SOCIO–ECONOMIC PROJECTION OF ANALYTICAL CHEMISTRY FOUNDATIONS OF ANALYTICAL CHEMISTRY BLOCK III SOCIO–ECONOMIC PROJECTION OF ANALYTICAL CHEMISTRY Chapter 7. Chapter 8. Chapter 9. Analytical problem-solving Analytical Chemistry and quality Social responsibility of Analytical Chemistry BLOCK I. INTRODUCTION TO ANALYTICAL CHEMISTRY BLOCK II. THE ANALYTICAL PROCESS ANNEX 1. GLOSSARY OF TERMS ANNEX 2. ANSWERS TO THE QUESTIONS 7-1

Chapter 7: Analytical problem-solving BLOCK III SOCIO–ECONOMIC PROJECTION OF ANALYTICAL CHEMISTRY Chapter 7: Analytical problem-solving Contents 7.1.1. Introduction to Block III 7.1.2. Introduccion to the chapter 7.1.3. The concept of “problem” in Analytical Chemistry 7.1.4. Integral definition of “analytical problem” 7.1.5. Elements of an analytical problem 7.1.6. Steps of the analytical problem-solving process 7.1.7. Concluding remarks: 7.1.7.1. Consistency between required and delivered information 7.1.7.2. Analytical problem and quality Teaching objectives To introduce students to the concept “analytical problem” and its elements. To describe the general steps of the analytical problem-solving process. To compare required information and delivered information. To emphasize the applied side of Analytical Chemistry. 7-2

7.1.1. Introduction to Block III (I) Chapter 7: Analytical problem-solving 7.1.1. Introduction to Block III (I) ♣ The block is concerned with the socio–economic consequences of the results and knowledge obtained from analytical processes (Chapter 4), whether quantitative(Chapter 5) or qualitative (Chapter 6). The topic dealt with in the last block of this book is the SOCIO–ECONOMIC PROJECTION OF ANALYTICAL CHEMISTRY. ♣ It uses the third basic standard [(bio)chemical information requirements (see Slide 1.12)] to facilitate decision-making in the social and economic realms, and to assess to what extent such requirements are fulfilled. ♣ The three chapters in Block III are concerned with ♦ A practical analysis of analytical problem-solving, that is, of the fulfilment of information requirements (Chapter 7). ♦ The integral characterization of the socio–economic projection of Amalytical Chemistry in the form of a definition of analytical quality (Chapter 8). ♦ Social responsibility in Analytical Chemistry beyond analytical quality (Chapter 9). 7-3

Chapter 7: Analytical problem-solving 7.1.1. Introduction to Block III (II) CHAPTER 7 ANALYTICAL PROBLEM- SOLVING 3 1 BLOCK III CHAPTER 9 CHAPTER 8 SOCIAL RESPONSI- BILITY OF ANALYTICAL CHEMISTRY ANALYTICAL QUALITY 2 7-4

7.1.2. Introduction to the chapter (I) Chapter 7: Analytical problem-solving 7.1.2. Introduction to the chapter (I) ANALYTICAL CHEMIST ANALYTICAL CHEMISTRY OBTAINING (BIO)CHEMICAL INFORMATION PRACTICAL PURPOSES Chapter I Block I THEORETICAL Knowledge Scientific and techno-logical developments Fulfilling INFORMATION REQUIREMENTS ANALYTICAL PROBLEM Fitness for purpose Required information: CLIENT Chapter 7 Block III 7-5

Chapter 7: Analytical problem-solving ANALYTICAL INFORMATION 7.1.2. Introduction to the chapter (II) QUALITY OF ANALYTICAL INFORMATION FITNESS FOR PURPOSE ACCURACY REPRESENTATIVENESS Chemical metrology 7-6

7.1.3. The concept of “problem” in Analytical Chemistry Chapter 7: Analytical problem-solving 7.1.3. The concept of “problem” in Analytical Chemistry ANALYTICAL PROBLEM PRACTICAL THEORETICAL APPLIED SIDE BASIC SIDE Delivering the chemical information required R&D in Analytical Chemistry 1 2 3 Socio–economic, scientific and technical problems Improving the internal foundations of Analytical Chemistry Incorporating advances from other scientific or technical areas Chapter 7 Block III 7-7

Chapter 7: Analytical problem-solving 7.1.4. Integral definition of “analytical problem” (I) ANALYTICAL CHEMIST CLIENT 1 Socio– economic problem ANALYTICAL PROBLEM Analytical process 2 Information requirements to be fulfilled ANALYTICAL PROBLEM Analytical properties 3 Analytical quality ANALYTICAL PROBLEM External quality Quality of results Quality of CMP 7-8

Chapter 7: Analytical problem-solving PRODUCTIVITY-RELATED 7.1.4. Integral definition of “analytical problem” (II) PROBLEM 1 Conceptual hierarchy OBJECT SAMPLE ANALYTE INTERNAL QUALITY EXTERNAL QUALITY QUALITY OF RESULTS QUALITY OF CMP CAPITAL PROPERTIES BASIC PROPERTIES PRODUCTIVITY-RELATED PROPERTIES REPORTS RESULTS PRIMARY DATA TO ANALYSE TO CHARACTERIZE TO DETECT TO SENSE 2 ANALYSER INSTRUMENT APPARATUS DEVICE Relationship between leading concepts PROCESS TECHNIQUE METHOD PROCEDURE ANALYSIS DETERMINATION MEASUREMENT 7-9

Chapter 7: Analytical problem-solving 7.1.4. Integral definition of “analytical problem” (III) ANALYTICAL PROBLEM SOCIO– ECONOMIC PROBLEM PLANNING 2 TRACEABILITY SOLUTION TRACEABILITY SAMPLE ALIQUOT INTERNAL REPRESENTATIVENESS (orthodox) + TRACING (history of the sample and aliquot) 3 TRACEABILITY HIGHEST REPRESENTATIVENESS (fitness for purpose) + TRACING (history of the sample and aliquot) 1 RESULTS 7-10

7.1.4. Integral definition of “analytical problem” (IV) Chapter 7: Analytical problem-solving 7.1.4. Integral definition of “analytical problem” (IV) AN EXAMPLE OF “ANALYTICAL PROBLEM” IN THE CONTEXT OF TRACEABILITY R1. Content in GOLD 1 µg/100 kg mineral R2.Content LEAD 1 g/100 kg Results SUITABILITY Socio–economic problem Suitability of a pyrite mine for obtaining GOLD MINE UNSUITABLE PLANNING SOLUTION Analysis ANALYTICAL PROBLEM Determination of the amount of GOLD in samples from a stack of mined pyrite Portions of mined mineral collected at different depths in the stack: surface, mean depths… Sample aliquot Collection of sample/aliquots 7-11

7.1.4. Integral definition of “analytical problem” (V) Chapter 7: Analytical problem-solving 7.1.4. Integral definition of “analytical problem” (V) 2 TOP LEVEL IN AN ANALYTICAL HIERARCHY CONNECTED TO THE TOP LEVELS IN OTHER HIERARCHIES 1 INTERFACE BETWEEN THE “CLIENT” AND THE ANALYTICAL CHEMIST ANALYTICAL PROBLEM CROSSING THE TRADITIONAL “BOUNDARIES” OF ANALYTICAL CHEMISTRY TOP LEVEL OF REPRESENTATIVENESS OF THE RESULTS 4 3 7-12

7.1.5. Elements of an analytical problem Chapter 7: Analytical problem-solving 7.1.5. Elements of an analytical problem ECONOMIC, SOCIAL, SCIENTIFIC OR TECHNICAL PROBLEM ANA LYTICAL PROBLEM Planning OBJECT Design SAMPLE(S) ANALYTICAL CHEMISTRY TODAY Evaluation MEASURAND(S) CLASSICAL ANALYTICAL CHEMISTRY Correction ANALYTE(S) INTANGIBLE SIDE TANGIBLE SIDE 7-13

1 2 3 4 5 7.1.6. Steps of the analytical problem-solving process (I) Chapter 7: Analytical problem-solving 7.1.6. Steps of the analytical problem-solving process (I) 1 IDENTIFYING AND CONFIRMING THE ECONOMIC, SOCIAL, SCIENTIFIC AND TECHNICAL INFORMATION REQUIRED 2 Analytical problem SPECIFYING THE ANALYTICAL INFORMATION REQUIRED 3 PLANNING THE STRATEGY YES CHECK 4 END MONITORING THE RESULTS NO 5 CORRECTIVE ACTIONS 7-14

1 7.1.6. Steps of the analytical problem-solving process (II) 2 1 Chapter 7: Analytical problem-solving 7.1.6. Steps of the analytical problem-solving process (II) 1 IDENTIFYING AND CONFIRMING THE INFORMATION REQUIRED Required information CLIENT DECISION- MAKING Characteristics of the information required SOCIO–ECONOMIC PROBLEM COMMUNICATION 2 What? How? When? Where? Why? What…for? 1 Information producer ANALYTICAL CHEMIST 7-15

2 7.1.6. Steps of the analytical problem-solving process (III) 2 1 3 4 Chapter 7: Analytical problem-solving 7.1.6. Steps of the analytical problem-solving process (III) 2 SPECIFYING THE ANALYTICAL INFORMATION REQUIRED Socio–economic information ANALYTICAL information ANALYTICAL CHEMIST MEASURAND(S) ANALYTE(S) SAMPLE SIZE 2 QUALITATIVE QUANTITATIVE, STRUCTURAL 1 TYPES OF ANALYSIS SPECIFIC FEATURES OF THE ANALYTICAL INFORMATION REQUIRED TEMPORAL, STATIC AND/OR SPATIAL 3 4 LEVELS OF ANALYTICAL PROPERTIES GLOBAL DISCRIMINATE 7-16

3 7.1.6. Steps of the analytical problem-solving process (IV) Chapter 7: Analytical problem-solving 7.1.6. Steps of the analytical problem-solving process (IV) 3 PLANNING THE ANALYTICAL STRATEGY (I) PLANNING THE ANALYTICAL STRATEGY SELECTING THE METHOD DESIGNING THE ANALYTICAL PROCESS SAMPLE How? RESULTS 7-17

3 7.1.6. Steps of the analytical problem-solving process (V) 1 2 4 3 Chapter 7: Analytical problem-solving 7.1.6. Steps of the analytical problem-solving process (V) 3 PLANNING THE ANALYTICAL STRATEGY (II) 1 2 TYPE OF INFORMATION GENÉRICA ANALÍTICA CHARACTERISTICS OF THE OBJECT/SAMPLE AND ANALYTES GENERAL ANALYTICAL 2nd step 1st step 2nd step FACTORS INFLUENCING SELECTION OF A CMP AGREED OVERALL OR PER ANALYSIS COST MATERIAL AND HUMAN RESOURCES AVAILABLE 4 3 7-18

4 7.1.6. Steps of the analytical problem-solving process (VI) 2 1 Chapter 7: Analytical problem-solving 7.1.6. Steps of the analytical problem-solving process (VI) 4 MONITORING THE RESULTS 2 1 ANALYTICAL PROPERTIES VALIDATING THE RESULTS INFORMATION REQUIRED BY THE CLIENT INTERNAL (ANALYTICAL) QUALITY EXTERNAL (REQUIRED) QUALITY Convergence ERROR CORRECTION PROBLEM SOLVED 7-19

5 4bis 7.1.6. Steps of the analytical problem-solving process (VII) Chapter 7: Analytical problem-solving 7.1.6. Steps of the analytical problem-solving process (VII) 5 APPLYING CORRECTIVE ACTIONS CORRECTING ERRORS INVALID RESULTS AND INFORMATION MINOR (standards, parameters, instruments) Changes CHECKING THE ANALYTICAL STRATEGY Changes PARTIAL (equipment calibration) Changes VALIDATING THE RESULTS 4bis OVERALL (method) 7-20

1 2 7.1.6. Steps of the analytical problem-solving process (VIII) Chapter 7: Analytical problem-solving 7.1.6. Steps of the analytical problem-solving process (VIII) EXAMPLE: SOLVING A SPECIFIC ANALYTICAL PROBLEM (I) SOCIO–ECONOMIC PROBLEM: Rejecting (action) orange ice creams (what?) if they contain colorant E-127 (erythrosine) because it may cause thyroid disorders (why?). 1 IDENTIFYING THE INFORMATION REQUIRED: Amount of eythrosine in orange ice creams from different manufacturers. Highest allowed additive concentration: 1 ppm. Best before date of the ice creams: 2 weeks. 2 SPECIFYING THE INFORMATION: A qualitative and quantitative study of orange ice cream samples from different manufacturers (is there any erythrosine?, how much?). Highest limit of quantitation: 1 ppm. Expeditiousness needed. 7-21

3 4 5 7.1.6. Steps of the analytical problem-solving process (IX) Chapter 7: Analytical problem-solving 7.1.6. Steps of the analytical problem-solving process (IX) EXAMPLE: SOLVING A SPECIFIC ANALYTICAL PROBLEM (II) 3 PLANNING THE STRATEGY: 1) I f a liquid chromatograph is available: liquid–liquid extraction and chromatography. 2) If only a photometer is available: Preliminary operations (to remove interferents) and photometry. 4 MONITORING THE RESULTS: 1) The limits of detection and quantitation are both acceptable (CLOD < 1 ppm, CLOQ < 1 ppm). 2) The limit of detection is acceptable (CLOD < 1 ppm), but the limit of quantitation is not (CLOQ > 1 ppm). 5 CORRECTIVE ACTIONS: 2) Preconcentration is added to the preliminary operations in order to obtain an acceptable limit of quantitation (CLOQ < 1 ppm). PROBLEM SOLVED 7-22

7.1.7. Concluding remarks (I) Chapter 7: Analytical problem-solving 7.1.7. Concluding remarks (I) 7.1.7.1. CONSISTENCY BETWEEN REQUIRED INFORMATION AND DELIVERED INFORMATION A IDEAL situation = ANALYTICAL CHEMIST B CLIENT ≠ ANALYTICAL INFORMATION DELIVERED ANALYTICAL INFORMATION REQUIRED C < D > DIVERGENT situations 7-23

= 7.1.7. Concluding remarks (II) EXAMPLE A Chapter 7: Analytical problem-solving 7.1.7. Concluding remarks (II) EXAMPLE A DELIVERED INFORMATION = REQUIRED INFORMATION ANALYTICAL CHEMIST CLIENT DELIVERED INFORMATION REQUIRED INFORMATION - 200 yoghourt samples - Total fat (4.00 ± 0.01) g in 125 g of yoghourt = Total fat content of 125 g fruit yoghourts in a batch 7-24

≠ 7.1.7. Concluding remarks (III) EXAMPLE B Chapter 7: Analytical problem-solving 7.1.7. Concluding remarks (III) EXAMPLE B DELIVERED INFORMATION ≠ REQUIRED INFORMATION ANALYTICAL CHEMIST CLIENT DELIVERED INFORMATION REQUIRED INFORMATION - 200 yoghourt samples - Total sugar content (5.50 ± 0.01) g in 125 g of yoghourt ≠ Total fat content of 125 g fruit yoghourts in a batch 7-25

< 7.1.7. Concluding remarks (IV) EXAMPLE C Chapter 7: Analytical problem-solving 7.1.7. Concluding remarks (IV) EXAMPLE C DELIVERED INFORMATION < REQUIRED INFORMATION CLIENT ANALYTICAL CHEMIST REQUIRED INFORMATION DELIVERED INFORMATION Contents in - saturated - monounsaturated - polyunsaturated fat of 125 g fruit yoghourts in a batch - 200 yoghourt samples - Content in saturated fat (2.70 ± 0.01) g in 125 g of yoghourt < 7-26

> 7.1.7. Concluding remarks (V) EXAMPLE D Chapter 7: Analytical problem-solving 7.1.7. Concluding remarks (V) EXAMPLE D DELIVERED INFORMATION > REQUIRED INFORMATION ANALYTICAL CHEMIST CLIENT DELIVERED INFORMATION REQUIRED INFORMATION - 200 samples - Advanced technology - Fat: → Saturated (2.70 ± 0.01) g → Monounsaturated (0.60 ± 0.01) g → Polyunsaturated (0.70 ± 0.01) g > Total fat content of 125 g fruit yoghourts in a batch Total (4.00 ± 0.01) g in 125 g of yoghourt 7-27

1 3 3 2 7.1.7. Concluding remarks (VI) A B QUALITY ANALYTICAL QUALITY Chapter 7: Analytical problem-solving 7.1.7. Concluding remarks (VI) 7.1.7.2. ANALYTICAL PROBLEM AND QUALITY QUALITY 1 BASIC APPLIED BODY OF INDICATORS CLIENT SATISFACTION 3 3 A B ANALYTICAL PROPERTIES ANALYTICAL PROBLEM-SOLVING BASIC APPLIED 2 ANALYTICAL QUALITY 7-28