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NABL 103

National Accreditation Board for Testing and Calibration Laboratories (NABL)

Specific Criteria for Chemical Testing Laboratories

ISSUE NO. : 04 ISSUE DATE : 25-Apr-2016

AMENDMENT NO. : 01 AMENDMENT DATE : 09-Mar-2017

National Accreditation Board for Testing and Calibration Laboratories Doc. No: NABL 103 Specific Guidelines for Chemical Testing Laboratories

Issue No: 04 Issue Date: 25-Apr-2016 Amend No: 01 Amend Date: 09-Mar-2017 Page No: 1/53

AMENDMENT SHEET

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Page No.

Clause No.

Date of Amendment

Amendment Reasons Signature QM

Signature Director

1 11/53 5.2.5 09.03.2017 Quality Manager qualification

Uniformity with other discipline

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3

4

5

6

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8

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ABBREVIATIONS

AOAC : Association of Official Analytical Chemists

APHA : American Public Health Association

APLAC : Asia Pacific Laboratory Accreditation Cooperation

AS : American Standard

ASTM : American Society for Testing and Materials

BIS : Bureau of Indian Standards

BIPM : Bureau International des Poids et Measure (International Bureau of Weights and Measures)

BS : British Standard

CRM : Certified Reference Material

ISO : International Organization for Standardization

EA : European Cooperation for Accreditation

FTIR : Fourier Transform Infrared

GFAAS : Graphite Furnace Atomic Absorption Spectrometer

e.g. : For Example

GUM : Guide to the Expression of Uncertainty in Measurement

ICP-AES : Inductively Coupled Plasma - Atomic Emission Spectrometer

ICP-MS : Inductively Coupled Plasma – Mass Spectrometer

IEC : International Electrotechnical Committee

ILAC : International Laboratory Accreditation Cooperation

IUPAC : International Union of Pure and Applied Chemists

NABL : National Accreditation Board for Testing and Calibration Laboratories

NATA : National Association of Testing Authorities

NIST : National Institute of Standards and Technology

NMR : Nuclear Magnetic Resonance

QC : Quality Control

w.r.t. : With Respect To

NBC : National Building Code



CONTENTS

Sl Title Page

Amendment Sheet 1

Abbreviations 2

Contents 3

1. Introduction 4

2. Terms and Definitions 5

3. Scope 6

4. Management Requirements 8

5. Technical Requirements 10

6. GroupWise Codification for Chemicals Tests 29

7. References 45

Annexure – A : Scope of Accreditation 46

Annexure – B : Equipment Calibration Intervals 49

Appendix – A : Calibration of Common Test Equipment 50

Appendix – B : Calibration of Instrumentation (Comparative Techniques) 53



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 Traceability ‘Property 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 laboratory‟s accreditation certificate. A laboratory‟s 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 laboratory‟s 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.

3.4 Laboratory 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 only like instrument breakdown, unavailability of trained staff for a short

period. The subcontracting of any test, 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 clearly identify the subcontracted tests in the test reports as described

in NABL 133.

If an accreditation body allows CAB 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

subcontractor‟s report or certificate;

the subcontractor is itself accredited for the specific tests or calibrations

concerned and the results have been included in the subcontractor laboratory‟s

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 requirement of 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 5.2 Personnel 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.

Note: The technical personnel who perform chemical testing should be free from colour

blindness, evidence for which is necessary.

5.2.2 Authorized signatory should fulfill either of the following requirements:

Minimum Years of Experience

Minimum Qualifications

Two Five Ten

Degree (Engg.) / Post Graduate in Science

Same field of testing

Similar field of testing

--

Diploma (Engg.) / Graduate in Science

-- Same field of testing

Similar field of testing

ITI / Equivalent

-- -- Same field of testing

Note -

(a) Similar field may be considered when that particular subject / field of testing is

covered in at least one year of the course;

(b) Qualification with specialized field like food, civil, textile, pharma, metallurgy,

plastic, rubber etc. shall be considered eligible for groups falling under multi-

disciplines;



(c) In each case, merely requisite qualifications and experience is not sufficient to

become the Authorized signatory; the technical competence will be verified by

NABL assessment team before recommending as authorized signatory.

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 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, 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 Quality Manager shall have undertaken at least 4-day training course on requirements of

ISO/IEC 17025:2005.

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 manufacturer‟s 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.

Laboratory should ensure that it has taken necessary steps to meet the

Regulatory requirement of respective pollution control board for waste disposal.

5.4 Test Methods and Method Validation: 5.4.1 Laboratory should generally use standard methods/internationally published methods/in-

house validated methods.

5.4.2 The 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.

5.4.3 Methods 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.

5.4.4 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; Eurachem Guide for Method Validation and

Related Topics (1998) may be referred.

5.4.5 The 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 determined

Note: 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 Quantification: Limit of Quantification 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:

Quantification: 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 inter-comparison 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.

5.4.6 When 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

5.4.7 When 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 validated

5.4.8 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 Quantification

- 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

5.4.9 Kits : 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.

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

ASTM, AOAC, etc may be followed.

5.4.11 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 labeled as obsolete. The revised method must be fully

documented, and indicate under whose authority the new method was issued (signed

and dated).

5.4.12 Lab 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 discussion

Internationally 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.

5.4.14 Use 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 software‟s. 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 program 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 is 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 types of equipment

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 program 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

5.6.3.1 Laboratories shall use CRM wherever applicable.

5.6.3.2 In 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.

5.6.3.3 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 and records should be maintained.



5.6.3.4 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 Sampling and Handling of Test Items

5.7.1 Sampling may refer to following set of procedures and or activities

1. Where a sample is to be collected for analysis from outside the laboratory by

laboratory personal (may be customer‟s premises) e.g. collecting a sample of water

from customer‟s tube well or taking a sample of cement from a lot at customer‟s

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.

5.7.2 The 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.

5.7.3 Sample 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.



5.7.4 Sample registration

Laboratory shall uniquely identify and register the sample received in the laboratory to

establish audit trail.

5.7.5 Sample 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

above.

5.7.6 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.

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.

5.9 Assuring 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



5.9.1 Proficiency 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 as per the plan submitted to NABL

during the next accreditation cycle. Refer NABL 163.

5.9.2 Internal 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.

5.10 Reporting the Results

In 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 Adhesives

Starch based adhesives

Natural gums

Glues

Polymer based adhesives (Synthetic)

Physical Properties

Other

6.2 Animal Food & Feeds

Pet Foods

Rapeseed Meal

Cotton seed cake

Guar Meal

Poultry feed additives

Animal Nutrition Supplements

Oil Cake

Groundnut meal

Miscellaneous



6.3 AYUSH Products

Ayurvedic drugs

Unani Drugs

Siddha Drugs

Homeopathic Drugs

Herbal formulations

Other

6.4 Atmospheric Pollution

Ambient air

Work Environment and Indoor Air Qualitly

Stack emission

Process/Vent Emissions

Vehicle emission

Fugitive emission

Ambient Noise Levels (Excluding vibration)

Source Noise Levels (Excluding vibration) Particular Source to be specified

Meteorological Parameters

6.5 Building Material

Aggregates

Bitumens & asphalts

Bricks & pre-casted blocks

Cement

Ceramics

Concrete

Construction chemicals

Fly ash

Gypsum & its products

Lime

Mortars



Pozzolanic materials

Refractory materials

Sand

Water-proofing compounds

Other

6.6 Cosmetics & Essential Oils

Essential oils and other natural fragrant raw materials

Aromatic chemicals

Fragrances and Indian attars

Synthetic essential oils

Cosmetics and toiletries

Intermediates and miscellaneous chemicals for cosmetics

Herbal based cosmetics

Other

6.7 Corrosion tests

Salt Spray Tests

Dezincification Tests

Other

6.8 Drugs & Pharmaceuticals

Physical and Physiological Methods

Chemical Methods

Pharmaceutical Aid (Raw material except API)

Drug Substance (API)

Capsules

Creams

Ear Drops

Eye Ointment

Gels

Ointment



Oral Liquids

Oral Powders

Parenteral Preparations

Tablets

Vitamins

Harmones

Other

6.9 Explosives & Pyrotechnics

Ammunitions

Industrial explosives & associated materials

Pyrotechnics

Explosive chemicals & allied materials

Physical Properties

Other

6.10 Fertilizers

Nitrogenous Fertilizers

Phosphatic Fertlizers

Potassic Fertlizers

Fertiliser Mixtures

Micronutrients

Macrnutrients

Fortified Fertilizers

Bio-Fertilizer

Other

6.11 Fire Fighting Equipments & Accessories

Aqueous film forming foam concentates

Dry Chemical Powder

Foam Concentrates

Other



6.12 Food & Agricultural products

Bakery & confectionery products

Beverages (Alcoholic / Non-alcoholic)

Canned & processed foods

Cereals, pulses & cereal products

Coconut and coconut products/Narural Plant Derivatives/Products

Coffee & cocoa products

Edible colours & flavours

Edible oils & fats

Food additives & preservatives

Fruit & fruit products

Herbs, spices & condiments

Honey & honey products

Infant foods

Jams, juices, sauces & concentrates

Meat & meat products

Milk & dairy products

Natural waxes

Nuts & nut products

Oil seeds & by-products

Pet foods

Poultry & poultry products

Starch & starch products

Sugar & sugar products

Tea

Tobacco & tobacco products

Vegetables & vegetable products

Other



6.13 Gases

Industrial Gases

Liquefied Gases

Compressed Natural Gas (CNG)/ Piped Natural Gas (PNG)

Gases for medical use and diving

Reference Gases & Mixtures

Other

6.14 Glass

Clear glass

Tinted glass

Reflective Glass

Stain Glass

Textured or pattern glass

Laminated Glass

Wired Glass

Other

6.15 Hazardous & Restricted Chemicals

Textile & Textile products

Toys and sports equipment

Computing & communications equipment

Consumer electronics

Lighting: lamps, lighting fixtures, light bulbs

Power tools

Automatic dispensers

Small household appliances

Large household appliances

Plastics & other polymeric products

Leather products

Prints

Zippers

Paints

Other



6.16 Industrial & Fine Chemicals

Organic Chemicals

Inorganic Chemicals

Electroplating Chemicals

Chemicals used in Leather Industry

Chemical used in Rubber Industry

Chemical used in Textile Industry

Chemicals used in Electronic industry

Chemicals used in Photographic Industry

Chemicals used in Refrigeration industry

Chemicals used in Agriculture

Alcohols & Alcohols based Chemical

Disinfectants

Other

6.17 Inks, dyes & pigments

Duplicating inks

Dye intermediates

Inorganic pigment powder & pastes

Natural dyes & colouring materials

Organic pigment powder & pastes

Printing inks

Synthetic dyes

Writing inks

Other

6.18 Lac & lac products

Lac

Lac products

Other



6.19 Leather

Finished leather

Leather accessories

Leather products

Semi-finished leather

Synthetic leather

Other

6.20 Lubricants

Oils & greases

Solid lubricants

Aviation lubricants

Lubricant additives

Microcrystalline wax

Insulation oils

Other

6.21 Marine /Aqua culture Food Products

Prawn & Prawn Products

Fish& Fish Products

Shrimps

Artemia & Artemia Products

Shrimps

Oyester

Molecular identification of bacterial, fungal, viral pathogens

Crab & Crab Products

Other

6.22 Metallic coatings & treatment solutions

Anodising solutions

Conversion coatings

Metal finishing materials

Metallic coatings

Plating solutions

Others



6.23 Metals & Alloys

Ferro-alloys

Carbon Steel (low carbon, medium carbon & high carbon steel)

Alloy steel

Stainless steel

Tool steel

Special Steel

Copper & its alloys

Aluminium & its alloys

Tin and tin alloys

Zinc & inc alloys

Lead & lead alloys

Magnesium & its alloys

Nickel & its alloys

Chromium & its alloys

Cobalt & its alloys

Titanium & titanium alloys

Tungsten & its alloys

Other metal alloys

Precious metals

Rare earth alloys

Amalgam

Others

6.24 Nutraceuticals & Functional Foods

Probiotics

Dietary Fibres

Carotenoids

Flavonoids

Prebiotics

Soy Proteins

Fortified Food

Phytoestrogens

Others



6.25 Ores & Minerals

Iron ores

Copper ores

Zinc ores

Nickel ores

Manganese ores

Tin ores

Lead ores

Titanium ores

Molybdenum ores

Tungsten ores

Chromium ores

Precious metals ores

Rare metals ores

Radio active metals ores

Aluminium Ores

Barium ore

Cobalt ore

Mercury ore

Alkali Metal Ores

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

Mercury



6.26 Paints & Surface Coating

Drying oils

Gums, driers & paint removers

Paints & enamels

Pigments & extenders

Polishes

Powder coatings

Resin coatings

Solvents & thinners

Varnishes

Physical Properties

Others

6.27 Paper and Pulp

Paper

Paper board

Pulp

Pulpwood

Newsprint and board packing material

Composite packing material

Others

6.28 Pesticide Formulations

Technical Concentrates(TK)

Dustable Powders(DP)

Powders for Dry Seed Treatment(DS)

Granules(GR)

Tablets for Direct Application(DT)

Wettable Powders (WP)

Water Dispersible Powders for Slurry Seed Treatment(WS)

Water Dispersible Granules(WG)

Water Dispersible Tablets(WT)



Emulsifiable Granules(EG)

Emulsifiable Powders (EP)

Water Soluble Poweders (SP)

Water Soluble Poweders for Seed Treatment (SS)

Water Soluble Granules (SG)

Water Soluble tablets( ST)

Soluble Concentrates(SL)

Solutions for Seed treatment(LS)

Oil Miscible Liquids(OL)

Ultra Low Volume Liquids(UL)

Emulsifiable Concentrates(EC)

Dispersible Concentrates(DC)

Emulsions,Oil in Water(EW)

Emulsions for Seed Treatment(ES)

Micro- Emulsions (ME)

Aqueous Suspension Concentrates(SC)

Suspension Concentrates for Seed Treatment(FS)

Aqueous Capsule Suspensions (CS)

Oil based Suspension Concentrates(OD)(Oil Dispersion)

Aqueous Suspo-Emulsions(SE)

Mixed Formulations of CS and SC(ZC)

Mixed Formulations of CS and EW(ZW)

Mixed Formulations of CS and EW(ZW)

Mosquito Coils (MC)

Vaporizing Mats(MV)

Liquid Vaporizers(LV)

Long lasting insecticidal NETS or NETTING(LN)

Others

6.29 Petroleum and Products

Crude petroleum

Petroleum products

Petrochemicals, Petroleum solvents



Liquefied / compressed gases

Aviation fuels

Waxes and jellies

Petroleum additives

Petroleum feed stocks

Others

6.30 Plastic & Resins

Resin

Plastics & polymers

Raw materials

Plastic films

6.31 Pollution & Environment

Waste Water (Effluents/Sewage)

Municipal Solid wastes

Wastes (Liquid/Slurry/Sludge/Solid/Semi-Solid)

Soil/Sediments

Used/Waste oil

Effluents toxicity (Bioassay only qualitative- 90% survival of fish after 96 hours in 100

percent effluent)

Others

6.32 Residues in Food Products

Antibiotics

Pesticides

Mycotoxins

Trace metal elements

Chlorinated dioxins & dibenzofurans

Halogenated hydrocarbons

Phenols

Polycyclic aromatic hydrocarbons



Polyhalogenated biphenyls

Others

Poly Chlorinated Biphenyl

Others

6.33 Residues in Water

Antibiotics

Pesticides

Mycotoxins

Trace metal elements

Chlorinated dioxins & dibenzofurans

Halogenated hydrocarbons

Phenols

Polycyclic aromatic hydrocarbons

Polyhalogenated biphenyls

Others

Poly Chlorinated Biphenyl

Others

6.34 Rubber & Rubber Products

Natural rubber

Synthetic rubber

Rubber compound

Rubber vulcanizates

Rubber Products

Thermoplastic elastomers

Hard rubber / ebonite Rubber

Natural / synthetic Latex

Latex goods

Textile rubber composite

Others



6.35 Soap detergent & Toiletries

Soaps

Detergent

Wetting & Emulsifying agent

Others

6.36 Soil and Rock

Clays & Soils

Stones

Others

6.37 Solid Fuels

Coal

Coke

Charcoal

Briquettes

Oil Shale

Coal tar/Bitumen

Others

6.38 Textile (Woven & Non woven)

Fibre & filaments

Yarns & chords

Grey Fabrics

Finished fabric

Apparels/Garments

Made-ups

Carpet & rugs

Terry Fabrics & its products

Technical textiles

Geo-textiles



Medical textile

Automotive textiles

Protective Textiles

Sports textiles

Packaging textiles

Industrial Textiles

Domestic Textiles

Agro-textiles

Others

6.39 Warfare Chemicals

Choking Agents

Blister Agents

Blood Agents

Nerve Agents

Riot Control Agents

Potential CW Agents

Mustard Agents

Psychotomimetic Agents

Toxins

Others

6.40 Water

Surface Water

Ground Water

Drinking Water

Packaged Drinking water

Construction Water

Swimming Pool Water

Industrial Water

Industrial water

Irrigation water

Water from purifiers

Others



7 REFERENCES

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.

ISO/IEC Guide 98-3:2008 Uncertainty of measurement -- Part 3: Guide to the expression of uncertainty in measurement (GUM:1995)

ISO/IEC Guide 99:2007

ISO 78-2:1999, 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)

http://www.iso.org/iso/home/store/catalogue_ics/catalogue_detail_ics.htm?csnumber=45324



Annexure – A Scope of accreditation

Sl no

Group of products, materials or items tested

Specific tests or types of tests performed

Specification, standard (method) or technique used

Range of testing/ Limit of detection / quantification

MU

( )

This column is for explanation only and not part of format

1. Pollution and Environment

This is group 6.25 in section-6

Effluents This is sub group in 6.25

Alkalinity as HCO3

APHA-21st Ed.

2005- 2320 B IS 3025 (P-23) 1986 R1998 Amnd.1

5-600mg/L

6 + 0.2 mg/l 553.7+ 8.8 mg/l

This 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 it‟s different. The complete details of test methods including year/edition and amendments needs to be written

Residual Chlorine

APHA-21st Ed.

2005- 4500-Cl:B Iodometric method APHA-21

st Ed.

2005- 4500-Cl:G DPD Colorimetric method

>1 mg/l 0.1-2 mg/l

1.2+ 0.1 mg/l 0.2+ 0.02 mg/l

Ambient Air / Work Zone / Fugitive Monitoring

Sulphur dioxide

IS: 5182 (Pt-2) 2001

5-1050 µg/m

3

Clubbing 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 Air PM 2.5 Manufacturer‟s manual and Draft CPCB Guidelines- (Lab/SOP/ AIR /06)

1-300 µg/m

3

This is correct

Sludge Ni in Leachate

IS 3025 : Part 54 : 2003 or APHA 21

st

Ed.2005 (Leachate preparation by LATS/9/2008-09)

0.1 -3 mg/kg

1.1 0.08 This is correct



Wastewater PAH APHA, 21stEd.6440B

0.1 mg/l PAH, 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 Matter

IS: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 residues 4-Bromo-2-chlorophenol, Aldrin, Chlordane,

GC-MS 0.0001 mg/l It is not correct to just write instrument name used for analysis

Pesticide residues Aldrin, Chlordane, Cyfluthrin, Cypermethrin

Laboratory Validated Methods (Number and date) Based on AOAC and International Standards & QuEchers using GC-MS (Lab/SOP/Resi

0.0001 mg/kg (for solid matrix) and mg/L for liquid matrix)

This is correct .Lab to specify the product



due/Fruit & Vegetables/06)

8.. Synthetic Drugs like Alkylating Agents

Clarity and Colour of solution

IP.2007/BP.2010/USP-32.2009

Qualitative This is correct

Pharmaceutical Raw materials

(i) Identification (ii) Impurities

IP.2007/BP.2010/USP-32.2009

Qualitative Items (like paracetamol) to be specified with specific tests such as identification, impurities

/drugindex/category/idx-drugcateg_alkylating-agents.html

/drugindex/category/idx-drugcateg_alkylating-agents.html



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.

Sl. Type of Equipment / Instrument / Calibration Item

Recommended Frequency of Calibration

Intermediate Checks Remarks

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 weight

Reference weights to be used should be standard class F2 or better with established permissible errors.

2 WEIGHTS

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

- -

3. Temperature Controlled Enclosures/ Thermostatically Controlled Equipment 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, furnances

To 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 the uncertainty of the calibration, complete recalibration is required.

5 rRTD, PRT, Thermocouple with indicator

Every year, across working range or at points of use from an accredited calibration laboratory.

6. TIMING DEVICES Stop watches, clock,

Every Year



7. Hygrometer Calibration by an accredited calibration laboratory

8. Pressure Gauge Calibration 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 meters

Initial and recalibration after two years from an accredited calibration laboratory

Once a year against standard soap bubble meter

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

Pitot tube Initial and recalibration after three years from an accredited calibration laboratory

Orifice Plate Initial calibration from an accredited calibration laboratory

13. Gas sensors Initial, recalibration after two years

Using standard gases.

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

Quarterly-Photometric Absorbance and wavelength accuracy for the working range

Using CRM

15 Atomic Absorption Spectrophotometer

Performance check by f Cu CRM as per manufacturer‟s instruction.

When used, Standard solution of specific element

Generally the performance check is done against the initial value checked at the time of installation.



16 Conductivity Meter Once a year, Full range calibration with CRM

Monthly, Reference standard, One point calibration. Adjust cell constant if necessary. When used, Standard solution

17 Gas Chromatograph, GC-MS/HPLC / LC-MS

Quarterly, System performance including: Resolution, sensitivity, repeatability, retention time and noise level

When used, Standard solution / mixture

18 pH Meter Once a year, Full range calibration with CRM

To be checked with working standard before use.

19 Micropipettes Once 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, NATA b. 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 Program d. Manufacturer‟s 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 manufacturer‟s instructions and maintenance schedules

must be available and details of critical checks must be recorded.

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

National Accreditation Board for Testing and Calibration Laboratories (NABL) NABL House

Plot No. 45, Sector 44,

Gurgaon - 122002, Haryana

Tel. no.: 91-124-4679700 (30 lines)

Fax: 91-124-4679799

Website: www.nabl-india.org

http://www.nabl-india.org/

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