TWODIMENSIONAL CHROMATOGRAPHY

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CONVENTION OF THE METRE

The metric system was first developed during the French Revolution to replace the various measures used at that time. During the nineteenth century the metric system was adopted by both the world-wide scientific community and many countries as the system of measurement. This confirmed the international need to establish a measurement institute for the purpose of coordinating international metrology.
The development of the metric system called for a treaty that would coordinate international measurement and establish associated organisations to oversee the running of the institute (BIPM c. 2005a, Naughtin 2008). The Convention of the Metre is a treaty that created the International Bureau of Weights and Measures (BIPM), an intergovernmental organisation under the authority of the International Committee for Weights and Measures (CIPM). The CIPM has established a number of Consultative Committees that ensures the world’s experts, in their specified fields, meet as advisers on scientific, technical and administrative matters (BIPM c. 2005b). The Metre Convention was signed in Paris in 1875, thus establishing a permanent organisational structure for member governments to act in mutual agreement on all matters relating to units of measurement (BIPM c. 2005c).
A ‘Mutual Recognition Arrangement’ framework document (CIPM MRA), designed for national measurement standards and for calibration and measurement certificates issued by National Metrology Institutes (NMIs), was signed in Paris in response to a growing global need for reliable quantitative information on the comparability of national metrology services and to provide the technical basis for wider agreements negotiated for international trade, industry and regulatory activities (BIPM 2003). The task of the BIPM is to ensure world-wide uniformity of measurements and their traceability to the International System of Units (SI) under the auspices of the Metre Convention. The BIPM operates through the Consultative Committees (BIPM c. 2005d), whose members are the national metrology institutes (NMIs) of the Member States of the Convention, and through its own laboratory work. 2.2 ACCURATE MEASUREMENT IN SOUTH AFRICA The National Metrology Institute of South Africa (NMISA), is mandated by an Act of Government, Act No. 18, 2006 (Act of Parliament 2006), to provide for the use of measurement units of the International System of Units and certain other measurement units. In August 1964, South Africa became the 40th signatory to the Metre Convention and signed the CIPM MRA in October 1999 on behalf of the Department of Trade and Industry (the dti). NMISA was initially established in 1947 as the National Physics Laboratory in the Council for Scientific and Industrial Research (CSIR). It was later renamed the National Metrology Laboratory (McDowell 1997). Under the Measurement Act of 2006, NMISA was promulgated in May 2007 as an independent public entity, forming part of the Technical Infrastructure of the dti. 2.2.1 Why is Measurement Important? Accurate measurement is paramount for fair trade, competitive manufacturing, efficient health care and effective environmental monitoring and law enforcement (the dti 2014). NMISA links the South African and regional measurement system to the international measurement system through its participation in the Convention of the Metre and its organs, the CIPM and the BIPM. The expanding global trade and pressure to eliminate technical barriers to trade (TBTs) creates a constant demand for greater accountability and demonstrated competence in NMIs and plays a leading role in the development of a sound metrology infrastructure in Africa, especially in support of South Africa’s immediate neighbours in the Southern African Development Community (SADC). The brief outline described above for the establishment of the Metre Convention and the BIPM is intended to inform the reader of the measurement framework within which NMISA functions and to better understand the role of chemical metrology in NMISA to provide measurement traceability for analytical measurements for the South African industry and for measurement collaboration in Africa.

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TABLE OF CONTENTS :

  • SUMMARY
  • ACKNOWLEDGEMENTS
  • PUBLICATIONS AND PRESENTATIONS
  • ACRONYMS AND ABBREVIATIONS
  • LIST OF FIGURES
  • LIST OF TABLES
  • CHAPTER 1: INTRODUCTION
  • CHAPTER 2: BACKGROUND
    • 2.1 CONVENTION OF THE METRE
    • 2.2 ACCURATE MEASUREMENT IN SOUTH AFRICA
      • Why is Measurement Important in South Africa?
    • 2.3 PERSISTENT ORGANIC POLLUTANTS
      • 2oxicology and Health Aspects
    • 2.4 SOUTH AFRICAN SITUATION
      • 2.4.1 National Implementation Plan
    • 2.5 PCDD/F ANALYTICAL REQUIREMENTS
    • Alternative Approach
  • CHAPTER 3: GC×GCTOFMS
    • 3.1 GAS CHROMATOGRAPHY
      • Capillary Columns
    • 3.2 TWODIMENSIONAL CHROMATOGRAPHY
      • GC×GC Column Sets and Orthogonality
    • 3.3 GC×GC TOFMS
      • 3.3.1 Detection, Data Processing and Reporting
    • 3.4 TARGET COMPOUND ANALYSIS USING GC×GCTOFMS
      • 3 Analytical Benchmarking in South Africa using GC×GCTOFMS
  • CHAPTER 4: SOUTH AFRICAN APPROACH
    • 4.1 BIOANALYTICAL (BIOASSAY) APPROACH
    • 4.2 ANALYTICAL MEASUREMENT APPROACH
    • 4.3 COMBINED APPROACHES
      • .3 PCDD/F Method Development using GC×GCTOFMS
    • 4.4 RESULTS AND DISCUSSION
    • 4.5 CONCLUDING REMARKS
  • CHAPTER 5: SAMPLE PREPARATION
    • 5.1 GENERAL SAMPLE PREPARATION FOR POP ANALYSIS
    • 5.2 PLE/ SOXHLET APPROACH IN SOUTH AFRICA
      • E Extraction of Waste Samples
    • 5.3 AUTOMATED PREPARATION APPROACH
      • .2 Cleanup
    • 5.4 NMISA EXTRACTION METHOD FOR PCDD/Fs
      • .3 Method Summary
  • CHAPTER 6: SCREENING AND SELECTIVITY
    • 6.1 SCREENING WITH GC×GCTOFMS
    • 6.1.1 Toxic Waste Disposal
    • 6.2 NONTARGETED SCREENING
      • 6.2.1 Scripting and Classifications
    • 6.3 ISOMER SPECIFICITY/ SELECTIVITY
      • .4 Selectivity using a Dioxin Specific Column
    • 6.4 CONCLUDING REMARKS
  • CHAPTER 7: QUANTITATIVE ANALYSIS
    • 7.1 QUANTITATIVE ANALYSIS
      • .4 GCHRMS and GC×GCTOFMS Instrument Methods
    • 7.2 SAMPLE RESULTS
      • 4 KruskalWallis Test
    • 7.3 CONCLUDING REMARKS
  • CHAPTER 8: METHOD VALIDATION
    • 8.1 NMISA VALIDATION APPROACH
    • 8.2 REGRESSION ANALYSIS
      • .2.2 Limit of Detection and Quantitation
    • 8.3 CONCLUDING REMARKS
  • CHAPTER 9: METROLOGICAL RESULTS
    • 9.1 RESULTS FOR VALIDATION STUDY
    • 9.2 VALIDATION CONCLUSIONS
  • CHAPTER 10: CONCLUSIONS
    • 10.1 CONCLUSIONS
    • 10.2 FUTURE WORK
  • CHAPTER 11: REFERENCES

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