Томск, ТПУ, ИГНД, ГЭГХ1 Methods of radioactive ores and minerals investigation Volostnov Alexander Valerievich

Томск, ТПУ, ИГНД, ГЭГХ2 Methods of the substance investigation (general concepts)

Lecture plan Introduction The course content Purpose of the investigation methods Classification of methods Requirements to quality of analytical works Metrological bases of the analytical work quality control Types of errors Metrological characteristics of analytical methods Certification of analytical methods Methods of metrological monitoring Standard samples of composition Томск, ТПУ, ИГНД, ГЭГХ3

Томск, ТПУ, ИГНД, ГЭГХ4 Methods of investigation of material and mineral constitution are the component of all geological prospecting process. Detail of mineral deposit studying, quality of prospecting works, establishing of new kinds of mineral raw materials, development of modern advanced technological schemes and enhancement of mineral extraction depend on quality of these investigations. Introducti on

Томск, ТПУ, ИГНД, ГЭГХ5 The course content I Meteorological bases of analytical works II The bases of sample preparation III Methods of studying of radioactive ores and minerals phase composition 1 Optical methods of studying substance 1.1 Petrography 1.2 Mineragraphy 1.3 Schlich analysis 2 Uranium and thorium microchemical reactions 3 Methods of prints 4 Luminescent methods 4.1 Photoluminescence 4.2 Cathodol uminescence 4.3 Radiol uminescence 4.4 Chemol uminescence 4.5 Thermol uminescence 4.6 Tribol uminescence 5 Methods of electron microscopy 5.1Transparent electron microscopy (TEМ) 5.2 Scanning electron microscopy (SEМ) 5.3 Electron-probe microanalysis (EPMA)

Томск, ТПУ, ИГНД, ГЭГХ6 Содержание курса IV Method of the elemental composition studying 9 Perl-luminescent analysis 10 Spectral methods 10.1 Emission-spectral analysis (ESA) 10.2 Atomic-emission spectrometry with inductively coupled plasma (IСP-AES) 10.3 Mass-spectrometry with inductively coupled plasma (ICP- MS) 10.4 X-ray fluorescence spectral analysis (RFSA) 10.5 Atomic-absorption analysis (ААА) 11 Activation methods 11.1 Neutron-activation analysis (NАА) 11.2 Method of delayed neutrons (МDN) 12 Radiometric methods 12.1 γ-method 12.2 β-method 12.3 α-method

Томск, ТПУ, ИГНД, ГЭГХ7 The course content 6 Thermal analysis 6.1 Differential thermal analysis (DTA) 6.2 Thermogravimetry 6.3 Thermodilatometry 6.4 Thermomagnetometry 6.5 Thermovolumetry 6.6 Differentially scanning colorimetry (DSC) 6.7 Emanation method 7 X-ray structure analysis 8 Radiographic methods 8.1 Macroradiography 8.2 Microradiography 8.3 Fission-fragment radiography

Томск, ТПУ, ИГНД, ГЭГХ8 Purpose of the investigation methods – detailed analytical information about material and elemental composition. To get such kind of information it is necessary: 1. to concretize a defined problem 2. to choose correctly the method of investigation, founding on previous investigations and know detection limit of method 3. to carry out sampling and sample preparation according to the chosen method 4. to carry out analysis (carrying conditions of analyses, change mode, combination of methods, errors in analyses) 5. to interpret the results (accuracy, convergence) 6. to conclude (analysis repeat, other methods)

Томск, ТПУ, ИГНД, ГЭГХ9 Classification of methods and requirements to quality of analytical works In accordance with origin  optical (mineragraphy)  physical (radiometry)  chemical (use of chemical agents)  combined (X-ray spectral with chemical preparation of sample)

Томск, ТПУ, ИГНД, ГЭГХ10 Classification of methods In accordance with influence on substance  destructive (thermal, chemical)  non-destructive (luminescent, optical)

Томск, ТПУ, ИГНД, ГЭГХ11 Classification of methods In accordance with results  Determination of material constitution (minerals, alloys – thermal analysis)  Determination of elemental composition (chemical elements – spectral analysis)  Qualitative (qualitative assessment of phase, if there are etalons)  Quantitative (quantitative assessment of phase and mineral, ion, molecule content in it; if there are standards)

Requirements to quality of analytical works Range of solved problems, variety and complexity of objects, quantity of determined components, wide range of their contents lead to that practically all modern analytical methods are used to solve geological problems. Method number are increased according to expansion and complication of geological investigation problems. At present more than 400 methods are applied in production analytical laboratories. Correct formulation of analytical problem, rational choice of methods to solve it can favour an increase of geological investigation effectiveness, reduce the time of their carrying out and at the same time they can supply with necessary information. One of the most important things is objective justification of the required analysis accuracy Томск, ТПУ, ИГНД, ГЭГХ12

Томск, ТПУ, ИГНД, ГЭГХ13 Metrological bases of the analytical work quality control Information content obtained from analysis data is determined by their reliability, i.e. degree of conformity of obtained component content in analyzed substance to real one. «Any experimental result should be considered as approximation to quantity assessment, which remain unknown»

Томск, ТПУ, ИГНД, ГЭГХ14 Reliability of analysis results The basic characteristic of reliability of analysis results is error. The error of the determination result is a difference between the determination result and the real content of determined component. The errors of measurement results have different origin. In connection with this it is necessary to determine nature and type of errors which can influence on the result of analysis.

Certification of analytical methods Томск, ТПУ, ИГНД, ГЭГХ15 Most methods presented in literature (approved by State Standard and recommended for application in determinative branch), as a rule, don’t contain detailed metrological characteristic and economic evaluation. That’s why it is necessary to make objective estimate and metrological certification of all methods of analysis used in analytical laboratories. Certification of methods is carried out according to common plan and data is combined in common document – “«Metrological certificate of analytical methods» (MCAM). Comparison some analytical certificates will allow to choose more optimal method of analysis in this situation.

Methods of metrological monitoring Methods of monitoring are intended for assessment of the quality of analytical determination. It is supposed that all analytical methods, used in laboratories, obtained metrological assessment both in the process of development and in the process of introduction. However, any method of analysis can yield poor results if the analysis is carried out not carefully. All analytical methods must be under the test! Томск, ТПУ, ИГНД, ГЭГХ16

External laboratory monitoring is necessary to give the assessment of the result correctness – to give the assessment of systematic discrepancy between the results of determination carrying out either in different laboratories or by different methods. Samples passed internal laboratory monitoring and had two results of analysis can be sent to external laboratory monitoring Томск, ТПУ, ИГНД, ГЭГХ17 There are two types of metrological monitoring: internal laboratory monitoring and external laboratory monitoring

Standard samples of composition Physical methods of composition studying are applied now very often. They are relative and require calibration of instruments. In addition to that the supplying of uniformity of measurements of mineral chemical composition and objective metrological assessment of methods of analysis are very important. One of the way of solving this problem is to use standard samples of minerals composition (SSC). Standard samples of chemical composition of minerals are specially prepared materials; all component content or their parts are identified with required accuracy Томск, ТПУ, ИГНД, ГЭГХ18

Standard samples of composition Томск, ТПУ, ИГНД, ГЭГХ19