No

NABL 103 DRAFT

NABLNATIONAL ACCREDITATION BOARD FOR TESTING AND CALIBRATION LABORATORIES

SPECIFIC CRITERIAfor CHEMICAL TESTING LABORATORIES

ISSUE NO : xxAMENDMENT NO : 00

ISSUE DATE: -AMENDMENT DATE: --

AMENDMENT SHEET

SlPage No.Clause No.Date of AmendmentAmendment madeReasonsSignature QMSignature Director

1

2

3

4

5

6

7

8

9

10

National Accreditation Board for Testing and Calibration Laboratories

Doc. No: NABL 103 DraftSpecific Criteria for Chemical Testing Laboratories

Issue No: XXIssue Date: -Last Amend No: 00Amend Date: --Page No: i

ABBREVIATIONS

AOAC:Association of Official Analytical ChemistsAPHA:American Public Health AssociationAPLAC:Asia Pacific Laboratory Accreditation CooperationAS:American StandardASTM:American Society for Testing and MaterialsBIS:Bureau of Indian StandardsBIPM:Bureau International des Poids et Measure (International Bureau of Weights and Measures)BS:British StandardCRM:Certified Reference MaterialISO:International Organization for StandardizationEA:European Cooperation for Accreditation FTIR:Fourier Transform InfraredGFAAS:Graphite Furnace Atomic Absorption Spectrometere.g.: For ExampleGUM:Guide to the Expression of Uncertainty in MeasurementICP-AES:Inductively Coupled Plasma - Atomic Emission Spectrometer ICP-MS:Inductively Coupled Plasma Mass SpectrometerIEC:International Electrotechnical CommitteeILAC:International Laboratory Accreditation Cooperation IUPAC:International Union of Pure and Applied ChemistsNABL:National Accreditation Board for Testing and Calibration LaboratoriesNATA:National Association of Testing AuthoritiesNIST:National Institute of Standards and TechnologyNMR:Nuclear Magnetic ResonanceQC:Quality Controlw.r.t.:With Respect To

NBC: National Building CodeNational Accreditation Board for Testing and Calibration Laboratories

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

Issue No: xxIssue Date: -Last Amend No: 00Amend Date: --Page No: ii

CONTENTS

SlTitlePage

Amendment Sheeti

Abbreviationsii

Contentsiii

1. Introduction1

2. Terms and Definitions2

3. Scope3

4. Management Requirements6

5. Technical Requirements8

6. GroupWise Codification for Chemicals Tests30

7. References41

Annexure A38

Annexure B41

Appendix A42

Appendix B45

National Accreditation Board for Testing and Calibration Laboratories

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

Issue No: xxIssue Date: -Last Amend No: 00Amend Date: --Page No: iii

1. INTRODUCTION

1.1 The requirements for accreditation are laid down in the International Standard ISO/IEC 17025: 2005 (General requirements for the competence of calibration and testing laboratories). These requirements apply to all types of objective testing but in certain instances additional guidance is necessary to take account of the type of testing and the technologies involved.

1.2 This document has been prepared by a Technical Committee constituted by NABL as a supplement for ISO/ IEC 17025: 2005 standard and sets out additional technical requirements specific to chemical testing discipline.

1.3 Laboratories conducting tests on food/water should also consult NABL Specific Criteria on Biological testing (NABL 102).

2. TERMS AND DEFINITIONS:

For the purpose of reference few definitions have been described, however the final version of VAM definitions would prevail.2.1 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.

2.2 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.2.3 Sample

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

2.4 Sample handling

This refers to the manipulation to which samples are exposed during the sampling process, from the selection of the original material through to the disposal of all samples and test portions.

2.5 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

2.6 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.

2.7 Test portion

This refers to the actual material weighed or measured for the analysis.

2.8 TraceabilityProperty of the result of a measurement or the value of a standard whereby it can be related to stated references, usually national or international standards, through an unbroken chain of comparisons all having stated uncertainties (VIM 1993 - Ref B6).

3. SCOPE

3.1 The Scope of accreditation of a laboratory is the formal statement of the range of activities for which the laboratory has been accredited; the scope is recorded in detail on a laboratorys accreditation certificate. A laboratorys scope should be defined as precisely as possible so that all parties concerned know accurately and unambiguously the range of tests / Limit of Quantification (LOQ)/Limit of Detection (LOD) and/or analyses covered by that particular laboratorys accreditation. The guideline for the applicant laboratories to describe group of products, material or items tested for scope of accreditation is given in section-6. The format to write scope of accreditation is given in NABL-151 and is presented with few examples for understanding (Annexure A).

3.2 There are many tests where 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. In such cases the statement in the column, Specification, standard (method) or technique used, of format to write scope of accreditation will normally take the form of Documented In-House Methods, which should elaborate on methods used to prepare samples or both standard method for preparation for sample and for measurement stage may be written.

3.3 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 standard method in the conventional sense with an instrument specifying 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-MS/NMR/FTIR, ICP-MS, XRF and XRD etc. (Refer ISO/IEC 17025: 2005 para 5.4.2, 5.4.3, 5.4.4 and 5.4.5). Whenever there are deviations from standard method or inadequate clarification in Standard Method, the laboratory needs to develop effective procedure for ensuring the quality of results.

Note: Wherever Sampling is a part of Test method, it shall not be included as test in the recommended scope.

3.4Laboratory can apply for addition or amendment in the scope at any time by writing to NABL of the tests, which it wishes to add to its scope, by providing the following information to NABL in the formats given in NABL 151: Scope to be added List of authorized manpower, List of equipments List of CRMs Quality assurance including PT/ILC participation In addition to the above the laboratory should also provide a layout plan showing the area where it plans to conduct additional tests as relevant.

4. Management REQUIREMENTS

4.1 The internal management system documents shall be comprehensively reviewed for suitability at appropriate frequency to be documented by the lab. The procedure for document control shall include the control of external documents including standard test methods. Evidence of ensuring the revision status of the standard test methods shall be available.

4.2 Laboratory can subcontract testing to another accredited laboratory under unavoidable circumstances like instrument breakdown, unavailability of trained staff for a short period. The subcontracting of any test(s), for which the laboratory is not accredited is done, then the laboratory cannot claim accreditation status while incorporating the results of these test(s) in their test report, even if the test(s) is/are performed in an accredited laboratory.Laboratory shall identify the subcontracted tests in the test reports.

If an accreditation body allows an accredited laboratory to include results of subcontracted tests or calibrations in its endorsed reports or certificates, the accreditation body shall define such circumstances. These shall include: the accredited laboratory takes full responsibility for the subcontracted tests or calibrations and, unless it is an accredited branch of the same laboratory, has informed the customer of the proposed subcontracting and has obtained his/her prior approval; approval has been obtained from the subcontractor to report excerpts from the subcontractors report or certificate; the subcontractor is itself accredited for the specific tests or calibrations concerned and the results have been included in the subcontractor laboratorys endorsed report or certificate.

4.3 Storage requirements and shelf life (where applicable) of the various chemicals and other critical consumables which can deteriorate over a period of time shall be documented. In case of various solutions prepared, the container should be labeled incorporating the name of the solution, date of preparation and date of expiry. The quality of water used shall be checked to ensure its compliance with the requirements of the intended use.

4.4 Verbal complaints shall also be registered by the laboratory.

4.5 Deficiencies encountered such as poor performance in ILC/PT, non repeatability of test results while performing quality checks shall be registered as non conforming testing work and suitable corrective actions taken after conducting root cause analysis.

4.6 Records of personnel including training records shall be kept permanent - i.e. so long as the person is working in the laboratory. Similarly, history of individual equipments shall be kept permanent so long as the equipment is used in the laboratory.

4.7 Internal audit of the laboratory shall be conducted at least once in 12 months and shall cover all the sections including the testing section(s) and covering all the applicable requirements of ISO/IEC 17025:2005 and NABL 103. The technical audit should be conducted by a trained auditor who is qualified and conversant with the technical activities performed. Specific observations about the key requirements of the standard ISO/IEC 17025:2005, both positive and negative shall be recorded by the auditor to give evidence of having covered all the elements of the standard. Apart from conducting horizontal audit covering all applicable elements of ISO/IEC 17025:2005, VERTICAL AUDIT should also be conducted. For this purpose different samples or test reports covering the entire period and commensurate with the number of samples between internal audits shall be selected and compliance with management and technical requirements shall be verified.

For meeting the Internal Audit in the Laboratory having different Section must have sufficient no's of Technical Personnel (apart from Technical Manager & Quality Manager) having formal training on Internal Audit for avoiding the conflict of Interest.

5. TECHNICAL REQUIREMENTS

5.2Personnel

5.2.1 The Technical Manager of a Chemical testing laboratory shall be a person preferably having a recognized post graduate degree in science or Bachelor degree in engineering or specialized course and at least two years experience in analysis/R&D/quality control.

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, food etc. The staff shall have sufficient training and exposure in analytical chemistry and in analysis and testing of appropriate products. All technical staff must have minimum training in requirements of ISO/IEC 17025. Training record and evaluation for effectiveness of training for the System must be documented.

Lower formal qualifications (minimum higher secondary in science or equivalent) may be acceptable when staff have extensive relevant experience and/or the scope of activities covering simple tests. Chemical analysis should be carried out under adequate supervision.

Note: The technical personnel who perform chemical testing should be free from colour blindness, evidence for which is necessary.

5.2.2 Authorized signatory is one whose signatures must be there on all the reports issued by laboratory. (Note: There may be other persons signing on the test reports as per in-house requirements of a laboratory) The minimum requirement for an authorized signatory shall be graduate in Science (relevant field) with 4 years experience or graduate in Engineering/ Post graduate in Science /Engineering (relevant field) with 2 years experience. Personnel having Doctorate degree may be exempted from experience requirement if the research work commensurate with the relevant field.The person should also have knowledge of laws or protocols in the group of products, material or items tested so as to enable him to give opinions and interpretations in test reports.

5.2.3 Chemical testing laboratory involved in testing different group of products, material or items must have a minimum one number of technical staff involved in testing of that group of products, material or items in addition to authorized signatory. The laboratory should justify total staff with reference to volume of work handled. 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 trainings must be documented in detail providing identity of trainer, training contents, duration, methodology, identity of participants.

Internal Training alone may not be considered adequate to make the staff knowledgeable on the latest status of science and technology. It must be supplemented if required with external training. The duration of the external training should commensurate with contents and conducted/organized by Universities, Research Institutes, Professional Bodies, Industry, NABL accredited laboratories Associations/NGOs or other recognized organizations. The certificate of successful completion of training should be available.

In addition relevant laboratory staff particularly technical manager/authorized signatory should also participate in awareness programs/workshops/conferences to update them on knowledge of laws or protocols in the group of products, material or items tested so as to remain updated on latest in their field.

Feedback by participants on training and evaluation of participants by laboratory are two important elements of the training activity and must be documented.

5.2.5 The Quality Manager of a Chemical testing laboratory should be a person having a recognized graduate degree in science or Bachelor degree / diploma in engineering or specialized course and at least two years experience.

Quality Manager shall have undertaken at least 4-day training course on requirements of ISO/IEC 17025.

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.

5.3 Environment and Accommodation Condition

5.3.1 Laboratory accommodation and layout should consider provision of areas for - (a) Sample receipt and customer dealing (b) Sample pre-treatment (c) Sample storage (d) Storage for chemicals/ consumables (e) Test areas as for wet analysis; heating, digestion & extraction; instrumentation (f) In-house calibration (g) Maintenance (h) Stores say for records (i) Waste management (j) Reporting (k) miscellaneous as per the requirements of the lab. This does not necessarily mean separation by walls and may vary widely depending upon group of products, material or items tested for which the laboratory seeks or maintains accreditation.

Samples, reagents, measurement standards and reference materials must be stored so as to ensure their integrity. In particular, samples must be stored in such a way that cross contamination is not possible. The laboratory should guard against their deterioration, contamination and loss of identity.

Floor wise laboratory layout giving dimensions and highlighting the above provisions should be provided in Quality Manual. Drawings shall show key equipment. Future space requirements can be shown in shaded.

Laboratory shall maintain, monitor and record environmental conditions (air quality, ventilation, temperature, humidity, luminance, noise and vibration levels, radiation, and electromagnetic disturbances) for proper working as per the requirements of the test specifications. The laboratory environment should be sufficiently uncrowned, clean and tidy to ensure the quality of the work carried out is not compromised. See 5.3.2 for more details.

5.3.2 There shall be effective separation between neighbouring areas in which incompatible activities are being performed in laboratories that cover different products and tests. Typical Examples are separate areas for handling of test items and sample preparation. Even though analysis of trace metals/residues may be done on same AAS/GC-MS, but sample handling, storage and preparation areas for food samples and sewage shall be different. Separate area shall be available for proper storage and maintenance of field monitoring equipments.

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 Health and Safety

One key responsibility of the laboratory management is to provide safe working environment which include the following: head and eye shower cleaning and decontamination procedures for radioactive spills, waste disposal evacuation procedures including a plan of the facility showing the location of safety equipments and fire extinguishers/sand bucket, protective clothing eg. gowns, coats, gloves, goggles etc Appropriate fume evacuation system routine cleaning and disinfection for work benches, floors, centrifuges, Refrigerators, etc handling hazardous substances

Fire Safety: Laboratory shall follow latest norms as per NBC of India.

Fume hoods: Laboratory operations often involve use of toxic, hazardous or odoriferous chemicals. The handling of these chemicals particularly digestion activities should be safely performed in a fume hood. The size and type of fume hood (Bench or Walk-in) shall depend upon lab requirements and volume of work. The non AC labs may use conventional type or automatic by-pass fume hoods. The AC labs shall use auxiliary or variable flow volume fume hoods.

A dedicated fume hood is required for extensive usage of perchloric acid greater than 50% of total chemical usage. Note: A dedicated hood is required because; organic chemicals should not be used with perchloric acid. Explosion may occur when perchloric acid reacts with organic materials. Fume hood manufacturer shall be contacted for specific materials requirements if any for explosion proof electrical fixtures or for radiological purposes.

Personal Protection Equipments: Suitable protective clothing/equipment must be available at all the times in the laboratory. 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. The laboratory should list out its requirements depending upon material or items tested in its health and safety manual.

Dedicated emergency Safety Shower/Safety-cum Eye shower shall be available in clear approachable area away from electrical service within easy accessibility from relevant work areas). Individual eye wash units may also be provided. Unit design shall provide twin stream nozzles to flush both eyes at once, and in a hands-free mode. Unit shall be securely positioned in place, universally reachable, preferably installed at a sink, away from any obstructions. Safety shower signage/ Eyewash signage shall be provided. These shall be installed as per manufacturers instruction and shall be standard equipments.

Gas Cylinder Storage: Cylinders shall not be stored in test areas. Cylinders storage areas shall be prominently identified as to the type gas contained. All gas cylinders shall be secured with appropriate restraints (like chain). Where permanent connection hoses and lines are provided for cylinder gases, they shall be marked to identify the gas they contain and the direction of gas flow.

5.4 Test Methods and Method Validation:

5.4.1Laboratory should generally use standard methods/internationally published methods/in-house validated methods.

5.4.2The validation of a standard or collaboratively tested methods should not be taken for granted, no matter how impeccable the method's pedigree - the laboratory should satisfy itself that the degree of validation of a particular method is adequate for the required purpose, and that the laboratory is itself able to verify any stated performance criteria.5.4.3Methods developed in-house must be adequately validated, documented and authorised before use. Where they are available, matrix matched reference materials should be used to determine any bias, or where this is not possible, results should be compared with other technique(s), preferably based on different principles of measurement. Measurement of the recovery of gravimetrically added spike analyte, measurement of blanks and the study of interferences and matrix effects can also be used to check for bias or imperfect recovery. Estimation of uncertainty must form part of this validation process and in addition to covering the above factors, should address issues such as sample homogeneity and sample stability.

5.4.4Laboratory, 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; Eurachem Guide for Method Validation and Related Topics (1998) may be referred.

5.4.5The important performance characteristics for method validation include:a) 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.

b) 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 uncertainty 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 it is usually sufficient to plot a calibration curve using measurement standards at 5 different concentration levels (+ blank). More measurement standards will be required where linearity is poor. In qualitative analysis, it is common place to examine replicate samples and measurement standards over a range of concentrations to establish at what concentration a reliable cut-off point can be drawn between detection and non-detection

c) 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 determinedNote: Linearity to be conducted for standard as well as matrix match standard.

d) 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.

e) 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

f) 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

Note: Quantitation: The batch of unknown samples for estimation of an analyte must be analysed in parallel with Spiked sample for quantitative estimation of an analyte. The calculation of an analyte should not be on standard solutions. Confirmatory Analysis: The positive detection of an analyte in any matrix has to be confirmed by using the confirmatory technique of analysis including the mass spectrometry.

g) 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

h) 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.

Note: Accuracy to be estimated at LOQ level and further at 5, 10 or 50 times of LOQ.

i) 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.

Note : Laboratories are estimating the linearity during validation of method where the performance of different linear concentration of standards are studied, however for Pesticide residue analysis along with linearity standard the laboratory must estimate matrix match standard linearity. For this laboratory must have the pesticide free matrix at initially least one matrix from the group of products.

Pesticide Residue Testing Laboratories should include in the validation that the accuracy studies by spiking the matrix or sample at LOQ level, five times of LOQ and ten or fifty times of LOQ.

Accreditation is normally granted only for nationally or internationally accepted standard test procedures or non-standard procedures (in-house methods) that have been appropriately validated and which are performed regularly.

5.4.6When standard methods are used, laboratories should verify their own satisfactory performance against the documented performance characteristics of the method, before any samples are analyzed. 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.

Laboratory Procedures can be written to document the above aspects. 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

5.4.7When In-house methods (Non Standard methods) validation shall be undertaken. In-house methods could include but not be restricted to:(a) Methods developed in the laboratory(b) Methods developed by a client(c) Methods developed for an industry group(d) Modified standard test methods(e) Methods from scientific publications but which have not been validated5.4.8Validation 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

5.4.9Kits :Commercial test systems (kits) will require further validation if the laboratory is unable to source the validation data from manufacturers with a recognized quality assurance system, reputable validation based on collaborative testing e.g. AOAC Official Methods and/or associated JAOAC publications, or independently reviewed methods e.g. AOAC Performance Tested Methods.

5.4.10Test and calibration methods and method validation/verification published by BIS, ASTM, AOAC, etc may be followed.

5.4.11Developments 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 labeled as obsolete. The revised method must be fully documented, and indicate under whose authority the new method was issued (signed and dated).

5.4.12Lab should provide UOM in different individual range in absolute unit terms instead of percentage. It is important for testing laboratories to understand the concept of uncertainty of measurement. Laboratory management should be aware of the effect that their own uncertainty of measurement will have effect on test results produced in their laboratory.

While the concept and application of measurement uncertainty estimations have been well established in metrology and calibration laboratories, the same cannot be said for testing laboratories. The publication of ISO/IEC 17025 has prompted rigorous discussionInternationally on uncertainty of measurement in chemical testing and a consensus agreement on the definitive methodology to be used for estimating uncertainty is still to be finalised.

The following details the current requirements for laboratories accredited by NABL:

Laboratories need to make a formal estimate of measurement uncertainty for all tests in the scope of accreditation that provide numerical results. Where an estimate of measurement uncertainty is required, laboratories need to document their procedures and processes on how this is to be done. This should be on the basis of EURACHEM and GUM where standard methods include uncertainty factors, laboratories may use them for the estimates.

5.4.14Use of Computer

When laboratories use equipment/instruments that make use of computers or have built in computers or laboratories use Laboratory Information Management Systems (LIMS) for the acquisition, processing, recording, reporting, storage or retrieval of test data, the laboratory shall ensure that it uses licensed softwares. The laboratory should be able to demonstrate if required control of access to computer systems and various functions including that procedures are established and implemented for protecting the data.

5.5 Equipment

5.5.1 As part of quality system, a laboratory is required to operate a programme for the maintenance and calibration of equipment used in the laboratory. Equipment normally found in the chemical laboratory can be categorised as:

i) general service equipment not used for making measurements or with minimal influence on measurements (eg hotplates, stirrers, non-volumetric glassware and glassware used for rough volume measurements such as measuring cylinders) and laboratory heating or ventilation systems;ii) volumetric equipment (e.g. flasks, pipettes, pyknometers, burettes etc);iii) measuring instruments (e.g. hydrometers, U-tube viscometers, thermometers, timers, spectrometers, chromatographs, electrochemical meters, balances etc);iv) physical standards (weights, reference thermometers);

5.5.2 General Service Equipment

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 as per Appendix B. 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 General Guidelines on calibration requirements and intermediate checks for specific items of equipment are detailed in Appendix B.

It must be stressed that these frequencies of calibration are considered to be the minimum appropriate, provided that the Laboratory uses standard equipments, perform regular intermediate checks and or regular performance checks.

Performance checks e.g to check the response, stability and linearity of sources, sensors and detectors, the separating efficiency of chromatographic systems, the resolution, alignment and wavelength accuracy are needed for many equipments as spectrometers. 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.

Where the above criteria cannot be met or the relevant standard methods have specified more stringent requirements, the same may be adopted. Chemical testing laboratories are recommended to have these items calibrated by an accredited external agency. If chemical testing laboratories wish to calibrate these items themselves, a full measurement uncertainty budget is expected to be estimated along with the necessary infrastructure. Records of calibrations carried out in-house must confirm traceability of measurement. This is normally achieved by the record specifically identifying the reference item used, the date and the person performing the work using the documented procedure.Uncertainty of measurement estimations for periodic checks conducted on in-house on calibrated equipment (i.e. conducted between full calibrations) are not required.

5.5.4.2 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 access to the relevant reference standard, as a means of calibration.

5.5.5.2 Reference standards and accompanying certificates should be stored and used in a manner consistent with preserving the calibration status. Particular consideration should be given to any storage advice given in the documentation supplied with the standard.

5.6 Calibration & Measurement Traceability

5.6.1 The overall programme for the calibration of measuring equipment in the chemical laboratory shall be designed to ensure that, where the concept is applicable, all measurements are traceable through certificates held by the laboratory, either to a national or international standard or to a certified reference material. Where no such reference standard or certified reference material is available, a material with suitable properties and stability should be selected or prepared by the laboratory and used as a laboratory reference. The required properties of this material should be characterized 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 traceable and certified chemicals. (iv) Laboratories may use chemicals of known purity in case on non-availability of CRM.

5.6.3 Reference materials and Chemical standards

5.6.3.1Laboratories shall use CRM wherever applicable.

5.6.3.2In case of matrix interferences, a standard 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.

5.6.3.3Reference 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 and records should be maintained.

5.6.3.4Reference materials and standards should be handled in order to safeguard against contamination or loss of determinant. Training procedures should reflect these requirements.

5.7Sampling and Handling of Test Items

5.7.1Sampling may refer to following set of procedures and or activities1. Where a sample is to be collected for analysis from outside the laboratory by laboratory personal (may be customers premises) e.g. collecting a sample of water from customers tube well or taking a sample of cement from a lot at customers godown or collecting a sample of ambient air in a city. The sampling shall be undertaken as per standard sampling procedures. Laboratory should have proper sampling formats to be used by its staff to record all information that is required as per clause 5.10 of ISO-17025:2005 including any deviations from standard test methods.2. Where customer provides a sample for analysis (sampling is not done by laboratory) even in this case laboratory should have procedures to verify from customer atleast those aspects (sample conditions as fitness for testing) that may have a bearing on the results and maintain records of same. 5.7.2The test reports should clearly identify whether sampling is done by laboratory (in which case sampling procedure followed should be mentioned) or sample is provided by customer. Once a sample is received in laboratory (test item) further sub-samples may be need to be taken/prepared as per standard test methods. The observations in many cases taken on site as recording environmental conditions as pressure, temperature, measuring onsite DO-levels, checking pH at the time of sampling on site also does not constitute field laboratory, such measurements shall be recorded as Field Observations in the test reports.

5.7.3Sample identification

The samples should be collected in containers or otherwise, preserved and transported to laboratory as per Standard methods and any deviations should be recorded. The laboratory should have written procedures on sample collection, preservation and transportation including providing identification labels in field and in laboratory.

5.7.4Sample registration

Laboratory shall uniquely identify and register the sample received in the laboratory to establish audit trail.

5.7.5Sample retention and storage

Laboratory shall define Sample retention criteria based on the sample stability and conditions. Laboratory may appropriately retain the sample to enable retesting wherever possible. The retention and storage should also be based on applicable regulatory requirements. 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 organized so that there is no risk of contamination or cross-contamination, nor of packaging and any related seals being damaged. Adequate environmental conditions should be maintained, to avoid damage or degradation of the test material. Records of environmental monitoring to be maintained. An appropriate level of security should be exercised to restrict unauthorized access to the samples.

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 above5.7.6Reagents

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.

Labeling 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 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.

5.9Assuring the quality of Test Results

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:

certified reference materials / reference materials

internally generated quality control materials

independent checks by other analysts/examiners

statistical quality control charts

positive and negative controls

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

5.9.1Proficiency Testing / Inter Laboratory Comparisons (PT/ILC)

Laboratories have to successfully participate in one PT/ILC program prior to applying for accreditation as per ILAC P: 9. The PT/ILC participation shall be done not more than one year prior to application date of accreditation. NABL strongly encourages the laboratories to participate in the PT services accredited to ISO/IEC 17043. In case laboratory conducts ILC program they should be conducted with 8-11 accredited laboratories to evaluate the results statistically. In exceptional cases few reputed non accredited laboratories can also be considered as participant.

Laboratory shall have a plan for PT/ILC participation as per NABL 162 / 163. The requirements of initial accreditation shall be applicable when the laboratory adds additional scope particularly new group or sub-group.

Laboratory shall submit the PT participation records during the next accreditation cycle. 5.9.2Internal Quality Control

NABL strongly encourages the laboratory to use statistical QC chart as Internal QC measures. The level and frequency adopted for internal quality control checks 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 analyzed should be a QC sample. For more complex procedures, even 20% is not unusual. For analyses performed infrequently, a full system validation should be performed 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.

5.10Reporting the ResultsIn addition to the compliance to the requirements of clause 5.10 of ISO/IEC 17025:2005, laboratory shall define its policy on use of NABL symbol and follow the same. NABL symbol shall be used strictly as per NABL-133. 6. GROUPWISE CLASSIFICATION FOR CHEMICAL TESTS

The Chemical discipline is described in terms of groups and subgroups of test. Application for accreditation may be made for one or more groups of tests or for subgroups or specific test within a single group or subgroup. Where the existing group does not appear to cover the needs of a laboratory, NABL secretariat welcomes proposals for additional groups or tests to be included in this discipline. The scope of accreditation may be reviewed and extended on request, provided that the laboratory complies with conditions for accreditation for the groups of test or specific tests involved.6.1. Air, Gases & Atmosphere Industrial gases Gases for medical use & diving Reference gases & mixtures Compressed gases Miscellaneous

6.2. Building and Construction Materials Cement & other mortars Cement concrete Refractories Refractory cement Sand Clays & soils Pozzolonic materials Fly-ash Waterproofing compounds Thermal insulation materials Masonry bricks/blocks, etc. Ceramics (glass, porcelain, refractories) Aggregates Rocks Admixtures inorganic & organic

6.3. Coal, Coke & other Solid Fuel Coal/coke Coal carbonization products Charcoal Briquetted solid fuels Bitumen

6.4. Cosmetics & Essential Oils Perfumes Essential oils Cosmetics Intermediates and miscellaneous chemicals for cosmetics Herbal-based cosmetics

6.5. Dye , Pigments and Inks Synthetic dyes Dye intermediates Natural dyes & colouring materials Pigments Inks (Printing, writing, duplicating inks)

6.6. Disinfectants Disinfectants and their formulation Sanitizer6.7. 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 Ayurvadic Homeopathic natural drugs and supplements

6.8. Explosives & Pyrotechnics Ammunitions Industrial explosives & associated material Pyrotechnics Explosives chemicals and allied materials

6.9. Fertilizers Nitrogeneous fertilizers Phosphatic fertilizers Fertilizer mixtures Potash fertilizers Micronutrients Organic manure and Compost Liquid Fertilizers

6.10. Agricultural Products Alcoholic drinks & beverages Products of Cereals pulses and others (atta, maida, semolina, etc) Coffee, cocoa and by-products Tea and tea products Starch and starchy products Honey and honey products Fruits and vegetable products Spices condiments and Herbs Nuts & nut products Organic foods GM Foods Seed Tobacco and tobacco products Cereals, grains, pulses, oil seeds

6.11. Non Agricultural Products Animal feeds Milk and dairy products Fish and fishery products Meat and meat products Egg & egg products

6.12 Processed food and Food additives Bakery and confectionery products Food additives Colour, flavour & preservatives Infant foods Sugar and by-products Fruit juices & concentrates Vitamins in foods Oil, fats and related products Enzymes

6.13 Food Packaging Material

Paper packaging Plastics and polymer Aluminium foils Metal cans Others6.14. 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 Carbon black Wood and timber treatment chemicals Industrial alcohols Alcohols based chemicals 6.15. Lac & Lac Products Lac Lac products

6.16. Leather and Leather products Leather products Natural and Synthetic Leather

6.17. Lubricants 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 (like asbestos, glass wool, rock wool, mineral wool) Other minerals Minor elements 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 Zinc & inc alloys Lead & lead alloys Magnesium & magnesium alloys Nickel, chromium, cobalt & their alloys Titanium & titanium alloys Tungsten & its alloys Other metal alloys

6.20. 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 Anti corrosive coatings

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

6.22. Petroleum and products Crude petroleum Fuels-gaseous, liquid & solid Aviation fuels Waxes and jellies Miscellaneous products, white oil, anti-freeze, solvents insulation oils, feed-stock Pour point depressants (flow improvers) Petrochemical feedstocks De-icing fluids Hydraulic fluids Fuel additives including corrosion preventives

6.23. Plastics and Polymers Plastics & polymers Raw materials Plastic films

6.24. Rubber, Resins and Adhesives Natural rubber Synthetic rubber Resin Starch based adhesives Natural gums Glues Polymer based adhesives (Synthetic)

6.25. Agrochemicals Synthetic pesticides (insecticides, weedicides, herbicides, fungicides, etc) & their formulations Natural pesticides (Biopesticides) & their formulations Pheromones, chitin inhibitors Growth Regulators

6.26. Pollution & Environment Ambient Air Quality Indoor air quality (to review the test method and equipment) Fugitive/Process Emissions Stack Emissions Wastewater (Effluents/Sewage) Solid wastes Hazardous wastes Soil/sediments Surface/Ground water Ambient Noise Levels (Excluding vibration) Source Noise Levels (Excluding vibration) Meteorological Vehicular Emission Effluents toxicity (Bioassay) Used/Waste oil

6.27. Rubber Resins and Adhesives Natural rubber Synthetic rubber Resin Starch based adhesives Natural gums Glues Polymer based adhesives (Synthetic)

6.28. Soap Detergents and Toiletries Soaps Synthetic detergents Wetting and emulsifying agents

6.29. Textile & Textile Auxiliaries Fibre & filaments Yarns & chords Fabrics, garments, coated and laminated fabrics and made-ups Technical textiles (geo-textiles, medical textile, automotive textiles) Non-woven textile Woven textile Textiles accessories like zippers, buttons. Jute and Jute products

6.30. Water Drinking water- Potable and domestic Packaged drinking water Packaged Natural Mineral Water Reagent Grade Water Water for Swimming Pools Water for ICE Manufacture Water for Processed Food Industry Feed Water, Boiler Water, and Condensate for High Pressure Boilers Water for Storage Batteries Water for Construction purpose Water for Injection/Medicinal purpose Water for use for irrigation purpose Others6.31. Metallic Coatings and Treatment Solutions Metallic coatings Conversion coatings Plating solutions Anodizing solutions Metal finishing materials

6.32. Group Residues and Trace Elements Food products Agricultural products Water Environment Textile products Toys Drugs and Pharmaceuticals Cosmetics Nutritional supplements Industrial and Fine chemicals OthersNote: Residues include pesticides, antibiotics, toxins, and contaminants as PAH, PCB, VOC etc.

6.33. Gem & semi-precious stones Gem & semi-precious stones Precious metals Gold Silver Platinum Miscellaneous6.34. Bituminous products Bitumen Asphalt Coal tars 6.35Toys Plastic toys Soft toys Wooden toys Metal toys6.36Ceramics Glass Porcelain Tiles

7REFERENCES

ISO/ IEC 17025: 2005 General Requirements for the Competence of Testing and Calibration Laboratories

ISO Guide 30 Terms and Definitions used in connection with reference materials.

Guide to the Expression of Uncertainty in Measurement, 1st Ed.,(1995), ISO/BIPM/IEC/IFCC/IUPAC/IUPAP/OIML

ILAC-G9:2005 "Guidelines for the Selection and Use of Reference Materials"

VIM 1993 - Ref B6

ISO 78-2:1982, Layout for Standards part 2: Standards for chemical Analysis

Eurachem Guide: The Fitness for Purpose of Analytical Methods A Laboratory Guide to Method Validation and Related Topics (1998) Annexure AScope of accreditation

Sl no Group of products, materials or items testedSpecific tests or types of tests performedSpecification, standard (method) or technique usedRange of testing/ Limit of detection / quantificationMU( )This column is for explanation onlyand not part of format

1. Pollution and Environment

This is group 6.25 in section-6

EffluentsThis is sub group in 6.25

Alkalinity as HCO3APHA-21st Ed. 2005- 2320 BIS 3025 (P-23) 1986 R1998 Amnd.15-600mg/L

6 + 0.2 mg/l

553.7+ 8.8 mg/lThis is correct way of writing. For each specific test if laboratory uses different methods than it should write each method for which it wants accreditation and describe range of testing/ LOQ and MU for each method if its different. The complete details of test methods including year/edition and amendments needs to be written

Residual ChlorineAPHA-21st Ed. 2005- 4500-Cl:B Iodometric method

APHA-21st Ed. 2005- 4500-Cl:GDPD Colorimetric method

>1 mg/l

0.1-2 mg/l1.2+ 0.1 mg/l

0.2+ 0.02 mg/l

Ambient Air /Work Zone /Fugitive Monitoring

Sulphur dioxide

IS: 5182 (Pt-2) 20015-1050 g/m3Clubbing of sub group here is wrong as the test method IS: 5182 are for ambient air and not for work zone and fugitive monitoring.

Ambient AirPM 2.5Manufacturers manual and Draft CPCB Guidelines- (Lab/SOP/ AIR /06)1-300 g/m3This is correct

SludgeNi in LeachateIS 3025 : Part 54 : 2003 or APHA 21st Ed.2005 (Leachate preparation by LATS/9/2008-09)

0.1 -3 mg/kg1.1 0.08This is correct

WastewaterPAHAPHA, 21stEd.6440B

0.1 mg/lPAH, PCB or VOC represent a group of compounds. Methods as referred here are for detection of multiple compounds. The laboratory should specify which individual compounds it can detect, if it cannot detect all compounds as given in method referred and does not have CRM for that particular compound

Poly Chlorinated Biphenyls (PCB)Annex. M of IS:13428(GC-ECD)

0.01 mg/l

Volatile Organic Compounds (VOC)

APHA, 21st Ed.

0.01mg/l

2. Textile and Textile Auxiliaries

This is group 6.28 in section-6

- Fibre & Filaments- Yarns & Chords,- Fabrics, Garments and made-ups- Auxiliaries- Technical textile (Geo-Textiles, Medical Textiles, Automotive Textiles)

Solvent Extractable MatterIS:4390-2001,(RA-07)

0.1-10%These are sub groups in 6.28.

If the same test method is applicable to different test items, these items can be clubbed together.

3. Agricultural Products

Fruits and vegetables

Pesticide residues4-Bromo-2-chlorophenol,Aldrin,Chlordane,

GC-MS0.0001 mg/lIt is not correct to just write instrument name used for analysis

Pesticide residuesAldrin,Chlordane,Cyfluthrin, Cypermethrin

Laboratory Validated Methods (Number and date) Based on AOAC and International Standards & QuEchers using GC-MS(Lab/SOP/Residue/Fruit & Vegetables/06) 0.0001 mg/kg (for solid matrix) and mg/L for liquid matrix) This is correct .Lab to specify the product

8..Synthetic Drugs likeAlkylating AgentsClarity and Colour of solution

IP.2007/BP.2010/USP-32.2009QualitativeThis is correct

Pharmaceutical Raw materials (i) Identification (ii) ImpuritiesIP.2007/BP.2010/USP-32.2009QualitativeItems (like paracetamol) to be specified with specific tests such as identification, impurities

Annexure - B

EQUIPMENT CALIBRATION INTERVALS

Laboratory equipment calibration and check programs should cover:

a) Commissioning of new equipment (including initial calibration and checks after installation);

b) Operational checking (checking during use with reference standards or reference materials);

c)Intermediate checks

d) Scheduled maintenance by in-house or specialist contractors;

e) Complete recalibration.

Some items of equipment, such as balances, require rechecking if they are moved and recalibration if they are repaired.

For in house calibrations, by laboratory staff, the laboratory shall be suitably equipped with appropriate calibration procedures (along with the applicable measurement of uncertainty) and the staff shall demonstrate its competence to perform in house calibrations.

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.

CALIBRATION APPENDIX A: CALIBRATION OF COMMON TEST EQUIPMENT

.

The guidelines detailed below are provided as a reference to benefit laboratories and their users and the laboratory can demonstrate the reasons for not following the same.

S.No.Type of Equipment/Instrument/ Calibration ItemRecommended Frequency of Calibration Intermediate ChecksRemarks

1.BALANCES

Every years or on repair ;

(a) Each weighing do Zero check(b) One Month- One point check using a calibrated weight close to working capacity (c) Six months- Repeatability checks at the upper and lower ends of the scale using a calibrated weightReference weights to be used should be standard class F2 or better with established permissible errors.

2WEIGHTS

Weights have to be calibrated externally by an accredited laboratory, at least once in two years. --

3.Temperature Controlled Enclosures/ Thermostatically ControlledEquipment as Ovens, Incubators, Aging, Vacuum; ; Environmental Conditioning chambers; Preferably from an accredited calibration laboratory.

Six monthly temperature check around working range

Maintain parameters to an accuracy of within a range as stipulated in methods.

Temperature Controlled enclosure

Autoclave, Temp controlled waterbath, furnancesTo be carried out based on usage

4.

Thermometers (Liquid in glass)Calibration from accredited laboratory. Once a year Check at ice point or at points of use.Ice point. If outside five times theuncertainty of the calibration,complete recalibration is required.

5rRTD, PRT, Thermocouple with indicatorEvery year, across working range or at points of use from an accredited calibration laboratory.

6.TIMING DEVICESStop watches, clock, Every Year

7. HygrometerCalibration by an accredited calibration laboratory

8.Pressure GaugeCalibration by an accredited calibration laboratory

10.Volumetric labware (Burette, Pipette and Volumetric flask)*Internal calibration on receipt.It should be verified that the tolerance is in desired acceptable limit (Class A & Class B glasswares)

12.Flow Rota metersInitial and recalibration after two years from an accredited calibration laboratory Once a year against standard soap bubble meter

Dry Gas MeterInitial and recalibration after three years from an accredited calibration laboratory

Pitot tubeInitial and recalibration after three years from an accredited calibration laboratory

Orifice PlateInitial calibration from an accredited calibration laboratory

13.Gas sensorsInitial, recalibration after two years Using standard gases.

14.UV-Visible / IR / FT-IRSpectrophotometer/ Colorimeter

Quarterly-PhotometricAbsorbance and wavelength accuracy for the working range

Using CRM

15Atomic AbsorptionSpectrophotometerPerformance check by f Cu CRM as per manufacturers instruction.When used, Standard solution ofspecific elementGenerally the performance check is done against the initial value checked at the time of installation.

16Conductivity MeterOnce a year, Full range calibration with CRMMonthly, Reference standard, One point calibration. Adjust cell constant if necessary.When used, Standard solution

17GasChromatograph, GC-MS/HPLC / LC-MSQuarterly, Systemperformanceincluding:Resolution,sensitivity,repeatability,retention timeand noise levelWhen used, Standard solution / mixture

18pH MeterOnce a year, Full range calibration with CRM To be checked with working standard before use.

19MicropipettesOnce a year internal calibration

Note 1: the staff should be trained to handle the lab ware appropriately, to avoid abuse (avoid overheating and use of corrosive solutions and ensure appropriate cleaning) of the volumetric labwares, so as to ensure the validity of calibration through its life. Note 2; For instruments/ equipments not covered above, the following guidance documents may be followed; a. ISO/IEC 17025 Field Application Document Chemical Testing, NATAb. Specific criteria chemical testing-International Accreditation, New Zealand; c. Technical Notes C&B 002 Quality Assurance of Equipment Commonly Used in Chemical and Biological Testing Laboratories SAC Accreditation Programmed. Manufacturers instruction manual. Note 3 ; The calibration history for each instrument must be recorded. Note 4 ; Calibrations using 2 or 3 points (and zero) must adequately cover the range. One point must be between 75% and 90% of full scale.

CALIBRATION APPENDIX B --: CALIBRATION OF INSTRUMENTATION (COMPARATIVE TECHNIQUES)

The following general principles apply to the major analytical instruments used in the laboratory that are calibrated primarily in-house by use of reference materials of known composition.

a) Sufficient and appropriate reference materials* must be used to calibrate instruments over the full analytical range required to establish the measurement characteristics of the instrument (linearity, sensitivity, etc).

b) Stability of measurement must be assessed with reference materials to establish the required frequency of calibration.

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

d) Limits of detection must be established if the instrument is to be used at concentrations approaching the limit of detection.

e) Operating parameters as set in manufacturers instructions and maintenance schedules must be available and details of critical checks must be recorded.

Note*: For use of appropriate reference material, guidance provided in ILAC-G9:2005 "Guidelines for the Selection and Use of Reference Materials" may be referred.

.

Note: This annexure may be treated as a guideline and not as NABL requirement.

National Accreditation Board for Testing and Calibration LaboratoriesSecretariat: Plot No. 45, Sector-44,Near HUDA City Centre,Gurgaon-122002, HaryanaTele: 0124-4679700 (30 lines)Fax: 0124-4679799Website: www.nabl-india.org

National Accreditation Board for Testing and Calibration Laboratories

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

Issue No: xxIssue Date: -Last Amend No: 00Amend Date: --Page No: 47 / 46