Nabl - Chemical Testing Laboratories Guidelines

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 Issue No: 03 Specific Guidelines for Chemical Testing Laboratories Issue Date: 25.03.2008 Last Amend No: 00 Amend Date: -Page No: i
ABBREVIATIONS
AOAC APHA APLAC AS ASTM BIS BIPM BS CRM ISO EA FTIR GFAAS e.g. GUM ICPAES ICP-MS IEC ILAC IUPAC NABL NATA NIST NMR QC w.r.t. : : : : : : : : : : : : : : : : : : : : : : : : : : Association of Official Analytical Chemists American Public Health Association Asia Pacific Laboratory Accreditation Cooperation American Standard American Society for Testing and Materials Bureau of Indian Standards Bureau International des Poids et Measure (International Bureau of Weights and Measures) British Standard Certified Reference Material International Organization for Standardization European Cooperation of Testing Authorities Fourier Transform Infrared Graphite Furnace Atomic Absorption Spectrometer For Example 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 Quality Control With Respect To

Doc. No: NABL 103 Issue No: 03 Specific Guidelines for Chemical Testing Laboratories Issue Date: 25.03.2008 Last Amend No: 00 Amend Date: -Page No: ii
CONTENTS
Sl Title
Amendment Sheet Abbreviations Contents 1. 2. 3. 4. 5. 6. Introduction References Terms and Definitions Scope Technical Requirements Groupwise Codification for Chemicals Tests Annexure A Annexure B Annexure C
Page
i ii iii 1 2 3 7 9 28 37 40 78

Doc. No: NABL 103 Issue No: 03 Specific Guidelines for Chemical Testing Laboratories Issue Date: 25.03.2008 Last Amend No: 00 Amend Date: -Page No: iii
1.
1.1
INTRODUCTION
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).

Doc. No: NABL 103 Issue No: 03 Specific Guidelines for Chemical Testing Laboratories Issue Date: 25.03.2008 Last Amend No: 00 Amend Date: -Page No: 1/ 88
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

3.
3.1
TERMS AND DEFINITIONS

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

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

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.

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.

4.
4.1
SCOPE
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: (i) (ii) (iii) (iv) 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
4.2
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.

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.

5.
5.2 5.2.1
TECHNICAL REQUIREMENTS
Personnel 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.

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.

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.
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.

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 5.4.1
Validation 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

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.

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

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.

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 5.5.1
Equipment 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) iii) volumetric equipment (e.g. flasks, pipettes, pyknometers, burettes etc); measuring instruments (e.g. hydrometers, U-tube viscometers, thermometers, timers, spectrometers, chromatographs, electrochemical meters, balances etc); iv) physical standards (weights, reference thermometers);
5.5.2
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).

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.
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 5.6.1 Calibration & Measurement Traceability 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.

(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.

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.

5.7 5.7.1
Sampling and Sample Preparation 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: The quantity of the sample The extraction system
5.7.2
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.

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.

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

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

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

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.

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.
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
6.2.
Alcohols & Alcohols based Chemical Industrial alcohols Alcohols based chemicals
6.3.
Adhesives Starch based adhesives Natural gums Glues Polymer based adhesives (Synthetic)
6.4.
Building Materials Cement & other mortars Cement concrete Refractories Refractory cement Sand Clays & soils

6.5.
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
6.6.
Cosmetics & Essential Oils Perfumes Essential oils Cosmetics and toiletries Intermediates and miscellaneous chemicals for cosmetics Herbal-based cosmetics
6.7.
Dye & Dye Intermediates Synthetic dyes Dye intermediates Natural dyes & colouring materials
6.8.
Disinfectants Disinfectants and their formulation

6.9.
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
6.10.
Explosives & Pyrotechnics Ammunitions Industrial explosives & associated material Pyrotechnics Explosives chemicals and allied materials
6.11.
Fertilizers Nitrogeneous fertilizers Phosphatic fertilizers Fertilizer mixtures Potash fertilizers Micronutrients Bio-fertilizers
6.12.
Foods & Agricultural Products Alcoholic drinks & beverages Animal feeds Bakery and confectionery products Cereals, pulses, and by-products Coffee, coca and by-products

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

6.14.
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
6.15.
Lac & Lac Products Lac Lac products
6.16.
Leather Leather Synthetic leather
6.17.
Lubricants Trace elements Oils & greases Solid lubricants Aviation lubricants Lubricant additives Microcrystalline wax

6.18.
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
6.19.
Metals and Alloys Iron, steel and ferro-alloys Special steel Copper & its alloys Aluminium & its alloys Tin and tin alloys

6.20.
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
6.21.
Paper and Pulp Pulp Paper, paper board and speciality papers Newsprint and board packing materials Composite packing materials
6.22.
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)

6.23.
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
6.24.
Pesticides Synthetic pesticides & their formulations Natural pesticides & their formulations Pheromones, chitin inhibitors Weedicides Herbicides Fungicides
6.25.
Pollution & Environment Liquid effluents Solid wastes Hazardous solid wastes Toxic waste Tests related to work place environment & hazards
6.26.
Rubber & Synthetic Rubber Natural rubber Synthetic rubber
6.27.
Soap Detergents and Toiletries Soaps Synthetic detergents Wetting and emulsifying agents
Specific Guidelines for Chemical Testing Laboratories Issue Date: 25.03.2008 Last Amend No: 00 Amend Date: --

Doc. No: NABL 103 Issue No: 03 Page No: 35/ 88
6.28.
Textile & Textile Auxiliaries Fibre & filaments Yarns & chords Fabrics, garments and made-ups Auxiliaries Technical textiles (geo-textiles, medical textile, automotive textiles)
6.29.
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
6.30.
Metallic Coatings and Treatment Solutions Metallic coatings Conversion coatings Plating solutions Anodizing solutions Metal finishing materials
6.31.
Corrosion Tests Salt spray tests Dezincification tests Other tests

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.

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

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.

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) b) commissioning of new equipment (including initial calibration and checks after installation); operational checking (checking during use with reference standards or reference materials); c) periodic checking (interim but more extensive checking, possibly including partial calibration); d) e) scheduled maintenance by in-house or specialist contractors; 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.

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) Initial 1 Initial 1 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 6 1 Each weighing BAROMETERS Fortin Aneroid CALLIPERS (VERNIER) DIAL GAUGES Initial 1 2 2 60 One point check with transfer instrument. AS 1984 AS 2103 Service Repeatability check. One point check Zero point check Checking Interval (months) 12 Procedures and References AIR FLOW NOZZLES ANEMOMETERS AUTOCLAVES Check throat diameter
Each Cycle BALANCES See also weighing instruments 3

ELECTRICAL INSTRUMENTS Digital multimeters Analog meters Data loggers ENVIRONMENTAL CONDITIONING CHAMBERS FORCE TESTING MACHINES Dead weight Elastic dynamometer Hydraulic, pneumatic FURNACES 5 2 2 Initial 12 On use HYDROMETERS Reference Working - glass 5 12 Check against reference hydrometer or in newly prepared solutions of known density. AS 2026, ASTM-E126 Working - metal HYGROMETERS Assmann and psychrometers Thermohygrographs Electronic types MANOMETERS Reference, liquid Working, liquid Electronic MASSES Reference of integral stainless steel or nickel chromium alloy Working stainless steel, nickel chromium alloy Working other alloy MICROMETERS 1 5 1 ORIFICE PLATES Initial 6 AS 2102 Check zero and one point against gauge block. Inspect anvils. BS 1042.1 Visual check for wear and damage. 3 then 6 subsequent 3 10 3 1 36 36 Check the cleanliness of the fluid Check the cleanliness of the fluid 1 sling 10 6 Compare thermometers at room temperature with wick dry. AS 2001.1 Appendix C. Check against a calibrated psychrometer 6 ISO 649.1, .2, ISO 650 AS 2193 AS 2193 AS 2193 AS 2853 Check variation within the working zone at the working temperature Monitor temperature 1 2 1 3 On use 6 6 1 Compare with meters of similar resolution. Compare with meters of similar resolution. Check at zero and the maximum point. IEC 600688-2-1,-2,-3,-33,-38,-39 Check at the working temperature
Weekly

PRESSURE EQUIPMENT Test gauges used for calibration of industrial gauges Industrial gauges not subject to shock loading Industrial gauges subject to shock loading Pressure transducers Calibrators SIEVES 1 AS 1349
1 6 months 1 1 Initial 12
AS 1349 AS 1349
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.
On use TAPE MEASURES, RULES Tape measures Steel rules Initial Initial 2 to 5
AS 1290.4, BS 4035 Check at maximum length, depending on use and accuracy required. BS 4372
TEMPERATURE CONTROLLED ENCLOSURES Ageing 5 Daily BOD On use AS 2853 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 1 Initial Calibrate against a reference temperature measuring system. Check efficacy of automatic cold junction compensation with the temperature sensor at the ice point. Check at ice point.
Drying
Initial

THERMOMETERS Reference, platinum resistance 10 Before use Reference, liquid-in-glass 10 Before use AC temperature bridge Working - liquid-in-glass 5 Initial 6 Check at ice point Check linearity and resistance ratio. Check at ice point or at one point in the working range against a reference thermometer. Check R at ice point CSIRO/NML Temperature Course Book 2 Check at ice point Measurement
Working - resistance
5 6
Working - digital display
1 6 Check at ice point or at one point in the working range against a reference thermometer.
THERMOCOUPLES K type, sheathed Initial For use up to 400C. For use above 400C to 1100 C the same immersion must always be used. For use up to 400C. Replace if used above 400C. For use up to 350C. 6 Check at ice point.
K type, wire
Initial (reel of wire) Initial (reel of wire)
T type, wire K and T types TIMING DEVICES Stop watches, clock
Test aurally against the Telstra speaking clock. Two measurements separated by one hour (ie. a one hour period) must be carried out. Non-automatic weighing instruments. Uniform Test Procedures, Inspectors Handbook No 2 for class III and IV Instruments.
WEIGHING INSTRUMENTS See also balances

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 Note 1: Procedures and Comments Balances with in-built calibration check facilities must also have monthly and 6monthly checks carried out. Electronic balances with more than one range must have monthly and 6-monthly checks carried out on all ranges.
BALANCES
Note 2:
BAROMETERS
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 DENSITY BOTTLES, PYKNOMETERS DENSITY METERS *1 year *Initial; whenever test temperature is changed or cell cleaned * Daily *1 week FLOWMETERS Rotameters (Reference) High flow, ie >1 L/min Low flow, ie <1 L/min Rotameters (Working) *2 years *2 years *Each time on use ASTM D3195 Soap bubble flow meter. Soap bubble flow meter. AS 2378; BS 733 App A; IP 190 *2 year Check condition of discs (this check could be done with a spectrophotometer referenced to standards)
ASTM D4052 With pure substance of known density. Air and double-distilled water.

Orifice plates
Initial
BS 1042 Part 1 (calibration by an approved testing authority) Visual inspection for damage, wear or contamination. ASTM D1071 Calibration by an approved testing authority. Check dimensional compliance with BS 1042 Sec 2.1 Annex A. Inspect tip for damage, blockage, etc as required by BS 1042 Sec 2.1 Monitor temperature with an appropriate sensor
*6 months Wet test meters Anemometers Pitot tubes *2 years 2 years *Initial *On use
FURNACES (FOR USE AT SPECIFIED TEMPERATURES) (In addition to other requirements) GAS METERS GAUGE BLOCKS
*On use
*2 years 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
(2)
Piston operated *Initial AS 2162.2 volumetric apparatus (see below) Pipetters
*Initial
AS 2162.1
*Initial *3 months
Check volume delivered. For adjustable devices check volume delivered at several settings (refer to AS 2162.2). 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. Check sample and diluent volumes or dilution ratio and total volume (refer to AS 2162.2). 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. Check volume delivered at maximum and two other settings.
Dispensers
*Initial *3 months
Diluters
*Initial *6 months
Displacement burettes
*Initial *When barrel/plunger is changed
HYDROMETERS In addition to other requirements OVENS In addition requirements Ageing Drying to other *On use *Daily *On use Monitor temperature throughout use, with appropriate sensor, and record temperature daily. Monitor with appropriate sensor and record. Monitor with appropriate sensor and record. *On use Check that scale has not slipped.

PENETRATION NEEDLES
CONES
AND
5 years *On use
Calibration by an approved testing authority. ASTM D217; IP 50; ASTM D5; ASTM D1321. Visually inspect needle tips.
POTENTIOMETERS Reference Working PRESSURE GAUGE TESTERS Deadweight Manometers PYROMETERS Reference Working REFRACTOMETERS 3 years *6 months *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. 5 years 10 years Calibration by an approved testing authority 5 years *One year Calibration by an approved testing authority. Check against reference potentiometer.
TACHOMETERS Reference Working VISCOMETERS U-tube Reference *Initial *10 years Working *Initial *2 years Others Brookfield *Initial *2 years *1 month Ferranti *Initial *3 months Zahn *Initial *1 year * IS commonly done by laboratory staff Volumetric plasticware is not acceptable because it is prone to irreversible volume changes and deformation. Against reference oils Against reference oils. Against reference oils. ASTM D2556 Against quality (ie. manufacturers) oils Using quality oils against reference tubes or using reference oils. ASTM D2162/D445; IP 71 Against reference oils. ASTM D2162 5 years *1 year BS 3403. Calibration by an approved testing authority Check against reference tachometer

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 Maximum period between successive Calibrations or Checks *On use *3 months Pressure, mechanical and dimensional tests on bombs 3 years or 1000 firings depending on use Procedures and Comments Checks on calorimeter dimensions and for thread slackness Determination of the water equivalent (bomb factor) Refer AS1038 Part 5 Checks as prescribed in AS 1038 (see also BS 4791). More frequent checks required if calorimeter is damaged or used repeatedly. Calibration by an appropriate testing authority. CRUCIBLE SWELLING NUMBER BURNERS DENSITY BOTTLES DILATOMETER FROTH FLOTATION CELLS FURNACES Ash *12 months Measure and record test zone temperature by the 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 Tube Volatile Matter Ash Fusion GIESELER PLASTOMETER Bath temperatures Torque Test Rabble Arms * 6 months *1 month *Initial *50 determinations Remove thermocouple and check against reference. Refer AS 1038.12.4.1 Check against torque meter. Check dimensions. Check for wear. *12 months *12 months *6 months *3 months *1 month *3 months *6 months *12 months Heating profiles of all burners Refer AS 1038 Part 12.1 Refer AS 1038 Part 21 Temperature (absolute and gradient), piston assembly mass and tube wear. Refer AS 1038 Part 12.3 Check cell block and impeller dimensions. Refer AS 4156.2.1
BOMB CALORIMETERS

HARDGROVE GRINDABILITY Apparatus *12 months Calibrate against four national reference coal samples with certified grindability indices. Refer AS 1038 Part 20. Check number of revolutions per minute.
Mill revolutions HYDROMETERS Working, for float and sink testing
*12 months
*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.
INSTRUMENTAL ANALYSERS For carbon, hydrogen, nitrogen or sulphur MICROSCOPE PHOTOMETER For reflectance measurements Prior to each sample, at fifteen minute intervals and at end of sample measurement Calibrate using glass or mineral reflectance standards. Refer AS 2486 *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.
OVENS Direct gravimetric Drying Minimum free-space SHALE BREAKDOWN APPARATUS Andreasen sizing apparatus * Initial Check flask volume, height of stem and pipette volume. Refer AS 4156.1 Drum tumbler * commonly done by laboratory staff 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. Accredited coal laboratories must maintain adequate quality control in supervision of equipment performance by the use of appropriate reference materials on a regular basis. Whenever possible, unless otherwise stated in the relevant standard, equipment should contain all items of apparatus specified in the test method when being calibrated. 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. * 12 months Check revolution counter on tumbler. Refer AS 4156.1 *12 months *12 months *12 months Check temperature gradient over sample area Check temperature of working space Check temperature
(II) (III) (IV)

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 Psychrometer *1 month (retain charts) 10 years *6 months Anemometer 2 to 5 years depending on use. Against calibrated psychrometer Complete. Against reference thermometer
Illumination meter METHOD 101.3 Forced draught oven Stoving *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.
METHOD 107.3 Reference wheel gauge Working gauges METHOD 108.1 Shims
Calibration by an approved testing authority Calibration by an approved testing authority, or Against reference wheel gauge.
Magnetic instruments METHOD 108.2 Paint inspection gauge METHODS 202.1; 202.2 Pycnometer (at least 50ml capacity) METHOD 204.1 Fineness of grind gauge block and scraper Reference
Initial only plus frequent visual examination *On use
Shims bearing ASTM or NIST stamps do not require initial external calibration. Against calibrated shims
* Initial only *Initial *6 months
Graticule and cutting angle of cutting tip Check capacity.
5 to 10 years depending on use. *1 year plus frequent visual examination
Calibration by approved testing authority.
Working
Against reference using at least four paints covering the working range

METHOD 211.1, 211.2 Settling spatula
*Initial only *6 months
Dimensions and mass Re-examine for wear and change +Masses and paddle dimensions ++Against standard oils stored in sealed container Replace. Store as directed, well sealed, clean
METHOD 214.1 Krebs-Stormer Viscometer
*Initial only *Initial, then 1 year
Reference oils METHOD 214.2 Flow cup
2 years
*Initial only *Initial, then *3 months (for cups in constant use), or *1 year (other)
Dimensions ++ Against standard oils stored in sealed container ++Against standard oils stored in sealed container
++Against standard oils stored in sealed container As for 214.1
Reference oils METHOD 214.3 Cone and plate viscometer Reference oils METHOD 214.4 Roto thinner viscometer Reference oils METHOD 214.5 Brookfield viscometer
2 years
Initial *On use 2 years
Verification of plate temperature ++Against standard oils stored in sealed container As for 214.1
* Initial, then 1 year 2 years * Initial, then 1 year *1 month
++Against standard oils stored in sealed container. As for 214.1 ++Against standard oils stored in sealed container Against manufacturers oils As for 214.1
Reference oils METHOD 301.1, 301.2 Oven
2 years
*6 months *2 years
Oven thermometer against reference thermometer Temperature variation in working space.
METHOD 401.1 Spoon METHOD 401.6 Mechanical thumb * Initial * Initial only Dimensions and mass of beads delivered Dimensions and masses (those that disassembled must be checked against one known to conform). Hardness of rubber plunger Dimensions and mass Hardness. cannot be
2 years METHOD 401.8 Ramp/roller Roller rubber bands * Initial 2 years

METHOD 402.1 Bend test mandrels METHOD 403.1 Scratch test apparatus Initial only *1 year METHODS 408.1, 408.3 Adhesion test apparatus Initial only *1 year METHOD 459.1 Sponge and holder machine METHODS 459.1, 461.1, 481.1,481.2, 482.1 Grey scales Reference Working METHOD 601.1 Light booth Colour blindness test METHODS 601.2, 601.3 Colour master Colour eye METHOD 602.1 Specular gloss standards METHOD 602.2 Gloss tiles Primary Secondary Instrument * 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 5 years *6 months *On use Supplied by manufacturer Against primary tiles Against secondary gloss tiles Initial External certificates (NIST) *On use Calibration of photometer scale using reference tiles supplied by manufacturer 100 hours * Initial Check lamps, voltage and illumination levels. Refer Tests for Colour Blindness by S Ishihara 10 years *3 months Replace. Check against reference set. * Initial Mass, length and rate of travel Dimensions of cutting tips and points Re-examine under microscope Needle dimensions. Inspect under microscope for wear and damage apparatus and * Initial only Dimensions.
++ 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).

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.

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 Maximum period between successive Calibrations or Checks Before use Span and zero check (weekly on field instruments used for continuous monitoring) *6 months complete recalibration Procedures and Comments
GAS DETECTION INSTRUMENTS for use in mines, and also for industrial and commercial applications
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). 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 REFERENCE GASES Non-reactive reference gases at a concentration greater than 100 ppm Non-reactive reference gases at a concentration of 100ppm or less whichever comes first. Reactive reference gases 4 years or once the cylinder pressure drops below 700kPa (100 psi), whichever comes first. 2 years or once the cylinder drops below 700kPa (100psi) 2 years or once the cylinder pressure drops below 700kPa(100psi), whichever comes first Full calibration, including maintenance and overhaul to be conducted above ground.
commonly done by laboratory staff

NOTES (i) (ii) (iii) (iv) Frequency given is MAXIMUM period between calibrations. Instruments must be completely recalibrated after significant maintenance. The calibration history for each instrument must be recorded. 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.

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.

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 Positive Displacement Pump Critical Flow Venturi
*500 hours of use after stabilising period or major maintenance *As indicated by CVS system verification
ADR 37/00 - Appendices 5 (Method), 12
Reference Standard; Air Flow Meter (Laminar Flow Element, Subsonic Venturi or orifice plate). Calibration traceable to NIST. Accuracy 1 % of air flow. Using CP Propane (C3H8) or Carbon Monoxide or Carbon Dioxide.
System verification Propane Carbon Monoxide Carbon Dioxide Correlation car
*1 week or after maintenance or servicing of system
System accuracy in the order of 2% critical flow orifice or bomb method NOTE: Precautions for use of pure carbon monoxide *As required to supplement other methods Approved in-house laboratory methods.

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

FLOWMETERS Air Flow Meter Laminar Flow Element (LFE) *100 hours of use or more frequently if drift occurs 10 years Visual inspection contamination for damage, wear and
Orifice Plate
Calibration traceable to NIST Master within 1%, ADR 37/00, Appendix 5
Venturi Flow Meter Anemometers Rotameters (see Note below) Reference High flow >1 L/Min Low flow <1 L/Min Working Fuel Flowmeters Gas analyser For motor emissions vehicle exhaust
10 years 2 years
*2 years *2 years
ASTM D3195 Soap bubble flow meter
*On use *6 months
Soap bubble flow meter
*Span and zero check before and after each analysis on each analyzer *Complete recalibration of all analysers at one month intervals
ADR 37/00 Appendices 10, 12, 13
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.

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 HC Optimisation of performance HC oxygen quenching effect *1 week *On first commissioning; 1 year and after major maintenance *On first commissioning; 1 year and after major overhaul *On first commissioning; 1 year and after major overhaul *Electrical check before each reading ADR 37/00 Appendix 10 ADR 37/00 Appendix 10
SAE J1094a Constant Volume Sampler Systems for Exhaust. Emissions or recommendations. instrument manufacturers
CO Analyser interference of CO2, H20 Exhaust emissions of engines at idle NDIR CO, CO2, HC
*1 week span and zero *1 month SHED (Sealed housing for evaporative determinations) Background emissions HC retention check HC analyser (FID) Homogeneity test Homogeneity response time Recovery or validation test Volume of SHED 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 cylinder pressure falls below 700kPa (100psi) whichever occurs first 2 years or once the cylinder pressure falls below 700kPa (100psi) whichever occurs first *1 year *1 month *1 month *On commissioning and after major service *On commissioning and after major service *On commissioning and after major service *On commissioning and after major service
Gas check. Multi-point calibration using standard gases. ADR 37 Appendices XI, XII
Six point calibration not including zero (see gas analysers)
Time to achieve homogeneity
commonly done by laboratory staff

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.

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 Atmospheric pressure Ambient temperature Air temperature into LFE Pressure depression upstream of LFE Pressure differential across LFE Air temperature at: PDP inlet; or CFV inlet Pressure depression at: PDP inlet; or CFV inlet Pressure at PDP outlet Air temperature at PDP outlet (optional) PDP revolutions during test phase Elapsed time for test phase Air flow (litres/minute) PPi PPO PTO 0.01 kPa 0.01 kPa 0.3C Manometer Manometer Thermometer PTi Tv 0.3C 0.3C Thermometer Thermometer SYMBOL PB TA ETi EPl TOLERANCE 0.03 kPa 0.3C 0.15C 0.01 kPa INSTRUMENT Barometer Thermometer Thermometer Manometer
EDP
0.001 kPa
Manometer
one
Revolution counter
t Qs
0.1 s 0.5%
Stopwatch or equivalent Laminar flow element or subsonic venturi flowmeter
RAMETER ARAMETER SYMB SYMBOL OL TOLERANCE INSTRUMENT

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 * Yearly service * Regular cleaning Procedures and Comments
MICROSCOPE
Details at end of table The microscope, lenses and objectives must be kept clean
HSE/NPL TEST SLIDE WALTON BECKETT GRATICULE
*On use *Measured on installation then every 12 months and whenever the interpupiliary distance, objective, intermediate magnification, or, on some microscopes, the eyepieces are changed. Note: For microscopes embodying a magnification change, the graticule must be measured prior to counting each batch of slides.
Used when setting up the microscope prior to counting each batch of slides. Use to be recorded NOHSC Guidance Note, 1988
PUMPS (Where accreditation is held/sought for volume measurement.) Direct automatic flow control consecutive tests
*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. *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
Constant flow compensation. Refer to calibration Appendix J
Indirect control
automatic
flow-
As above

ALL PUMPS
*On use
Where accreditation for volume measurement is held, the flow rate must be checked in the field before and after use Records must be kept
*Regular maintenance and battery checks ROTAMETERS 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 *As above except, if the measurements are within 3% of the expected result, the interval can be lengthened to 2 years
Against primary flow meter over the range of use (including high flow rates where used)
Large bore, short/medium flow meter, cylindrical float
Against primary flow meter over the range of use(including high flow rates where used)
ELECTRONIC SOAP FILM FLOW METER (eg. gilibrator, mini-buck)
*Monthly for 3 months then, if measurements are within. 3% of the expected result, the interval can be lengthened to 6 months. *On commissioning *On commissioning and whenever the filter, filter holder or any aspect of the filter clearing is changed *1 year *3 months
Against primary flow meter over the range of use (including high flow rates where used)
MANUAL SOAP FILM FLOW METER EFFECTIVE FILTER AREA
Check volume using an appropriate measuring device NOHSC Guidance Note, 1988
REFRACTIVE INDEX OILS
High grade proprietary oils Chemical blends mixed by laboratory
FURNACE * commonly done by laboratory staff
* Initial
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.

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 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. Checking directions of polariser, analyser and accessory plate. Checking correct operation of iris diaphragm in relation to dispersion staining.
3. Stereo Microscopes Checking, lubricating (as necessary) and adjusting all mechanical moving parts, such as focusing rack and zoom controls. Checking all optical alignments such as oculars, binocular tube, objective and illumination system for surface and mount defects. ISO/IEC
Cleaning all optical components as necessary. Checking and adjusting for parfocal operation throughout zoom range.

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) e) Without adjusting the pump, re-measure the flow rate. If the flow rate changes by more than 5%, the pumps constant flow compensation must be reset. f) g) Repeat steps a) to e) with the pump set to each relevant flow rate. 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.

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. ii. iii. iv. v. vi. set pump at initial nominal flow rate program pump to start at least 1 hour later measure and record pump flow rate within 5 minutes to auto switch-on repeat steps i to iii for each flow rate used repeat steps i to iv for each pump used 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
b)
reliably deliver the correct flow rate immediately before automatic switch-off over the time cycle chosen i. ii. iii. iv. v. vi. set pump at initial nominal flow rate program pumps to finish at least 1 hour later measure and record final pump flow rate within 5 minutes before auto switch-off repeat steps i to iii for each flow rate used repeat steps i to iv for each pump used 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. iii. iv. v. d) repeat step i for each sampling period likely to be used repeat steps i to ii for each pump used repeat steps i to iii on three separate occasions accept a pump if pump timer elapsed time is within +/-1% of actual elapsed time
ISO/IEC 1 7025 APPLIC APPLICATION TION DOCU DOCUMENT
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. iii. iv. v. vi. set pump at initial nominal flow rate progressively restrict pump suction so as to cause flow fault condition during step ii measure and record pump flow rate just before auto switch-off repeat steps i to iii for each flow rate used repeat steps i to iv for each pump used 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

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. iii. iv. v. vi. set pump at initial nominal flow rate progressively reduce voltage supply to pump so as to cause low battery fault during step ii, measure and record pump flow rate just before auto switch-off repeat steps i to iii for each flow rate used repeat steps i to iv for each pump used 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.

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) d) Effects of interfering substances and differing matrices must be assessed. 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.

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.

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.

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 ASTM E169 ASTM E275 Terminology relating to molecular spectroscopy. Practices for general techniques of ultraviolet quantitative analysis. Practices for describing and measuring performance of ultraviolet, visible and near infrared spectrophotometers. ASTM E925 ASTM E958 Practice for periodic calibration of narrow bandpass spectrophotometers. Practice for measuring practical spectral bandwidth of ultraviolet-visible spectrophotometers.
b)
Infrared: ASTM E168 ASTM E275 Practices for general techniques of infrared quantitative analysis. 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:

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 ASTM E663 ASTM El184 APHA 3111 APHA 3112 APHA 3113 APHA 3114 Glossary of terms used in flame atomic absorption spectroscopy. Practice for flame atomic absorption analysis. Practice for electrothermal (graphite furnace) atomic absorption analysis. Metals by flame atomic absorption spectrometry. Metals by cold-vapour atomic absorption spectrometry. Metals by electrothermal atomic absorption spectrometry. 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 AS 2563 Glossary of terms used in X-ray spectroscopy. 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.

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
Practice for use of statistics in the evaluation of spectrometric data.
(c)
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 chromatography (or high omatography liquid omatography, chromatographs , including and high ion
performance
pressure)
(HPLC)
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.

Relevant standards for the checking and use of chromatographic instrumentation include: AS 3741 ASTM D1945 ASTM D4626 ASTM E260 ASTM E355 ASTM E516 Recommended practice for chemical analysis by ion-chromatography. Test methods for analysis of natural gas by gas chromatography. Practice for calculation of GC response factors. Practice for packed column gas chromatography. Practice for gas chromatography terms and relationships. Practice for testing thermal conductivity detectors used in gas chromatography. ASTM E594 Practice for testing flame ionization detectors used in gas
chromatography. ASTM E682 ASTM E685 Practice for liquid chromatography terms and relationships. Practice for testing fixed wavelength photometric detectors used in liquid chromatography. ASTM E697 ASTM E840 ASTM E958 Practice for use of electron capture detectors in gas chromatography. Practice for using flame photometric detectors in gas chromatography. Practice for measuring practical spectral band width of UV/Vis spectrophotometery. ASTM E1151 ISO 6326 Practice for ion chromatography terms and relationships. 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 ISO10301 Natural gas - simple analysis by gas chromatography. 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.

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 ASTM E627 ASTM E792 Guide for computerised systems. Guide for documenting computerised systems. Guide for selection of a clinical laboratory information management system. ASTM E1013 Terminology relating to computerised systems.

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. 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. This is an

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 %
R2
Appropriateness Error : 0.5 %
Standard Solution (0.1 % relative) Calibration without CRM
Composition CRM (0.5% relative) 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.

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.

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 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) o 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). o Limitation of the field of application.

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: Comparative method: 2) Water in powders Calculable method: Relative method: Comparative method: Karl Fisher Titration Extraction of H2O by isopropanol, GC detection Infra-red Reflexion on solid sample Atomic Absorption after acid digestion of sample X-ray Fluorescence on solid sample

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.

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.

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.

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.

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.

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.

National Accreditation Board for Testing and Calibration Laboratories 3rd Floor, NISCAIR 14, Satsang Vihar Marg New Mehrauli Road New Delhi 110 067 Tel.: 91-11 26529718 20, 26526864 Fax: 91-11 26529716 Website: www.nabl-india.org

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NABL 103

NATIONAL ACCREDITATION BOARD FOR TESTING AND CALIBRATION LABORATORIES

CHEMICAL TESTING LABORATORIES

ISSUE NO : 03 ISSUE DATE: 25.03.2008

AMENDMENT NO : 00 AMENDMENT DATE: --

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

TERMS AND DEFINITIONS

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

Sample A portion of material selected to represent a larger body of material.

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

Assuring the quality of Test Results

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

GROUPWISE CODIFICATION FOR CHEMICAL TESTS

National Accreditation Board for Testing and Calibration Laboratories

Disinfectants Disinfectants and their formulation

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

Inks Printing inks Writing inks Duplicating inks

National Accreditation Board for Testing and Calibration Laboratories

Lac & Lac Products Lac Lac products

Leather Leather Synthetic leather

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

Rubber & Synthetic Rubber Natural rubber Synthetic rubber

National Accreditation Board for Testing and Calibration Laboratories

Corrosion Tests Salt spray tests Dezincification tests Other tests

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

ISO/IEC APPLIC APPLICATION TION DOCU DOCUMENT MENT Annexure

EQUIPMENT CALIBRATION INTERVALS (as per NATA Document)

National Accreditation Board for Testing and Calibration Laboratories

CALIBRATION APPENDIX A: CALIBRATION OF COMMON TEST EQUIPMENT

Each Cycle BALANCES See also weighing instruments 3

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

National Accreditation Board for Testing and Calibration Laboratories

Initial When barrel/plunger is changed

* Initial only Initial 6 months

Initial only 6 months

Initial only Initial, then 1 year

On use 6 months