What is What is QUALITYQUALITY??

QUALITYQUALITY is “the degree to which a set of inherent is “the degree to which a set of inherent characteristics fulfils requirements” characteristics fulfils requirements”

[ISO 9000-2000].[ISO 9000-2000].

In analytical work, In analytical work, QUALITY QUALITY can be defined as can be defined as “delivery of reliable information within an agreed “delivery of reliable information within an agreed spare of time and under agreed conditions, at spare of time and under agreed conditions, at agreed costs and with necessary aftercare”.agreed costs and with necessary aftercare”.

ToTo achieve achieve QualityQuality and optimal performanceand optimal performance it is it is necessary to develop and put in practicenecessary to develop and put in practice the the concepts of:concepts of:

QUALITY MANAGEMENTQUALITY MANAGEMENT

QUALITY ASSURANCEQUALITY ASSURANCE

QUALITY CONTROLQUALITY CONTROL

QUALITY MANAGEMENTQUALITY MANAGEMENT (QM)(QM) represents represents “the coordinated activities to direct and control “the coordinated activities to direct and control an organization with regard to qualityan organization with regard to quality”.”. [ISO 9000-2000].[ISO 9000-2000].

In testing laboratories, QM means:In testing laboratories, QM means:

creating a good structure;creating a good structure;

providing support for developing;providing support for developing;

validating methodologies;validating methodologies;

verifying performance.verifying performance.

QUALITY MANAGEMENT SYSTEMQUALITY MANAGEMENT SYSTEM (QMS) (QMS) is “the management system to directis “the management system to direct and and control an organization with regard to control an organization with regard to quality” [ISO 9000-2000].quality” [ISO 9000-2000].

QMS includesQMS includes::

organizatoric structure;organizatoric structure;

procedures / processes;procedures / processes;

resources necessary for resources necessary for

implementation of QM.implementation of QM.

QUALITY ASSURANCEQUALITY ASSURANCE (QA) (QA) isis “part of the “part of the QM focused on providing confidence that QM focused on providing confidence that quality requirements will be fulfilled”quality requirements will be fulfilled” [ISO 9000-2000].[ISO 9000-2000].

QA implies that the organization of the QA implies that the organization of the activities and the conditions under which activities and the conditions under which this takes place are:this takes place are:

controlled;controlled;

reported;reported;

filed.filed.

In short, QA means:In short, QA means:

SAY WHAT YOU DO SAY WHAT YOU DO DO WHAT YOU SAY DO WHAT YOU SAY DO IT BETTER DO IT BETTER BE ABLE TO SHOW WHAT YOU HAVE BE ABLE TO SHOW WHAT YOU HAVE DONE DONE

QA implementation conduct to:QA implementation conduct to:

better laboratory management; better laboratory management; improve efficiency; improve efficiency; minimize errors; minimize errors; stimulate and motivate personnel; stimulate and motivate personnel; improve reputation of the laboratory. improve reputation of the laboratory.

QUALITY CONTROLQUALITY CONTROL (QC) (QC) is a “major part is a “major part of QM, focused on fulfilling quality of QM, focused on fulfilling quality requirements” [ISO 9000-2000].requirements” [ISO 9000-2000].

For analytical activity, For analytical activity, QCQC represents: “a represents: “a set of procedures undertaken by the set of procedures undertaken by the laboratory for continuous monitoring of laboratory for continuous monitoring of operations and results in order to decide operations and results in order to decide whether the results are reliable enough to whether the results are reliable enough to be realized”.be realized”.

QC is divided into three levels:QC is divided into three levels:

1. 1. first level of control (internal control):first level of control (internal control): realized by the analyst; realized by the analyst;

2. 2. second level of control (internal control):second level of control (internal control): realized by the QA Manager/Head of realized by the QA Manager/Head of Laboratory; Laboratory;

3. 3. third level of control (external control):third level of control (external control): interlaboratory proficiency testing interlaboratory proficiency testing

Third LevelLaboratory

performance study

Third LevelLaboratory

performance study

QC sampleQC sample

Sample data

Sample data

Second levelCheck samples given

by Qality manager

Second levelCheck samples given

by Qality manager

Quality ControlQuality Control

Data QC samplesData QC samples

Quality assesment

Quality assesment

Measurement process

Measurement process

Accept/use data

Accept/use data

SpecificationSpecification

SampleSample

The main QMS elements areThe main QMS elements are::

Quality policy;Quality policy;

Quality objectives;Quality objectives;

Quality Manual;Quality Manual;

Procedures, instructions;Procedures, instructions;

RecordsRecords..

Function of their importance, they have aFunction of their importance, they have a

pyramidal structure.pyramidal structure.

QUALITY STANDARD

RECORDS

PROCEDURESINSTRUCTIONS

QUALITY POLICYQUALITY

OBJECTIVES

QUALITY MANUAL

QUALITY POLICYQUALITY POLICY attest the intentions and attest the intentions and direction for maintaining a high level of quality in the direction for maintaining a high level of quality in the activity of the laboratory.activity of the laboratory.

QUALITY POLICY QUALITY POLICY is established by the highest is established by the highest level of authority from the laboratory.level of authority from the laboratory.

QUALITY POLICY QUALITY POLICY must be written down and must be written down and familiar to all personnel from the laboratory.familiar to all personnel from the laboratory.

QUALITY OBJECTIVES ARE BASED ON:QUALITY OBJECTIVES ARE BASED ON:

particular laboratory priorities and particular laboratory priorities and field of interest; field of interest;

results of audits; results of audits;

customer complaints; customer complaints;

requirements of regulatory or requirements of regulatory or accreditation body. accreditation body.

QUALITY OBJECTIVES SHOULD BE:QUALITY OBJECTIVES SHOULD BE:

quantified in so far as possible quantified in so far as possible (numerical values, target dates); (numerical values, target dates);

attainable and very clear defined attainable and very clear defined

THE MAIN QUALITY OBJESTIVES IN A TEST LABORATORY ARE:

- To maximize the quality of the data by improving precision and accuracy;

- To ensure that all personnel is trained at high level of technology;

- To make changes in the routine methodology in order to respond to the performance needs;

- To achieve and maintain consistent, uniform levels of quality.

QUALITY MANUAL is the “document specifying the QMS of the organization”[ISO 9000-2000].

The QUALITY MANUAL includes:

a short presentation of the Laboratory and of the Company;

the Quality Policy;

the responsibilities and authorities of the personnel;

the procedures of QMS or a short presentation of them;

a specification concerning elaboration, beginning ,up to date and

control of the Manual;

The QUALITY MANUAL is elaborated by the Manager of the Laboratory and the Quality Manager.

PROCEDURES are “specified ways to carry out an activity or process” [ISO 9000-2000].

Types of procedures function of the activities described:

general or fundamental procedures – how to

elaborate procedures;

system procedures – for the management and the

technical requirements from ISO 17025 standard;

standard operating procedures – for testing

methods

PROCEDURES MUST CONTAIN A MINIMUM NUMBER OF REQUIREMENTS:

ON EACH PAGE TO BE MENTIONED:

- the complete title;

- the code and number of the procedure;

- the version and revision number;

- number of copies;

- page number and the total number of

pages.

PROCEDURES MUST CONTAIN A MINIMUM NUMBER OF REQUIREMENTS:

THE FIRST PAGE SHOULD CONTAIN:

- general information mentioned above;

- name and signature of author, including date

of signing ;

- name and signature of person who

authorized the implementation of the

procedure.

PROCEDURES MUST CONTAIN A MINIMUM NUMBER OF REQUIREMENTS:

THE CONTENT MUST INCLUDE:

- purpose and field of application;

- list of references;

- a clear description of the activity;

- responsibilities for achieving the

activities.

RECORDS represent the objectives proofs for the laboratory clients, accreditation body and regulatory authorities concerning the quality of the analytical activity of the laboratory.

Records are the basic elements of the QMS;

Records are produced every day;

Records must be kept in order and good conditions to

prevent damage, loss or change of original data.

QMS for environmental laboratories (I):

ISO/IEC 17025ISO/IEC 17025 General requirements for General requirements for

competence of testing and competence of testing and calibration laboratoriescalibration laboratories

ISO 9001ISO 9001 Quality Management System Quality Management System

requirementsrequirements

ISO 14001ISO 14001 Environmental Management Environmental Management

Systems. Specification with Systems. Specification with guidance for use guidance for use

For first, second and third party For first, second and third party laboratories which perform laboratories which perform tests, including samplingtests, including sampling

For laboratories which conduct For laboratories which conduct

research and development research and development activities activities

For laboratories which perform For laboratories which perform monitoring of the environment monitoring of the environment

QMS for environmental laboratories (II):

Function of the activity an environmental laboratory can implement integrated QMS: ISO 9001 – ISO 17025 ISO 17025 – ISO 14001 ISO 9001 – ISO 17025 – ISO 14001

Management responsability

Measurement,analysis and improvement

Product realisation

Resource management

ISO 9001

Personnel

Management and Organization

Quality System(politics,objectives,documentat

ion)

Managementrewiews

Accomodation and

environmental conditions

Sub-contracting ot tests

Purchasing services and

supplies

Test and method

validation

Equipment

Handeling of test items

Rewiew of requests, tender and contracts

Sampling

ISO 17025

Services to the clients

Complaints

Control of nonconforming

testsCorrective and

preventive actions

Traceability

Assuring Qualityof tests

Internal Audit

Document controlControl of records

Reporting results

Procedures in the integrated quality system ISO 9001-ISO 17025

ACCREDITATION ISO 17025 offers:

Independent assessment of quality

management system and technical

competence of the laboratory.

Confirm or recognize the competence of

the laboratory towards :

- clients;

- regulatory authorities;

-accreditation bodies.

ACCREDITATION ISO 17025 process is

voluntary;

ACCREDITATION ISO 17025 is realized by

the National Accreditation Body;

REACCREDITATION at 2-5 years.

ACCREDITATION ISO 17025

Requirements for accreditation ISO 17025:

to respond to the 14 management requirements;

to respond to the 10 technical requirements.

MANAGEMENT REQUIREMENTS

4.1 ORGANIZATION (I)

Laboratory must:

be entity legally responsible;

satisfy the needs of the client, regulatory authorities or accreditation body;

identify potential conflicts of interest (if laboratory is part of an organization);

be able to demonstrate the impartiality and that the personnel is free from commercial, financial or other pressures which might influence their technical judgment;

have an organigram in which to define the organization, structure and management

ORGANIZATION (II):

have sufficient qualified staff for all the activities (professional requirements described in the Job Description);

have technical management with responsibilities for technical activities and of provisions of the resources needed to ensure the required quality;

have a quality manager;

have deputies for key managerial personnel.

4.2 QUALITY SISTEM

For implementing and maintaining the QMS the laboratory must have:

Quality policy statement

- commitment to good professional practice and to quality

of the test services;

- commitment to compliance with the standard;

- objectives of the quality system;

- commitment that all personnel concerned with testing

activity will know and implement the policies and

procedures in their work.

Quality Manual

4.3 DOCUMENT CONTROL (I)

Document is “written down or digital information, which define, describe or report an activity, procedure, result”.

[ISO 9000-2000]

Laboratory must maintain full control over the:

evaluation of documents – drafting;

- verifying;

- authorizing.

distribution of documents;

possession and/or changing of documents;

destroying and archiving of documents.

DOCUMENT CONTROL (II)

Quality Documents can be:

DOCUMENTS

INTERNALLY GENERATED

EXTERNAL SOURCES

Quality Manual;

Procedures;

Instructions;

Quality policy and objectives.

Quality Manual;

Procedures;

Instructions;

Quality policy and objectives.

Standards;

Books, manuals;

Norms, regulations;

Technical specification.

Standards;

Books, manuals;

Norms, regulations;

Technical specification.

DOCUMENT CONTROL (III)

Documents generated by the laboratory should be:

uniquely identified by :

- a code/number;

- date of issue;

- date of revision;

- page numbering;

- the issuing authority.

periodically reviewed /revised;

destroyed when are out of use to avoid unintended

use;

original with all accompanying change notice

retained as historical file.

4.4 REVIEW OF REQUESTS, TENDERS AND

CONTRACTS (I)

Before doing a contract, laboratory must proof that:

it posses the skilled personnel for the performance of the

tests in question;

the financial, legal and time schedule aspects were taken

into account;

methods to be used are adequately defined, documented

and capable of meeting the clients requirements.

REVIEW OF REQUESTS, TENDERS AND CONTRACTS (II):

The contract, or the agreement between the client and the laboratory shall be:

signed by both partners;

any deviations announced to the client.

4.5 SUBCONTRACTING OF TESTS

Temporary subcontracting activity - workload;

- temporary incapacity;

- need for further expertise.

Permanent subcontracting activity

Selection of subcontracting laboratories by:

- audit;

- certificate of accreditation.

Maintain a register with all subcontractors;

Laboratory is responsible to the client for subcontractor’s work.

4.6 PURCHASING SERVICES AND SUPPLIES (I)

Procedures for purchasing and storage of:

- reagents;

- equipment;

- consumable materials;

- services.

Purchase order must contain:

- complete name of the product/service;

- quantity;

- quality specification.

Purchase documents, like purchase order, receiving documents, accompanying certificate are used for identification of the material received.

PURCHASING SERVICES AND SUPPLIES (II)

Inspection of the purchase services and supplies before being used;

Records of actions taken;

Evaluation of suppliers and maintaining records of these evaluations.

4.7 SERVICE TO THE CLIENT

Co-operation with clients:

- providing the client access to relevant areas of the

laboratory for the witnessing of tests performed for the

clients;

- preparation, packaging and dispatch of test items needed

by the client for verification purposes;

- technical advices and interpretation based on results.

Information of the client of any major deviations and

delays.

Feedback (positive and negative) from the client.

4.8 COMPLAINTS

Received from clients, regulatory or accreditation bodies.

Steps for solving a complaint:

- preliminary investigation to determine the nature and

validity of the complaint;

- solving the problem which generated the complaint;

- initiating a request for corrective actions, if necessary;

- report to manager about the status of the complaint.

Records of complaints, of investigations and corrective

actions taken

4.9 CONTROL OF NONCONFORMING TESTING WORK (I)

Nonconformity may occur :

Within the Quality System:

- internal or external audits;

- customer complaints;

- staff observations;

- management review.

Within technical operation:

- instrument calibration;

- data validation;

- test report checking.

4.9 CONTROL OF NONCONFORMING TESTING WORK (II)

Procedure must include:

- reporting and recording the occurrence of a

nonconforming event ;

- suspension of work and commencement of an

investigation ;

- report to the customer;

- repetition of the test;

- initiation of corrective action.

4.12 CONTROL OF RECORDS (I)

Records are “written objective proofs concerning the activities performed and the results” [ISO 9000-2000].

Records can be classified as:

RECORDS

QUALITY RECORDS

TECHNICAL RECORDS

- Report of audit;- Report of nonconforming activities;- Report of corrective/preventive actions;- Training report;- Management review report.

- Report of audit;- Report of nonconforming activities;- Report of corrective/preventive actions;- Training report;- Management review report.

- Test reports;- Laboratory notebooks;- Cheek sheets;- Work notes;- Control charts;- Calibrations certifications.

- Test reports;- Laboratory notebooks;- Cheek sheets;- Work notes;- Control charts;- Calibrations certifications.

RECORDS

CONTROL OF RECORDS (II)

Laboratory must maintain procedure for:

- identification;

- collection;

- access;

- filling;

- storage;

- maintenance;

- disproval;

of Quality and technical records.

CONTROL OF RECORDS (III)

Records must be: - legible; - stored in proper conditions; - protected of damage, loss or degradation due to atmospheric conditions; - protected of unauthorized access.

Equivalent measures must be taken for records stored electronically for avoiding loss or change of original data.

4.10 CORRECTIVE ACTIONS

Corrective actions have “the role to eliminate the causes of a nonconformity and to prevent recurrence of the undesirable potential situation”.

Steps for implementing a corrective action:

- investigation of the root cause of the problem (possible causes:

sampling, method of analysis, staff skills, equipment, etc.);

- selection and implementation of corrective action;

- monitor the results to ensure that the corrective action was

effective.

4.17 PREVENTIVE ACTIONS

“Pro-active process of identification of potential sources of

nonconfomities either technical or concerning the Quality

System”.

Preventive actions can result from:

- market analysis;

- feed-back from clients;

- results of the management review;

- participation to interlaboratory schemes;

- participation to trainings or changes of experience.

4.13 INTERNAL AUDIT

“A systematic, independent and documented process for verifying and obtaining evidence that operations in the laboratory continue to comply with the requirements of the QMS and the referential standard”.

Carried out by trained personnel.

Planned by the QA Manager at least annually.

All the Management and Technical elements of the

QMS are checked.

Corrective actions must be taken.

4.14 MANAGEMENT REVIEWS

The executy manager shall conduct once by year a review of the QMS in which to take account of:

- corrective and preventive actions;

- the outcome of internal and external audits;

- clients feedback;

- complaints;

- results of interlaboratory proficiency tests;

- changes in the type and volume of work

Findings from the management reviews represent:

- goals;

- objectives;

- action plans;

for the next year and must be recorded.

TECHNICAL REQUIREMENTS

5.2 PERSONNEL AND TRAINING (I)

The laboratory must have sufficient qualified and experienced personnel

The laboratory must maintain current job description for managerial, technical and key support personnel involved in test activity

All information about personnel should be recorded

PERSONNEL AND TRAINING (II)

All personnel involved in any function affecting quality should have sufficient training in their appointed job

The training program may concern:

- development in analytical techniques;

- data handling;

- use of the new equipment, use of computers;

- laboratory QMS.

PERSONNEL AND TRAINING (III)

Trainings developed:

- within the laboratory;

- by outside specialist;

- centrally conducted courses, if necessary abroad.

At the end of the training:

- evaluation of the effective training;

- certificates / diplomas.

The laboratory shall maintain up-to-date records of the trainings received by the staff of the laboratory.

5.3 ACCOMODATION AND ENVIRONMENTAL

CONDITIONS (I)

Laboratories must have uncrowded, clean and tidy room divided into “chemical” and “not chemical” areas:

- room for receipt and registration of the samples;

- rooms for preliminary operation (extraction, distillation, acid

digestion, etc.):

- room for general chemical analysis;

- “clean room” for equipment;

- storage room for chemicals;

- storage room for samples (with shelves, refrigerators);

- service rooms (storage of distilled water, washing of glassware);

- rooms for administration office.

ACCOMODATION AND ENVIRONMENTAL CONDITIONS (II)

Appropriate environmental conditions: - temperature; - humidity; - freedom of vibration; - freedom of air borne and dust; - clean air.Monitoring of temperature and humidity

Admission in laboratory only for authorized persons

Visitors, inspectors must be in charge of one member of the laboratory

5.4 TEST METHODS AND METHOD VALIDATION

Appropriate methods and procedures for all test activities

Test methods must be:

- technically justified;

- authorized;

- verified for use in the laboratory.

METHOD VALIDATION (I)

Validation means “confirmation by examination and provision of objective evidence that the particular requirements for a specific intended use are fulfilled “

(ISO- 8402-94).

Verification means “ confirmation by examination and provision of objective evidence that specified requirements have been fulfilled” (ISO 8402-94).

METHOD VALIDATION (II)

Verification is applied for checking the standard

method;

Validation is applied for:

- non-standard methods;

- laboratory- designed/developed methods;

- standard methods used outside their intended scope;

- changes of standard methods

METHOD VALIDATION (III)

In validation process are established the performance

characteristics of the method:

- detection limit;

- quantification limit;

- specificity /selectivity;

- ruggedness or robustness;

- recovery;

- repeatability;

- reproducibility.

UNCERTAINTY OF MEASUREMENT (I)

Testing laboratories must implement procedures for estimating uncertainty of measurement.

Uncertainty is “the parameter associated with the result of a

measurement that characterizes the dispersion of the values that

could be reasonably attributed to the measurand ”.

Type A components – may be evaluated from statistical distribution

of the result of a series of measurements and is expressed as

standard deviations.

Type B components - may be evaluated from assumed probability

distributions based on experience or other information. Is expressed

as standard deviation.

UNCERTAINTY OF MEASUREMENT (II)

Standard Uncertainty – u (xi), is “the uncertainty of the result of a

measurement expressed as a standard deviation”.

Combined Standard Uncertainty - uc(y), is ‘the uncertainty of

the result of a measurement when the result is obtained from the

values of a number of other quantities, equal to the positive square

root of a sum of terms being the variances or co-variances of these

other quantities weighted according to how the measurement result

varies with the quantities’.

UNCERTAINTY OF MEASUREMENT (II)

Expanded Uncertainty – U=K.uc, is “the quantity

defining an interval about a result of a measurement

that may be expected to encompass a large fraction of

the distribution of the values that could reasonably be

attributed to the measurand”.

CALCULATION AND DATA TRANSFER

Nominated persons from the laboratory must check the calculations and the data transfer in a systematic manner, during they are generated

When computers are used, it is necessary to ensure that:

- software are suitable validated;

- the protection of data is established;

- computers are maintained in proper

condition.

EQUIPMENT (I)

The laboratories must be furnished with all categories of equipment, like:

- sampling equipment;

- primary measuring equipment (balances, thermometers,

flow meters, etc.);

- analytical equipment (spectrometers, chromatographs,

electrochemical meters, etc.);

- miscellaneous equipment (ovens, furnaces, stirrers, etc.);

- computers and data processors.

EQUIPMENT (II)

Records must be maintained for all equipment:

- identification list for each equipment;

- list of all available equipment;

- a Plan for Instrument Calibration / Maintenance;

- Maintenance Logbook;

- Operational Instructions Manual.

EQUIPMENT (III)

All equipment must be labeled.

On the label must be mentioned:

- the identification number, or code of the

equipment;

- the status of the calibration;

- the date when last calibration was done.

EQUIPMENT (IV)

Equipment that have been subject of:

- mishandlings;

- overloading;

- give suspect results;

- are defective or outside specified limits;

must be clearly labeled or marked and isolated to

prevent unintended use.

5.5 MEASUREMENT TRACEABILITY (I)

Traceability concerns the requirements to relate the

results of measurements to the values of reference

standards, preferably to SI.

Measurement traceability is realized by:

- calibration of equipment and glassware;

- use of reference materials.

MEASUREMENT TRACEABILITY (II)

Calibration is “the process establishing how the response of a measurement process varies with respect to the parameter being measured”.

Calibration is realized by the use of:

- certified reference materials;

- reference materials;

- secondary reference materials (prepared in the

laboratory and characterized by repeated tests,

preferably by more than one laboratory or using

different validated methods)

MEASUREMENT TRACEABILITY (III)

Individual calibration program must be establish

depending on:

- the analytical technique;

- recommendation of the manufacturer;

- the level of uncertainty required.

Action to be taken for calibration of equipment must be

included in procedure for analytical method.

REFERENCE MATERIAL (I)

Reference material (RM) is a “material or substance

whose property values are sufficiently homogenous and

well established to be used for the calibration of an

apparatus, the assessment of the measurement

method or the assigning values to the materials”

(ISO Guide 30).

REFERENCE MATERIAL (II)

Certified reference material (CRM) is a “reference

material, accompanied by a certificate, one or more of

whose property values are certified by a procedure

which establishes traceability to an accurate realization

of the unit in which the property values are expressed

and for which each certificate value is accompanied by

an uncertainty at a stated level of confidence”

(ISO Guide 30).

REFERENCE MATERIAL (III)

Reference materials must be:

- clearly labeled;

- accompanied by certificates or other

documents;

- handled in order to safeguard against

contamination or loss of determinand;

- used only during the shelf life.

5.6 SAMPLING (I)

Sampling – “taken a part of a substance, material or

product for testing as a representative sample of the

whole”.

Sampling is an error generating process (40 % from

the total error induced during a test).

SAMPLING (II)

A Sampling Plan must be elaborated in which to be mentioned:

- location; - number of samples; - type of samples; - packaging of sample; - preservation of samples; - equipment used for sampling; - transport of samples; - personnel involved in this activity.

SAMPLING (III)

Documentation of sampling activity by:

- labels;

- records with relevant data about sampling

(sampling report).

When laboratory is not responsible for the sampling

stage, it should state in the report that samples were

analyzed as received from the client

5.7 HANDLING OF TEST ITEMS (I)

Handling of samples includes:

- transportation;

- receipt;

- storage;

- retention;

- disposal.

All these activities must be realized in such a way to

protect:

- the integrity of the samples;

- the interests of the laboratory and of the client.

HANDLING OF TEST ITEMS (II)

“Chain of custody” refers to the maintenance of unbroken

record of possession of a sample from the time of its

collection till the end of analytical investigation.

A person properly trained from the laboratory is

responsible for the custody and identification of the

sample and its accompanying documentation.

HANDLING OF TEST ITEMS (III)

The receipt of the test items implies:

- inspection of packaging, condition of samples,

correspondence between information from the

labels and the sampling report;

- identification of the sample with an unique code

(number);

- registration of sample into a sample logbook;

- observation in case the sample does not

correspond to the description provided.

HANDLING OF TEST ITEMS (IV)

Samples must be stored in such conditions:

- to maintain its integrity;

- to avoid contamination or cross-contamination;

- to avoid extremes environmental conditions

(e.g. temperature, humidity).

Disposal of the samples must be done in a way

prescribed by the local authorities and function of their

composition.

5.8 ASSURANCE THE QUALITY OF TESTS RESULTS

INTERNAL QC

The first level of control is assured by:

- blank of reagents (for reagent contamination);

- spiked samples (for effect of matrix);

- replicate analysis (for check of repeatability);

- control samples, control charts (drift of the

system);

- checks and correlations of the results.

CONTROL CHART (I)

The control chart is a graphic method realized by systematic checks (per day or per batch), which shows that the test result remain reproducible and that the methodology of measuring the analyte is respected.

Most used types of control charts:

- Control charts of the mean ( x -chart) for the control

of bias;

- Control chart of the Range of Duplicates (R- chart)

for the control of precision.

CONTROL CHART (II)

The X- chart is realized by plotting the analytical data,

in specific units, on the vertical scale, against time or

sequence of tests, on the horizontal scale.

Are realized :

- minimum 10 replicates results in each batch;

- calculation of mean value (x) and standard

deviation;

- calculation of: x±2s – warning levels

- calculation of: x±3s – control levels

Control chart of the Mean:

+3s UCL

+2s UWL

X X

-2s

LWL-3s

LCL Data/Batch

CONTROL CHART (III)

The R chart is obtained by running duplicate analysis

in the same batch, on control samples or test samples;

Are realized:

- minimum 10 initial pairs of duplicates;

- mean difference between duplicate, R:

- standard deviation of the range of all pairs of

duplicates;

- calculation of x±2s – warning levels

- calculation of: x±3s – control levels

+3s CL

+2s

R R

Data/Batch

Control chart of the Range of Duplicates :

WL

CONTROL CHART (IV)

Warning rule: one result beyond warning limits

Rejection rules:

- one result beyond control limit;

- two successive results beyond warning limit:

- ten successive results on the same side of the mean value;

- six out of seven successive points are in decreasing or

increasing order.

Specific actions have to be taken.

INTERNAL QC (I)

Second level of control is assured by:

- intra laboratory testing or in-house proficiency

testing of analysts;

- organized by QA Manager and the Head of

Laboratory.

The role is to establish the potential sources of errors induced by:

- the analyst;

- the equipment;

- the operating conditions;

- the calibration.

INTERNAL QC (II)

Problems in assessing intra-laboratory tests:

No.Problem Solutions and decision criteria

1 Kind of samples -Replicate samples of unknowns of reference

materials

-Samples must be exposed by the analyst to the

same preparatory steps as normal unknown

samples

2 Introducing the sample -Samples should have the same labels and

appearance as unknowns

-Supervisor can place knowns or replicates in the

system occasionally

-An aliquot from one day can be introduced for

analysis by another analyst

3 Frequency of checking performance

-Function of the method precision

-Function of the degree of automation

-Function of the analyst’s training, attitude and

performance record

EXTERNAL QC(I)

The third level of control is represented by participation

to interlaboratory comparisons organized at local,

regional, national or international level.

Accreditation laboratories are required to participate to

proficiency tests as a request of the accreditation bodies.

Participation to interlaboratory comparisons offers to a

laboratory the possibility to monitor its performance

against its own requirements and the norms of other

laboratories.

EXTERNAL QC(II)

Types of interlaboratory comparisons:

Method performances studies:

- collaborative studies

- comparative studies

Laboratory performance studies:

- proficiency tests

Material certification studies:

- certification studies

- consensus studies

5.10 REPORTING THE RESULTS (I)

The results must be reported:

- accurately;

- clearly;

- unambiguously;

- objectively;

- in accordance with the test methods.

REPORTING THE RESULTS (II)

The results are reported in a test report

The test report may be issued as a hand copy or by

electronic date

Amendments to a test report shall be made on a

special form with the mention “Supplement to Test

Report no. “