Presented by:Presented by:Farzad DadgariFarzad Dadgari

Soils & Environmental Soils & Environmental Specialist,Specialist,

SWHISASWHISA

What is quality? “The totality of features & characteristics of a product or service that bear on its ability to satisfy sated or implied needs

(ISO definition) Simply put, a product has good quality when it complies with the requirements specified by the client, or in laboratory terms, “delivery of reliable information within an agreed span of time under agreed conditions, at agreed costs, and with necessary aftercare”

(FAO, 1998)

The introduction and proper running of a “quality system” in laboratories.

There should be a statement of objectives and policy to produce quality should be included in the QA/QC manual by the organization and department concerned (Regional labs, ARARI, BoARD).

The statement should also state the internal organizational structure and responsibilities for the effective operation of the Quality System.

Quality management is a wider interpretation of “Good Laboratory Practice (GLP).

“The assembly of all planned and systematic actions necessary to provide adequate confidence that a product, process, or service will satisfy given quality requirement”. (ISO 9000 definition)

QA results should (ideally) be checked by someone who has not been involved in the work (the QA officer).

If no QA officer is available, this is the job of the head of the laboratory as part of his quality management tasks.

“the operation techniques and activities that are used to satisfy quality requirements” (ISO 9000 definition)

Important part of QC is quality assessment: the system of activities to verify if the quality control activities are effective (an evaluation of the product, the lab results, themselves).

QC’s main goal is to prevent laboratory errors. However, no matter how hard we try, errors will be made.

Therefore, a control system should be in place to detect the errors.

The “Five Ws” is a means to study the source of identified or suspected errors:What error was made?Where was it made?When was it made?Who made it?Why was it made?

When all these questions are answered, proper measures can be taken to correct and prevent the same errors to be made again.

QC related activities and techniques can be divided to three major levels:

1st-line of control: Instrument performance check & calibration or standardization.

2nd-line of control: Batch control (control sample, identity check).

3rd-line of control: Overall check/external checks (reference samples, inter-laboratory exchange programs, etc).

As a general rule 10-20% of the total costs of analysis should be spent on quality control.

To ensure quality lab work, at least four conditions should be made:

Means should be available (adequate personnel and facilities);

Efficient use of time and resources(costs aspect);

Expertise should be available (answering questions; aftercare); and

Upholding and improving level of output (continuity of QC related activities).

"GLP is concerned with the organizational process and the conditions under which laboratory studies are planned, performed, monitored, recorded, and reported." (OECD definition)

Therefore, GLP recommends that laboratory should work according to a system of procedures and protocols (controlled activities and working conditions, reporting, & filing).

GLP should be considered as a policy for all aspects of the laboratory work that influence the quality of the analytical work.

Therefore, implementation of GLP should:Allow for better laboratory management (including QM);

Improve efficiency (thus reducing costs)

Minimize errors;Allow quality control (including tracking of errors and their causes);

Stimulate and motivate all personnel;Improve safety; andImprove communication possibilities, both internally and externally.

Implementation of GLP should also result:improvement of laboratory performance and control of its working efficiency.

Documentation of quality standards (QS) and demonstration of QS to authorities and clients; thus, improving laboratory reputation. In short, GLP provide a venue to: say what you do; do what you say; do it better; and be able to show what you have done.

All relevant plans, activities, conditions and situations should be recorded, safely filed, and be able to easily be reproduced or retrieved when necessary.

The GLP related activities are normally compiled in the so-called Quality or QA/QC Manual that should comprise all relevant information on: Organization and Personnel; Facilities; Equipment and Working materials; Analytical or testing systems; Quality control; and Reporting and filing of results.

An important aspect of a quality system is that labs should use clear and easily understandable SOPs.

The whole process from sampling to filing of the analytical result should be described by a continuous series of SOPs. A SOP for a laboratory can be defined as

"A document which describes the regularly recurring operations relevant to the quality of the investigation”.

The purpose of a SOP is to carry out the operations correctly & always in the same manner.

SOP should be available at the work location.

SOP is a compulsory instruction. If deviations from SOP instruction are

allowed, the conditions should be documented including who is allowed to give permission for this and what exactly the complete procedure will be.

The original SOP should always kept at a secure place and working copies should be authenticated with stamps and/or signed by authorized person(s).

In addition, worksheets used for any analytical procedure must be standardized to prevent mistakes due to writing of, say, instrument readings and calculations on pieces of scrap paper.

Major types of SOP used in labs include: Fundamental SOPs: Providing instructions

on how to make SOPs of the other categories;

Methodical SOPs: Describing a complete testing system or method of investigation;

SOPs for receiving and registration of samples.

SOPs for safety precautions. SOPs for instruments, apparatus and other

equipment. SOPs for the preparation of reagents. SOPs for analytical methods. SOPs for Quality Assurance. SOPs for archiving and how to deal with

complaints.

The process of preparing and initiating an SOP in itself is an SOP. Such SOP should at least include:

Who can or should make which type of SOP;

To whom proposals for a SOP should be submitted, and who approves and legalizes the draft;

The procedure of approval; Who decides on the date of implementation, and who should be informed;

How revisions can be made or how a SOP can be withdrawn.

Establish and record who is responsible for the proper distribution of the documents, the filing and administration of the original and further copies;

Frequency of evaluation and possible revision of a valid SOP (say every two years) and by whom.

Only after such SOPs are in place, it is guaranteed that the proper laboratory operating instruction is going to be implemented.

Laboratory head (LH) should by himself or through assigning a senior staff member draft a SOP.

In principle, the author is the person who will work with the SOP, but he/she should always remember that the SOP should be understood by all others.

The author should request a new registration number from the SOP administrator or custodian (in our case, the LH).

The LH should verify whether the SOP already exists (or is drafted).

If the SOP does not exist, the title and author should be entered into the registration system.

Once the writing of a SOP is undertaken, the management must actively support this effort and allow authors adequate preparation time.

In case of methodical or apparatus SOPs the author should ask one or more qualified colleagues to try out the SOP.

In case of execution procedures for investigations or protocols, the project leader or LH could do the testing.

In this phase the wording of the SOP is fine-tuned.

Only after the test is passed the scrutiny, the SOP should be submitted to the SOP administrator/LH for acceptance.

Revisions of SOPs should follow the same procedure.

A SOP document should meet a minimum number of requirements:

1. Each page should have a heading and/or footing mentioning:

a.date of approval and/or version number;

b.unique title (abbreviated if desired);c.the number of the SOP (preferably with category);

d.page number and total number of pages of the SOP.

e.the heading (or only the logo) of originals should preferably be printed in another colour than black.

Categories can be denoted with a letter or combination of letters, e.g.:

F for fundamental SOP A or APP for apparatus SOP M or METH for analytical method SOP P or PROJ for procedure to carry out a

special investigation (project) PROT for a protocol describing a sequence

of actions or operations ORG for an organizational document PERS for describing personnel matters RF for registration form (e.g. chemicals,

samples) WS for worksheet (related to analytical

procedures)

2. The first page, the title page, should mention:

a.General information mentioned under item 1 (last slide), including the complete title;

b.A summary of the contents with purpose and field of application (if not evident from the title). If desired, the principle may be given, including a list of points that may need attention;

c.Any related SOPs (of operations used in the present SOP);

d.Possible safety instructions; e.Name and signature of author, including

date of signing; f.Name and signature of person who authorizes

the introduction of the SOP (including date).

3. The necessary equipment, reagents (including grade) and other means should be detailed.

4. A clear, imperative description should be given in a language mastered by the user.

5. It is recommended to include criteria for the control of the described system during operation.

6. It is recommended to include a table of contents, especially if the SOP is long.

7. It is recommended to include a list of references.

Matrix of information organization Laboratorie

s & personnel

SOP Documents

Involvement Code

A filing system for all documents should be established from the beginning to ease the process and avoid any confusion, inconvenience, and/or embarrassment, not only in internal use but also with respect to the bureau’s management, authorities, clients and, in future, inspectors of the accreditation body.

In ANRS, since labs are not accredited, the administration can be done by laboratory head or his deputy.

After accreditation, administration of SOPs will be the responsibility of Quality Assurance Officer, otherwise an officer of the department of Personnel at the bureau.

Administration may be done in a logbook, by means of a card system or, with a computerized database.

The most logical system should make an appropriate grouping of SOPs to categories and a master index for easy retrieval.

Normally, SOP files are kept at a central place such as the office of the laboratory head.

This does not apply to working documents, used at the work place in the laboratory, such as instrument logbooks, operation instruction manuals and laboratory notebooks.

The data which should be stored per document are:

SOP number; version number; date of issue and date of expiry; Title; Author; status (title submitted; being drafted;

draft ready; issued); department of holders/users; names of holders; number of copies per holder if more than

one; registration # of SOPs to which reference is

made; and historical data (dates of previous issues).

The SOP administrator should keep at least two copies of each SOP; one for archiving and one as the back-up file.

Same applies to revised versions. Superseded versions should be collected and destroyed (except the copy for archiving) to avoid confusion and unauthorized use.

The contents of a SOP for management & administration of SOPs should be extracted from the above.

Raw data and readings of measurements should be written down on worksheet, prepared for each analytical method or procedure, including calibration of equipment.

Each laboratory staff member should have a personal Notebook in which all observations, remarks, calculations and other actions connected with the work are recorded in ink, not with a pencil, so that they will not be erased or lost.

To ensure integrity such a notebook must meet a few minimum requirements: on the cover it must carry a unique serial number,

the owner's name; and the date of issue.

The copy should be issued by the QA officer or LH who keeps a record of this (e.g. in his/her own Notebook).

The user should sign for receipt, the QA officer or LH for issue.

The Notebook should be bound and the pages numbered before issue (loose-leaf bindings are not GLP!).

The first one or two pages can be used for an index of contents (to be filled in as the book is used).

The Notebooks can be an ordinary notebook (before issuance, the page numbering should be done by hand or with a special stamp) and then printed and bound.

Date/Signature Subject

Verified by:Signature ________________Test no._________________Date: ____________________File: ___________________

Do not overdo the documentation; Step-by-step approach should be adopted in implementation of all new Quality Management rules;

Protocols and SOPs, as well as the administration involved, should be kept as simple as possible, especially in the beginning.

Quality Management system must grow by trial and error, with increasing experience, by group discussions and with change in perceptions.

In the beginning, attention will be focused on basic operational SOPs, shifting to record keeping and filling gaps as missing links in the chain of Quality Assurance are revealed through practice.

When problems are identified, talk with people in other laboratories who have faced similar problems.

Do not forget! Quality Management is a tool rather than a goal. The goal is quality performance of the laboratory.

A typical SOP should have the following fields after providing the title of the SOP:1. Purpose2. Principle3. Field of application4. Related SOPs5. Requirements6. Procedure (Administration, initiating

SOP, revision of SOPs, Distribution of SOPs)

7. Archiving8. References

Internal structure should include: job description of the various positions throughout the organization (all laboratories):

list of personnel involved at each lab; their qualification, Their knowledge level, Their experience; and Their responsibilities.

Because of work continuity in the lab, well qualified replacement colleagues should be identified in case of illness or other absence of staff.

1. Function & aims of the institute;2. Scope of the laboratory;3. Organization chart (Organogram): A

chart depicting the laboratory structure that should be updated frequently;

4. Description of the process: The way work is organized in the laboratory should be described in a SOP:

kind and frequency of consultations and meetings;

how jobs are assigned; how instructions are given; and how results are reported).

5. Job descriptions, personnel records, job allocation, replacement of staff process;

6. Education and training of staff; and7. Introduction of new staff.

When an institution (BoARD/ARARI) establishes a laboratory, it is expecting quality analytical data.

Provision of quality data, beside trained and qualified staff requires:Supply of adequate equipment and working materials;

Presence of suitable housing structure; and

Enforcement of proper health & safety measures.

All BoARD laboratories are “planned laboratories, but that is not the case in ARARI. Whatever the case, the conditions should be optimized to allow for obtaining the desired quality;

In ideal condition, the building layout should consist of 2 separate blocks: Scientific block for analytical determination, staff training and administration; and

A storage block for receipt, preparation, and storage of samples. The dusty analytical work (crushing, sieving) should be done in storage block.

Transport of prepared soil and plant samples should be through a covered passageway or buffer room.

There should not be direct connection such as a simple door between crushing/milling room and analytical room.

Ideally, the scientific block should include separate laboratory room such as:

1. Preliminary operation room(s) for a)weighing, including sub-sampling, and b) extraction, oxidation, ad drying;

2. Room(s) for physical analysis of soils such as soil moisture retention, specific surface area, bulk density, and particle size analysis;

3. Room(s) for general chemical processes involving the use of concentrated acids, alkalies, or ammonia, where fumes may be involved;

4) “Clean” room(s) where instruments can be used without danger of being affected by fumes or adverse atmospheric conditions such as balance room and rooms for specialized purposes such as AA, auto-analyzer, optical mineral analysis, GC-MS, HPLC, or X-ray diffraction, etc. These rooms must have UPS and should be well sealed and air conditioned;

5) Storage room for chemicals and maintenance supplies. Large amounts of inflammable liquid such as alcohol and acetone should be stored separately;

6. Workshop or service room(s) for the central preparatio and storage of distilled and.or deionized water for general washing and drying of lab-ware, construction and repair of instruments, and for glass blowing; and

7. Room(s) for administration, filing of records, staff meeting, seminars, reception of visitors, etc.

Room types 3 and 4 should be arranged so that no sample need to be taken into them except those already weighed for analysis and contained in covered vessels.

Storage block should consist of three rooms:

1. Room for receipt and registration of samples with adequate bench and shelf space to cope with the “normal” input;

2. Drying, crushing, grinding/milling and sieving room with measures to exhaust dust;

3. Room for storage of samples, bith before and after analysis with adequate shelf space. QA requires that samples be kept for at least a year after the date of analysis.

Air temperature of the laboratory should ideally be maintained at a constant level between 18 and 25oC and the humidity steady at about 50%;

Most often (the case in Amhara labs) air conditioning of the lab is neglected;

Analytical processes, carried out at room temperature, can be affected by differences in temperature and humidity;

Analysis performed in “cold” room can give a different result to one performed in “hot” room;

P extraction, for example, normally is influenced by temperature;

Temperature (at small scale) can be controlled by using thermostatic water baths or immersion coolers but this is impractical for shakers or other large scale routine operations;

1. Temperature correction factor can be applied in some cases, say pH measurement, but these have to be established first and may be inaccurate for wide temperature variations;

2. Many chemicals are affected by temperature and humidity under which they are stored (absorb water in humid condition, effloresce in dry air or decompose in high temperature);

3. Modern scientific equipment such as AA and GC/MS can be quickly and permanently damaged by changes in temperature and humidity; and

4. Personnel efficiency can also be significantly affected by temperature and humidity fluctuation or [presence of dust and fumes in the work place.

Most accidents in laboratories occur as a result of negligence and casual behaviour either in operation of equipment or their maintenance;

Therefore maintenance log books should be available where all particulars should be recorded;

Maintenance, calibrations, malfunctioning and actions to rectify problems & other relevant remarks for optimal functioning should be detailed;

If a sensitive equipment (AA, autoanalyzer) is used by more than one person, each user should record the operation in the journal to make him/her responsible for proper use (specific SOP)

Chemicals, reagent, and gases should be handled carefully, especially toxic and inflammable ones;

SOPs/protocols should be prepared for their handling;

Quantity of inflammable chemicals such as acetone and alcohol in excess of 10 litre should be kept outside the building in a shed;

Someone should be assigned to routinely check and ensure that safety kits such as first aid kits, chemical spill kits, eye wash in bottle/station are in order, safety shower is working condition and fire extinguishers are present and maintained properly;

To facilitate inspection, a floor-plan indicating all safety appliances and emergency exits should be available;

One option to incorporate the safety related activities is to prepare a safety logbook where the records of safety inspections should be kept with the head of the lab;

Oxidizing and reducing agents should not be stored together;

Acids should not be stored with organic liquids;

Each chemical has a label that indicate if it is hazardous. Keep close attention!

For efficient working and inspection purposes a list of chemicals in stock and the place they are stored should be prepared and kept up-to-date;

Copies of the list should be kept in or near all storage places so that any container or bottle removed can be counted for easy stock-management;

Some chemicals used in soils lab such as common acids, bases, and salts maybe disposed of in dilute form, but do not try to dilute concentrated solutions to make them disposable. Dilution is no solution to pollution!

Chemicals such as toxic compounds, persistent mineral oil, chromates, arsenic, molybdates, vanadates, selenium, cyanide, cobalt, and several other metals and their compounds have to be collected in proper containers to be disposed of in a way prescribed by the local environmental authorities. It is the lab’s responsibility to learn the regulation & prescribed & appropriate actions to be taken.

1. All employees must receive the locally applicable Workplace Hazardous Materials information guidance by management;

2. A positive attitude toward laboratory safety should be developed: prevention is better than cure.

3. Develop & strictly observe general laboratory safety practices.

4. Good housekeeping is extremely important. Maintain a safe, clean work environment.

5. You may work hard, but never be in a rush.

6. Safety precautions provided by the manufacturer should be followed when operating instruments.

7. Monitor instruments during operation. 8. Avoid working alone. If it is a must,

have someone contact you periodically. 9. Learn what to do in case of

emergencies (e.g., fire, chemical spill).

10.Learn emergency first aid. 11.Seek medical attention immediately if

affected by chemicals. Use first aid until medical aid is available.

12.Report all accidents and near-misses to the management.

13.Access to emergency exits, eye-wash fountains and safety showers must not be blocked. Fountains and showers should be checked periodically for proper operation.

14.Wash hands immediately after contact with potentially hazardous or toxic chemicals.

15.Clean up any spillage immediately. Use appropriate materials for each spillage.

16.Dispose of chipped or broken glassware in specially marked containers.

17.Use forceps, tongs, or heat-resistant gloves to remove containers from hot plates, ovens or muffle furnaces.

18.Eating, drinking or smoking in the laboratory is prohibited.

19.Laboratory glassware should not be used for eating or drinking.

20.Do not store food in the laboratory. 21.Telephone calls to analytical laboratory

should be restricted to urgent cases. 22.Visitors should always be accompanied by

authorized personnel. 23.All electrical, plumbing, and instrument

maintenance work should be done by qualified personnel.

24.Use fume hoods when handling concentrated acids, bases, and other hazardous chemicals. Fume hoods should be checked routinely for operating efficiency. Do not use them for storage

25.Muffle furnaces must be vented to the atmosphere (e.g. via a fume cupboard).

26.AA spectrophotometers must be vented to the atmosphere. Ensure that the drain trap is filled with water prior to igniting the burner.

27.Avoid unnecessary noise in the laboratory. Noise producing apparatus such as centrifuges, or continuously running vacuum pumps should be placed outside the working area.

28.Cylinders of compressed gases should be secured at all times.

29.Use personal safety equipment as described below.

a) Body protection: laboratory coat and chemical-resistant apron.

b) Hand protection: gloves, particularly when handling concentrated acids, bases, and other hazardous chemicals.

c) Dust mask: when crushing or milling/grinding samples, etc.

d) Eye protection: safety glasses with side shields.

e) Full-face shields: wear face shields over safety glasses in experiments involving corrosive chemicals.

f) Foot protection: proper footwear should be used. Do not wear sandals in the laboratory.

30.Never open a centrifuge cover until the machine has stopped completely.

31.Acids, hydroxides, and other hazardous liquid reagents should be kept in plastic or plastic coated bottles.

32.Do not pipette by mouth. 33.When diluting, always add acid to water,

not water to acid. 34.For chemicals identified for waste

disposal, write down contents on the label. 35.Always label bottles, vessels, wash

bottles, etc., containing reagents, solutions, samples, etc., including those containing water and also those you use for a short period (this short period may become days!).

36.Extreme care is required when using perchloric acid, otherwise fires or explosions may occur. Work must be performed in special fume cupboards, certified as perchloric acid safe, with a duct wash down system and no exposed organic coating, sealing compound, or lubricant. Safety glasses, face shield, and gloves must be used. When wet-digesting soil or plant samples, treat the sample first with nitric acid to destroy easily oxidizable matter. Oxidizable substances (e.g. tissue, filter paper) should never be allowed to come into contact with hot perchloric acid without pre-oxidation with nitric acid. Do not wipe spillage with flammable material. Do not store on wooden shelves. Do not let perchloric acid come into contact with rubber.

37.Read labels before opening a chemical container. Use workplace labels for all prepared reagents indicating:

a) kind of reagent and concentration;b) date of preparation;c) date of expiry; andd) the name of the person who prepared it.

Ideally every employee of a laboratory should have knowledge of emergency first aid and about 10%t of every ten employees of a whole institute should have a valid First Aid certificate including ability to for resuscitate.

Major equipment required at each lab include: Names and phone numbers of employees with First Aid certificate.

Telephone numbers of physicians and hospitals as well as the general emergency number.

First Aid kit Eye wash fountains or bottles. Safety showers (at least one per laboratory).

Responsibility for the First Aid kit should be given to one person who should keep a logbook of regular content, and purchased supplements. He/she should also inspect eye-wash equipment and safety showers regularly. When an eye-wash bottle has been used, it should be replaced or refilled and the expiration date revised.

The most important general points to observe in case of an acciden twhen there is no time to wait for qualified aid are: 1. Stay calm, try to oversee the situation and

watch out for danger. 2. Try to find out what is wrong with the

casualty. 3. Take care that the casualty keeps

breathing.4. If breathing stops, try to apply artificial

respiration by mouth-to-mouth or mouth-to-nose insufflations. When unconscious, turn casualty on his/her side with the face tilted to the floor (support head by kind of cushion).

5. Staunch serious bleeding. If necessary, arterial bleeding may be stopped by pressing a thumb in the wound.

6. Do not move the casualty unless he/she is in a dangerous position (e.g., in case of gas, smoke, fire or electricity), then carefully move casualty to a safe place.

7. Put the casualty's mind at rest. 8. Call qualified help as soon as possible:

medical service, a physician and/or an ambulance, and if necessary, the police. Do not leave casualty unattended.

Some of the accidents that may occur in the laboratory are:1. Burns: Hold affected parts of the skin for

at least 10 minutes in cold water. Try to keep the burn sterile. Do not apply ointment.

2. Corrosive burns: wash the affected part of the skin thoroughly with water.

3. Eye (corrosive) burns: Wash eye thoroughly with tap water. Use an eye fountain or eye-wash bottle or a tubing connected to a tap.

4. Hydrofluoric acid burn: Wash the affected part with dilute ammonia (1-2%) or NaHCO3 bicarbonate solution.

5. Poisoning by swallowing:a) Corrosive solutions (acids, bases): Let the

casualty drink one or two glasses of water to dilute the poison. Vomiting should not be induced.

b) Petroleum products: Do not induce vomiting (the products may get into the bronchial tubes).

c) Non-corrosive solutions (e.g. herbicides, fungicides): Try to induce vomiting. Swallow activated charcoal.

d) In all cases the casualty must immediately be taken to a physician or hospital. Try to bring the original container (with or without some of the poison).

As in the case of First Aid, a number of laboratory employees should be properly trained in fire fighting.

Necessary items and equipments are: Fire-proof blanket; Safety shower; Bucket with sand; Portable fire extinguishers of two types: CO2 or b.c.f. (halon, halogenated hydrocarbons). The b.c.f. has 6 times more fire fighting power than CO2.

When fire is detected stay calm, oversee the situation, and watch out for danger;

Then the following actions should be taken:1. Close windows & doors;2. Give fire alarm by shouting, telephone call,

and fire alarm, whichever available;3. Rescue people;4. Switch off electricity; and5. Fight fire, if possible with at least two

persons. Person with burning clothing should be wrapped in a blanket on the floor, sprayed with water or pulled under a safety shower.

When using fire extinguishers, the fire must be fought at the seat of the fire i.e., at the bottom of the flames, not in the middle of the flames.

If gas cylinders are present there is the danger of explosion by overheating. If they cannot be removed, take cover first and then and try to cool them with a fire-hose.

When the situation looks out of control, evacuate the building. Let everybody assemble outside and check if no one is missing.

To practice this, a regular fire drill (once a year), should be held.

Due to safety issues, only authorized personnel should have admittance to the laboratory blocks.

Visitors may only enter the laboratory after permission. This permission can be given by the head of laboratory or his/her deputy and they should be accompanied by a staff.

The entrances should be marked with a sign “No admittance for unauthorized persons".

To perform quality analytical work, availability of properly organized and suitable material is paramount;

Sample materials should have also received proper attention with respect to handling, storing and disposal;

The tools used for analysis are divided to:1. Primary measuring equipment (pipettes,

diluters, burettes, balances, thermometers, …;

2. Analytical apparatus or instruments (flame photometer, spectrophotometer, AAS, …;

3. Miscellaneous equipment and materials (ovens, furnaces, fridges, stills, glassware,…; and

4. Reagents.

Dirty cuvette improper dial location can cause erroneous readings of very well preapred extract, causing costly need for repeat of the analysis, even when using blind, dup and spike samples;

Calibration of thermometer, automatic burrette, pipette, etc may exceed acceptable tolerance level.

New Glassware may look clean, but should always be washed with deionized water after washing;

When glassware is shared, all lab patrons should follow the GLP to minimize errors.

Most prominent source of lab error is the use of wrongly prepared or old reagents;

Reagents have to be prepared carefully, exactly following the procedure, be well labelled, and the expiry date should be observed closely. Filtering a pH buffer solution in which fungus is growing may save time & reagent, but it is centim wise and Birr foolish;

Improper sample preparation, handling, and storage (chain of custody) is another major source of laboratory error.

To ensure implementation of proper QA, the following requirements should be met:1. Apparatus used for data generation, &

for controlling environmental factors relevant to the study should be suitably located and of appropriate design & capacity.

2. The apparatus used should be routinely inspected, cleaned, maintained, and calibrated according to SOP. Records of procedures should be maintained.

Instrument identification list: Record should include description and registration #, supplier info (phone/address), installation date, name of the responsible person(s) in card box or computerized form;

Instrument maintenance list; Instrument calibration list;

Apparatus needing routine maintenance & calibration need such lists (can be combined).

List(s) should include instrument ID, reference to equipments’ logbook and fixed dates for actions. Actions themselves, however, should be recorded in the logbook.

Operation Instruction Manual: The manual for every equipment should be available.

SOP for operation of each equipment should be prepared.

Instrument maintenance logbook: Each equipment should have a maintenance logbook.

All relevant actions should be recorded as well as problems encountered and repairs made.

For older apparatus, the current status of the equipment must be provided in the logbook.

Major maintenance and repair should be done by qualified technician from inside or ouside.

It is sensible to have a supply of essential parts such as hollow cathode lamp or nebulizer needles for AAS, necessary tools, blue prints and maintenance manual for major equipments.

User Logbook: For all sensitive equipment (AAS, UV-Vis spectrophotometer, flame photometer, etc a user logbook should be prepared to report: Name of the user; Type of use (elements measured and matrix used);

Date of operation; Duration of use; Any problems observed (should also be recorded in maintenance logbook).

SOPs for use of equipment: SOPs should be prepared for use of each apparatus. A number of example SOPs for equipment such as pH meter, auto-pipette, electronic balance, and a standard instruction for writing SOPs is provided in the handout.

Advisable to use analytical grade chemicals throughout. If not available, chemically pure grade is satisfactory for most soil analyses.

The minimum chemical purity requirement, including water and other solvents should be included in the procedure description;

When chemicals (and gases) arrive in the laboratory the containers need to be labelled.

The label should include Date of receipt, Date it was first opened; and Expiry date.

When chemicals & gases arrive, containers should be labelled with following info: Reagent Name: Date received and signature: Date opened; Opened by (name and signature): Storage location: Expiry date; Remarks.

Basic rules for taking chemicals from the bottle:1.Use a clean spoon or spatula;2.Do not return chemical to the bottle; and3.Close the bottle tightly after use.

Two types of standards are needed for chemical analysis in soils labs:1. Standard reagents for standard reagent

solutions for calibration of measuring instruments (1st line of control):

2. Standard sample material to be divided into primary (certified) standard material & the “home-made” control samples (2nd & 3rd line of control).

Success of an analysis depends on reliability of the used standards & other reagent solutions & they should be prepared with great care and by experienced staff.

Every standard and reagent preparation should be recorded in “reagent or standards book”;

Reagent book can be designed in one of two layouts:1. All reagents prepared are recorded

chronologically; or2. For each reagent, a separate page is

reserved. Each bottle of reagent solution should be labelled.

Label for reagent or standard bottle should include the following info:1. Reagent name:2. Concentration;3. For Analysis:4. Store Location:5. Expiry Date:6. Prepared by (name and signature)7. Date:

Proper label for standard solution should include the following info:1. Standard Name:2. Matrix:3. For Analysis:4. Expiry Date:5. Prepared by: (Name and signature);6. Date:

Same rules as reagent chemicals is applied for reagent solutions:1. Do not return unused solution to the bottle

(contamination!); 2. Close the analyte bottle tightly; and3. Write concentration with a marker in large

characters for easy recognition on the bottle. Reagent solution/standards should not be kept for more than 6 months, some for only few days.

Color labels should be used for different reagents, say red for short life reagents, blue for reagents to be refrigerated and yellow for those to be kept in the dark.

Soil, plant & water samples vary highly in nature and condition.

We do not discuss sampling in this training, but it can have significant impact on laboratory results.

Lab should require proper packaging, labelling & administration of samples before they arrival at the lab.

SOPs, protocols, registration form and labels can be prepared & issued by the lab & issued to clients prior to sampling.

Probably no laboratory exist that has not experienced problems with field sampling.

GLP aims at proper administration scrutiny of sample identity and unbroken chain of custody.

Process should be in place to prevent accidental sample interchange, sample contamination (broken bags), or loss of identity (losing label).

No system can be full-proof and even fire or malicious acts of sample tampering are possible.

Lab should have a plan to minimize such occurrences through proper QA/QC.

From the moment sample arrives, their identity, integrity, and knowledge of their location must be safeguarded by including: Inspection of packaging, sample condition, moisture status, status of labels (are they readable?);

Registration of samples by authorized lab staff who should plan the routing of the sample as per lab protocol that may include handing over of the sample to person in charge of drying, sieving and transfer to the analytical lab.

Sample particulars & sample numbers should be entered to the sample logbook.

A physical copy of registration should be filed with each work order, stating the proposed completion date.

Use of computerized Laboratory Information and Management System (LIMS) is encouraged.

Use of such program is a powerful tool in the organization and QC of the laboratory.

I the chain of custody, LIMS can be used to facilitate sample registration and analytical programs and can produce ready-to-use printed sticker labels with all required information for the sample container.

The way samples are stored and disposed of also have to be described in protocol.