Performance Evaluation of the Food and Environmental Monitoring Radio- Analytical Laboratory in Ghana A thesis presented to the: DEPARTMENT OF NUCLEAR SAFETY AND SECURITY UNIVERSITY OF GHANA By Lilian Ataa Agyeman, 10507915 Dip. (Laboratory Technology) BSc (Laboratory Technology) In fulfilment of the requirements for the degree of MASTER OF PHILOSOPHY in RADIATION PROTECTION June, 2016 University of Ghana http://ugspace.ug.edu.gh i DECLARATION This dissertation is the result of research work undertaken by Lilian Ataa Agyeman in the department of Nuclear Safety and Security, University of Ghana, under the supervision of Dr. A. Faanu and Prof. G. Emi-Reynolds. Sign________________ Lilian Ataa Agyeman (Student) Sign____________________ Dr. A. Faanu (Principal Supervisor) Sign____________________ Prof. G. Emi-Reynolds (Co-Supervisor) University of Ghana http://ugspace.ug.edu.gh ii DEDICATION I thank the Almighty God for how far He has brought me. This work is dedicated to my Husband, Yaw Saarah Adu-Gyamfi for his Absolute Support, Prayers and Encouragement during this work; to my Children, Abena, Akwasi and Danyame Saarah Adu- Gyamfi and my Mother Ms. Margaret Adomako. University of Ghana http://ugspace.ug.edu.gh iii ACKNOWLEDGEMENT I am grateful to the Lord God for the Protection, Good Health and Spiritual Guidance during the entire duration of my Mphil Programme. I wish to express my gratitude to my supervisors, Dr. Augustine Faanu and Prof. G. Emi-Reynolds for their excellent support, directions, suggestions and patience in guiding me through the research. I would like to acknowledge the Management of Radiation Protection Institute of the Ghana Atomic Energy Commission, for their assistance during the evaluation process; and, to all the Scientists and Technologists of the Food and Environmental Laboratory for their support during the entire research. I would also like to acknowledge, Prof. Emmanuel Ofori Darko, the Acting Director of the Radiation Protection Institute, Mr. Henry Lawluvi, Dr. David Kpeglo, Mr Oscar Adukpo, Miss Racheal Paintsil, Ms. Doreen Smith, Mrs Cynthia Engman, Mrs. Rita Kporzro and Mr. James Ayariga for their diverse support. University of Ghana http://ugspace.ug.edu.gh iv TABLE OF CONTENTS DECLARATION .......................................................................................................... i DEDICATION ............................................................................................................. ii ACKNOWLEDGEMENT .......................................................................................... iii TABLE OF CONTENTS ............................................................................................ iv LIST OF TABLES ...................................................................................................... ix LIST OF FIGURES .................................................................................................... xi LIST OF ABBREVIATIONS .................................................................................... xii CHAPTER ONE .......................................................................................................... 2 INTRODUCTION ....................................................................................................... 2 1.1 Background ................................................................................................... 2 1.2 Radiation Protection, Food and Environmental Monitoring Laboratory ........... 5 1.3 Statement of Problem .................................................................................... 7 1.4 Objectives ...................................................................................................... 7 1.5 Scope of the Study ......................................................................................... 8 1.6 Relevance of Study ........................................................................................ 8 CHAPTER TWO ......................................................................................................... 9 LITERATURE REVIEW............................................................................................. 9 2.1 The Analytical Laboratory as a Service Organisation ..................................... 10 2.2.1 Primary Standard Dosimetry Laboratories (PSDLs)............................ 10 2.2.2 Secondary Standard Dosimetry Laboratory ......................................... 11 2.2.3 National Reference Laboratory ........................................................... 11 University of Ghana http://ugspace.ug.edu.gh v 2.3 Analytical Laboratory Performance ............................................................ 12 2.2 Laboratory Performance Evaluation............................................................ 12 2.2.1 Evaluation of Performance Indicators ............................................... 13 2.2.2 Measurement Uncertainty .................................................................... 14 2.2.2 Certified Reference Materials .............................................................. 15 2.2.3 Traceability .......................................................................................... 17 2.3 Instrumentation Performance Indicators ..................................................... 18 2.3.1 Instrument Background Measurements................................................ 18 2.3.2 Efficiency Calibrations......................................................................... 19 2.3.3 Calibration of Apparatus Used for Mass and Volume Measurements . 22 2.4 Statistical Means of Evaluating Performance Indicators - Control Charts.. 22 2.4.1 Statistical Quality Control .................................................................... 22 2.4.2 Control Charts for Instrument Response .............................................. 24 2.5 Quality Assurance in the Laboratory Environment ..................................... 25 2.6 Laboratory Information Managing Systems ................................................ 27 2.7 Laboratory Personnel Competency and Performance Measurement .......... 28 2.8 Description of ISO 17025 ............................................................................ 29 2.8.1 Organisation ......................................................................................... 29 2.8.2 Management System ............................................................................ 30 2.8.2.11 Control of Records .............................................................................. 33 2.8.12 Internal Audits ......................................................................................... 34 2.8.13 Management Reviews ............................................................................. 34 University of Ghana http://ugspace.ug.edu.gh vi 2.8.14 Technical Requirements ....................................................................... 34 2.8.15 Personnel .......................................................................................... 35 2.8.16 Accommodation and Environmental Conditions ............................. 35 2.8.17 Test and Calibration Methods and Method Validation ........................... 35 2.8.18 Equipment ........................................................................................ 36 2.8.19 Measurement Traceability ................................................................ 36 2.8.20 Sampling ........................................................................................... 36 2.8.21 Handling of Test and Calibration Items ............................................... 37 2.8.22 Assuring the Quality of Test and Calibration Results ............................. 37 2.8.23 Reporting the Results ....................................................................... 37 2.9 Benefits of ISO 17025 certification ............................................................. 38 2.10 IAEA Technical Report Series 295 Requirements for Food and Environmental Laboratories ................................................................................... 39 2.10.1 Accommodation ...................................................................................... 39 2.10.2 Laboratory Design ................................................................................ 40 2.10.3 Ventilation ............................................................................................ 40 2.10.4 Temperature ......................................................................................... 41 2.10.5 Instrumentation required for Gamma Radiation Measurement: .......... 41 2.10.6 TRAINING .......................................................................................... 42 2.10.7 ANALYTICAL QUALITY CONTROL ............................................. 42 2.10.8 Internal Control Programmes .............................................................. 43 2.10.9 Data Presentation ................................................................................. 44 University of Ghana http://ugspace.ug.edu.gh vii CHAPTER 3 .............................................................................................................. 46 METHODOLOGY ..................................................................................................... 46 3.1 Description of the Facility ................................................................................ 46 3.2 Administration of Questionnaire ................................................................. 47 3.3 Physical Examination and Observation of Documents and Procedures ...... 48 3.3 Equipment Performance Test ...................................................................... 52 3.3.1 Energy calibration ................................................................................ 52 3.3.2 Efficiency Calibration .......................................................................... 53 3.3.3 Instrument Background Measurement ................................................ 54 3.3.4 Determination of Minimum Detectable Activity (MDA) .................... 55 3.4 Statistical Analysis of the Performance of the Gamma Spectrometry System 56 RESULTS AND DISCUSSIONS .............................................................................. 57 4.1 Compliance with ISO 17025 ....................................................................... 57 4.1.1 Personnel Training Records ................................................................. 57 4.1.2 Accommodation and Environmental Conditions ................................. 59 4.1.3 Quality assurance for the screening process ........................................ 60 4.1.4 Equipment ............................................................................................ 62 4.1.5 Traceability of measurement ................................................................ 63 4.1.6 Administration of work and sample tracking ....................................... 65 4.1.7 Recording of Results and Associated Data .......................................... 66 4.1.8 Computer Systems ............................................................................... 67 University of Ghana http://ugspace.ug.edu.gh viii 4.1.9 Reporting Requirements....................................................................... 68 4.1.10 Purchasing Services and Supplies ........................................................ 69 4.2 Complying with IAEA Technical Report Series 295 (TRS 295) ................ 70 4.3 Quality Assurance Tests .............................................................................. 71 4.3.1 Energy Calibration ............................................................................... 71 4.3.2 Efficiency Calibration .......................................................................... 72 4.3.3 Minimum Detectable Activities ........................................................... 73 4.3.4 Background Measurements .................................................................. 74 4.3.5 Calibration of other Measuring Instruments ........................................ 74 4.3.6 Statistical Quality Control .................................................................... 75 CHAPTER 5 .............................................................................................................. 76 CONCLUSIONS AND RECOMMENDATION ....................................................... 76 5.1 Conclusions ................................................................................................. 76 5.2 Recommendations ....................................................................................... 77 REFERENCES ........................................................................................................... 80 APPENDIX A ............................................................................................................ 82 APPENDIX B ............................................................................................................ 87 APPENDIX C .......................................................................................................... 106 University of Ghana http://ugspace.ug.edu.gh ix LIST OF TABLES Table 2. 1: Rooms and Area Recommended for a Central Environmental Laboratory .............................................................................................................. 40 Table 3. 1: The checklist below developed to assist in the workplace inspection . 50 Table 4. 1: Average response to questions on personnel training records ............ 58 Table 4. 2: Approximated Average Score of responds to questions on accommodation and environmental conditions existing in the laboratory 60 Table 4. 3: Approximated Average Score of responds to questions on quality assurance for the screening process ........................................................ 61 Table 4. 4: Approximated Average Score of responds to questions on equipment in the RPI lab ............................................................................................ 63 Table 4. 5: Approximated Average Score of responds to questions on traceability of measurement ......................................................................................... 64 Table 4. 6: Approximated Average Score of responds to questions on administration of work and sample tracking ......................................... 65 Table 4. 7: Approximated Average Score of responds to questions on Recording of Results and Associated Data ................................................................. 66 Table 4. 8: Approximated Average Score of responds to questions on computer systems .................................................................................................. 67 Table 4. 9: Approximated Average Score of responds to questions on reporting requirements ............................................................................................ 68 Table 4. 10: Approximated Average Score of responds to questions on purchasing services and supplies ............................................................................. 69 University of Ghana http://ugspace.ug.edu.gh x Table 4. 11: Comparison of facilities recommended by TRS 295 and existing Infrastructure at the RPI Lab. ............................................................... 70 Table 4. 12: Minimum Detectable Activities of the 238 U, 232Th and 226Ra and 137Cs ……………………………………………………………………...74 University of Ghana http://ugspace.ug.edu.gh xi LIST OF FIGURES Figure 4. 1: Percentage responds to questions on personnel training records ..... 58 Figure 4. 2: Percentage responds to questions on accommodation and environmental conditions existing in the laboratory .................................................. 59 Figure 4. 3: Percentage responds to questions on quality assurance for the screening process ....................................................................................................... 61 Figure 4. 4: Percentage responds to questions on equipment in the RPI lab ....... 62 Figure 4. 5: Percentage responds to questions on traceability of measurement .. 64 Figure 4. 6: Percentage responds to questions on administration of work and sample tracking .......................................................................................................... 65 Figure 4. 7: Percentage responds to questions on Recording of Results and Associated Data .......................................................................................................... 66 Figure 4. 8: Percentage responds to questions on computer systems .................. 67 Figure 4. 9: Percentage responds to questions on reporting requirements........... 68 Figure 4. 10: Percentage responds to questions on Purchasing services and supplies .......................................................................................................... 69 Figure 4. 11: Plot of gamma ray energy against channel number.......................... 72 Figure 4. 12: Efficiency calibration curve as a function of energy for mixed radionuclides standard ................................................................................................ 73 Figure 4. 13: Statistical Control chart for daily counting of a check source.......... 75 University of Ghana http://ugspace.ug.edu.gh xii LIST OF ABBREVIATIONS ADC: Analogue- to- Digital Converter Bq/Kg: Becquerel per Kilogram Bq/m2: Becqueral per square meter Bq/m3 : Becquerel per cubic meter CL: Control Limit CN: Channel Number CRM: Certified Reference Material DPS: disintegration per second FEML: Food and Environmental Monitoring Laboratory FWHM: Full Width at Half Maximum GAEC: Ghana Atomic Energy Commission GLP: Good Laboratory Practices HPGe: High Purity Germanium detector IAEA: International Atomic Energy Agency IEC: International Electrotechnical Commission ISO: International Standard Organization K: Potassium KeV: Kilo ElectronVolts University of Ghana http://ugspace.ug.edu.gh xiii LCL: Lower Control Limit LIMS: Laboratory Information Management System LWL: Lower Warning Limit MCA: Multichannel Analyser MDA: Minimum Detectable activity NaI: Sodium Iodide NORM’s: Naturally Occurring Radioactive Materials PSDL: Primary Standard Dosimetry Laboratories QA: Quality Assuarance QC: Quality Control RPB: Radiation Protection Board RPI: radiation Protection Institute SI: Systeme Internationale SOP: Standard Operating Procedures SSDL: Secondary Standard Dosimetry Laboratory Th: Thorium TRS: Technical Report Series U: Uranium UCL: Upper Control Limit University of Ghana http://ugspace.ug.edu.gh xiv UNIDO: United Nations Industrial Development Organization UNSCEAR: United Nations Scientific Committee on Effect of ATOMIC Radiation UWL: Upper Warning Limit WHO: World Health Organization WNO: World Nuclear Organization University of Ghana http://ugspace.ug.edu.gh 1 ABSTRACT Since the establishment of the Radiation Protection Institute’s Food and Environmental Laboratory in 1988, there has never been any thorough evaluation of the activities of the facility to provide assurance of the quality of analytical results produce by the laboratory. The objective of this study, therefore, was to assess the performance level of the Food and Environmental monitoring laboratory with respect to the requirements for a standard analytical laboratory (IAEA, 1989) and ISO 17025. The study focused on the performance of the Gamma Spectrometry laboratory of the Radiation Protection Institute, Ghana Atomic Energy Commission which has been involved in monitoring of radionuclides in food and environmental samples. In doing that, data from 1988 to 2015 was reviewed to ascertain whether the Laboratory has being performing as required in providing quality results on food and environmental samples measured. Besides this data (records kept), the evaluation also covered some Technical Quality Control measures, such as Energy and Efficiency Calibration, that need to be put in place for such laboratories. The laboratory meets almost all conditions and equipment requirements of IAEA (1989), however the laboratory falls short of the management requirements of ISO 17025. Based on the results it was recommended, among others, that management of the laboratory should ensure there are procedures for how calibration and testing is performed for different types of equipment and also the competence of all who operate specific equipment, perform tests, evaluate results and sign test reports ensured. University of Ghana http://ugspace.ug.edu.gh 2 CHAPTER ONE INTRODUCTION The quest for a cost effective performance-based evaluation for the assessment of the technical ability of an analytical laboratory to perform acceptably over its lifetime, has been a subject of much concern in recent years. This chapter provides the background information and explains the reason for the study, its importance, objectives and scope. 1.1 Background The world is said to be radioactive and has been since it was created. Over 60 radionuclides (radioactive elements) can be found in nature, and they can be placed in three broad categories namely: a) Primordial – in existence since creation of the Earth b) Cosmogenic - formed as a result of cosmic ray interactions with the atmosphere. c) Human produced - enhanced or formed due to human actions (minor amounts compared to natural) Radionuclides are found naturally in the atmosphere, water, soil as well as human beings. Every day, humans ingest and inhale radionuclides in the air, food and drinking water . This is because natural radioactivity is common in the rocks and soil that make up our planet, in water and oceans, and in building materials and homes. As a result of human activities such as industrial, nuclear accidents, weapon testing, radionuclide from both natural and artificial origin could widely spread in the environment. University of Ghana http://ugspace.ug.edu.gh 3 In addition, humans can also be exposed to radiation in the environment from man- made activities, such as medical diagnostic intervention in nuclear medicine procedures. As a result of these human activities, radionuclides from both natural and artificial origin could be released into soil and water bodies. Human beings could possibly be exposed to these radionuclides through the direct ingestion of contaminated water. Indirectly, crops grown on contaminated soil could eventually be consumed by man. Similarly, animals grazing on contaminated grass could be a source of exposure through the consumption of meat and milk products. Whether, man-made or natural in origin, radioactive element passes through the food chain in the same way as non-radioactive material. The level of harm to human health depends on the type, amount of radionuclides, and the exposure time. The exposure of radiation to humans differs from place to place and among individuals. When there is a release of radioactivity following an emergency at a nuclear power plant; land, rivers, sea and structures in the vicinity of the power plant can become contaminated with a fission product generated inside the reactor. Individuals can therefore become exposed to these radionuclides released into the environment. When these radioisotopes are discharged into the environment, they affect foods by either falling onto the surface of foods like fruits and vegetables or animal feed as deposits from the air or through contaminated rainwater. Radioactivity in water can also accumulate in rivers and the sea, contaminating fish and seafood. Once in the environment, radioactive material can also get into food as it is taken up by plants, seafood or ingested by animals. Assessment of any release of radioactivity into the environment is therefore important in ensuring protection of the public, especially if University of Ghana http://ugspace.ug.edu.gh 4 the released radioactivity can enter the food chain. Such assessment demands rapid, reliable and practical techniques for analyses of various radionuclides. In April 1986, the Chernobyl nuclear power plant disaster in Ukraine was the product of a flawed Soviet reactor design coupled with serious mistakes made by the plant operators. The accident caused the largest uncontrolled radioactive release into the environment ever recorded for any civilian operating nuclear power plant, and large quantities of radioactive substances were released into the environment for 10 days. This caused serious social and economic disruption for large populations in Belarus, Russia and Ukraine. Two radionuclides, the short-lived iodine-131 and the long-lived caesium-137, were particularly significant for the radiation dose delivered to members of the public, (WNO, 2016). Several organisations reported on the impacts of the Chernobyl accident, but had problems assessing the significance of their observations because of the lack of reliable public health information before 1986 (WNO, 2016). Some Member States of the International Atomic Energy Agency (IAEA) requested the assistance of the Agency in conducting radio analyses on a large number of food and environmental samples and in developing their own laboratory capabilities for this purpose. In the course of the IAEA’s response to these requests it became evident that there was a need for laboratories capable of performing rapid and reliable measurements of radionuclides on a variety of sample materials and capable of handling large numbers of samples. As a result of the above, Ghana instituted a monitoring programme to ensure food safety. Through the assistance of the IAEA, Ghana instituted the Food and Environmental monitoring programme during the 1980’s. Through the IAEA’s University of Ghana http://ugspace.ug.edu.gh 5 support, Ghana was able to develop the basic manpower and acquired basic equipment to carry out food monitoring, particularly on milk and milk products imported into the country. The Radiation Protection Board (RPB) through the Radiation Protection Institute (RPI) of the Ghana Atomic Energy Commission (GAEC) was given the mandate to carry out the monitoring programme. Since the food and environmental monitoring programme was instituted, the capability of the program has evolved, therefore this study seeks to evaluate the programme over the years and compare with the requirements as provided for in the IAEA Technical Report Series number 295 (IAEA, 1989). 1.2 Radiation Protection, Food and Environmental Monitoring Laboratory a. The Food and Environmental Monitoring Laboratory (FEML) b. Food Monitoring Programme The Ghana Atomic Energy Commission (GAEC) has been monitoring food products both imports and exports since 1986 before the Radiation Protection Board was established in 1993. In pursuance of the provisions of the Radiation Protection Instrument of the Radiation Protection Board (RPB), Legislative Instrument (LI 1559) of 1993 (RPB, 1993), and in line with international requirements as well as to satisfy some importing countries requirements on some Ghana goods/products, for export, the RPB has continued to monitor milk and milk products for radioactivity contamination. The RPB carries out radiation contamination test on food products such as cocoa beans, cocoa cake, tuna fish, and Nestle products (such as Cerelac and other milk products), which are to be exported to countries like Egypt, Algeria Nigeria, Abidjan and Tunisia. It is important to note that before these products are University of Ghana http://ugspace.ug.edu.gh 6 accepted into the importing countries, the product must be accompanied by an appropriate Radiation Contamination Test Certificate from the country of origin. In pursuance of the LI 1559, the RPB monitors food products such as meat/poultry, milk and milk products imported into Ghana in order to quantify the activity concentrations of caesium-134 (134Cs) and caesium-137 (137Cs) that might be found in the sample. c. Environmental Monitoring Programme Naturally occurring radionuclides are present in the environment at varying levels depending on the geological formation of the area. In addition, human activities including mining have the potential to increase the levels. Mining has been identified as one of the potential sources of exposure to Naturally Occurring Radioactive Materials, [NORMs] (UNSCEAR, 2000). However, mining companies are not being regulated for NORM in most countries including Ghana. On the average, about 342 metric tonnes of gold ore is processed annually yielding about 13,365,000 oz. of gold (Goldfields, 2007). These mining operations turn out large volumes of solid and liquid wastes in the form of waste dams, slime dams and tailing dams, which could contain elevated levels of NORMs. These materials could wash off onto surface water bodies and farmlands during run-offs. Risk assessment and contamination test is conducted on environmental samples like soil and water from some of the mining areas by the Food and Environmental Monitoring Laboratory. The laboratory has been in existence for over 25years, and therefore it has become necessary to carry out an assessment of the monitoring programme to ascertain the effectiveness and standard of measurements, procedures and processes at the Food and Environmental Laboratory, Radiation Protection Institute. University of Ghana http://ugspace.ug.edu.gh 7 1.3 Statement of Problem The food and environmental monitoring laboratory has been in existence since the late 1980’s following the nuclear disaster in Chernobyl in 1986. The laboratory has provided services to various stakeholders in Ghana including exporters, researchers, and students. However, since the establishment of the laboratory, there has never been a thorough evaluation of the activities of the laboratory to provide assurance of the quality of analytical results emanating from the laboratory. In addition, the laboratory does not participate in International Inter-comparison Exercises enabling the RPI-FEML to monitor its performance and to evaluate the quality of data churn out by the laboratory. In view of that, this study is being conducted to help establish the status and performance of the laboratory in providing quality analytical services to its cherished clients. 1.4 Objectives The objective of this study is to assess the performance level of the Food and Environmental monitoring laboratory of the RPI with respect to the requirements of the IAEA standard analytical laboratory practices (IAEA, 1989) and the Management and Technical Requirements of ISO 17025. Specifically to: i. To review records of the laboratory from 1988 to 2015; ii. Evaluate the performance of the RPI-FEML radio-analytical laboratory against the requirements of the IAEA Guide for measurement of University of Ghana http://ugspace.ug.edu.gh 8 Radionuclides in Food and the environment (IAEA Technical Report Series No.295; 1989), and the International Standard Organization’s ISO/ IEC 17025 17025. iii. To provide useful recommendations for laboratory management in the quest to obtain ISO/IEC 17025 accreditation. 1.5 Scope of the Study This study is focused on the performance of the Food and Environmental Monitoring Laboratory of the Radiation Protection Institute of the Ghana Atomic Energy Commission which has been involved in monitoring of radionuclides in food and environmental samples. 1.6 Relevance of Study In addition to routine radio-analytical measurements, the RPI’s Food and Environmental Lab contributes knowledge to applied research projects funded by individuals and industries. These include studies in the field of radiation protection as well as scientific research targeted at development of improved radio-analytical methods. This study would contribute to improvement in the quality of data produced by the RPI’s Food and Environmental Laboratory. University of Ghana http://ugspace.ug.edu.gh 9 CHAPTER TWO LITERATURE REVIEW This Chapter reviews literature related to the concept of operations and laboratory standards. Literature on ISO 17025 and IAEA Technical Report Series 295 will also be reviewed. 2.0 ANALYTICAL LABORATORY An analytical laboratory undertakes tests, or analyses, of samples or materials in a purpose built laboratory. The tests are undertaken to identify and to quantify, as necessary, the composition of the sample, or the material, that is analysed. Different laboratories have different functions, and support either a single scientific discipline, example chemistry, or a number of different scientific disciplines, e.g., chemistry, biology and physics, within the same facility. For the purposes of this study, an analytical laboratory is a laboratory that practices one, or more, of these scientific disciplines in a purpose built laboratory facility. Traditionally, analytical laboratories have some level of interaction with their customers, who supply, or arrange to supply, laboratory samples to the laboratory for processing. Laboratories also interact with their suppliers, who provide various inputs, such as chemical reagents, laboratory consumables and scientific technology, for use in the analysis processes and other associated activities. As a result of these various activities, there are many opportunities for improved, laboratory performance across all of the activities involved in delivering results of an analysis. University of Ghana http://ugspace.ug.edu.gh 10 2.1 The Analytical Laboratory as a Service Organisation Analytical laboratories are generally classified as being part of the service industry. They primarily act as a reporting service, which supplies analytical results, or data, to their customers in the form of a test report. Customers then use the output analysis data to address their particular issues and problems. This perception of a laboratory as a service provider often means that laboratory selection by a customer is driven by factors such as quality, price, and turn-around time. These drivers have the potential, in turn, to influence laboratory decision-making in relation to the selection of test processes and analytical technology. Poor decisions by the laboratory may adversely influence the quality of the data provided. The potential also exists for environmental harm to arise from poorly conceived sampling and analysis programs driven only by financial considerations and operating under the traditional approach. 2.2.1 Primary Standard Dosimetry Laboratories (PSDLs) A PSDL is a national laboratory designated by the government for the purpose of developing, maintaining and improving primary standards in radiation dosimetry. A PSDL participates in the international measurement system by making comparisons through the medium of the ˝Bureau Internationale des Poids et Mesuresʺ (International Bureau of Weights and Measures), and provides calibration services for secondary standard instruments (ISO 17025). University of Ghana http://ugspace.ug.edu.gh 11 2.2.2 Secondary Standard Dosimetry Laboratory Secondary Standard Dosimetry Laboratory (SSDL) is an international network of dosimetry laboratories established by the International Atomic Energy Agency (IAEA) and the World Health Organization (WHO). The network provides a framework of international comparisons of the absorbed dose measurements that help to maintain consistency and accuracy particularly amongst the radiotherapy community. The SSDLs are designated by national laboratories (such as Primary Standard Dosimetry Laboratories, PSDL) to provide national and international radiation dosimetry traceability to users, (ISO 17025). 2.2.3 National Reference Laboratory The national reference laboratory is an internationally recognised centre for the study of nuclear, non-nuclear, isotopic or elemental analysis of trace elements. Its wide- ranging roles encompass testing, non-testing, administrative, advisory and supervisory roles. Other roles include guiding the standards of training of personnel to be deployed in laboratories, standardisation of equipment, reagents and consumables, and the quality control of the testing procedures and results. In order to perform these roles, the laboratory is expected to achieve and maintain certain minimum standards. Key considerations are the premises, the people working in them, policies that guide operations, the equipment and other tools of the trade, competency in the use of the equipment, mechanisms for the communication of test results and the availability of financial resources. Standards are essential for the realisation of these functions, (ISO 17025). University of Ghana http://ugspace.ug.edu.gh 12 2.3 Analytical Laboratory Performance There are several factors that influence laboratory operational performance, these include the equipment performance, adequacy of facility, trained personnel and QA/ QC, this section reviews the operations and the functions of analytical laboratories. 2.2 Laboratory Performance Evaluation Some laboratories evaluate their performance based on the types of measures employed and the type of laboratory involved. In most cases, laboratory performance evaluation is based on outputs, but this is rarely applied across laboratories. For example, a university might look to the number and quality of publications and research; a routine laboratory to the number of samples completed, or profit generated; an industrial laboratory to the number of problems solved; and a government laboratory to the value to society (Lifshin, 1996). Another approach to performance evaluation suggests that a better evaluation of laboratory performance is the value contributed to achieving organisational goals and objectives (Collins, 2001). Many laboratories support the need to achieve recognition from a parent organisation by applying performance evaluation and benchmarking based on cost effectiveness and the timely delivery of services. Laboratory benchmarking and performance evaluation has the potential to impact on the laboratory’s management. Customer satisfaction measures not only the performance of the laboratory, but also reflect on the performance of the laboratory manager. Laboratories are rated on the quality of results they submit. An individual result is acceptable if it falls within acceptable performance limits and is unacceptable if it University of Ghana http://ugspace.ug.edu.gh 13 falls outside that limits. Once again, these performance limits are established by calculation of the mean and standard deviation from values reported by a pre- selected group of reference laboratories. 2.2.1 Evaluation of Performance Indicators Performance indicators are measures of the analytical process that the laboratory monitors as part of its routine QC programme. Performance indicators demonstrate whether the analytical process is performing as planned, when it has exhibited a statistical anomaly that requires investigation, and when a system has failed. Accordingly, monitoring performance indicators using established statistical techniques provides the laboratory with an effective tool for self-assessment that allows the identification of trends or conditions that, while still within the established bounds of acceptability, are drifting or trending out of control. These conditions can be addressed prospectively, allowing the laboratory to maintain analytical control. Additionally, this process allows the development of a database regarding a protocol's or system's behavior over time or under a specified set of conditions. 2.2.1 Tolerance Limits In some situations, the acceptance limits for a QC parameter may be based on professional judgment rather than statistics. Tolerance limits are used much like the control limits on a control chart to determine whether investigation and corrective action are required. Tolerance limits may be used when it is important to detect large changes in the variable. For example, tolerance limits could be used when variability within the limits has no significant impact on the measurement process. University of Ghana http://ugspace.ug.edu.gh 14 An example of a variable that may sometimes appear to shift by small amounts is the resolution of a high-purity germanium detector. It also tends to be true that even statistically significant changes in the resolution are often so small that they have no practically significant effect on analytical results. So, it is reasonable to specify tolerance limits for the resolution at full width at half maximum (FWHM), rather than statistically based control limits. Another example of a variable that is commonly monitored using tolerance limits is the chemical yield for an analytical process. Typically the yield is measured with relatively small uncertainty; so, fluctuations of the yield over some range of values may have no substantial impact on the quality of the measurement. However, a yield that is significantly greater than 100 percent generally indicates a spurious error of some kind, and a yield that is very low may indicate a spurious error or other problem in the measurement process that deserves investigation. 2.2.2 Measurement Uncertainty Every analytical measured result is uncertain to some degree. If these measurement uncertainties are large relative to the tolerances needed for decision making, the data may not be useful for their intended purpose. In order to determine the significance of a sample result, all reported values should be accompanied by the laboratory's best estimate of the uncertainty associated with the result. The "combined standard uncertainty" (one-sigma uncertainty) is obtained by propagating the uncertainties of all the input quantities that contribute to the calculation of the derived value. University of Ghana http://ugspace.ug.edu.gh 15 The combined standard uncertainty is used to indicate the statistical confidence in interpreting the performance indicator's ability to assess analytical quality. The estimated statistical confidence level that is usually associated with 1 combined standard uncertainty is about 68%, the confidence level for 2 combined standard uncertainties is about 95%, and the confidence level for 3 combined standard uncertainties is about 99%. It is important that the combined standard uncertainty be a fair estimate because it will indicate when the analytical process could be approaching the limits of statistical control and corrective actions should be initiated. A performance indicator exceeding ±2 combined standard uncertainty limits from the indicator's historical mean value may indicate that corrective action should be considered, and a performance indicator exceeding ±3 combined standard uncertainty limits from the indicator's historical mean value may indicate that an investigation must be conducted and corrective action may be necessary. Because statistical confidence never reaches 100 percent, it probably would be prudent to confirm the measurement for the performance indicator when it exceeds ±2 combined standard uncertainty limits. If the performance indicator value for repeat measurements do not exceed ±2 combined standard uncertainty limits, one may conclude that the first measurement was a statistically allowable event. However, if the excursion is repeated, appropriate investigative actions should be considered. 2.2.2 Certified Reference Materials Certified reference materials (CRMs) are well-characterized, stable, homogeneous materials with physical or chemical properties that are known within specified uncertainty limits. Laboratories that analyze CRMs can compare their performance to University of Ghana http://ugspace.ug.edu.gh 16 the certified concentration and uncertainty levels. CRMs are used for the calibration of an apparatus or the assessment of a measurement method. Metrology organizations issue CRMs in various matrices with critically evaluated concentration values for the radionuclide constituents. The usefulness of a reference material depends on the characterization of the radionuclide source, activity levels, and their estimated uncertainties. CRMs can be used as internal laboratory QC samples to evaluate the ability of analytical methods to handle the matrix. CRMs need not be known to the analyst but can be introduced into the analytical stream as a blind. A numerical performance indicator for the analysis of a CRM is essentially the same as that for a laboratory control sample. Excursions in the CRM results can be used to identify various out-of-control situations. The advantage of the CRM is that the sample matrix is always the same, and the levels of analytes are known to a high degree, so uncertainties in matrix effects and radionuclide content should not be a factor in evaluating excursions. A rapid and one-time excursion in the Standard Reference Material usually indicates that a mistake was made in the procedure. A rapid change with continued occurrences suggest that something occurred that is out of the ordinary, such as a new analyst performing the procedure or the use of a new batch of calibration solutions or reagents. Slow changes showing a trend usually indicate degradation or contamination of equipment or reagents. If a CRM result shows elevated concentrations, analysts should check for contamination sources or poor instrument or tracer calibration. If the results show University of Ghana http://ugspace.ug.edu.gh 17 decreased concentrations, the analyst should check for poor techniques or expired or poorly prepared reagents and solutions. CRM results may indicate a bias in the measurement process. Tracking the performance of several consecutive CRM measurements will show if the method or the laboratory consistently obtains high or low results. If the results are consistently higher or lower than the certified values, they should be evaluated for a statistical difference, example, tested. When the test indicates a statistical difference, a bias is indicated and the laboratory should investigate the cause of the bias and correct or characterize it. 2.2.3 Traceability Comparing results from different laboratories or from the same laboratory at different times, with confidence is important. This can be achieved by ensuring that all laboratories are using the same measurement scale, or the same ‘reference points’. This is also achieved by establishing a chain of calibrations leading to primary national or international standards, ideally (for long-term consistency) the Systeme Internationale (SI) units of measurement. A clear example is the case of analytical balances; each balance is calibrated using reference masses which are checked against national standards and to the primary reference kilogram. This chain of comparisons leads to a known reference value which provides ‘traceability’ to a common reference point, ensuring that different operators are using the same units of measurement. In routine measurement, the consistency of measurements between one laboratory and another is greatly aided by establishing traceability for all relevant intermediate measurements used to obtain or control a measurement result. University of Ghana http://ugspace.ug.edu.gh 18 Traceability is therefore an important concept in all branches of measurement. (Eurachem, 2012) 2.3 Instrumentation Performance Indicators Radiometric and non-radiometric instruments are used currently to quantify radionuclides in a variety of environmental matrices, and quality control measures are necessary to ensure proper instrument performance. This section presents radiometric instrument performance measures that indicate a measurement system is in control. The specific quality control procedures to be followed depend on the measurement equipment. Sufficient checks are needed to demonstrate that the measurement equipment is properly calibrated, the appropriate background has been recorded, and that all system components are functioning properly. QC measures for instrumentation should include at a minimum: (1) instrument background measurements, (2) instrument calibration with reference standards, and (3) periodic instrument performance checks subsequent to the calibration. Acceptable control limits should be specified in appropriate laboratory documents. 2.3.1 Instrument Background Measurements Radiation detection instruments have a background response even in the absence of a sample or radionuclide source. In determining the instrument's response to radioactivity contributed by the sample alone (net), the instrument background response is subtracted from the sample-plus-background response (gross). Background correction is more critical when the instrument net response is small relative to the background. Control of contamination and routine monitoring of instrument background are therefore integral parts of a control program. Improper University of Ghana http://ugspace.ug.edu.gh 19 background correction results in analytical error and will increase the uncertainty of data interpretation. Differences in instrument backgrounds may indicate instrument malfunction. Variations may take the form of rapid increase or decrease in background, slow increase or decrease in backgrounds, and highly variable or erratic backgrounds. These variations can result in the measurement system's reduced precision and decreased detection capability. Rapid or significant increases in background measurements may be due to instrument or blank contamination, insufficient shielding with relocation of nearby radionuclide sources, or large scale equipment malfunction (example, a broken window on a gas proportional system). When the instrument background is more variable than expected, the reliability of measurements becomes questionable, resulting in loss of confidence and increased uncertainty. This indicates a loss of control over the measurement environment, or limitations of the data handling software. The root cause of the variability should be identified and corrected to re-establish statistical control over the instrument background. 2.3.2 Efficiency Calibrations The number of counts recorded by a detector is converted to activity (actual radionuclide transformations) by empirically determining this relationship with traceable radionuclide sources when available. This relationship is expressed in the system's efficiency calibration. A separate efficiency is determined for each detector- source combination and is typically energy or radionuclide specific. University of Ghana http://ugspace.ug.edu.gh 20 Detector efficiency is critical for converting the detector's response to activity. Routine performance checks can evaluate several aspects simultaneously (sample geometry, matrix) and provide a means to demonstrate that the system's operational parameters are within acceptable limits. These are typically included in the assessment of the analytical method's bias and are specified in terms of percent recovery based on the source's known disintegration rate. Performance checks for measurement efficiency are usually determined statistically from repeated measurements with a specific check source. Detection of a shift in measurement efficiency should be investigated. 2.3.3 Energy Calibrations All radiation measurements are energy dependent to a certain extent. However, spectrometric techniques such as gamma and alpha spectrometry identify radionuclides based on the energy of the detected radiations. For these techniques a correct energy calibration is critical to accurately identify radionuclides. Problem with energy calibration may result in misidentification of peaks. Spectrometry systems should be calibrated so that each channel number is correlated with a specific energy. To identify radionuclides correctly, this energy calibration needs to be established initially and verified at regular intervals. The energy calibration is established by determining the channel number of the centroid of several peaks of known energy over the applicable energy range. Typically, a minimum of three peaks is used, and commercially available sources contain nine or ten photopeaks. The relationship between energy and channel number can be determined by a least squares fit. To account for non-linearity, a second or third order fit may be used. However, these require more points to define the curve. For example, a first order calibration requires at least two points, while a second order University of Ghana http://ugspace.ug.edu.gh 21 calibration requires a minimum of three points. The end points of the curve define a range of applicability over which the calibration is valid, and peaks identified outside the curve's range should be used carefully. The uncertainty associated with the curve should be available at any point along the calibration curve. Quality control checks for energy calibration can be combined with checks for efficiency calibration and resolution. Radiations emitted over the energy range of interest are measured, and two or more peaks are used to demonstrate that the energy calibration falls within acceptable limits. Check sources may consist of a single radionuclide or a mixture of radionuclides (example, mixed gamma). Because only the location of the peak is of concern, there is no requirement that the check source be calibrated or certified, except for ensuring that it does contain the radionuclide(s) of interest at a specified level of purity. The energy calibration is determined by setting the system initially and then adjusting the gain of the amplifier, analog-to-digital conversion (ADC) gain, and zero. The criteria that indicate when readjustment is required because of gradual and abrupt changes in the energy versus channel calibration should be established as an integral part of the system's operating procedure. These changes usually are monitored by the measurement system's software, and the user specifies the allowable difference between that the system's response and the radionuclide's known energy. The tolerable difference often relates to the instrument's resolution. For example, a high resolution instrument such as an intrinsic germanium detector typically will have acceptable limits on the order of a few keV, while a low resolution instrument such as a NaI detector typically will have acceptable limits on the order of several tens of keV. University of Ghana http://ugspace.ug.edu.gh 22 Spectra also can be analyzed by identifying each peak manually. With manual identification, the acceptable limits for the energy calibration are determined for each spectrum based on the professional judgment of the person analyzing the spectrum. The frequency of QC checks for energy calibrations can be related to the expected resolution of the instrument, the electronic stability of the equipment, or the frequency needs of QC measurements for efficiency calibration or resolution. (MARLAP, 2004). 2.3.3 Calibration of Apparatus Used for Mass and Volume Measurements Fundamental to quantitative analysis is the use of the proper masses and volumes. The analysts must be careful in performing gravimetric and volumetric measurements such as preparation of calibration solutions, test sources, and reagent in order to achieve the desired levels of precision and bias in each analytical method. Laboratory balances and volumetric glassware and equipment should be calibrated and checked periodically to maintain the desired method performance levels. 2.4 Statistical Means of Evaluating Performance Indicators - Control Charts 2.4.1 Statistical Quality Control The term statistical quality control refers to QC based on statistical principles. Generally, statistical QC in the laboratory applies the principles of hypothesis testing, with varying degrees of rigor, to make inferences about a measurement system or process, (MARLAP, 2004). University of Ghana http://ugspace.ug.edu.gh 23 An important reason to establish statistical QC in the laboratory is to ensure that measurement uncertainties are properly estimated. The uncertainty estimate that accompanies a measured value may be misleading unless the measurement process is in a state of statistical control. Statistical control implies that the distribution of measured results is stable and predictable. It exists when all the observed variability in the process is the result of random causes that are inherent in the process. The existence of variability due to .assignable causes, including instrumental and procedural failures and human blunders, which are not inherent in the process, implies that the process is unpredictable and hence “out of control” (MARLAP, 2004). Statistical QC procedures are designed to detect variations due to assignable causes. When such variability is detected, specific corrective action is required to determine the cause and bring the measurement process back into a state of statistical control. Laboratory QC procedures should be definitive enough to detect variations in the measurement system that could have a significant impact on measurement uncertainties, (MARLAP, 2004). Statistical QC also may be used in the laboratory to monitor method performance parameters, such as chemical yield, to ensure that the measurement system is performing as expected. However, the need for corrective action in the case of a low yield may not be as urgent as in the case of a malfunctioning radiation counter, since the latter is much more likely to cause underestimation of measurement uncertainties. The primary tool for statistical QC is the control chart. (MARLAP, 2004). University of Ghana http://ugspace.ug.edu.gh 24 2.4.2 Control Charts for Instrument Response Every control chart has control limits, which define the acceptable range of the monitored variable. Many charts have both upper and lower limits. However, when changes in only one direction are of concern, only one limit is necessary. Most control charts have a central line, or reference line, which is an estimate of the expected value of the monitored variable. Many control charts also have warning limits, which lie between the central line and the control limits (UNIDO, 2009) By definition, control limits are action limits. A single measured value that falls outside these limits normally requires that one stop the measurement process, and investigate the problem, and if necessary take corrective action. The warning limits are optional but recommended, since they help one to identify and investigate possible problems before control limits are exceeded (UNIDO, 2009) Control charts based on grouped observations often are more powerful tools for detecting shifts of the monitored variable than charts based on individual observations. Average charts, or X charts, are used to monitor the arithmetic means of measured values obtained in rational sub-groups, which are sub-groups of equal size chosen to ensure that the measurement variability within each sub-group is likely to represent only the inherent variability of the measurement process produced by non-assignable causes. When an X chart is used, a range chart, or R chart, is generally used in tandem to monitor within-group variability. (The range of a set of values is the difference between the largest value and the smallest.) A control chart for individual values (X chart or I chart) is used when it is impractical to obtain measured values in the groups needed for an 𝑋 chart. In this case, a moving range chart (MR chart) is often used as well to monitor variability. University of Ghana http://ugspace.ug.edu.gh 25 The moving range chart is an R chart based on the absolute differences between consecutive measured values. (MARLAP, 2004) A radioactive check source is normally used to monitor the radiation response/efficiency of every radiation counting instrument. It is recommended that the activity and count time for the source be chosen to give no more than 1 percent counting uncertainty (ANSI N42.23). In other words, at least 10,000 counts should be obtained in each measurement of the source. There may be cases when placing a high-activity source in a detector is undesirable, so obtaining 10,000 counts is impractical. The instrument response may not have a Poisson distribution. In this case, if the check source is long-lived, an X or 𝑋 chart based on replicate measurements should be set up. An X or 𝑋 chart is the appropriate radiation response/efficiency chart for a high-purity germanium detector when the area of a specific photopeak is monitored, since the calculated size of the photopeak may have significant sources of uncertainty in addition to counting uncertainty. An X or 𝑋 chart may be used even if the response is truly Poisson, since the Poisson distribution in this case is approximated well by a normal distribution, but slightly better warning and control limits are obtained by using the unique properties of the Poisson distribution. 2.5 Quality Assurance in the Laboratory Environment Globally, everyone is concerned with the quality of services offered by the laboratories (Kiline, 2008). For a laboratory to be able to produce accurate and precise results, laboratory personnel must be well-trained, motivated, and have documented standard operating procedures. Standard operating procedures must be University of Ghana http://ugspace.ug.edu.gh 26 formulated in a way that they can identify and correct erroneous results before they reach the customers (Kiline, 2008). Suksai et al. (2010) reported that hospital mortality rates can be lowered if testing laboratories produce the correct first time results that assist physicians with their diagnosis. Kiline (2008) describes a quality management framework as one that will include the “5Q’s”. The “5Q’s” stands for quality assurance, quality control; quality improvement; quality indicators and quality systems. A quality framework must be designed in a way that there is continuous feedback to ensure that root causes to arising issues are identified and corrective and/or preventive actions implemented. Critical factors for a successful implementation of a quality standard include acceptance and commitment by each member of the team involved to generate “quality culture”. The documentation of the system should be simple and flexible, so that employees can identify with it. The system as a whole should be self-sustainable and add value to the organization (Grochau et. al., 2010). The main purpose of laboratories is to produce and deliver accurate and reliable measurement results at all times. In order to ensure that laboratories produce accurate and reliable results, there are control programs and quality assurance that can be implemented (Klinkner, 2008). Laboratories produce and issue a test/calibration certificate as their end product. The product produced by the laboratory is delivered to the customer in the form of a document, which is a test/calibration certificate. The test/calibration certificate is the only document which goes out of laboratory shelves in the form of ‘product’ (Gupta, 2010). When selecting a laboratory to provide service of testing or calibration, the potential customer needs to be sure that the supplier can issue valid results. There are a lot of factors that contribute to a University of Ghana http://ugspace.ug.edu.gh 27 laboratory’s technical competence. These include: the competence of laboratory personnel, the reliability of equipment, documented and validated test methods, proper sampling procedures and traceability of measurement to national and international standards (Robertson, 2010). 2.6 Laboratory Information Managing Systems Dlamini (2005) reports that, the Laboratory Information Management System (LIMS) impacts operations of the laboratory positively. Nowadays managing information in the organisations has become an integral part of business. Test results issued by the laboratories are very important in the production processes. They have a direct impact on the process of meeting the requirements of the customers. Management must show leadership and implement corrective action and/or preventive actions. This can only be achieved using an effective laboratory management system (Dlamini, 2005). According to Van Eeden (2005) the implementation of LIMS results in major improvements within the laboratory. The major improvement in the laboratory is identified as the turn-around time from receiving the sample until the approved results are issued. The systems eliminate non-value-adding debates about who is responsible for delaying tests results because every activity is traceable. Employing qualified and competent employees in laboratories gives them confidence when issuing results. Sometimes, the importance of hiring skilled laboratory personnel is taken lightly and not recognised. Highly automated measurement systems and test equipment cannot replace the importance of competent laboratory personnel. It is precisely when highly automated systems are used that competent University of Ghana http://ugspace.ug.edu.gh 28 personnel are needed. Staffs that are competent would be able to utilise equipment to its full potential. Equipment reproducibility would be even more consistent (Apps, 2006). 2.7 Laboratory Personnel Competency and Performance Measurement Laboratories face the challenge of running short of skilled personnel. This shortage and the availability of automated equipment tempt laboratories to go down the path of utilising sophisticated instruments that are operated by low skilled personnel. While this might appear to be a cost saving exercise and is attractive, it has costly consequences. There is higher throughput per person due to automated systems which means that one mistake affects output. Personnel depend largely on the supplier even for minor equipment service and troubleshooting. When laboratories use low skilled personnel, skilled personnel spend time verifying the results produced by those low skilled personnel. That practice is counter-productive (Apps, 2006). One of the methods used by laboratories to measure the performance of laboratory personnel includes observing the person conducts a test or analysis. This method is time consuming and counterproductive. It can even be seen by personnel as discriminatory and unfair labour practice. Most laboratories have a procedure in place of handling an out of specification instrument. But most do not have an equivalent procedure for laboratory personnel, even though the testing of personnel plays a critical role in laboratory testing (Apps, 2006). University of Ghana http://ugspace.ug.edu.gh 29 2.8 Description of ISO 17025 Requirements that laboratories have to satisfy according to ISO 17025 include validation protocols, measurement traceability, competence of personnel, and environmental conditions of the laboratory (Bednarova & Waddington, 2010). The clauses of ISO 17025 are discussed below. 2.8.1 Organisation The laboratory or organisation should be an entity that can be held legally responsible. If the laboratory is part of an organisation it should not be directly under functions like production, finance or marketing. An arrangement like that will ensure that laboratory management is free from undue pressures where the quality of results may be sacrificed for profit, production volumes or speedy sample turnaround time. In cases of commercial laboratories, it should not act as a consultant for its customers. This could result in the laboratory’s integrity of results and independent judgment being at stake (Gabi, 2006) Clause 4.1.5(b) on organization of the ISO 17025 standard covers a requirement which ensures that both management and personnel are free from undue pressures that may adversely affect the quality of their work (Gabi, 2006). Factors like basic compensation, fringe benefits, leave, grievance procedures and economic protection against hazards are included in the employment contract of laboratory personnel and these factors help to reduce undue pressures, but they do not necessarily provide total protection unwarranted pressure and influences (Gabi, 2006). The importance of deputies for key positions in the laboratory is very critical. This can relieve management from some of the pressures resulting from the heavy University of Ghana http://ugspace.ug.edu.gh 30 workloads (Gabi, 2006). There must be adequate staffing in the entire laboratory to avoid pressures associated with work overload (Gabi, 2006). 2.8.2 Management System The laboratory should establish, implement, and maintain a management system that is relevant to the scope of its activities (Gabi, 2006). The policies, systems, programmes, procedures to ensure the quality of results need to be documented and presented in the form of a quality manual (Gabi, 2006). Quality objectives should also form part of the quality manual and should be reviewed during the management reviews. The quality policy statement should be issued under the authority of top management (Gabi, 2006). 2.8.2.1 Document Control According to Gabi (2006), a laboratory should establish and maintain procedures to control all the documents that form part of the management system. Documents could be of either internal or external origin and can include regulations, software, standards, drawings and specifications in any media (Gabi, 2006). The document control procedure should cover the process of approving documents, issuing documents and also the changes to documents (Gabi, 2006). 2.8.2.2 Review of Requests, Tenders and Contracts The laboratory should have clearly defined procedures to review requests, tenders and contracts (Gabi, 2006). The lead times agreed upon should be within the laboratory’s capability. Lead times should incorporate allowances for contingencies University of Ghana http://ugspace.ug.edu.gh 31 (Gabi, 2006). All the records of reviews should be maintained in accordance with the document control procedures (Gabi, 2006). 2.8.2.3 Subcontracting of tests and calibrations When a need for a laboratory to subcontract has been identified due to unforeseen reasons, competent suppliers should be used. A competent supplier could be one who is certified to ISO 17025 (Gabi, 2006). The customer whose work is tested by a subcontractor needs to be informed in writing and the laboratory will still be responsible to the customer for the subcontractor’s work, except in the case where the customer or a regulatory authority specifies which subcontractor is to be used, (Gabi, 2006). 2.8.2.4 Purchasing services and supplies The laboratory should have a documented policy and procedure for the selection and purchasing of services and supplies it uses that affect the quality of the results (Gabi, 2006). The laboratory needs to be given a reasonable budget to avoid undue financial pressures (Gabi, 2006). The laboratory should be at liberty to select quality brands and grades of analytical materials to be used in the testing processes (Gabi, 2006). 2.8.2.5 Service to the customer The laboratory should be willing to cooperate with customers on clarifying the customer’s requests and in monitoring the laboratory’s performance in relation to the work performed. But the laboratory should always ensure confidentiality to other customers (Gabi, 2006). University of Ghana http://ugspace.ug.edu.gh 32 2.8.2.6 Complaints A systems approach to the analysis of root causes and corrective actions should be defined in the form of a policy and procedure (Gabi, 2006). Complaints from customers should not be regarded as an indication of poor performance of laboratory management and testing personnel (Gabi, 2006). They should be seen as an opportunity for continuously improving the quality management system. If complaints are not viewed from a systems perspective that may result to laboratory personnel issuing results that will please their customers in order to protect their jobs (Gabi, 2006). 2.8.2.7 Control of Non-Conforming Testing and/or Calibration Work The laboratory should have policies and procedures that are implemented when any aspect of its testing or calibration work do not conform to its own procedures or the agreed requirements of the customer (Gabi, 2006). 2.8.2.8 Improvement The only way to ensure continuous improvement in the laboratory system is through management reviews (Theodorou & Anastasakis, 2008). The management review agenda should include discussion points like suitability of policies and procedures, reports from managerial and supervisory personnel, outcome of recent internal audits, non-conformances, corrective/preventive actions, results of external quality assessments, inter-laboratory comparisons or proficiency testing schemes, changes in the volume and type of work, customer feedback, complaints and improvement suggestions (Theodorou & Anastasakis, 2008). Issues such as QC activities, University of Ghana http://ugspace.ug.edu.gh 33 resources and staff training can also be included on the agenda (Theodorou & Anastasakis, 2008). 2.8.2.9 Corrective Action The laboratory should establish a policy and a procedure that will assist them in implementing corrective action if any non-conformances occur in the form of non- conforming testing or deviations from procedures (Gabi, 2006). Once the corrective action to be implemented has been chosen, it should be implemented and monitored to ensure its effectiveness (Gabi, 2006). Additional audits can be conducted to verify the effectiveness of the implemented corrective action (Gabi, 2006). 2.8.2.10 Preventive Action When improvements and potential sources of non-conformities have been identified, a preventive action should be developed, implemented and monitored to reduce the likelihood of the occurrence of non-conformance and to take advantage of the opportunities for improvement (Gabi, 2006). The preventive action procedure should include the initiation of the action and the application of controls to ensure that they are effective (Gabi, 2006). 2.8.2.11 Control of Records The laboratory should establish and maintain procedures for identification, collection, indexing, access, filing, storage, maintenance and disposal of quality and technical records (Gabi, 2006). That should include records from internal audits, management reviews, as well as corrective and preventive action. Records should be stored in a secure space and in confidence (Gabi, 2006). University of Ghana http://ugspace.ug.edu.gh 34 2.8.12 Internal Audits The laboratory should develop a pre-determined audit schedule and procedure to conduct internal audits. The internal audit programme should address the elements of the management system including the testing or calibration activities (Gabi, 2006). If resources permit, audits should be conducted by qualified personnel who are independent of the activity being audited (Gabi, 2003). 2.8.13 Management Reviews Certified laboratories or laboratories aiming at certification put a lot of effort into meeting the technical requirements of the accreditation standards (training, calibration and method validation) but some managerial requirements, for example management review are considered of lesser importance; however they are very critical (Theodorou & Anastasakis, 2008). Management reviews are key processes in many quality management systems. These include laboratory management systems like ISO 17025 and ISO 15189. These reviews are an opportunity to understand and manage all the inputs and outputs of a quality management system. In many quality management systems, management review is a critical requirement of the system. Laboratory standards like ISO 17025 are no exception (Theodorou & Anastasakis, 2008). 2.8.14 Technical Requirements There are factors that determine the validity and reliability of the tests performed by the laboratory (Sithole, 2006). Those include human factors, accommodation and environmental conditions, test and calibration methods and method validation, University of Ghana http://ugspace.ug.edu.gh 35 equipment, measurement traceability, sampling and the handling of test and calibration items (Sithole, 2006). 2.8.15 Personnel The laboratory management should ensure the competence of all who operate specific equipment, perform tests, evaluate results and sign test reports (Sithole, 2006). If personnel are undergoing training, they need to work under the supervision of a person who has already been declared competent. Personnel’s competence should be assessed on a continuous basis, to keep up with changes in technology (Sithole, 2006). 2.8.16 Accommodation and Environmental Conditions The clause on accommodation and environmental conditions, stipulates that the environment in the laboratory should allow laboratory personnel to produce valid and reliable results (Gabi, 2006). Incompatible materials and activities should be segregated to avoid cross contamination (Gabi, 2006). The environmental conditions may be stated in the method but also requires the competency of personnel to be able to establish if the validity of result will be affected if there is no control (Sithole, 2006) 2.8.17 Test and Calibration Methods and Method Validation The laboratory should use appropriate methods and procedures for all tests and calibrations within its scope (Sithole, 2006). Those include sampling, handling, transport, storage and preparation of items to be tested or calibrated, and where appropriate, an estimation of the measurement uncertainty as well as statistical techniques for analysis (Sithole, 2006). The laboratory can use laboratory developed University of Ghana http://ugspace.ug.edu.gh 36 methods, non-standard methods, these must be done in consultation with the customer (Sithole, 2006). The test methods used by the laboratory should be validated, that is confirmed by objective evidence that the particular requirements for a specific intended use are fulfilled (Sithole, 2006). 2.8.18 Equipment The laboratory should be properly furnished with items for sampling, measurement and test equipment required for the correct performance of the tests or calibrations (Sithole, 2006). All the equipment and software used for testing, calibration and sampling should be capable of achieving the accuracy required (Sithole, 2006). 2.8.19 Measurement Traceability Laboratories need capable equipment that is maintained and calibrated at set intervals to ensure traceability to national and international standards (Sithole, 2006). Records of equipment maintenance and calibration should be maintained. Reference standards, reference material, and intermediate checks should be used to ensure traceability of testing or calibration (Sithole, 2006). 2.8.20 Sampling The process of sampling is a critical requirement that needs to be taken into account to achieve valid results (Sithole, 2006). Where the laboratory is involved in sampling, the laboratory should have established and unbiased sampling procedures and adhere to that (Gabi, 2006). Gabi (2006) points out that laboratories involved in the regulatory testing field, should receive samples that are identified by codes and true identities withheld. It University of Ghana http://ugspace.ug.edu.gh 37 should be a practice for laboratory personnel not to be in direct contact with the sample owners. The arrangement guards laboratory personnel from being offered bribes and victimization by sample owners. 2.8.21 Handling of Test and Calibration Items The laboratory should have procedures for the transportation, receipt, handling, protection, storage, retention and disposal of test or calibration items including all provisions necessary to protect the integrity of the test or calibration item, and to protect the interests of the laboratory and the customer (Sithole, 2006). 2.8.22 Assuring the Quality of Test and Calibration Results The laboratory should have quality control procedures for monitoring the validity of tests and calibrations undertaken (Sithole, 2006). The monitoring of tests or calibration could include participation in inter-laboratory or proficiency testing programmes, retesting or recalibration of retained items, replicate tests or calibration using the same or different methods, regular use of certified material or internal quality control using secondary reference materials (Sithole, 2006). 2.8.23 Reporting the Results The results of each test or calibration carried out by the laboratory should be reported accurately, clearly, objectively and in accordance with any specific instructions in the test or calibration methods (Sithole, 2006). An approved template needs to be used to generate all the test reports or calibration certificates (Sithole, 2006). When opinions and interpretation are included in the reports, the laboratory should document them on the basis upon which they have been made. Opinions and interpretation should be clearly marked as such in the report (Sithole, 2006). University of Ghana http://ugspace.ug.edu.gh 38 2.9 Benefits of ISO 17025 certification Governments and regulators can benefit a lot by using ISO 17025 certified laboratories. Certification to ISO 17025 increases confidence in data issued by laboratories. It reduces uncertainties associated with decisions that affect the protection of human health and the environment. It is seen as a seal of approval, and therefore increases public confidence. It facilitates trade and economic growth, gives laboratories a marketing advantage, international recognition and can be used as a benchmark for performance (Robertson, 2010). Sithole (2006) reports that implementing a laboratory quality standard and certifying it can benefit laboratories. It serves as a standard to transmit information; encourages transparency as activities are documented and accessible to all personnel, assist personnel in the understanding and application of policies, it is a good marketing tool to give customers confidence about the reliability and consistency of their service providers. It is a training tool for new employees, ensures uniformity of the organisation’s practices and tasks, and assists personnel to make decisions (Sithole, 2006). Bailey (2003) warns that ISO 17025 has been criticised for the emphasis it places on documentation, records and record keeping. Experience has shown that this criticism is to some extent true, but careful drafting of laboratory policies and procedures can significantly reduce the record keeping workload (Bailey, 2003). Care must be taken to select the correct data and information for inclusion in laboratory records. Records are essential and the effective use and interpretation of recorded information and data is essential to maintaining a consistently high laboratory performance (Bailey, 2003). University of Ghana http://ugspace.ug.edu.gh 39 2.10 IAEA Technical Report Series 295 Requirements for Food and Environmental Laboratories During the course of the Supplementary Programme on Nuclear Safety, it became evident to the IAEA that there was a serious lack of analytical capabilities within its Member States to cope with nuclear releases. The IAEA therefore relied on experts and specialists in the radioanalytical field to provide guidelines for collecting, preparing and analysing relevant environmental material and basic food for radionuclides of interest. This resulted in the publication of Technical Report Series 295 (TRS 295). 2.10.1 Accommodation Table 2.0 lists the number of rooms and the area recommended by TRS 295 for a central laboratory's activities. However, organizations that are just beginning to set up monitoring facilities need not establish a full-scale operation as outlined. However, good judgement in selecting the appropriate facilities and equipment will facilitate the establishment of a scaled down and adequate monitoring laboratory (IAEA, 1989) University of Ghana http://ugspace.ug.edu.gh 40 Table 2. 1: Rooms and Area Recommended for a Central Environmental Laboratory Operations No. of Rooms Area (m ) Sample registration, storage and preparation: Evaporation and drying Grinding Ashing Handling of higher activity samples 7-8 130-180 Gamma ray spectrometry laboratory: Preparation and storage of samples Counting room Computer room 3-4 90-120 Alpha spectrometry laboratory Radiochemical laboratory Counting room Computer room 3-4 60-70 Offices, Administration Social rooms, Library, 4-10 80- 150 Source: IAEA Technical Report Series 295(1989) 2.10.2 Laboratory Design The central laboratory should be designed and built according to the requirements of a normal analytical laboratory with a few additional features such as special ventilation, specially designed rooms for receiving and storing samples, and specially constructed nuclear measurement facilities (counting room(s)). Storage space should be available to accommodate all types of sample materials. Storage shelves or bins should be constructed of materials that are easily decontaminated in case of spills. (IAEA TRS 295, 1989). 2.10.3 Ventilation The ventilation system should be designed to filter incoming air to all areas and to maintain the lowest pressure in areas used for handling high activity samples and for preparing the samples. The sample receiving room(s) should be at low pressure to prevent any possible contamination of other laboratories by incoming samples. University of Ghana http://ugspace.ug.edu.gh 41 Wet chemistry laboratories should have well ventilated fume hoods. Counting rooms should be under positive pressure at all times. (IAEA Technical Report Series 295, 1989) 2.10.4 Temperature Constant temperature and humidity should be maintained in counting and computer rooms and should be set according to the recommendations of the manufacturers of instruments and equipment. Normal temperatures recommended for counting rooms are between 20 °C and 26 °C (IAEA Technical Report Series 295, 1989) 2.10.5 Instrumentation required for Gamma Radiation Measurement: A fully integrated gamma spectrometry system for qualitative and quantitative determination of gamma emitters is required by Technical Report Series 295. According to IAEA (1989), the system should comprise a germanium detector, shield, multichannel analyser (MCA), high-speed printer, and (optionally) a plotter. Nal(Tl) detector (8% resolution), a 2048-channel analyser and a lead shield with an inside diameter of about 20 cm and a wall thickness of 5-10 cm. Other laboratory equipment, for sample collection and preparation, listed in IAEA (1989) are: i. Large refrigerator for preserving samples; ii. Freezer for storing samples; iii. Crusher and/or grinder ; iv. Evaporator or evaporation lamps; v. Large drying oven; and vi. Freeze dryer (as an option). University of Ghana http://ugspace.ug.edu.gh 42 2.10.4 Personnel requirements Personnel required to staff a central environmental laboratory includes: a. A Manager (Chief Scientist); b. 2 Scientists; c. 3 Senior Technicians; d. 6 Technical Assistants; e. 1 Secretary f. 1 Field Technician to operate trucks, other vehicles and boats for sample collection; g. 1 maintenance and service Technician familiar with electronic equipment. 2.10.6 TRAINING The staff of local laboratories must undergo continuous training in order to maintain the radioactivity measurement capability adequate for routine measurements and to be ready for any possible emergency. 2.10.7 ANALYTICAL QUALITY CONTROL Quality control measures are necessary to provide documentation to show that the analytical results are reliable. 2.10.7.1 Analysis by different methods. In cases where agreement is good, results are assumed to be accurate. Control analysis with reference materials that are as similar as possible to the materials to be University of Ghana http://ugspace.ug.edu.gh 43 analysed. Agreement between certified and observed values is then a direct measure of accuracy for that particular determination. (MARLAP, 2004) 2.10.7.1 Participation in an Inter-laboratory Comparison. Samples used in such an inter-comparison should be, as far as possible, similar in composition and concentration to the samples to be analysed on a routine basis. The agreement of results received from a particular laboratory with the most probable mean value obtained from statistical evaluations of all the results will be a measure of the accuracy for that particular determination. Participation on a regular basis will detect a systematic error that is those due to improper calibration, contamination or incorrect methods of calculation. 2.10.7.2 Calibration and Standards It is desirable and often necessary that calibrations of measurement systems be carried out with standards of the radionuclides to be determined. Standards should be accompanied by certificates which specify activity, purity and accuracy (IAEA Technical Report Series 295, 1989). 2.10.8 Internal Control Programmes The laboratory should operate a routine programme to maintain the equipment and the validity of the results (IAEA Technical Report Series 295, 1989) University of Ghana http://ugspace.ug.edu.gh 44 2.10.8.1 Equipment performance The laboratory should routinely check the status of equipment by checking background and standard samples. Quality control charts be kept for each system on a routine basis. m 2.10.8.2 Analytical control samples The validity of the analytical results should be checked by an internal standards programme which incorporates the use of blind duplicates, blanks and standards. These results often give the first indication of analytical difficulties. Analytical control samples, submitted with each group of samples to be analysed, generally constitute 10-15% of the total samples. Laboratory control standards can be developed by preparing large, homogeneous batches of material for various sample types. By analysing these controls in duplicate or triplicate, sufficient data will be available in a short time to establish the "standard" value. This material can also be run by several other reliable laboratories as a check. 2.10.9 Data Presentation The results of the sample analysis should be presented in such a way that the reader can evaluate the data and the conclusions. The presentation should discuss as a minimum: i. Location, collection method and preparation procedures; ii. Analytical method and specifications of the equipment. The report on environmental radioactivity should contain tables with the following characteristics: University of Ghana http://ugspace.ug.edu.gh 45 (a) The International System (SI) units and symbols should be used (b) Some standard units of presentation are: a. Air in Bq/m3 b. Water and milk in Bq/L c. Deposition in Bq/m2 d. Soil in Bq/kg dry mass and Bq/m2 e. Grass in Bq/kg dry mass and Bq/m2 f. Foods in Bq/kg fresh mass. (c) The value should be given to the correct number of significant figures; (d) The precision of the data should be indicated and the form of expressing this data should be clearly explained, for example the standard error, the two-sigma error, and the counting error. Where possible the accuracy of the data should be indicated, generally by reference to the supporting data for the particular method used. (e) Where low levels of activity are indicated, the lower limit of detection should be indicated and the method used for its calculation should be referenced (IAEA Technical Report Series 295, 1989). University of Ghana http://ugspace.ug.edu.gh 46 CHAPTER 3 METHODOLOGY This Chapter presents the method for evaluating the performance indicators of the RPI Food and Environmental Monitoring Laboratory. 3.1 Description of the Facility The Food and Environmental Monitoring Laboratory is part of the Environmental Protection and Waste Management Centre, Radiation Protection Institute, Ghana Atomic Energy Commission. The Laboratory is located within the same building with the Ghana Research Reactor- 1 on the premises of the Ghana Atomic Energy Commission (GAEC). The facility has a registry room which also serves as technologist office, sample preparation room, a counting/ computer room, store room and a wash room. The Radiation Protection Institute serves as the technical arm of the Radiation Protection Board which is the competent national authority for environmental radioactivity monitoring among others. The RPI laboratory performs detailed analyses on all types of environmental materials such as water, soil and air, as well as imported and exported food samples, in order to quantify the radionuclides concentration in them. The laboratory is capable of performing the required radioactive contamination measurements for determination of Gamma emitters by non-destructive gamma ray spectrometry. The Food and Environmental Laboratory is equipped with two low background gamma ray spectroscopic systems, the High Purity Germanium detectors (HPGe) and the Sodium Iodide Detector. University of Ghana http://ugspace.ug.edu.gh 47 In-situ measurements are usually included in the environmental radioactivity monitoring programme. In situ measurements are performed for: the qualitative and the quantitative determination of a potential radiological contamination, Radon analysis and characterization of the materials. The laboratory also serves as a National Central Reference Laboratory and a research laboratory for students from the School of Nuclear and Allied Sciences (SNAS), College of Basic and Applied Sciences, University of Ghana- Atomic. 3.2 Administration of Questionnaire This took the form of a list of questions (Appendix A) given to twelve (12) respondents to answer with the rationale of getting data on the topic under study. The respondents included; the Director, previous Centre Managers, Research Scientist and Technologist working in the Laboratory. Self-administered questionnaires as opposed to the postal questionnaires was used. The questions in the questionnaire took the form of Close-ended Questions and offered a set of alternative answers from which the respondents were asked to choose the one that most closely represents their view. It is to be emphasized that the questionnaire allowed respondents time to think through the questions to provide accurate answers. The researcher conducted pre-testing of the draft questionnaire with few potential respondents in an informal manner before following up with the full scale questionnaire administration. The purpose of the study was explained to officials and those who responded to the questionnaires and interviews. The survey contained questions which respondents could choose from three relevant responses; No, Partially or Yes. The responses were coded (No = 0, partially = 1 and Yes = 2) and summarized on the basis of the information provided by the University of Ghana http://ugspace.ug.edu.gh 48 respondents. The most straightforward form of analysis, and one that often supplies much of the basic information need, to tabulate results, question by question, are ‘one-way tables’ (Statistical Services Centre, 2001). This was done using the original questionnaire and writing on it the approximated average score of each question. Though this method does not identify which respondents produced particular combinations of responses, this is often useful when a quick and/or simple summary is required. The analysis was done using Microsoft Excel, 2016 quantitative tool. 3.3 Physical Examination and Observation of Documents and Procedures This study was carried out by comparing information and data that existed in the Food and Environmental Laboratory of the RPI to the standard requirements that need to be available for the laboratory to perform effectively and efficiently. The requirements were based on the ISO 17025 International standard as well as the IAEA Guide for Laboratories performing the Measurement of Radionuclides in Food and the Environment (IAEA, 1989). The assessment covered the suitability and performance of the facility with respect to the following areas: i. Laboratory Design: Test facilities should be of suitable size, construction and location to meet the requirements of the study. The facility should be spacious enough to avoid overcrowding, cross contamination and confusion between projects. The area should be big enough to accommodate the number of staff working in it, and allow them to carry on their work without risk of getting in one another’s way or of mixing up different materials. Each operator should have a workstation sufficiently large to enable him/her to carry out the operation efficiently. To reduce University of Ghana http://ugspace.ug.edu.gh 49 the chance of mix-up of materials or of cross-contamination, there should also be a degree of physical separation between the workstations. The workstations must be built of materials that allow easy cleaning and that are not likely to allow test materials to accumulate and contaminate one another. There should be a ventilation system that provides air-flow away from the operator through filters which both protect personnel and prevent cross-contamination (GLP Hand, 2009). Arrangement There should be separate areas for: a. Storage of test items under different conditions. b. Storage of control items. c. Handling of volatile materials. d. Weighing. e. Mixing of different chemicals. f. Cleaning equipment. g. Offices and Changing rooms (GLP Hand, 2009). University of Ghana http://ugspace.ug.edu.gh 50 Table 3. 1: The checklist below developed to assist in the workplace inspection Department: Environmental Protection and Waste Management Centre. Date: 10 /03/ 2016 Area inspected: Food and Environmental Monitoring Laboratory Inspected by: Lilian Ataa Agyeman Laboratory Environment Inspection item Yes No N/ A Notes Adequate number of rooms x Number of rooms was counted and compared to the required number in the TRS 295 Adequate Laboratory Space x Lab. Space was measured and compared to the required space for each room in the TRS 295 Availability of adequate Laboratory bench x “AUTHORISED ENTRY ONLY” signage is displayed at the laboratory entrances x The laboratory is locked when unattended x Hand washing facilities are available adjacent to the main entry/exit x Benches, floors and furniture surfaces are smooth, impervious, chemically resistant and easy to clean x Benches are clean, tidy and uncluttered x Floor is clean, dry and uncluttered x All areas are adequately lit x Adequate Ventilation x Temperature is within acceptable limits e.g. 20- 260C x University of Ghana http://ugspace.ug.edu.gh 51 ii. Equipment available and Equipment Performance Test iii. Availability of qualified and well trained personnel iv. Reporting of results v. Record keeping vi. Maintenance: The requirement that equipment be properly maintained is based on the assertion that this ensures the constant performance of equipment to specifications and that it reduces the likelihood of an unexpected breakdown and consequent loss of data (GLP, 2009). Routine maintenance should be documented such that users of equipment can be assured of its reliability. A label attached to the equipment or provision of a clear service plan may ensure this. Records of equipment calibration, checking and maintenance demonstrate that the respective SOPs have been followed and that equipment used was adequate for the task and operating within its specifications. Maintenance documentation in the laboratory was assessed. vii. Standard Operating Procedures: A full set of good Standard Operating Procedures (SOPs) is a prerequisite for successful good laboratory Practice compliance. All documents within the laboratory was reviewed but the was no written document or protocols found in the laboratory. viii. Management system to ensure quality services University of Ghana http://ugspace.ug.edu.gh 52 Data from 1988 to 2015 were reviewed to ascertain whether the Laboratory has been performing as required in providing quality results on food and environmental samples measured. 3.3 Equipment Performance Test For Gamma spectroscopy, energy and efficiency calibration of the detector system of the gamma spectrometer is vital and it forms an important part of the analytical technique in analysing environmental and food samples for radioactivity. This is to enable the identification and quantification of radionuclides in the samples. Standard sources are usually used for calibration. The calibration standard source must have the same geometry as the samples to be analysed, so that the deviation in the measured activity is minimized (Harb et al., 2008b). The energy and efficiency calibration of the system was carried out by using a multinuclide certified reference standard. The standard consists of an aqueous mixture of nine radionuclides in a 1.0 Litre Marinelli beaker. The standard consist of the following radionuclides with their corresponding energies; 241Am (4.694kBq), 109Cd (14.54kBq), 139Ce (1.355kBq), 57Co (1.156), 60Co (2.697), 137Cs (2.689kBq), 113Sn (4.000kBq), 85Sr (4.570kBq), and 88Y (5.323kBq). The standard was counted for 36,000 seconds. 3.3.1 Energy calibration The above described reference standard was used for the calibration. The energy calibration of the germanium detector system was done by counting the standard for 36,000 seconds. The gain of the system was adjusted so as to position the 662 keV of 137Cs to the channel number of the multichannel analyser in relation to the gamma ray energy. University of Ghana http://ugspace.ug.edu.gh 53 After these adjustments are made, the gain of the system should remain fixed. The channel number that corresponds to the centroid of each Full Energy Peak on the Multichannel Analyser was recorded and plotted on a linear graph on the X-axis against the gamma ray energy on the Y-axis. A linear curve was obtained in the plot of the data. The slope and intercept of the energy calibration line was determined by least squares calculations. The equation relating the energy and the channel number is given by the expression [Reguigui, 2006; Gilmore and Hemingway, 1995]. Eγ=A0+A1CN (Eq. 3.1) where Eγ is the energy in keV, CN is the channel number for a given radionuclide, and Ao and A1 are calibration constants for a given geometry. 3.3.2 Efficiency Calibration The radiation detector must be calibrated to determine the relationship between the observed count rate of the detector and the emission rate of the source being assayed. This relationship is called the efficiency calibration, typically expressed as counts per second/emissions per second, or cps/dps-and is an integral part of the measurement protocol. For alpha spectrometry systems, the efficiency of detection is energy- independent. Efficiencies for gamma spectrometry are energy dependent, and an efficiency calibration typically covers a range for a specific counting geometry. The mixed radionuclide standard used for the energy calibration was again used for the efficiency calibration by counting it on the High Purity Germanium Detector for another 36000 seconds. The net count for each of the spectrum was determined and their corresponding energies were used in finding the efficiencies. University of Ghana http://ugspace.ug.edu.gh 54 The efficiency at each energy was plotted as a function of the peak energy and extrapolated to determine the efficiencies at other peak energies for each of the measurement. To calculate the efficiency, Equation 3.2 was used )**()( tPA NE  (Eq. 3.2) Where N is the full peak energy net count corresponding to the gamma photons with energy Eγ and gamma emission probability P, A is the activity of the radionuclide in the calibration standard and t is the counting time. 3.3.3 Instrument Background Measurement In general, radionuclide detection covers more than 17 orders of magnitude of sample activity, from irradiated material that produces high radiation fields to environmental samples. All radiation detection instruments have a background response even in the absence of a sample or radionuclide source. (MARLAP, 2004). The instrument's background measurement was determined in the absence of a radionuclide source. The background was counted for 24 hours with an empty well sterile 1L Marineli beaker, and then a second counting was done with the above described standard on the detector for another 24 hours as the gross count. To determine the instrument's response to the radioactivity contributed by the sample (standard) alone (net), the instrument background response is subtracted from the sample (standard) - plus-background response (gross). The instrument background is an important factor in determining the ability to achieve a specific minimum detectable activity (MDA). University of Ghana http://ugspace.ug.edu.gh 55 3.3.4 Determination of Minimum Detectable Activity (MDA) Detection limits of a Gamma- ray spectrometry detector is used to express the detection capability of a measurement system under certain conditions. MDA is an estimate for the lowest amount of activity of a specific gamma-emitting radionuclide that can be detected at the time of measurement. (MARLAP, 2004). The background response of the detector was determined and then, the reference standard was counted on the detector for 36000 s. The average background peaks was used to determine the MDA. The minimum detectable activities were calculated using the equation below: (DWAF, 2002) 𝑀𝐷𝐴 = σ√𝐵 ƞ.𝑃.𝑇.𝑊 (𝐵𝑞/𝑘𝑔) (Eq. 3.3) Where; σ is the statistical coverage factor equal to 1.645 (confidence level 95%); B is the background for the region of interest of each radionuclide; T is counting time in seconds; W is the weight of the sample container; P is the gamma emission probability (gamma yield) of each radionuclide; and ƞ is the photopeak efficiency for the measured gamma ray energy. University of Ghana http://ugspace.ug.edu.gh 56 3.4 Statistical Analysis of the Performance of the Gamma Spectrometry System A radioactive check source (137Cs of activity1Ci) was counted 60 seconds for 100 times. The central line, and, control and warning lines for the X chat, were determined using the following procedure (assuming the system is under statistical control): Step 1: The sum of the counts ( ∑ 𝑋𝑖 ) and the mean of the counts ( 𝑋 ) were calculated Step 2: The experimental standard deviation was calculated from the relation; 𝑠 = √[ 1 𝑛−1 ∑ (𝑋𝑖 − 𝑋) 2 𝑛 𝑖=1 ] (3.5) Step 3: The unbiased estimate 𝜎 of the standard deviation was calculated from the relation; 𝜎 = 𝑠 𝑐4 (3.6) Where 𝑐4 = 4𝑛−4 4𝑛−3 The central line (CL), control limits (UCL and LCL) and warning limits (UWL and LWL) were calculated as follow: 𝐶𝐿 = 𝑋 (3. 7) 𝑈𝐶𝐿 = 𝑋 + 3𝜎 (3.8) 𝐿𝐶𝐿 = 𝑋 − 3𝜎 (3.9) 𝑈𝑊𝐿 = 𝑋 + 2𝜎 (3.10) 𝐿𝑊𝐿 = 𝑋 − 2𝜎 (3.11) After the construction of the X-Chart, another set of 100 counts (60 seconds each) of the Cs source was carried out. The data obtained was used to statistically monitor the radiation response/efficiency of the gamma detector. University of Ghana http://ugspace.ug.edu.gh 57 CHAPTER 4 RESULTS AND DISCUSSIONS The results and discussions of the research conducted are presented in this chapter. Data collected from managers and staff of the Laboratory provided evidence of the extent to which ISO 17025 and Technical Report Series 295 are used in the operational performance of the RPI Laboratory. 4.1 Compliance with ISO 17025 4.1.1 Personnel Training Records It is necessary for the laboratory to have staff training and competence records. These should include, at least, a record of each staff member’s formal qualifications, previous experience and date of recruitment; a list of the activities for which the staff member has been trained and record of regular re-assessment of the staff member’s competence at each of the activities. One purpose of the training records is to serve as a source of reference for supervisors who wish to ensure that the person whom they intend to allocate to a task is properly trained and that their training is up to date. The laboratory does not have an established quality assurance system that clearly defines procedure for declaring employees competent. Methods like training of personnel by a competent person, taking part in proficiency testing schemes and intra-laboratory test samples are not used. There are no procedures in place to measure the effectiveness of training once training has been conducted. The variability of the responses, as shown in Table 4.1, indicates there are no personnel records as such training records must be available in the laboratory. It must University of Ghana http://ugspace.ug.edu.gh 58 be noted that assessors will not accept training records held in the personnel office at Ghana Atomic Energy Commission. Figure 4. 1: Percentage responds to questions on personnel training records Table 4. 1: Average response to questions on personnel training records No. Personnel Training Records Approximated Average Score a1 Do you have a record of the qualifications and experience of your staff, with objective evidence of their qualifications, for example copies of certificates? 1 a2 Do you have a clear record with regard to your proposed scope of accreditation of which members of staff are authorized to conduct each test or calibration? 1 a3 Do you have a documented procedure for training staff in quality issues and technical procedures, including tests? 1 a4 Do you have a documented procedure for conducting evaluation of the competence of staff after training and before authorising them for the procedure in which they were trained? 0 a5 Do you have a system for recording training, including objective evidence of competence? 0 a6 Do you have a mechanism for identifying which staff conducted each procedure, test or calibration? 1 1 0 10 20 30 40 50 60 70 80 a1 a2 a3 a4 a5 a6 P er ce n ta ge o f R es p o n d en ts ( % ) Responds to Questions No Partial Yes University of Ghana http://ugspace.ug.edu.gh 59 4.1.2 Accommodation and Environmental Conditions Though staff members’ response indicated that there are some environmental factors in the laboratory which might impact on the validity of tests or calibrations and activities which need to be separated to avoid, for example, cross contamination, much has not been done to put measures in place to determine and minimise environmental factors in the laboratory which might impact on the validity of tests or calibrations. Also there are no documented requirements for test or calibration to be done under specific environmental conditions (Table 4.2). Figure 4. 2: Percentage responds to questions on accommodation and environmental conditions existing in the laboratory 0 10 20 30 40 50 60 70 a7 a8 a9 a10 a11 a12 P er ce n ta ge o f R es p o n d en ts ( % ) Responds to Questions No Partial Yes University of Ghana http://ugspace.ug.edu.gh 60 Table 4. 2: Approximated Average Score of responds to questions on accommodation and environmental conditions existing in the laboratory No. Accommodation and environmental conditions Approximated Average Score a7 Have you considered whether there are any environmental factors in your laboratory which might impact on the validity of tests or calibrations? 2 a8 Are you conducting any tests or calibrations where the published procedure which you claim to follow includes a requirement for the work to be done under specific environmental conditions, for example temperature or humidity? 1 a9 If there are such factors, do you have procedures in place to control and monitor them? 1 a10 Do you have any activities which need to be separated to avoid, for example, cross contamination? 1 a11 Do you have any activities which need to be separated to avoid, for example, cross contamination? 2 Average 1 4.1.3 Quality assurance for the screening process From Table 4.3, the laboratory seems to have determined the accuracy, precision and, where relevant, the limit of detection of the methods which are used, including standard published methods. However, all the other indicators of a good assurance for the screening process have not been properly established. University of Ghana http://ugspace.ug.edu.gh 61 Figure 4. 3: Percentage responds to questions on quality assurance for the screening process Table 4. 3: Approximated Average Score of responds to questions on quality assurance for the screening process No. Quality assurance for the screening process Approximated Average Score a13 Do you have a set of methods specified as acceptable for use in your laboratory? 1 a14 Are they documented to the extent necessary to ensure they are applied properly and consistently? 1 a15 If not, have you evidence to show that the methods you are using are fit for the purpose claimed and acceptable to your clients? 1 a16 Have you determined the accuracy, precision and, where relevant, the limit of detection of the methods which you use, including standard published methods? 2 a17 Do you run routine quality control samples and evaluate the results before releasing data? 1 a18 Do you monitor trends in quality control results in order to anticipate possible problems? 1 a19 Have you tested your methods and laboratory by use of certified reference methods and/or inter- laboratory comparison? 1 Average 1 0 10 20 30 40 50 60 70 80 a13 a14 a15 a16 a17 a18 a19 P er ce n ta ge o f R es p o n d er s (% ) Responds to Questions No Partial Yes University of Ghana http://ugspace.ug.edu.gh 62 4.1.4 Equipment The respondents indicated there is a plan for periodic calibration and verification of the performance of all equipment which affects the validity of measurements (Table 4.4). Nevertheless, there is only a partial system for commissioning equipment and verifying its performance and calibration before it is used for test or calibration work and to some extent there are some measures in place for commissioning equipment and verifying its performance and calibration. Figure 4. 4: Percentage responds to questions on equipment in the RPI lab 0 5 10 15 20 25 30 35 40 45 50 a20 a21 a22 a23 P er ce n ta ge o f R es p o n d en ts ( % ) Responds to Questions No Partial Yes University of Ghana http://ugspace.ug.edu.gh 63 Table 4. 4: Approximated Average Score of responds to questions on equipment in the RPI lab No. Equipment Approximated Average Score a20 Do you have a system for commissioning equipment and verifying its performance and calibration before it is used for test or calibration work? 1 a21 Do you have a plan for periodic calibration and verification of the performance of all equipment which affects the validity of measurements? 2 a22 Do you have records showing that this plan is followed and which enable the status of any equipment to be verified at any point in its history of use? 1 a23 Is equipment subject to regular checks or calibrations labelled so that its status can be seen immediately by users? 1 Average 1 4.1.5 Traceability of measurement Management policy to ensure that the calibration is maintained at all times, records which could be audited to confirm the calibration status of the equipment at any point in the past and means of identifying all the measuring equipment which is involved, directly or indirectly, in measurement are not well developed (Table 4.5). Despite this it must be noted the respondents claimed equipment are calibrated in a manner which provides traceability to the international measurement system. University of Ghana http://ugspace.ug.edu.gh 64 Figure 4. 5: Percentage responds to questions on traceability of measurement Table 4. 5: Approximated Average Score of responds to questions on traceability of measurement No. Traceability of measurement Approximated Average Score a24 Have you identified all the measuring equipment which is involved, directly or indirectly, in measurement or calibration and which, if not properly calibrated, would affect the validity of measurements? 1 a25 Is this equipment calibrated in a manner which provides traceability to the international measurement system? 2 a26 Do you have a management procedure to ensure that the calibration is maintained at all times, i.e. recalibration is conducted as necessary and, where possible, equipment is monitored so that any drift away from calibration will be detected? 1 a27 Do you have records which could be audited to confirm the calibration status of the equipment at any point in the past? 1 Average 1 0 10 20 30 40 50 60 70 80 a24 a25 a26 a27 P er ce n ta ge o f R es p o n d en ts ( % ) Responds to Questions No Partial Yes University of Ghana http://ugspace.ug.edu.gh 65 4.1.6 Administration of work and sample tracking The answers to the questions on administration of work and sample tracking revealed that procedure for receiving samples into the laboratory, storage of samples and the procedures required to be carried out on samples by laboratory staff are not clearly spelt out. Samples are however numbered as soon as possible (Table 4.6). Figure 4. 6: Percentage responds to questions on administration of work and sample tracking Table 4. 6: Approximated Average Score of responds to questions on administration of work and sample tracking No. Administration of work and sample tracking Approximated Average Score a28 Do you have procedure for logging samples into your laboratory? 1 a29 Are all samples uniquely numbered as soon as practicable after receipt? 2 a30 Does your system ensure that samples are stored securely and in a way that will preserve them against any changes which may affect data generated from them? 1 a31 Do you have a system for ensuring that the procedures required to be carried out on samples are clearly communicated to laboratory staff? 1 a32 Do you have a procedure to ensure reports are checked to make sure they correspond to the raw data? 1 Average 1 0 10 20 30 40 50 60 70 a28 a29 a30 a31 a32 P er ce n ta ge o f R es p o n d en ts ( % ) Responds to Questions No Partial Yes University of Ghana http://ugspace.ug.edu.gh 66 4.1.7 Recording of Results and Associated Data According to the responses, there is a system in place to ensure that all observations are recorded at the time they are made (Table 4.7). Data recorded by the Laboratory in 2014 using a Sodium iodide detector is as shown in Appendix B. Though a recording has been established, data preservation, policy on how amendments to entries are to be made and the means of identification of persons making entries are not fully in operation. Figure 4. 7: Percentage responds to questions on Recording of Results and Associated Data Table 4. 7: Approximated Average Score of responds to questions on Recording of Results and Associated Data No. Recording of Results and Associated Data Approximated Average Score a33 Does your system ensure that all observations are recorded at the time when they are made? 2 a34 In this record, is the raw data always preserved so that any problems can be investigated? 1 a35 Do you have a policy on how amendments to entries on laboratory records are to be made? 1 a36 Does the system allow the person making any record to be identified? 1 Average 1 0 10 20 30 40 50 60 70 a33 a34 a35 a36 P er ce n ta ge o f R es p o n d er s (% ) Responds to Questions No Partial Yes University of Ghana http://ugspace.ug.edu.gh 67 4.1.8 Computer Systems There are no procedures for regular backup of data held on computers and software used is not secured against unauthorised changes. From Table 4.8, respondents insisted that there is control of what software may be loaded onto any of laboratories computers, and all computer systems are checked to ensure that they record and process data correctly. Figure 4. 8: Percentage responds to questions on computer systems Table 4. 8: Approximated Average Score of responds to questions on computer systems No. Computer systems Approximated Average Score a37 Do you have control of what software may be loaded onto any of your computers? 1 a38 Are all computer systems, including software, checked to ensure that they record and process data correctly? 1 a39 Is all software secured against unauthorised changes? 1 a40 Do you have a procedure for regular backup of data held on computers? 1 Average 1 0 10 20 30 40 50 60 70 a37 a38 a39 a40 P er ce n ta ge o f R es p o n d en ts ( % ) Responds to Questions No Partial Yes University of Ghana http://ugspace.ug.edu.gh 68 4.1.9 Reporting Requirements There is no defined or documented reporting format in use at the laboratory. There is on the other hand a partial system to ensure reports reach only those entitled to receive them. Figure 4. 9: Percentage responds to questions on reporting requirements Table 4. 9: Approximated Average Score of responds to questions on reporting requirements No. Reporting requirements Approximated Average Score a41 Do you have a defined report format? 1 a42 Does this comply with the detailed requirements of ISO 17025? 1 a43 Does your system ensure reports always reach only those entitled to receive them? 2 a44 Does the report acknowledge subcontracted work? 0 a45 Do you have a policy on how to deal with situations where it becomes apparent that suspect data has been reported? 1 a46 Do you have a clear identification of staff authorised to approve reports? 1 Average 1 0 10 20 30 40 50 60 70 a41 a42 a43 a44 a45 a46 P er ce n ta ge o f R es p o n d en ts ( % ) Responds to Questions No Partial Yes University of Ghana http://ugspace.ug.edu.gh 69 4.1.10 Purchasing Services and Supplies The laboratory attaches great value to the quality of any purchased goods or services which might affect the quality of data; as such a system for checking all received materials for conformity is in place. However, policies on selection and rejection of suppliers have not been established as stated in Table 4.10. Figure 4. 10: Percentage responds to questions on Purchasing services and supplies Table 4. 10: Approximated Average Score of responds to questions on purchasing services and supplies 0 10 20 30 40 50 60 70 80 a47 a48 a49 a50 P er ce n ta ge o f R es p o n d en ts ( % ) Responds to Questions No Partial Yes No. Purchasing services and supplies Approximated Average Score a47 Do you take steps to control the quality of any purchased goods or services which might affect the validity of your data? 1 a48 Do you have a list of approved suppliers and a policy on their selection? 1 a49 Do you keep this list under review and remove any suppliers found to be inadequate from a quality perspective? 1 a50 Do you have a system for checking all received materials against the order specifications? 1 Average 1 University of Ghana http://ugspace.ug.edu.gh 70 4.2 Complying with IAEA Technical Report Series 295 (TRS 295) The RPI Environmental Laboratory complies with all the conditions and equipment as required by TRS 295, except provisions for a ventilation system that has not been provided (Table 4.11). From the study, the number of personnel in the RPI Laboratory is about 38% below the requirement for a typical analytical laboratory. Technically, the Laboratory can be said to be rated as good. Table 4. 11: Comparison of facilities recommended by TRS 295 and existing Infrastructure at the RPI Lab. Description Recommendation by IAEA, 1989 Existing Infrastructure at RPI Gamma Lab Number of rooms a) Gamma ray spectrometry laboratory: b) Preparation and storage of samples c) Counting room d) Computer room 3-4 3 a) Sample registration, storage and preparation, Evaporation and drying b) Grinding c) Ashing d) Handling of higher activity 7-8 4 Room size 90-120 90-162 Ventilation Low pressure - Temperature 20-26 oC 16-26 oC Personnel - 1 Manager (Chief Scientist); - 3 Scientists; - 3 Senior Technicians - 6 Technical Assistants; - 1 Secretary; - 1 field technician to operate trucks, other vehicles and boats for sample - 1 Manager - 3 Scientists; - 3 Technologists - 1 Secretary; - Maintenance and service section - National Service personnel University of Ghana http://ugspace.ug.edu.gh 71 collection; - 1 maintenance and service technician familiar with electronic equipment. - Further assistance personnel according to the customs of the country. Equipment - Refrigerator - Crusher and/or grinder - Evaporator ; - Large drying oven; - Large muffle furnace - Freeze dryer - Fume chamber - Beta/gamma survey instruments - Portable gamma measurement systems - Refrigerator - Crusher - Evaporator - Large drying oven - Freeze dryer - Fume chamber - Beta/gamma survey instruments - Portable gamma measurement systems 4.3 Quality Assurance Tests 4.3.1 Energy Calibration Figure 4.1 shows the plot of gamma ray energy against channel number for the HPGe detector in use at the RPI Food and Environmental Laboratory. The linear curve obtained from the data points is an indication that the system is operating properly (IAEA, 1989) University of Ghana http://ugspace.ug.edu.gh 72 Figure 4. 11: Plot of gamma ray energy against channel number. 4.3.2 Efficiency Calibration Efficiency calibration curve as a function of energy for mixed radionuclides standard is shown in Figure 4.2 y = 0.244x + 0.2489 R² = 1 0 200 400 600 800 1000 1200 1400 0 1000 2000 3000 4000 5000 6000 g am m a ra y e n er g y / eV Channel number University of Ghana http://ugspace.ug.edu.gh 73 Figure 4. 12: Efficiency calibration curve as a function of energy for mixed radionuclides standard 4.3.3 Minimum Detectable Activities The results of the Minimum Detectable Activities of the 238U, 232Th and 226Ra are presented in Table 4.12 below. The minimum detectable concentration is defined as the smallest concentration of radioactivity in a sample that can be detected with a 5% probability of erroneously detecting radioactivity, when in fact none was present (Type I error) and also, a 5% probability of not detecting radioactivity, when in fact it is present (Type II error). University of Ghana http://ugspace.ug.edu.gh 74 Table 4. 12: Minimum Detectable Activities of the 238 U, 232Th and 226Ra and 137Cs Radionuclide MDA (Bq/kg) 238U 232Th 226Ra 137Cs 4.67 5.32 1.02 2.42 4.3.4 Background Measurements The background of a gamma- ray detection system has a very significant influence on the detection limit and accuracy of the measurement of low levels of activity. The counting system must have a background as low as is attainable with a minimum of spectral lines originating from natural radionuclides which may be present in the system components and the surrounding environment, that is the walls, floor, and benches of the counting facility IAEA (1989). The background measured produced a spectral line of energy 25.28 keV and 25.1 Counts /second originating from an X-ray from the components of the shielding. The shielding of the Gamma spectrometer of the RPI Food and Environmental Laboratory can therefore said to be intact. 4.3.5 Calibration of other Measuring Instruments An observation of the Balance and Marinelli beakers, used in the laboratory, reveals that the instruments have never been calibrated putting into doubt the quality of data fron the laboratory. The instruments were therefore sent to the Ghana Standards Authority’s laboratories for calibration. The results are presented in Appendix C. The University of Ghana http://ugspace.ug.edu.gh 75 results show that, while the Balance was 100% accurate, the beakers were not delivering 1000 mL as indicated. Test Results: Nominal Volume (ml) Mean Measured Volume (EUT) ml Deviation (ml) Uncertainty % 1000 930.540 -69.460 0.05 4.3.6 Statistical Quality Control Figure 4.3 shows a statistical quality control chart that was developed. The test Cs source was, after two months of development of the control chart, counted 100 successive times. All the results obtained were within the warning limits. This indicated a good instrument response. Figure 4. 13: Statistical Control chart for daily counting of a check source 9000 9400 9800 10200 10600 11000 11400 11800 12200 0 20 40 60 80 100 120 C o u n ts p e r Se co n d Number of Counts UCL UWL CL LWL LCL University of Ghana http://ugspace.ug.edu.gh 76 CHAPTER 5 CONCLUSIONS AND RECOMMENDATION This chapter focuses on the conclusions and recommendations based on the study conducted. 5.1 Conclusions The following conclusions are drawn after evaluating the operational performance of the RPI laboratory using ISO 17025 and the IAEA’s Technical Report Series 295: a. From the study, the number of personnel in the RPI Laboratory is 62% of the requirement for a typical analytical laboratory. Technically, the laboratory can rated as good. b. The laboratory does not have established staff training and competence records. List of activities showing training and record of regular re- assessment of the staff member’s competence at each of the activities was not available c. The laboratory does not have a quality assurance system that clearly defines procedure for declaring employees competent. Methods like taking part in proficiency testing schemes and intra-laboratory competencies have not been utilised. d. There are no documented requirements for test or calibration to be done under specific environmental conditions. e. Though the laboratory meets almost all conditions and equipment requirements of the IAEA Guide (1989), there is only a partial system for University of Ghana http://ugspace.ug.edu.gh 77 commissioning equipment and verifying its performance and calibration before it is used for test or calibration work. Management should take the necessary steps to work on these findings; it could accelerate the accreditation drive of the Laboratory. By having the laboratory management system accredited to ISO/IEC 17025, the laboratory stands to gain substantial benefits financially as well as gain the confidence of its clients. One of the main advantages is that the laboratory will gain international recognition for its commitment to quality, competency and reliable results. In addition, ISO/IEC 17025 accreditation will signify that the laboratory complies with an internationally recognized standard. 5.2 Recommendations The following recommendations are made, based on the findings of the study: i. The laboratory’s management should ensure the competence of all who operate specific equipment, perform tests, evaluate results and sign test reports. ii. The laboratory should have a plan for how to ensure adequate equipment function and performance before and during sample measurement. iii. Each laboratory should have processes for how calibration and testing is performed for different types of equipment. iv. Background measurements should be taken as frequently as is practicable and for counting times as long as possible in order to obtain good counting statistics. A good practice is to record the background measurements on a control chart with statistically fixed limits. This provides a means both for University of Ghana http://ugspace.ug.edu.gh 78 checking the stability of the electronics of the system and of checking for contamination of the detector and/or shield. Should the background exceed the control limits, an immediate and thorough investigation should be made and appropriate steps taken to maintain a minimum background. v. Equipment used for measurement should be tested before initial use to ensure acceptable performance. This should be performed through calibration of balance, and volume of the Marinelli beaker. vi. Equipment characteristics and performance can change over time. Therefore, equipment quality programs should be put in place to ensure that equipment is routinely tested on an ongoing basis. vii. The laboratory should have a maintenance plan to carry out preventive maintenance activities and a procedure for unplanned repair to ensure ongoing performance and reliability. viii. Computer systems and software used for acquisition, processing, recording, reporting, storage and retrieval of test and calibration data must be validated when the software is developed, configured, or customized by the user. ix. The laboratory should develop Quality manuals, Process & Standard Procedures, Step-by-step Operating Procedure and Work Instructions, Checklists, Forms and Records for use. Such documents when developed must be controlled. x. The management of the laboratory should, have a documented policy for deciding when the control chart indicates a condition where the method should come under investigation, and this policy should be expressed quantitatively so that it will be applied consistently. University of Ghana http://ugspace.ug.edu.gh 79 xi. There should be proper record keeping and these records must be kept for a considerable time frame. There should also be a computer backup system in place for all records in the laboratory. xii. The laboratory should have a clear policy in place for retention and disposal of samples. xiii. All observations, raw data, calculations and derived data in the form of work sheets, notebooks, instrument output, must be dated and should all be traceable to the person who made the observation or measurement and to the equipment used. xiv. The notebooks used in the laboratory must be properly controlled. The books should have numbered pages such that a record can be referenced by notebook numbers and that pages cannot be torn out without being detected. xv. Staff should not be allowed to remove notebooks from the laboratory except for field work, and books should be returned to management for archiving before a new one is issued. xvi. The laboratory should solicit for client feedback and must investigate client complaints thoroughly. University of Ghana http://ugspace.ug.edu.gh 80 REFERENCES Apps, P. (2006). Test and Measurement Conference: The Critical Role of Skilled Technicians in Laboratory Measurement. [Online]. Pretoria. Available from: http://www.nla.org.za/conferences. [Accessed 09/10/2015] Bailey, T. (2003). Test and Measurement Conference: Utilising LIMS for Quality Control. [Online]. Pretoria. Available from: http://www.nla.org.za/conferences. [Accessed 09/10/2015] Bednarova, M. & Waddington, C. (2010). Accredited Quality Assurance: Developments in accreditation of flexible scopes in Europe. Vol. 15, pp 539-542. Dlamini, M.J. (2005). Test and Measurement Conference: The cornerstone for laboratory performance and success – study on RWAS. [Online]. Pretoria. Available from: http://www.nla.org.za/conferences. [Accessed 09/10/2015] Grochau, I., Ferreira, C., Ferreira, J. & Ten Caten, C. (2010). Accreditation Quality Assurance. Implementation of a quality management system in university test laboratories-a brief review and new proposals. Vol. 15, pp 681-689. Gupta, M. 2010. Accredited Quality Assurance. Document control: status of calibration/test certificate. Vol. 15, pp 591-593. Horngen, C.T., Datar, S.M., Foster, G. 2006. Cost Accounting. 12th Edition. Eaglewood Cliffs: Pearson Prentice-Hall. IAEA, (1989). Guides for Measurement of Radionuclides in Food and the Environment, Vienna Kiline, C. (2008). Clinical Biochemistry: Laboratory quality management systems. Missions, goals and activities in quality assurance. Vol. 42, pp 301-302. Klinkner, R. (2008). Accredited Quality Assurance. Quality assurance in analytical chemistry. Vol. 13, pp 487-488. Multi-Agency Radiological Laboratory Analytical Protocols Manual (MARLAP), 2004. University of Ghana http://ugspace.ug.edu.gh 81 Robertson, R. June 2010. ISO 17025. http//www.ilac.org/documents/why use an accredited lab (Accessed: 15 September 2015) Sithole, M. (2006). Test and Measurement Conference. What is accreditation and its meaning. [Online]. Pretoria. Available from: http://www.nla.org.za/conferences. [Accessed 09/10/2015] Statistical Services Centre, 2001 Approaches to the Analysis of Survey Data. [Online] The University of Reading, UK. Available from: http://www.ilri.org. [Accessed 03/02/2016] Suksai S., Suksripanich, O. & Pobkeeree, V. (2010). International Journal of Healthcare and Quality Assurance. laboratory quality improvement in Thailand’s northernmost provinces. Vol. 23 (1), pp 22-34. Theodorou, D. & Anastasakis, P. (2008). Accreditation Quality Assurance. Management review checklist for ISO 17025 quality management systems. Vo. 14, pp 107-110. Van Eeden, F.J. 2005. Test and Measurement Conference. Improvement of laboratory performance through the integration and business systems. [Online]. Pretoria. Available from: http://www.nla.org.za/conferences. [Accessed 09/10/2015] UNIDO, 2009, Complying with ISO 17025, A practical guidebook for meeting the requirements of laboratory accreditation schemes based on ISO 17025:2005 or equivalent national standards, Vienna World-nuclear.org/information-library/safety-and-security/safety-of- plants/chernobyl-accident.aspx University of Ghana http://ugspace.ug.edu.gh 82 APPENDIX A Performance Evaluation of a Food and Environmental Monitoring Radio- Analytical Laboratory in Ghana Questionnaire Please provide your responses for this questionnaire for the study entitled Performance Evaluation of a Food and Environmental Monitoring Radio-Analytical Laboratory in Ghana Since this research is for academic purpose any information provided would be treated with utmost confidentiality. For each question below, indicate, with a tick, in the space provided your response Equipment, Documents and Procedures No Partially Yes a. Personnel Do you have a record of the qualifications and experience of your staff, with objective evidence of their qualifications, for example copies of certificates? Do you have a clear record with regard to your proposed scope of accreditation of which members of staff are authorized to conduct each test or calibration? Do you have a documented procedure for training staff in quality issues and technical procedures, including tests? Do you have a documented procedure for conducting evaluation of the competence of staff after training and before authorising them for the procedure in which they were trained? Do you have a system for recording training, including objective evidence of competence? Do you have a mechanism for identifying which staff conducted each procedure, test or calibration? b. Accommodation and environmental conditions Have you considered whether there are any environmental factors in your laboratory which might impact on the validity of tests or calibrations? Are you conducting any tests or calibrations where the published procedure which you claim to follow includes a requirement for the work to be done under specific environmental conditions, for example temperature or University of Ghana http://ugspace.ug.edu.gh 83 humidity? If there are such factors, do you have procedures in place to control and monitor them? Do you have any activities which need to be separated to avoid, for example, cross contamination? Do you have any activities which need to be separated to avoid, for example, cross contamination? Do you have clear instructions to staff on actions to be taken when conditions move out of specification? c. Quality assurance for the screening process Do you have a set of methods specified as acceptable for use in your laboratory? Are they documented to the extent necessary to ensure they are applied properly and consistently? If not, have you evidence to show that the methods you are using are fit for the purpose claimed and acceptable to your clients? Have you determined the accuracy, precision and, where relevant, the limit of detection of the methods which you use, including standard published methods? Do you run routine quality control samples and evaluate the results before releasing data? Do you monitor trends in quality control results in order to anticipate possible problems? Have you tested your methods and laboratory by use of certified reference methods and/or inter-laboratory comparison? d. Equipment Do you have a system for commissioning equipment and verifying its performance and calibration before it is used for test or calibration work? Do you have a plan for periodic calibration and verification of the performance of all equipment which affects the validity of measurements? University of Ghana http://ugspace.ug.edu.gh 84 Do you have records showing that this plan is followed and which enable the status of any equipment to be verified at any point in its history of use? Is equipment subject to regular checks or calibrations labelled so that its status can be seen immediately by users? e. Traceability of measurement Have you identified all the measuring equipment which is involved, directly or indirectly, in measurement or calibration and which, if not properly calibrated, would affect the validity of measurements? Is this equipment calibrated in a manner which provides traceability to the international measurement system? Do you have a management procedure to ensure that the calibration is maintained at all times, i.e. recalibration is conducted as necessary and, where possible, equipment is monitored so that any drift away from calibration will be detected? Do you have records which could be audited to confirm the calibration status of the equipment at any point in the past? Administration of work and sample tracking Do you have procedure for logging samples into your laboratory? Are all samples uniquely numbered as soon as practicable after receipt? Does your system ensure that samples are stored securely and in a way that will preserve them against any changes which may affect data generated from them? Do you have a system for ensuring that the procedures required to be carried out on samples are clearly communicated to laboratory staff? Do you have a procedure to ensure reports are checked to make sure they correspond to the raw data? f. Recording of results and associated data University of Ghana http://ugspace.ug.edu.gh 85 Does your system ensure that all observations are recorded at the time when they are made? In this record, is the raw data always preserved so that any problems can be investigated? Do you have a policy on how amendments to entries on laboratory records are to be made? Does the system allow the person making any record to be identified? g. Computer systems Do you have control of what software may be loaded onto any of your computers? Are all computer systems, including software, checked to ensure that they record and process data correctly? Is all software secured against unauthorised changes? Do you have a procedure for regular backup of data held on computers? h. Reporting requirements Do you have a defined report format? Does this comply with the detailed requirements of ISO 17025? Does your system ensure reports always reach only those entitled to receive them? Does the report acknowledge subcontracted work? Do you have a policy on how to deal with situations where it becomes apparent that suspect data has been reported? Do you have a clear identification of staff authorised to approve reports? i. Purchasing services and supplies Do you take steps to control the quality of any purchased goods or services which might affect the validity of your data? Do you have a list of approved suppliers and a policy on University of Ghana http://ugspace.ug.edu.gh 86 their selection? Do you keep this list under review and remove any suppliers found to be inadequate from a quality perspective? Do you have a system for checking all received materials against the order specifications? University of Ghana http://ugspace.ug.edu.gh 87 APPENDIX B Recorded Data for 2014 Country Sample type Cs - 134 Bq /kg Cs - 137 Bq/kg Total count Error Bq /kg Brazil Poultry 0.7 0.74 1.44 0.05 Brazil Poultry 0.43 0.51 0.94 0.02 Germany Food stuff 0.44 0.45 0.89 0.03 The Netherlands Fat filled milk powder 0.17 0.14 0.31 0.03 Ireland Cowbell vegetable fat filled milk 0.31 0.27 0.58 0.02 Belgium 0.17 0.29 0.46 0.07 Poland Whey powder 0.22 0.13 0.35 0.02 Poland Skimmed milk powder 0.59 0.34 0.93 0.04 Poland Whey powder 0.43 0.12 0.55 0.02 Holland Poultry 0.44 0.47 0.91 0.02 Belgium Antwerp Poultry 0.37 0.19 0.56 0.03 New Zealand Poultry 0.12 0.29 0.41 0.02 Brazil Poultry 0.32 0.21 0.53 0.03 Ireland Cowbell vegetable fat filled milk 0.17 0.31 0.48 0.02 Ireland Miksi vegetable fat filled milk 0.43 0.29 0.72 0.02 The Netherlands Poultry 0.41 0.31 0.72 0.02 Brazil Poultry 0.34 0.39 0.73 0.02 Altaics 0.72 0.57 1.29 0.03 Altaics Poultry 0.43 0.51 0.94 0.04 Poland Whey powder 0.34 0.41 0.75 0.03 University of Ghana http://ugspace.ug.edu.gh 88 Poland Whey powder 0.45 0.39 0.84 Poland Whey powder 0.27 0.31 0.58 0.03 Poland Whey powder 0.31 0.39 0.7 0.02 Poland Full cream milk powder 0.24 0.18 0.42 0.04 India Skimmed milk powder 0.29 0.34 0.63 0.02 Ghana Nescafe 3 in 1 cream chank sip 0.7 0.41 1.11 0.04 Ghana Nescafe 3 in 1 cream chank sip 0.65 0.61 1.26 0.04 Ireland Cowbell dairy based instant fortified 0.52 0.41 0.93 0.03 Ireland Miksi vegetable fat filled milk 0.82 0.9 1.72 0.07 Ghana Frozen tuna skipjack round 0.75 0.71 1.46 0.07 Ghana Frozen tuna skipjack round 1.02 1.01 2.03 0.42 Ghana Frozen tuna skipjack round 1.03 0.94 1.97 0.26 Ghana Frozen tuna skipjack round 0.56 0.5 1.06 0.06 Ghana Frozen tuna skipjack round 0.74 0.92 1.66 0.06 Beef feet 0.91 0.49 1.4 0.05 Ghana Nescafe 3 in 1 cream chank sip 0.42 0.4 0.82 0.04 Poland Moudy milk powder 0.31 0.28 0.59 0.02 Brazil Poultry 0.32 0.29 0.61 0.02 Modiglaus Beef feet 0.2 0.27 0.47 0.03 Ghana Nescafe 3 in 1 cream chank kp 0.21 0.28 0.49 0.03 Ghana Nescafe 3 in 1 cream sip 0.37 0.21 0.58 0.02 Ghana Nescafe 3 in 1 breakfast cup 0.41 0.43 0.84 0.03 University of Ghana http://ugspace.ug.edu.gh 89 Ghana Nescafe 3 in 1 cream 0.24 0.41 0.65 0.02 New Zealand Skimmed milk powder (medium heat) 0.53 0.31 0.84 0.08 Australia Skimmed milk powder 0.59 0.26 0.85 0.06 Brazil Poultry 0.39 0.28 0.67 0.02 Argentina Poultry 0.41 0.37 0.78 0.04 Brazil Poultry 0.43 0.29 0.72 0.04 The Netherlands Poultry 0.42 0.37 0.79 0.04 Poland Demicoralised whey powder 0.2 0.28 0.48 0.03 New Zealand Skimmed milk powder 0.43 0.29 0.72 0.02 Australia Skimmed milk powder (medium heat) 0.49 0.37 0.86 0.03 USA Whey powder 0.31 0.29 0.6 0.04 New Zealand Butter milk powder 0.25 0.38 0.63 0.03 New Zealand Skimmed milk powder 0 UK Skimmed milk powder 0.27 0.35 0.62 0.03 Ghana Milo actigen e 0.2 0.23 0.43 0.02 Ghana Nescafe 3 in 1 0.4 0.11 0.51 0.03 Ghana Nescafe 3 in 1 breakfast cup 0.24 0.28 0.52 0.02 Ghana Nescafe 3in 1 0.19 0.21 0.4 0.03 Ghana Nescafe 3 in 1 0.24 0.17 0.41 0.02 Ghana Nescafe 3 in 1 0.19 0.18 0.37 0.02 Ireland Filled milk powder 0.42 0.49 0.91 0.03 New Zealand Butter milk powder 0.29 0.31 0.6 0.02 Tunisia Tuna 0.27 0.19 0.46 0.02 University of Ghana http://ugspace.ug.edu.gh 90 Ghana Nescafe 3 in 1 breakfast 0.21 0.17 0.38 0.02 Ghana Nescafe 3 in 1 0.12 0.09 0.21 0.02 Ghana Nescafe 3 in 1 0.17 0.12 0.29 0.03 Ghana Nescafe 3 in 1 0.21 0.11 0.32 0.02 Ghana Nescafe 3 in 1 cream 0.09 0.12 0.21 0.02 Ghana Nescafe 3 in 1 chank 0.14 0.11 0.25 0.02 Ghana Nescafe 3 in 1 breakfast bulk 0.21 0.17 0.38 0.03 Ghana Nescafe 3 in 1 breakfast bulk 0.22 0.17 0.39 0.02 Ghana Nescafe 3 in 1 breakfast cup 0.17 13 13.17 0.02 Brazil Poultry 0.09 0.21 0.3 0.02 Brazil Poultry 0.21 0.11 0.32 0.03 Poland Millac milk powder 0.09 0.17 0.26 0.02 England Beef 0.14 0.17 0.31 0.03 The Netherlands Beef 0.14 0.09 0.23 0.02 England Beef product 0.09 0.11 0.2 0.02 Ghana Nescafe 3 in 1 cream chank pk 0.05 0.09 0.14 0.02 Ghana Nescafe 3 in 1 0.07 0.11 0.18 0.02 Ghana Nescafe 3 in 1 breakfast cup 0.09 0.14 0.23 0.03 Ghana 0.19 0.08 0.27 0.02 Ghana Nescafe classic tin 0.11 0.18 0.29 0.02 Ghana Nescafe classic tin 0.09 0.07 0.16 0.03 Ireland Vegetable fat filled milk 0.09 0.07 0.16 0.02 Ireland Dairyvale vegetable fat milk 0.11 0.06 0.17 0.02 The Netherlands Simmed milk powder 0.19 0.11 0.3 0.03 University of Ghana http://ugspace.ug.edu.gh 91 Ireland Filled milk powder 0.11 0.02 0.13 0.02 Demark Poultry 0.12 0.19 0.31 0.02 USA Sweet whey powder 0.12 0.11 0.23 0.02 New Zealand Butter milk powder 0.17 0.21 0.38 0.03 Netherland Skimmed milk powder 0.17 0.16 0.33 0.02 USA Sweet whey powder 0.14 0.18 0.32 0.03 Poland Full cream milk powder 0.09 0.11 0.2 0.02 Ireland Miskivegetable milk 0.19 0.13 0.32 0.03 Singapore Tuna 0.34 0.21 0.55 0.02 Brazil Poultry 0.09 0.17 0.26 0.02 Ghana Nescafe 3 in 1 breakfast cup 0.11 0.13 0.24 0.04 Ghana Nescafe 3 in 1 breakfasr bulk 0.05 0.1 0.15 0.02 Ghana Nescafe 3 in 1 cream 0.13 0.18 0.31 0.02 Ghana Nescafe 3 in 1 cream 0.07 0.09 0.16 0.02 Ghana Nescafe 3 in 1 cream sip 0.07 0.09 0.16 0.02 Ghana Nescafe 3 in 1 cream sachet 0.09 0.13 0.22 0.03 Ghana Nescafe 3 in 1 breakfast cup 0.13 0.18 0.31 0.02 England Beef feeder olf 0.19 0.18 0.37 0.03 Netherland Beef 0.19 0.29 0.48 0.02 Italy Fatted whey powder 0.04 0.08 0.12 0.02 Denmark Poultry 0.07 0.09 0.16 0.03 England Beef feeder olf 0.11 0.09 0.2 0.03 Denmark Beef 0.19 0.12 0.31 0.02 Ireland Cowbell vegetable fat filled milk 0.17 0.09 0.26 0.02 Ireland Cowbell vegetable fat filled milk 0.15 0.23 0.38 0.02 University of Ghana http://ugspace.ug.edu.gh 92 Ireland Cowbell vegetable fat filled milk 0.09 0.18 0.27 0.02 Netherland Skimmed milk powder 0.18 0.19 0.37 0.03 Germany Skimmed milk powder high heat 0.31 0.28 0.59 0.02 Germany Skimmed milk powder 0.19 0.31 0.5 0.02 Netherland Skimmed milk powder 0.09 0.59 0.68 0.02 Germany Skimmed milk powder 0.13 0.09 0.22 0.02 France Procream 0.13 0.21 0.34 0.02 Ireland Cowbell vegetable fat filled milk 0.21 0.37 0.58 0.02 New Zealand Skimmed milk powder dry mix 0.09 0.12 0.21 0.2 Ireland Filled milk powder 0.11 0.08 0.19 0.03 Netherland Skimmed milk powder medium heat 0.45 0.23 0.68 0.02 Ireland Filled milk powder 0.43 0.41 0.84 0.02 USA Sweet whey powder 0.41 0.37 0.78 0.02 Australia Skimmed milk powder medium heat 0.19 0.18 0.37 0.02 New Zealand Butter milk powder 0.23 0.19 0.42 0.02 Germany Colli food stuff (meat) 0.71 0.67 1.38 0.05 Netherland/ Germany Poultry/pig feet 0.63 0.61 1.24 0.05 Belgium, Antwerp Poultry 0.5 0.51 1.01 0.04 Ghana Nescafe 3 in 1 cream chank sip 0.51 0.44 0.95 0.05 Ghana Nescafe 3 in 1 cream chank sip 0.78 0.52 1.3 0.05 Ghana Nescafe 3 in 1 breakfast bulk 0.9 0.74 1.64 0.06 South Meat 0.7 0.44 1.14 0.07 University of Ghana http://ugspace.ug.edu.gh 93 Africa USA Poultry 0.51 0.39 0.9 0.04 Australia, Sydney Meat 0.91 0.71 1.62 0.09 Netherlands Poultry 0.7 0.5 1.2 0.05 Poland Full cream milk powder 0.32 0.3 0.62 0.02 Poland Whey powder 0.41 0.95 1.36 0.04 Poland Skimmed milk powder 0.26 0.23 0.49 0.03 Poland Skimmed milk powder 0.51 0.51 1.02 0.05 Ireland Cowbell vegetable fat filled milk powder 0.42 0.24 0.66 0.05 Netherlands Poultry/cow feet 0.81 0.62 1.43 0.05 USA Poultry 0.62 0.42 1.04 0.04 Ghana Nescafe 3 in 1 breakfast bulk 0.19 0.29 0.48 0.02 Ghana Nescafe 3 in 1 breakfast bulk 0.11 0.14 0.25 0.03 Ghana Nescafe 3 in 1 cream chank sip 0.17 0.19 0.36 0.04 Ghana Nescafe 3 in 1 cream sachet 0.21 0.34 0.55 0.02 Holland Poultry 0.34 0.29 0.63 0.02 Brazil Poultry 0.14 0.28 0.42 0.02 Ghana Nescafe 3 in 1 cream chank sip 0.43 0.23 0.66 0.02 Ghana Nescafe 3 in 1 cream sachet 0.49 0.09 0.58 0.03 Ghana Nescafe 3 in 1 cream chank kp sip 0.31 0.37 0.68 0.02 Ghana Nescafe classic tin 0.27 0.19 0.46 0.02 Tunisia Skipjack tuna 0.49 0.47 0.96 0.05 Brazil Poultry 0.78 0.49 1.27 0.02 University of Ghana http://ugspace.ug.edu.gh 94 Netherlands Poultry 0.48 0.43 0.91 0.02 Netherlands Meat Product 0.45 0.43 0.88 0.02 Italy Meat Product 0.49 0.58 1.07 0.02 Ghana Nescafe 3 In 1 Breakfast 0.43 0.29 0.72 0.02 Ghana Nescafe Cerelac Rice 0.37 0.48 0.85 0.03 Ghana Nescafe Cerelac 0.32 0.17 0.49 0.03 Poland Skimmed Milk Powder 0.49 0.23 0.72 0.02 Ghana 0.49 0.31 0.8 0.04 Ghana Nestle Cerelac 0.15 0.29 0.44 0.02 Ghana Nestle Cerelac 1 0.12 1.12 0.06 Ghana Nestle Cerelac 0.09 0.56 0.65 0.03 Ghana Nestle Cerelac 0.81 0.21 1.02 0.04 0.09 0.15 0.24 0.02 Ghana Nido Fortified 0.49 0.21 0.7 0.02 Ghana Nido Fortified 0.53 0.33 0.86 0.02 Ghana Nido Fortified 0.27 0.41 0.68 0.03 Ghana Nido Fortified 0.71 0.81 1.52 0.05 Ghana Nido Fortified 0.54 0.21 0.75 0.001 Netherlands Poultry/Beef Feet 0.53 0.21 0.74 0.04 Belgium Skimmed Milk Powder MDA MDA MDA Ireland Miksi Vegetable Fat Filled Milk Powder MDA MDA MDA Ireland Cowbell Filled Milk Powder MDA MDA MDA Ireland Dairyvale Filled Milk Powder MDA MDA MDA USA Poultry 0.19 0.34 0.53 0.03 Ghana Filled Milk Powder 0.61 0.37 0.98 0.03 Ghana Filled Milk Powder 0.19 0.41 0.6 0.03 Ghana Nido Fortified 0.9 0.21 1.11 0.02 University of Ghana http://ugspace.ug.edu.gh 95 Ghana Nido Nitripak Fortified 0.38 0.16 0.54 0.03 Ghana Nescafe 3 In 1 Breakfast Bulk 0.12 0.19 0.31 0.05 Ghana Nescafe 3 In 1 Breakfast Cup 0.42 0.21 0.63 0.03 Ghana Nescafe 3 In 1 Chank Sip 0.53 0.22 0.75 0.04 Ghana Nescafe 3 In 1 Cream Chank Sip 0.31 0.54 0.85 0.05 Netherlands Meat Product 0.42 0.45 0.87 0.02 Ireland Meat Feet 0.39 0.35 0.74 0.03 Ghana Nescafe 3 In 1 Cream Chank Sip 0.23 0.18 0.41 0.03 Ghana Nescafe 3 In 1 Cream Chank Sip 0.71 0.2 0.91 0.04 UK Meat 0.52 0.39 0.91 0.04 New Zealand Beef 0.21 0.42 0.63 0.01 UK Meat Product 0.53 0.16 0.69 0.05 Ireland Miksi Filled Milk Powder 0.21 0.39 0.6 0.06 Ireland Cowbell Filled Milk Powder 1 0.19 1.19 0.04 Ireland Dairyvale Filled Milk Powder 0.71 0.6 1.31 0.03 Ireland Cowbell Filled Milk Powder 0.43 0.28 0.71 0.02 Ireland Cowbell Filled Milk Powder 0.23 0.22 0.45 0.06 Argentina Doliat Full Cream Milk Powder 0.47 0.39 0.86 0.03 Ghana Nestl Cerelac Bl Millet 0.17 0.23 0.4 0.06 Ghana Nestle Cerelac Bl W.Frt 0.22 0.73 0.95 0.04 Ghana Nescafe 3 In 1 Breakfast Bulk 0.24 0.19 0.43 0.05 Ghana Nescafe 3 In 1 Breakfast 0.76 0.29 1.05 0.02 University of Ghana http://ugspace.ug.edu.gh 96 Cup Ghana 0.51 0.38 0.89 0.02 Ghana Nescafe Cerelac Bl Wheat 0.23 0.17 0.4 0.04 Ireland Beef Feet 0.43 0.38 0.81 0.02 Ghana Nido Fortified 0.29 0.36 0.65 0.02 Ghana Nido Fortified 0.16 0.39 0.55 0.04 Ghana Nescafe 3 In 1 Breakfast Bulk 0.26 0.28 0.54 0.02 Ghana Nescafe 3 In 1 Cream Chank Sip 0.16 0.29 0.45 0.03 Ghana Nescafe 3 In 1 Cream Chank Sip 0.28 0.41 0.69 0.06 Ghana Nescafe Classic Tin 0.17 0.19 0.36 0.04 Ghana Nescafe 3 In 1 Cream Chank Pk Sip 0.63 0.32 0.95 0.02 Ghana 0.09 0.26 0.35 0.05 Spain Beef Feet 0.11 0.32 0.43 0.02 Netherlands Poultry 0.21 0.37 0.58 0.03 USA Ecmu 4686792 0.65 0.12 0.77 0.08 Ghana Ideal Milk Coffee 0.18 0.01 Ghana Ideal Mliky Choco 0.03 0.07 0.1 0 Ghana Ideal Milky Tea 0.04 0.09 0.13 0.02 Ghana Cerelac Maize 0.09 0.11 0.2 0.03 Ghana Nido Fortified 0.21 0.38 0.59 0.02 Ghana Nestle Cerelac Bl Honey 0.11 0.21 0.32 0.02 Ghana Nescafe 3 In 1 Breakfast Bulk 0.1 0.29 0.39 0.02 Ghana Nestle Cerelac Bl Honey 0.11 0.38 0.49 0.03 Ghana Nestle Cerelac Millet 0.09 0.21 0.3 0.02 Ghana Nestle Cerelac Bl Frt Pcs 0.18 0.34 0.52 0.03 Ireland Beef MDA University of Ghana http://ugspace.ug.edu.gh 97 India Skimmed Milk Powder(Chl/268/14) MDA MDA MDA UK Poultry 0.035 0.247 0.282 0.02 Scotland UK Poultry MDA MDA MDA Netherlands Poultry MDA MDA MDA Denmark Poultry MDA MDA MDA Belgium Poultry MDA MDA MDA Ghana Nestle 3 In 1 MDA MDA MDA Ghana Nescafe 3 In 1 Breakfast MDA MDA MDA Ghana Nescafe Classic Tin MDA MDA MDA Ghana Nido Fortified MDA MDA MDA Ghana Nesccafe 3 In 1 Cream MDA MDA MDA Ghana Nescafe 3 In 1 Cream MDA MDA MDA Ghana Nescafe 3 In 1 Cream Chank MDA MDA MDA France Procream 151a MDA MDA MDA Belgium Skimmed Milk Powder MDA MDA MDA Netherlands Skimmed Milk Powder MDA MDA MDA UK Skimmed Milk High Heat MDA MDA MDA Poland MDA MDA MDA Netherlands MDA MDA MDA USA Poultry MDA MDA MDA Brazil Poultry MDA MDA MDA India Meat Product MDA MDA MDA BELGIUM Antwerp Meat Product MDA MDA MDA Denmark Poultry MDA MDA MDA South africa Poultry MDA MDA MDA Denmark Poultry MDA MDA MDA University of Ghana http://ugspace.ug.edu.gh 98 Ghana Nescafe 3 In 1 Creamchank Sip MDA MDA MDA Ghana Nescafe 3 In 1 Breakfast Bulk MDA MDA MDA Ghana Nescafe 3 In 1 Breakfast Bulk MDA MDA MDA Ghana Nescafe 3 In 1 Breakfast Cup MDA MDA MDA Ghana Nescafe 3 In 1 Breakfast Cup MDA MDA MDA Ghana Nestle Cerelac Bl Honey MDA MDA MDA Ghana Nestle Cerelac Rice MDA MDA MDA Ghana Nestle Cerelac Bl Frt Pcs MDA MDA MDA Ghana Nescafe 3 In 1 Cream Chank Kp Sip MDA MDA MDA Ghana Nescafe Classic Tin MDA MDA MDA USA Poultry MDA MDA MDA Belgium, Antwerp Poultry MDA MDA MDA Ireland Skimmed Milk Powder 0.11 0.18 0.29 0.03 Belgium Poultry MDA MDA MDA Belgium Poultry `MDA MDA Belgium Poultry MDA MDA Netherlands /Italy Poultry MDA MDA USA Poultry MDA MDA Ghana Nescafe Classic Tin MDA MDA Ghana Nescafe Classic Tin 0.43 0.39 0.82 0.04 Ghana Nescafe Classic Tin 0.17 0.29 0.46 0.04 Ghana Nescafe Classic Tin 0.4 0.28 0.68 0.02 Ghana Nescafe 3 In 1breakfast Cup 0.19 0.17 0.36 0.04 University of Ghana http://ugspace.ug.edu.gh 99 Ghana Nido Nitripak Fortified 0.11 0.17 0.28 0.02 Ghana Nido Fortified 0.09 0.2 0.29 0.03 Ghana Nido Fortified 0.21 0.4 0.61 0.03 Ghana Nido Fortified 0.19 0.21 0.4 0.02 Ghana Nido Fortified 0.21 0.23 0.44 0.04 Ghana Nestle Cerelac Bl Wheat 0.01 0.06 0.07 0 Ghana Nestle Cerelac Bl Wheat 0.23 0.14 0.37 0.04 Ghana Nestle Cerelac Bl Wheat 0.09 0.17 0.26 0.02 Ghana Nestle Cerelac Bl Wheat 0.52 0.16 0.68 0.05 Ghana Nescafe 3 In 1 Cream Chanpk Sip 0.29 0.18 0.47 0.02 Ghana Nescafe 3 In 1 Cream Chanpk Sip 0.11 0.46 0.57 0.06 Ghana Nestle Cerelac Bl W Frt Pcs 0.19 0.28 0.47 0 Ghana Nestle Cerelac Bl Honey 0.27 0.51 0.78 0.06 Ghana Nestle Cerelac Bl Rice 0.34 0.29 0.63 0.03 Ghana Nescafe Classic Tin 0.71 0.18 0.89 0.05 Ghana Nescafe Classic Tin 0.39 0.21 0.6 0.05 Ghana Nescafe Classic Tin 0.29 0.16 0.45 0.03 Netherlands Frozen Pork 0.05 0.11 0.16 0.03 Denmark Poultry 0.19 0.21 0.4 0.02 Netherlands Beef 0.19 0.23 0.42 0.04 Netherlands Beef 0.39 0.18 0.57 0.03 USA Beef 0.19 0.08 0.27 0.05 USA Poultry 0.16 0.23 0.39 0.02 Ireland 0.57 0.11 0.68 0.03 USA Poultry 0.16 0.09 0.25 0.05 New Zealand Skimmed Milk Powder Dry Mix 0.17 0.19 0.36 0.04 University of Ghana http://ugspace.ug.edu.gh 100 New Zealand Skimmed Milk Powder Dry Mix 0.31 0.21 0.52 0.03 Ireland Filled Milk Powder 18% 0.24 0.29 0.53 0.03 New Zealand Butter Milk Powder 0.23 0.19 0.42 0.02 Belgium Skimmed Milk Powder Medium Heat 0.21 0.18 0.39 0.02 Germany Golden Royal Unsweetened Evaporeted Milk 0.14 0.17 0.31 0.02 Ghana Nestle Cerelac Bl W Frt Pcs 0.08 0.36 0.44 0.02 Ghana Nestle Cerelac Bl Rice 0.29 0.09 0.38 0.06 Ghana Nestle Cerelac Bl Honey 0.19 0.17 0.36 0.03 Ghana Nescafe 3 In 1 Breakfast Cup 0.51 0.17 0.68 0.05 Ghana Nescafe 3 In 1 Cream 0.29 0.33 0.62 0.04 Ireland Cowbell Vegetable Fat Filled 0.29 0.27 0.56 0.03 Ireland Cowbell Filled Milk 0.19 0.23 0.42 0.02 Belgium Poultry 1 0.19 1.19 0.06 Netherlands Nescafe 3 In 1 Breakfast Cup 0.23 0.19 0.42 0.03 Ghana Nescafe 3 In 1 Breakfast Bulk 0.39 0.15 0.54 0.02 Ghana Nescafe 3 In 1 Breakfast Cup 0.27 0.08 0.35 0.04 Ghana Nescafe 3 In 1 Breakfast Bulk 0.28 0.15 0.43 0.03 Ghana Nescafe 3 in 1 Breakfast Bulk 0.16 0.18 0.34 0.04 Ghana Nescafe 3iIn 1 Breakfast Bulk 0.39 0.22 0.61 0.03 Ghana Nescafe 3 in 1 Breakfast Cup 0.43 0.29 0.72 0.06 University of Ghana http://ugspace.ug.edu.gh 101 Ghana Nestle Cerelac Bl Wheat 0.08 0.21 0.29 0.04 Ghana Nestle Cerelac Bl Wheat 1 0.16 1.16 0.06 Ghana Nescafe 3 In 1 Cream Chank Sip 0.17 0.09 0.26 0.05 Ghana Nescafe 3 In 1 Cream Chank Kp Sip 0.31 0.29 0.6 0.04 Ghana Nescafe 3 In 1 Breakfast Cup 0.23 0.13 0.36 0.05 Ghana Nescafe 3 In 1 Cream Chanpk Sip 0.17 0.29 0.46 0.05 Ghana Nescafe 3 In 1 Cream Chanpk Sip 0.37 0.33 0.7 0.04 Ghana Nescafe 3 In 1 Cream Chanpk Sip 0.19 0.54 0.73 0.04 Ghana Nido Nutripak Fortified 0.22 0.13 0.35 0.03 Ghana Nido Nutripak Fortified 0.91 0.21 1.12 0.04 Ghana Nescafe 3 In 1 Breakfast Cup 0.2 0.16 0.36 0.02 Malaysia Moi Sweetened Condensed Milk 0.49 0.23 0.72 0.05 Germany Golden Burger Long Life Milk 0.81 0.21 1.02 0.06 Belgium Skimmed Milk Powder 0.21 0.32 0.53 0.02 Malaysia Foodie Sweetened Condensed Milk 0.68 0.38 1.06 0.04 Malaysia Jago Sweetened Condensed Milk 1.02 0.21 1.23 0.06 Netherlands Skimmed Milk Powedr 0.17 0.16 0.33 0.03 USA Poultry 0.38 0.09 0.47 0.03 Ghana Natural Cocoa Cake 0.21 0.14 0.35 0.03 New Zealand Skimmed Milk 0.18 0.35 0.53 0.04 Germany Skimmed Milk Powder 0.32 0.19 0.51 0.03 Poland Sweet Whey Powder 0.21 0.15 0.36 0.04 University of Ghana http://ugspace.ug.edu.gh 102 Netherlands Skimmed Milk Powder` 0.21 0.14 0.35 0.03 New Zealand Skimmed Milk Powder 0.09 0.13 0.22 0.02 New Zealand Skimmed Milk Powder High Heat 0.16 0.29 0.45 0.05 Ghana Nescafe 3 In 1 Cream Chanpk Sip 0.21 0.09 0.3 0.03 Ghana Nescafe 3 In 1 Cream Sip 0.2 0.21 0.41 0.04 Ghana Nescafe 3 In 1 Crem Chanpk 0.31 0.28 0.59 0.03 Ghana Nescafe 3 In 1 Crem Chanpk 0.2 0.29 0.49 0.03 Ghana Nescafe 3 In 1 Crem Chanpk 0.28 0.27 0.55 0.02 Ghana Nescafe 3 In 1 Breakfast 0.17 0.23 0.4 0.02 Ghana Nescafe 3 In 1 Breakfast Bulk 0.11 0.19 0.3 0.03 Ghana Nestle Cerelac Bl Wheat 0.26 0.21 0.47 0.02 Ghana Nestle Cerelac Bl Wheat 0.17 0.18 0.35 0.03 Ireland Skimmed Milk Powder 0.16 0.41 0.57 0.05 Poland Sweet Whey Powder 0.14 0.13 0.27 0.02 Poland Demineralised Whey Powder 0.23 0.26 0.49 0.04 Poland Full Cream Milk Powder 0.13 0.15 0.28 0.04 Ireland Cowbell Vegetable Fat Milk 0.23 0.19 0.42 0.03 Ireland Cowbell Vegetable Fat Filled Milk 0.7 0.21 0.91 0.03 Ghana Nescafe 3 In 1 Crem Chanpk Sip 0.31 0.25 0.56 0.04 Ghana Nestle Cerelac Bl Millet 0.13 0.15 0.28 0.05 Ghana Nido Nutripak Fortified 0.21 0.09 0.3 0.04 Germany/B elgium Skimmed Milk Powder 0.52 0.24 0.76 0.02 University of Ghana http://ugspace.ug.edu.gh 103 UK Skimmed Milk Powder 0.21 0.35 0.56 0.03 Ghana Nestle Milo Actigen 0.32 0.16 0.48 0.02 Ghana Milo Actigen E 0.13 0.16 0.29 0.03 Ghana Nestle Cerelac Bl Wheat 0.14 0.21 0.35 0.02 Ghana Nescafe 3 In 1 Crem Chanpk Sip 0.11 0.13 0.24 0.04 Ghana Nestle Cerelac Bl Millet 0.24 0.11 0.35 0.02 Ghana Nestle Cerelac Bl Wheat 0.15 0.09 0.24 0.04 Ghana Nido Fortified 0.17 0.29 0.46 0.05 Ireland Beef Feet 0.11 0.19 0.3 0.03 Ireland Beef Feet 0.24 0.19 0.43 0.02 Holland Full Cream Powder 0.21 0.25 0.46 0.03 UK Whole Milk Powder 0.24 0.19 0.43 0.03 Germany Frozen Meat Product 0.24 0.4 0.64 0.03 Ghana Nestle Cerelac Bl Wheat 0.24 0.31 0.55 0.03 Ghana Nestle Cerelac Bl Honey 0.17 0.29 0.46 0.05 Ghana Nescafe 3 In 1 Breakfast Cup 0.21 0.4 0.61 0.05 Ghana Milo Actigen E 0.33 0.29 0.62 0.03 Ghana Milo Actigen E 0.13 0.36 0.49 0.03 Ghana Milo Actigen E 0.11 0.16 0.27 0.02 Ghana Milo Actigen E 0.43 0.15 0.58 0.05 Ghana Milo Actigen E 0.51 0.34 0.85 0.06 Poland Skimmed Milk Powder 0.23 0.17 0.4 0.04 Ireland Cowbell Filled Milk Powder 0.28 0.19 0.47 0.04 Ireland Dairyvale Filled Milk Powder 0.63 0.36 0.99 0.03 Ireland Cowbell Filled Milk Powder 0.18 0.23 0.41 0.03 Ireland Cowbell Filled Milk 0.16 0.15 0.31 0.04 University of Ghana http://ugspace.ug.edu.gh 104 Powder UK Skimmed Milk Powder 0.39 0.14 0.53 0.03 UK Sweet Whey Powder 0.19 0.33 0.52 0.02 Ghana Nestle Cerelac Bl Wheat 0.16 0.09 0.25 0.06 Ghana Nescafe 3in 1 Breakfast Cup 0.61 0.42 1.03 0.04 Ghana Milo Actigen E 0.29 0.15 0.44 0.05 Ghana Milo Actigen E 0.21 0.33 0.54 0.03 Ghana Milo Actigen E 0.41 0.24 0.65 0.02 Ghana Milo Actigen E 0.31 0.25 0.56 0.05 Ghana Milo Actigen E 0.72 0.51 1.23 0.06 Ghana Milo Actigen E 0.53 0.22 0.75 0.02 Ghana Milo Actigen E 0.49 0.26 0.75 0.04 Ghana Nido Fortified 0.16 0.29 0.45 0.03 Ghana Nido Nutripak Fortified 0.23 0.45 0.68 0.05 Ghana Nido Nutripak Fortified 0.59 0.42 1.01 0.06 Denmark Poultry/Beef 0.14 0.29 0.43 0.06 Germany Beef Product 0.36 0.2 0.56 0.05 Poland Sweet Whey Powder 0.3 0.35 0.65 0.03 Netherlands Skimmed Milk Powder Medium Heat 0.31 0.41 0.72 0.05 New Zealand Skimmed Milk Powder Dry Mix 0.12 0.14 0.26 0.02 New Zealand Beef/Poultry 0.32 0.54 0.86 0.06 Ghana Nestle Cerelac Bl Rice 0.39 0.21 0.6 0.02 Ghana Nestle Cerelac Bl Millet 0.21 0.15 0.36 0.05 Ghana Nestle Cerelac Bl Wheat 0.08 0.17 0.25 0.03 Ghana Milo Chocomilo 0.32 0.26 0.58 0.05 Ghana Nescafe Classic Tin 0.17 0.29 0.46 0.04 University of Ghana http://ugspace.ug.edu.gh 105 Ghana Nestle Cerelac Bl 0.22 0.13 0.35 0.06 Ghana Nestle Cerelac Bl Millet 0.09 0.3 0.39 0.05 Ghana Tuna Skipjack Round 0.29 0.43 0.72 0.03 Ghana Tuna Skipjack Round 0.15 0.34 0.49 0.05 University of Ghana http://ugspace.ug.edu.gh 106 APPENDIX C Calibration Certificates University of Ghana http://ugspace.ug.edu.gh 107 University of Ghana http://ugspace.ug.edu.gh 108 University of Ghana http://ugspace.ug.edu.gh 109 University of Ghana http://ugspace.ug.edu.gh 110 University of Ghana http://ugspace.ug.edu.gh 111 University of Ghana http://ugspace.ug.edu.gh 112 University of Ghana http://ugspace.ug.edu.gh