What is QUALITY? QUALITY? h QUALITY is the degree to which a set of inherent characteristics fulfils requirements [ISO 9000-2000].

9000-2000]

h In analytical work, QUALITY can be defined as

delivery of reliable information within an agreed spare of time and under agreed conditions, at agreed costs and with necessary aftercare. aftercare.

To achieve Quality and optimal performance it is necessary to develop and put in practice the concepts of:

h QUALITY MANAGEMENT h QUALITY ASSURANCE h QUALITY CONTROL

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

In testing laboratories, QM means: h creating a good structure; h providing support for developing; h validating methodologies; h verifying performance.

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

QMS includes: h organizatoric structure; h procedures / processes; h resources necessary for implementation of QM.

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

QA implies that the organization of the activities and the conditions under which this takes place are: are: h controlled; controlled; h reported; reported; h filed. filed.

In short, QA means: h h h h SAY WHAT YOU DO DO WHAT YOU SAY DO IT BETTER BE ABLE TO SHOW WHAT YOU HAVE DONE

QA implementation conduct to: h h h h h better laboratory management; improve efficiency; minimize errors; stimulate and motivate personnel; improve reputation of the laboratory.

QUALITY CONTROL (QC) is a major part of QM, focused on fulfilling quality requirements [ISO 9000-2000]. 9000For analytical activity, QC represents: a set of procedures undertaken by the laboratory for continuous monitoring of operations and results in order to decide whether the results are reliable enough to be realized.

QC is divided into three levels: 1. first level of control (internal control): realized by the analyst; 2. second level of control (internal control): realized by the QA Manager/Head of Laboratory; 3. third level of control (external control): interlaboratory proficiency testing

Quality Control

Sample
Measurement process

Sample data Quality assesment Data QC samples Specification Accept/use data

QC sample

Second level

Check samples given by Qality manager Third Level Laboratory performance study

The main QMS elements are:

h Quality policy; h Quality objectives; h Quality Manual; h Procedures, instructions; h Records.

Function of their importance, they have a pyramidal structure. structure.

QUALITY STANDARD

QUALITY POLICY QUALITY OBJECTIVES QUALITY MANUAL PROCEDURES INSTRUCTIONS RECORDS

h QUALITY POLICY attest the intentions and direction for maintaining a high level of quality in the activity of the laboratory. h QUALITY POLICY is established by the highest level of authority from the laboratory. h QUALITY POLICY must be written down and familiar to all personnel from the laboratory.

QUALITY OBJECTIVES ARE BASED ON:

h particular laboratory priorities and field of interest; h results of audits; h customer complaints; h requirements of regulatory or accreditation body.

QUALITY OBJECTIVES SHOULD BE:

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

h a short presentation of the Laboratory and of the Company; h the Quality Policy; h the responsibilities and authorities of the personnel;
h the procedures of QMS or a short presentation of them; h 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:
h general or fundamental procedures how to elaborate procedures; h system procedures for the management and the technical requirements from ISO 17025 standard; h 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.

h Records are the basic elements of the QMS; h Records are produced every day; h 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 17025
General requirements for competence of testing and calibration laboratories For first, second and third party laboratories which perform tests, including sampling

ISO 9001
Quality Management System requirements For laboratories which conduct research and development activities For laboratories which perform monitoring of the environment

ISO 14001
Environmental Management Systems. Specification with guidance for use

QMS for environmental laboratories (II):

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

Procedures in the integrated quality system ISO 9001-ISO 17025

ISO 17025 Management and Organization

ISO 9001 Quality System (politics,objecti ves,documentat ion) Management rewiews Services to the clients Complaints Management responsability Control of nonconforming tests Corrective and preventive actions Measurement, analysis and improvement Traceability Assuring Quality of tests Internal Audit

Document control Control of records

Personnel

Accomodation and environmental conditions

Resource management

Product realisation
Rewiew of requests, tender and contracts

Handeling of test items Sampling

Sub-contracting ot tests

Purchasing services and supplies

Test and method validation

Reporting results

Equipment

ACCREDITATION ISO 17025 offers:

h Independent assessment of quality

management system and technical competence of the laboratory. h Confirm or recognize the competence of the laboratory towards : - clients; - regulatory authorities; -accreditation bodies.

h ACCREDITATION ISO 17025 process is voluntary; h ACCREDITATION ISO 17025 is realized by the National Accreditation Body; h REACCREDITATION at 2-5 years.

ACCREDITATION ISO 17025 Requirements for accreditation ISO 17025: h to respond to the 14 management requirements; h to respond to the 10 technical requirements.

MANAGEMENT REQUIREMENTS
4.1 ORGANIZATION (I)
Laboratory must: h be entity legally responsible; h satisfy the needs of the client, regulatory authorities or accreditation body; h identify potential conflicts of interest (if laboratory is part of an organization); h be able to demonstrate the impartiality and that the personnel is free from commercial, financial or other pressures which might influence their technical judgment; h have an organigram in which to define the organization, structure and management

ORGANIZATION (II): h have sufficient qualified staff for all the activities (professional requirements described in the Job Description); h have technical management with responsibilities for technical activities and of provisions of the resources needed to ensure the required quality; h have a quality manager; h have deputies for key managerial personnel.

4.2 QUALITY SISTEM For implementing and maintaining the QMS the laboratory must have: h 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.

h 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:
h evaluation of documents drafting; - verifying; - authorizing. h distribution of documents; h possession and/or changing of documents; h destroying and archiving of documents.

DOCUMENT CONTROL (II) Quality Documents can be:

Quality Manual; INTERNALLY GENERATED Procedures; Instructions; DOCUMENTS Quality policy and objectives.

EXTERNAL SOURCES

Standards; Books, manuals; Norms, regulations; Technical specification .

DOCUMENT CONTROL (III) Documents generated by the laboratory should be:

h uniquely identified by : - a code/number; - date of issue; - date of revision; - page numbering; - the issuing authority. h periodically reviewed /revised;

hdestroyed when are out of use to avoid unintended use;

h 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: h it posses the skilled personnel for the performance of the tests in question; h the financial, legal and time schedule aspects were taken into account; h 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: h signed by both partners; h any deviations announced to the client.

4.5 SUBCONTRACTING OF TESTS

h Temporary subcontracting activity - workload; - temporary incapacity; - need for further expertise.
h Permanent subcontracting activity

h Selection of subcontracting laboratories by: - audit; - certificate of accreditation. h Maintain a register with all subcontractors; h Laboratory is responsible to the client for subcontractors work.

4.6 PURCHASING SERVICES AND SUPPLIES (I)

h Procedures for purchasing and storage of: - reagents; - equipment; - consumable materials; - services. h Purchase order must contain: - complete name of the product/service; - quantity; - quality specification. h Purchase documents, like purchase order, receiving documents, accompanying certificate are used for identification of the material received.

PURCHASING SERVICES AND SUPPLIES (II)

h Inspection of the purchase services and supplies

before being used; h Records of actions taken; h Evaluation of suppliers and maintaining records of these evaluations.

4.7 SERVICE TO THE CLIENT

h 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

h Received from clients, regulatory or accreditation bodies.

h 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.

hRecords of complaints, of investigations and corrective actions taken

4.9 CONTROL OF NONCONFORMING TESTING WORK (I) Nonconformity may occur :

h Within the Quality System: - internal or external audits; - customer complaints; - staff observations; - management review.

h Within technical operation:

- instrument calibration; - data validation; - test report checking.

4.9 CONTROL OF NONCONFORMING TESTING WORK (II) h 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:
- Report of audit; - Report of nonconforming activities; - Report of corrective/preventive actions; - Training report; - Management review report.

QUALITY RECORDS

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

h 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.

h Carried out by trained personnel.

h Planned by the QA Manager at least annually. h All the Management and Technical elements of the QMS are checked. h Corrective actions must be taken.

4.14 MANAGEMENT REVIEWS

h 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 h 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)

h The laboratory must have sufficient qualified and

experienced personnel

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

h All information about personnel should be recorded

PERSONNEL AND TRAINING (II)

h All personnel involved in any function affecting quality

should have sufficient training in their appointed job

h 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)

h Trainings developed:
- within the laboratory; - by outside specialist; - centrally conducted courses, if necessary abroad.

h At the end of the training:

- evaluation of the effective training; - certificates / diplomas. h 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)

h 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)

h Appropriate environmental conditions:

- temperature; - humidity; - freedom of vibration; - freedom of air borne and dust; - clean air. hMonitoring of temperature and humidity hAdmission in laboratory only for authorized persons h Visitors, inspectors must be in charge of one member of the laboratory

5.4 TEST METHODS AND METHOD VALIDATION hAppropriate methods and procedures for all test activities

h Test methods must be: - technically justified; - authorized; - verified for use in the laboratory.

METHOD VALIDATION (I)

h Validation means confirmation by examination and

provision of objective evidence that the particular requirements for a specific intended use are fulfilled (ISO- 8402-94).

h Verification means confirmation by examination and

provision of objective evidence that specified requirements have been fulfilled (ISO 8402-94).

METHOD VALIDATION (II)

hVerification is applied for checking the standard method;

h 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)

h 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.
h 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 . h Type A components may be evaluated from statistical distribution of the result of a series of measurements and is expressed as standard deviations. h 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) h Standard Uncertainty u (xi), is the uncertainty of the result of a
measurement expressed as a standard deviation.

h 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)

h 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

h Nominated persons from the laboratory must check

the calculations and the data transfer in a systematic manner, during they are generated
h

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)
h 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)

h 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) hAll equipment must be labeled.

h 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)

h 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)

h Traceability concerns the requirements to relate the results of measurements to the values of reference standards, preferably to SI.

h 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.
h 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) h Individual calibration program must be establish depending on: - the analytical technique; - recommendation of the manufacturer; - the level of uncertainty required. h 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.

h 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) h Documentation of sampling activity by: - labels; - records with relevant data about sampling (sampling report). h 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) h Handling of samples includes: - transportation; - receipt; - storage; - retention; - disposal. h 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)

h 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.

h 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) h 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). h 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 h 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)

h 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.

hMost 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) h 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. h Are realized : - minimum 10 replicates results in each batch; - calculation of mean value (x) and standard deviation; - calculation of: x 2s - calculation of: x 3s warning levels control levels

Control chart of the Mean:

+3s UCL +2s UWL X X -2s LWL -3s LCL Data/Batch

CONTROL CHART (III) h The R chart is obtained by running duplicate analysis in the same batch, on control samples or test samples;

h 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 - calculation of: x 3s warning levels control levels

Control chart of the Range of Duplicates :

+3s CL +2s WL

Data/Batch

CONTROL CHART (IV)

h Warning rule: one result beyond warning limits h 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. h Specific actions have to be taken.

INTERNAL QC (I)
h 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.
h 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:

Problem No. 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 analysts training, attitude and performance record Solutions and decision criteria

EXTERNAL QC(I)
h The third level of control is represented by participation

to interlaboratory comparisons organized at local, regional, national or international level. h Accreditation laboratories are required to participate to proficiency tests as a request of the accreditation bodies. h 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:

h Method performances studies: - collaborative studies - comparative studies h Laboratory performance studies: - proficiency tests

h 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)

h The results are reported in a test report

h The test report may be issued as a hand copy or by electronic date h Amendments to a test report shall be made on a special form with the mention Supplement to Test Report no.