM E876
(c)
Practice for use of statistics in the evaluation of spectrometric data.
Inductively Coupled Plasma

AS 3641.2
Recommended practice for atomic emission spectrometric analysis

Part 2 Inductively coupled plasma excitation
APHA 3120
Metals by plasma emission spectroscopy.
Direct Current Plasma spectrometric techniques may also be used in laboratories.

(d)
Nuclear Magnetic Resonance

ASTM E386
Practice for data presentation relating to high resolution NMR

spectroscopy.
Chromatographs
(a)
Gas chromatographs:
Instrument performance must be routinely monitored during use with reference materials.
System components (eg. integrators, ovens, electronic amplifiers and detectors) must also
be checked periodically, and records kept.
(b)
Liquid
chr
performance
chromatography
(or
high
omatography
pressure)
liquid
omatography,
chromatographs
including
(HPLC)
and
high
ion
chromatography:
The total system must be monitored during use with reference standards. Loss of
efficiency may be detected by chronological comparison of reference material
measurements. System components (eg. pumping system and detectors) must be subject
to periodic checks and details must be recorded.

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Relevant standards for the checking and use of chromatographic instrumentation include:
AS 3741
Recommended practice for chemical analysis by ion-chromatography.
ASTM D1945
Test methods for analysis of natural gas by gas chromatography.
ASTM D4626
Practice for calculation of GC response factors.
ASTM E260
Practice for packed column gas chromatography.
ASTM E355
Practice for gas chromatography terms and relationships.
ASTM E516
Practice for testing thermal conductivity detectors used in gas

chromatography.
ASTM E594
Practice
for
testing
flame
ionization
detectors
used
in
gas
chromatography.
ASTM E682
Practice for liquid chromatography terms and relationships.
ASTM E685
Practice for testing fixed wavelength photometric detectors used in liquid

chromatography.
ASTM E697
Practice for use of electron capture detectors in gas chromatography.
ASTM E840
Practice for using flame photometric detectors in gas chromatography.
ASTM E958
Practice for measuring practical spectral band width of UV/Vis

spectrophotometery.
ASTM E1151
Practice for ion chromatography terms and relationships.
ISO 6326
Gas analysis: Determination of sulphur compounds- in natural gas

Part 2 GC method using an electrochemical detector for the
determination of odoriferous sulphur compounds.
ISO 6326
Natural gas: Determination of sulfur compounds GC method using FID

for the determination of hydrogen sulfide, carbonyl sulfide and sulfur
containing oderants.
ISO 6568
Natural gas - simple analysis by gas chromatography.
ISO10301
Water quality Determination of highly volatile halogenated hydrocarbons

by gas chromatography.
BS 684
Methods of analysis of fats Sec 2.35 and fatty acids Other methodsAnalysis by gas-liquid chromatography of methyl esters of fatty acids.
BS 5443
Recommendations for a standard layout for methods of chemical analysis

by gas chromatography.

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Particle size analysis

Instrument performance should be routinely monitored during use with reference
materials.
ASTM F660
Practice for comparing particle size in the use of alternative types of

particle counters.
ASTM F661
Practice for particle count and size distribution measurement in batch

samples for filter evaluation using an optical particle counter.
ASTM F662
Method for measurement of particle count and size distribution in batch

samples for filter evaluation using an electrical resistance particle counter.
Computerised systems
ASTM E622
Guide for computerised systems.
ASTM E627
Guide for documenting computerised systems.
ASTM E792
Guide for selection of a clinical laboratory information management

system.
ASTM E1013
Terminology relating to computerised systems.

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Annexure C
(Taken from ILAC Proceedings, 1993)
INTRODUCTION
Purpose of the Guide
Quality assurance in a testing laboratory, particularly in the case of its assessment, highlights
the need to consider closely the question of the accuracy of its measurements and analytical
results, and to ensure that the principles necessary to establish demonstrated accuracy have
not been omitted.
The calibration of the parameters associated with chemical analyses and material tests
deserves particular attention. Because major errors can be made by neglecting or ignoring the
basic principles of metrology which also apply to these areas. This text identifies a number of
general recommendations for those who are faced with this problem, either as laboratories or as
assessors.
Basic considerations
Any measurements, particularly any quantitative chemical analysis, must employ reference
elements to ensure demonstrated traceability to the relevant basic quantities.
This is an
essential condition for the accuracy of the results.

The metrological quality of the calibration performed depends on:
The intrinsic uncertainty of the reference used {set of calibration masses, titrated solutions,
gas mixtures, composition CRMs* etc. (see remarks)}
The appropriateness (or fitness for purpose) of this reference under the practical
conditions of use, also taking account of the analytical method used and the samples
tested.

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The total uncertainty of calibration results from these two components, and it must be optimized
without ignoring either of them. Figure 1 as given below illustrates the problem. The combination
of uncertainties being presented as a quadratic function as recommended by BIPM.
Figure 1
R1 > R2
R1
Appropriateness
Error : 1 %
Appropriateness
Error : 0.5 %
R2
Standard Solution
(0.1 % relative)
Composition CRM
(0.5% relative)
Calibration without CRM
Calibration with CRM
The analyst should compare the uncertainty of calibration with the required total analytical
uncertainty (which should normally be agreed between the customer and the operator). This
comparison provides a useful guide for choosing between different available calibration
procedures and in the longer term, for improvements to the methods and procedures.
In tests based on measurements of physical quantities, the principle of traceability of the
standards and/or measuring instruments of the accredited laboratory to a national primary
standard through a national calibration system is generally applied.
Relevant principles for
ensuring the traceability of chemical analyses are presented later in this document; the use of
CRMs for that purpose has been gaining importance in the last decades and may be expected
to develop even more if and when they are available.

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Remarks:
a)
The definitions of RMs and CRMs can be found in ISO Guide 30. RMs can also be
sued to validate methods (see ISO Guide 33). They may also be used to check the
drift with time and possibly to correct an instrumental drift. They also serve as a
basis for a conventional scale (e.g. octane index). These aspects of the use of RMs
are not dealt with here, apart from a few remarks and the reader can refer to ISO
Guide 33. One can refer also to more general documentation, such as the VM
(International Vocabulary of Metrology).
b)
The analytical chemist is often a user of analytical materials or reagents. These

products must not be confused with CRMs.
A CRM in fact corresponds to in
identified batch of material of which the certified characteristics have been

determined with an optimized and defined accuracy. An analytical reagent is only
characterized by a nominal value determined without high accuracy. It is the users
duty to observe all necessary precautions to ensure, when used, that an analytical
reagent meets his needs.
1. SELECTION OF CALIBRATION PROCEDURES IN CHEMICAL ANALYIS
The first step is to classify the analytical procedure used by reference to the following
categories:
-
Calculable method
Relative method
Comparative method
Each of these categories is associated with:
a basic principle
a number of basic pre-requisites.
When the user classifies a method, it should be done by means of a detailed and close
examination of all the parameters of the analytical procedure. He must never be satisfied
with simplifications which would only be applicable to the detection principle applied under
idealized conditions.
This approach generally has the effect of under estimating the
necessary conditions for a reliable calibration and of generating systematic errors.

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Calibration does not make an inaccurate method true (e.g. presence of major interferences).
The variability of the factors of influence should only cause negligible variation in the
analytical signal.
The above classification is merely designed to identify the relevant calibration mode (s). It
must not be used as a scale of value of the methods.
Calculable method
This is a method that produces the anticipated result by performing a calculation defined on
the basis of the laws governing the physical and chemical parameters involved, using
measurements taken during the analysis, such as:
o
weight of the test sample, volume of titration reagent,
weight of precipitate, volume of titration product generated.
Relative method
This method compares the sample to be analysed with a set of calibration samples of known
content, using a detection system for which the response (ideally linear) is recognised in the
relevant working area (without necessarily being calculable by theory). The value of the
sample is determined by interpolation of the sample signal with respect to the response
curve of the calibration samples.
This implies that any other difference of composition, form, etc. between the calibration set
and the different samples analysed will have no effect, or a negligible effect compared with
the uncertainty on the signal. For this condition to be satisfied the analytical procedure
could include:
o
Means to reduce sensitivity to differences (e.g. spectral buffer, treatment of samples

before analysis)
A procedure to give similar form to the calibration set and the samples:
-
Reduce the complex sample to a simpler sample, by acid digestion, the removal of
major interferents or selective extraction of analyte.
Synthesize a more complex calibration set, by multi-element matrix simulation or

the use of a special medium (e.g. oils).
Limitation of the field of application.

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Comparative method
For this type of method, the sample to be analysed is compared to a set of calibration
samples, using a detection system which has to be recognised to be sensitive not only to
the content of elements or molecules to be analysed, but also to differences of matrix (of
any type whatsoever). If this influence is ignored it will generate a systematic error (bias).
For this type of method to be really appropriate for use, it is essential:
To identify the type(s) of samples routinely analysed (type of matrix, type of structure
etc.) and to draw up procedures to identify the introduction of abnormal samples in
comparison with the identified types.
To make up a set of CRMs suitable for each type of sample previously identified.
To evaluate whether or not intra-type differences are liable to generate an

unacceptable bias in the analysis.
Some examples of these three types of methods are given below:
EXAMPLES *
1) Nickel in alloy steel
Calculable method:
Gravimetry
of
Ni
after
selective
precipitation
as
Ni
dimethylglyoxImate
Relative method:
Atomic Absorption after acid digestion of sample
Comparative method:
X-ray Fluorescence on solid sample
2) Water in powders
Calculable method:
Karl Fisher Titration
Relative method:
Extraction of H2O by isopropanol, GC detection
Comparative method:
Infra-red Reflexion on solid sample

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3) Others.
Other methods
Any analytical method that fails to ensure traceability to the base units by one of these
approaches is liable not to yield results of demonstrated accuracy.
Even if it offers
appreciable advantages of repeatability and reproducibility, the results obtained are liable to
be distorted by a systematic error.
If it is used by a single laboratory to analyse drift, or to transfer information within a restricted
circle of users who are aware of the limitations of the result, vigilance will be necessary to
ensure that these results are not presented or used as accurate outside the circle.
Assessors giving accreditation to such methods should take great care to check that the
method is undertaken in such a way that appropriate accuracy is ensured through relevant
procedures and means and preferably that they are widely recognized as state of the art
methods.
2. CALIBRATION PROCEDURES
Calculable method
The basic procedure is to identify every quantity whose measurement is necessary to
establish the analytical result by calculation.
It is recommended that a provisional list of uncertainties be drawn up which will
estimate the uncertainty of each measured quantity, against the total analytical
uncertainty. This will help to identify the main sources of uncertainty and to exercise
special care in selecting the calibration procedures.
With this type of method, CRMs are used for verification (see ISO Guide 33). Note that
the CRM must be analysed as presumed unknown, the result obtained being compared
with the certified value.
If an abnormal deviation is observed, the laboratory must
identify the cause and correct it. It is not recommended (except for very specific cases)
to deduce a correction factor for the difference between the value found and the certified
value.

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Relative method
For this type of method, the working standards generally consist of a determined
quantity of analyte diluted in a larger quantity of diluent.
They are obtained by
measuring the masses or volumes of the different pure, dilute and diluent materials.
Depending on each case, metrological traceability implies the following:
Calibration of the mass measurements by calibration or verification of the balances

and/or calibration of the volume measurement system.
Calibration of the system for measuring the correction parameters applied to the
foregoing measurements (e.g. temperature, pressure, relative humidity). Since the
uncertainties of these quantities are generally of the second order with respect to
the total analytical uncertainty, a simplified calibration procedure is often adequate.
Knowledge of the purity of the basic materials used, together with their
uncertainties.
For the substance which is diluted, it is necessary to ensure that:

-
It is the compound of interest.
The nature of the impurities is identified (e.g. inorganics in an organic substance).
The stoichiometry is correct.
For diluents particular attention must be paid to the residual level of impurities such as:
-
The substance to be diluted.
Any substance exhibiting a similar analytical response
Any substance likely to react with the substance being diluted.
For practical or economic reasons, laboratories may decide to use commercial standard
solutions. If so, it is important to make sure that the uncertainty on their content is
known, as required, and that the basic rules set forth above are complied with by the
manufacturer, as attested by appropriate documentation.
For this type of method, CRMs are chiefly used as a means of verification.

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CRMs are sometimes used to prepare a calibration solution by a simple dissolution of a

known test sample of CRM, possibly followed by spiking. This practice is comparable to
that of using commercial standard solutions and must be treated as such.
Comparative method
Since these methods are sensitive to matrix effects, the calibration procedures employed
must take account of these effects. The use of an appropriate CRM is the preferable
calibration method. The choice of the CRM to be used must therefore satisfy two types
of necessary conditions:
-
That the certified property is known with sufficient reliability.
That the matrix of the standard is sufficiently similar to the samples being analysed
and that the existing differences are not liable to generate a bias in the results that is
incompatible with the total uncertainty desired.
The selection of a suitable CRM should aim to achieve an optimum between these two
types of necessity.
The CRM must initially be defined in the form of a tentative specification; the points to be
considered include:
-
What are the elements whose concentrations must be known with sufficient accuracy
to permit the establishment of the calibration? Over what concentration range? With
what uncertainty? For what sample size?
What should be the type of matrix; type of material and main components (which
could have a chemical or physical influence on the response of the analyzer)?
What other properties or characteristics of the samples and the standards should be
similar to avoid generating a bias in the responses of the analyzer? For example:
form, viscosity, particle size distribution, metallurgical structure, etc.

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SELECTION OF CRMs
The first approach in this search is to compare the tentative specification of the CRM
required with the lists of CRMs available on the international market. The laboratory
should consult:
-
The catalogues of the different manufacturers
The COMAR data bank
Branch publications or recommendations examining the best choices of CRM in a

specific field if they are available.
The laboratory must ensure that the CRMs that were short-listed after a first
examination:
-
Are effectively certified for the element concerned, and that the value is not merely
indicative (see certificate)
That the certification procedure exhibits an appropriate level of metrological reliability

(see ISO Guide REMCO 35) and that is sufficiently well documented (ISO Guide 31).
Any traceability defined in principle only, but without an evaluation of the uncertainty,
does not constitute a properly demonstrated traceability.
As to similarity of matrix, the laboratory must weigh the fact that it is not economically
and technically possible to obtain a perfect match between CRMs and samples in all
cases. Reasonable similarity must be deemed acceptable. If not, the entire analytical
procedure has to be reconsidered.
The use of a CRM available on the market is usually capable of ensuring:
The best guarantee of accuracy.
The best performance / cost ratio.
The laboratory that decides not to use appropriate available CRMs should accordingly
justify the reasons for this decision in its procedures.

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USE OF INTERNAL RMs

Should the market fail to offer a CRM to meet a laboratorys identified needs, it may
attempt to develop its own internal RM. Since this usually means a lengthy and costly
operation, involving the use of special resources and experience, it would be wise to
firstly explore the following possibilities:
-
Contact those manufacturer(s) of CRMs capable of developing such a new CRM. A

request for a new CRM for which the potential market would not amount to more
than several dozen per year over several years cannot normally be considered.
Contact groups of users with the same need and try to set up a joint project, possibly
with the assistance of the national laboratory responsible for CRMs.
The preparation and use of an internal RM must offer guarantees of metrological

traceability as well as the use of a CRM. It can allow for a lower level of accuracy than a
CRM, which is offset by better fitness for purpose or imposed by the absence of CRM.
An internal RM must therefore accordingly have been prepared by a procedure that
guarantees the following:
-
Sufficient availability over several years
Demonstrated homogeneity and stability
An internal certification analysis assuring demonstrated traceability and ensuring the

absence of bias which might have an effect on total analytical uncertainty.
A quantified estimation of uncertainty, which is also compatible with the total

analytical uncertainty; for the characterization of an internal RM, this requirement
usually entails the application of calculable or relative methods, preferably validated
by the use of CRMs.
In some cases, an internal RM is developed to help conserving an expensive CRM. It

can be calibrated (against a set of similar CRM) using a comparative method. As this
new link will deteriorate the uncertainty of the Working RM, the interest of such RMs
must be seriously assessed.

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Internal RMs must never be samples of which the reference value used is not known
through a procedure of demonstrated traceability with a definite and sufficient
uncertainty. If the development of an internal RM necessary to properly calibrate a given
method is not technically or economically feasible, the user will have to reconsider the
choice of method and/or procedure, and use on that does not demand the missing CRM.
General Remarks
Calibration is an integral part of analysis and its cost is an integral part of the cost of analysis. It
must be planned and provided for, especially if it involves purchasing CRMs or developing
internal RMs. An under estimation of these costs does not justify an inadequate calibration
procedure.
The calibration of chemical analyses must meet a number of essential requirements, such as
those set forth in this Guide. Compliance to such requirements may involve different forms in
different fields.
These general recommendations are not sufficient conditions for quality in
calibration. Every user must indicate:

-
His additional specific conditions.
Any exception to the general rules.
At all events, he must identify and analyse his need in its different aspects and draw up and
implement a response for each.
Accurate analyses depend not only on the metrological quality of the calibration but also on
other factors including random and systematic errors which occurs during the analysis.
Note: This annexure may be treated as a guideline and not as NABL requirement.

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NABL 103

National Accreditation Board for Testing and Calibration Laboratories

Specific Guidelines for Chemical Testing Laboratories

Association of Official Analytical Chemists

American Public Health Association

Asia Pacific Laboratory Accreditation Cooperation

American Society for Testing and Materials

Bureau of Indian Standards

Bureau International des Poids et Measure (International Bureau of

Certified Reference Material

International Organization for Standardization

European Cooperation of Testing Authorities

Fourier Transform Infrared

Graphite Furnace Atomic Absorption Spectrometer

Guide to the Expression of Uncertainty in Measurement

Inductively Coupled Plasma Atomic Emission Spectrometer

Inductively Coupled Plasma Mass Spectrometer

International Electrotechnical Committee

International Laboratory Accreditation Cooperation

International Union of Pure and Applied Chemists

National Accreditation Board for Testing and Calibration Laboratories

National Association of Testing Authorities

National Institute of Standards and Technology

Nuclear Magnetic Resonance

National Accreditation Board for Testing and Calibration Laboratories

Specific Guidelines for Chemical Testing Laboratories

Terms and Definitions

Groupwise Codification for Chemicals Tests

National Accreditation Board for Testing and Calibration Laboratories

Specific Guidelines for Chemical Testing Laboratories

Page No: iii

This document has been produced by a TECHNICAL COMMITTEE constituted by NABL

National Accreditation Board for Testing and Calibration Laboratories

Specific Guidelines for Chemical Testing Laboratories

National Accreditation Board for Testing and Calibration Laboratories

Specific Guidelines for Chemical Testing Laboratories

TERMS AND DEFINITIONS

National Accreditation Board for Testing and Calibration Laboratories

Specific Guidelines for Chemical Testing Laboratories

National Accreditation Board for Testing and Calibration Laboratories

Specific Guidelines for Chemical Testing Laboratories

Certified Reference Material

National Accreditation Board for Testing and Calibration Laboratories

Specific Guidelines for Chemical Testing Laboratories

National Accreditation Board for Testing and Calibration Laboratories

Specific Guidelines for Chemical Testing Laboratories

The Scope of accreditation of a laboratory is the formal statement of the range of

The range of products, materials or sample types tested or analysed;

Types of tests or analysis carried out;

The specification or method/technique used;

The concentration range and accuracy/precision

National Accreditation Board for Testing and Calibration Laboratories

Specific Guidelines for Chemical Testing Laboratories

It is accepted that sometimes it is not practicable for laboratories to use a (fully

The approach to extending or amending the scope of accreditation should be as flexible

National Accreditation Board for Testing and Calibration Laboratories

Specific Guidelines for Chemical Testing Laboratories

The minimum requirement for an Authorized Signatory shall be a Graduate in Science

National Accreditation Board for Testing and Calibration Laboratories

Specific Guidelines for Chemical Testing Laboratories

National Accreditation Board for Testing and Calibration Laboratories

Specific Guidelines for Chemical Testing Laboratories

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