Hans-Joachim Hübschmann graduated as Certified Food Chemist from the Technical University in Berlin, Germany, working on residue analysis of anabolic agents and pesticides in foods. He started his career in diagnostics, medical analytical instruments and application development working for a number of German companies in chromatography, mass spectrometry and in biotechnology. He joined Thermo Fisher Scientific in Bremen, Germany, and held several international positions covering inorganic and isotope ratio mass spectrometry specializing in food safety, forensic and dioxin analysis. In 2015 he established the independent consulting agency HANS Analytical Solutions for the development of automated sample preparation workflows. In his current capacity he is located in Osaka, Japan, as the Vice President Sales of CTC Analytics for the emerging Asia/Pacific region.

• Foreword xiiiPreface xv1 Introduction 11.1 A Perspective on Human Performance 2References 52 The Analytical Process 72.1 Laboratory Logistics 72.1.1 Analytical Benefits of Instrumental Workflows 92.1.1.1 Data Quality 112.1.1.2 Turnkey Operation 112.1.1.3 Green Analytical Chemistry 112.1.1.4 Productivity 122.1.2 Standard Operation Procedure 132.1.3 Economical Aspects 15References 163 Workflow Concepts 193.1 Sample Preparation Workflow Design 193.1.1 Transfer of Standard Methods to Automated Workflows 203.1.2 Method Translation 213.1.2.1 Sketching the Automated Workflow 223.1.2.2 Robotic System Configuration 223.1.3 Online or Offline Configuration 253.2 Instrumental Concepts 253.2.1 Workstations 253.2.2 Revolving Tray Autosamplers 263.2.3 Selective Compliance Articulated Robots 283.2.4 Cartesian Robots 283.2.5 Multiple Axis Robots 323.2.6 Collaborative Robots 333.3 Sample Processing 353.3.1 Sequential Sample Preparation 353.3.2 Prep-ahead Mode 353.3.3 Incubation Overlapping 363.3.4 Batch Processing 363.3.5 Parallel Processing Workflows 383.3.6 Sample Identification 383.3.6.1 Barcodes 383.3.6.2 Radio-Frequency Identification Chips 403.4 Tool Change 413.4.1 Manual Tool Change 413.4.2 Automated Tool Change 423.4.3 Tool Identification 443.5 Object Transport 463.5.1 Magnetic Transport 463.5.2 Gripper Transport 483.5.3 Needle Transport 503.6 Vial Decapping 50References 524 Analytical Aspects 554.1 Liquid Handling 554.1.1 About Drops and Droplets 554.1.2 Syringes 564.1.2.1 Precision and Accuracy 574.1.2.2 Syringe Needles 584.1.2.3 Syringe Needle Point Styles 594.1.2.4 Syringe Plunger Types 604.1.2.5 Syringe Termination 614.1.2.6 Operational Parameters 624.1.3 Vial Bottom Sensing 664.1.4 Pipetting 674.1.4.1 Air Displacement Pipettes 684.1.4.2 Positive Displacement Pipets 694.1.4.3 Pipetting Modes 694.1.4.4 Aspiration 714.1.4.5 Dispensing 734.1.4.6 Liquid-Level Detection 744.1.4.7 Liquid Classes 754.1.4.8 Pipet Tips 754.1.4.9 Functional Pipet Tips 784.1.4.10 Pipet Tip Materials 814.1.5 Dilutor/Dispenser Operation 824.1.6 Flow Cell Sampling 844.2 Solid Materials Handling 854.2.1 Workflows with Solid Materials 864.2.2 Automated Solids Dosing by Powder Dispensing 864.3 Weighing 884.4 Extraction 904.4.1 Liquid Extraction 914.4.2 Pressurized Fluid Extraction 924.4.2.1 Solvents and Extraction 934.4.2.2 Miniaturization and Automation 944.4.2.3 In-Cell Clean-Up 964.4.2.4 International Standard Methods 974.4.3 Liquid/Liquid Extraction 974.4.4 Dispersive Liquid/Liquid Micro-Extraction 1004.4.4.1 Automated DLLME Workflows 1034.4.4.2 DLLME for Soil and Urine 1034.4.4.3 DLLME for Pesticides in Food 1044.4.4.4 DLLME Hyphenation with LC 1044.4.5 Sorptive Sample Preparation 1044.4.5.1 Solid-Phase Micro-Extraction 1054.4.5.2 SPME Fiber 1094.4.5.3 SPME Arrow 1124.4.5.4 Solid-Phase Micro-Extraction with Derivatization 1164.4.5.5 Direct Solid-Phase Micro-Extraction Mass Spectrometry 1194.4.5.6 Stir Bar Sorptive Extraction 1214.4.5.7 Thin-Film Micro-Extraction 1234.5 Clean-Up Procedures 1244.5.1 Filtration 1244.5.1.1 Filter Materials 1254.5.1.2 Syringe Filter 1264.5.1.3 Filter Vials 1274.5.2 Solid-Phase Extraction 1294.5.2.1 The General SPE Clean-Up Procedure 1334.5.2.2 On-Line SPE 1344.5.2.3 Micro-SPE Clean-Up 1374.5.2.4 Syringe-Based Micro-SPE 1414.5.3 Gel Permeation Chromatography 1434.5.3.1 Standardized Methods 1454.5.3.2 Workflow and Instrument Configuration 1454.5.3.3 GPC-GC Online Coupling 1464.5.3.4 Micro-GPC-GC Online Coupling 1474.6 Centrifugation 1484.7 Evaporation 1504.8 Derivatization 1534.8.1 For LC and LC-MS 1544.8.1.1 Aromatic Acid Chlorides 1544.8.1.2 Dansylchloride 1554.8.1.3 Ninhydrin Reaction 1554.8.1.4 FMOC Derivatization 1554.8.2 For GC and GC-MS 1564.8.2.1 Silylation 1564.8.2.2 Acetylation 1574.8.2.3 Methylation 1574.8.2.4 Methoxyamination 1584.8.2.5 Fluorinating Reagents 1584.8.3 For GC and GC-MS In-Port Derivatization 1594.9 Temperature Control 1634.9.1 Heating 1634.9.1.1 Incubation Overlapping 1634.9.2 Cooling 1644.10 Mixing 1664.10.1 Vortexing 1664.10.2 Agitation 1674.10.3 Spinning 1694.10.4 Mixing with Syringes 1694.10.5 Cycloidal Mixing 169References 1715 Integration into Analysis Techniques 1915.1 GC Volatiles Analysis 1915.1.1 Static Headspace Analysis 1925.1.1.1 Overcoming Matrix Effects 1945.1.1.2 Measures to Increase Analyte Sensitivity 1955.1.1.3 Static Headspace Injection Technique 1955.1.2 Multiple Headspace Quantification 1975.1.3 Dynamic Headspace Analysis 2015.1.3.1 Purge and Trap 2025.1.3.2 Dynamic Headspace Analysis with In-Tube Extraction 2045.1.3.3 Dynamic Headspace Analysis Using Sorbent Tubes 2075.1.3.4 Needle Trap Microextraction 2085.1.4 Tube Adsorption 2105.2 GC Liquid Injection 2225.2.1 Sandwich Injection 2225.2.2 Hot Needle Injection 2225.2.3 Liquid Band Injection 2245.2.4 Automated Liner Exchange 2265.3 LC–GC Online Injection 2305.4 LC Injection 2335.4.1 Dynamic Load and Wash 2345.4.2 Using LC Injection Ports with a Pipette Tool 235References 2376 Solutions for Automated Analyses 247First About Safety 2486.1 Dilution 2486.1.1 Geometric Dilution of Reference Standards 2486.1.2 Dilution for Calibration Curves 2516.1.3 Preparation of Working Standards 2566.2 Derivatization 2596.2.1 Silylation 2606.2.2 SPME On-Fiber Derivatization 2626.2.3 Metabolite Profiling by Methoximation and Silylation 2666.3 Taste and Odor Compounds Trace Analysis 2716.4 Sulfur Compounds in Tropical Fruits 2766.5 Ethanol Residues in Halal Food 2846.6 Volatile Organic Compounds in Drinking Water 2896.7 Geosmin and 2-MIB 2956.8 Solvent Elution from Charcoal 3016.9 Semivolatile Organic Compounds in Water 3046.10 Polyaromatic Hydrocarbons in Drinking Water 3156.11 Fatty Acid Methylester 3216.11.1 Application 3216.12 MCPD and Glycidol in Vegetable Oils 3286.13 Mineral Oil Hydrocarbons MOSH/MOAH 3396.14 Pesticides Analysis – QuEChERS Extract Clean-Up 3476.15 Glyphosate, AMPA, and Glufosinate by Online SPE-LC-MS 3626.16 Pesticides, PPCPs, and PAHs by Online-SPE Water Analysis 3686.17 Residual Solvents 3756.18 Chemical Warfare Agents in Water and Soil 3826.19 Shale Aldehydes in Beer 3906.20 Phthalates in Polymers 394References 400A Appendix 413A.1 Robotic System Control 413A.1.1 Maestro Software 413A.1.2 Chronos Software 414A.1.3 Graphical Workflow Programming 415A.1.4 Sample Control Software 416A.1.5 Local System Control 417A.1.6 Script Control Language 418A.2 System Maintenance 418A.2.1 Syringes 418A.2.1.1 Manual Syringe Handling 418A.2.1.2 Syringe Cleaning 418A.2.1.3 Plunger Cleaning 419A.2.1.4 Needle Cleaning 419A.2.1.5 Confirming the Dispensed Volume of a Syringe 420A.2.1.6 Sterilization 420A.2.2 Pipettes 421A.2.2.1 Calibration 421A.2.2.2 Pipette Parts Maintenance 421A.2.3 System Hardware Maintenance Schedule 422A.3 Syringe Needle Gauge 423A.4 Pressure Units Conversion 425A.5 Solvents 425A.5.1 Solvent Miscibility 425A.5.2 Solvent Stability 428A.5.2.1 Halogenated Solvents 428A.5.2.2 Ethers 429A.5.3 Solvent Viscosity 429A.6 Material Resistance 429A.6.1 Glass 432A.6.2 Polymers 432A.6.3 Stainless Steel 433References 437Glossary 441References 451Index 453

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Hans-Joachim Hübschmann graduated as Certified Food Chemist from the Technical University in Berlin, Germany, working on residue analysis of anabolic agents and pesticides in foods. He started his career in diagnostics, medical analytical instruments and application development working for a number of German companies in chromatography, mass spectrometry and in biotechnology. He joined Thermo Fisher Scientific in Bremen, Germany, and held several international positions covering inorganic and isotope ratio mass spectrometry specializing in food safety, forensic and dioxin analysis. In 2015 he established the independent consulting agency HANS Analytical Solutions for the development of automated sample preparation workflows. In his current capacity he is located in Osaka, Japan, as the Vice President Sales of CTC Analytics for the emerging Asia/Pacific region.

• Foreword xiiiPreface xv1 Introduction 11.1 A Perspective on Human Performance 2References 52 The Analytical Process 72.1 Laboratory Logistics 72.1.1 Analytical Benefits of Instrumental Workflows 92.1.1.1 Data Quality 112.1.1.2 Turnkey Operation 112.1.1.3 Green Analytical Chemistry 112.1.1.4 Productivity 122.1.2 Standard Operation Procedure 132.1.3 Economical Aspects 15References 163 Workflow Concepts 193.1 Sample Preparation Workflow Design 193.1.1 Transfer of Standard Methods to Automated Workflows 203.1.2 Method Translation 213.1.2.1 Sketching the Automated Workflow 223.1.2.2 Robotic System Configuration 223.1.3 Online or Offline Configuration 253.2 Instrumental Concepts 253.2.1 Workstations 253.2.2 Revolving Tray Autosamplers 263.2.3 Selective Compliance Articulated Robots 283.2.4 Cartesian Robots 283.2.5 Multiple Axis Robots 323.2.6 Collaborative Robots 333.3 Sample Processing 353.3.1 Sequential Sample Preparation 353.3.2 Prep-ahead Mode 353.3.3 Incubation Overlapping 363.3.4 Batch Processing 363.3.5 Parallel Processing Workflows 383.3.6 Sample Identification 383.3.6.1 Barcodes 383.3.6.2 Radio-Frequency Identification Chips 403.4 Tool Change 413.4.1 Manual Tool Change 413.4.2 Automated Tool Change 423.4.3 Tool Identification 443.5 Object Transport 463.5.1 Magnetic Transport 463.5.2 Gripper Transport 483.5.3 Needle Transport 503.6 Vial Decapping 50References 524 Analytical Aspects 554.1 Liquid Handling 554.1.1 About Drops and Droplets 554.1.2 Syringes 564.1.2.1 Precision and Accuracy 574.1.2.2 Syringe Needles 584.1.2.3 Syringe Needle Point Styles 594.1.2.4 Syringe Plunger Types 604.1.2.5 Syringe Termination 614.1.2.6 Operational Parameters 624.1.3 Vial Bottom Sensing 664.1.4 Pipetting 674.1.4.1 Air Displacement Pipettes 684.1.4.2 Positive Displacement Pipets 694.1.4.3 Pipetting Modes 694.1.4.4 Aspiration 714.1.4.5 Dispensing 734.1.4.6 Liquid-Level Detection 744.1.4.7 Liquid Classes 754.1.4.8 Pipet Tips 754.1.4.9 Functional Pipet Tips 784.1.4.10 Pipet Tip Materials 814.1.5 Dilutor/Dispenser Operation 824.1.6 Flow Cell Sampling 844.2 Solid Materials Handling 854.2.1 Workflows with Solid Materials 864.2.2 Automated Solids Dosing by Powder Dispensing 864.3 Weighing 884.4 Extraction 904.4.1 Liquid Extraction 914.4.2 Pressurized Fluid Extraction 924.4.2.1 Solvents and Extraction 934.4.2.2 Miniaturization and Automation 944.4.2.3 In-Cell Clean-Up 964.4.2.4 International Standard Methods 974.4.3 Liquid/Liquid Extraction 974.4.4 Dispersive Liquid/Liquid Micro-Extraction 1004.4.4.1 Automated DLLME Workflows 1034.4.4.2 DLLME for Soil and Urine 1034.4.4.3 DLLME for Pesticides in Food 1044.4.4.4 DLLME Hyphenation with LC 1044.4.5 Sorptive Sample Preparation 1044.4.5.1 Solid-Phase Micro-Extraction 1054.4.5.2 SPME Fiber 1094.4.5.3 SPME Arrow 1124.4.5.4 Solid-Phase Micro-Extraction with Derivatization 1164.4.5.5 Direct Solid-Phase Micro-Extraction Mass Spectrometry 1194.4.5.6 Stir Bar Sorptive Extraction 1214.4.5.7 Thin-Film Micro-Extraction 1234.5 Clean-Up Procedures 1244.5.1 Filtration 1244.5.1.1 Filter Materials 1254.5.1.2 Syringe Filter 1264.5.1.3 Filter Vials 1274.5.2 Solid-Phase Extraction 1294.5.2.1 The General SPE Clean-Up Procedure 1334.5.2.2 On-Line SPE 1344.5.2.3 Micro-SPE Clean-Up 1374.5.2.4 Syringe-Based Micro-SPE 1414.5.3 Gel Permeation Chromatography 1434.5.3.1 Standardized Methods 1454.5.3.2 Workflow and Instrument Configuration 1454.5.3.3 GPC-GC Online Coupling 1464.5.3.4 Micro-GPC-GC Online Coupling 1474.6 Centrifugation 1484.7 Evaporation 1504.8 Derivatization 1534.8.1 For LC and LC-MS 1544.8.1.1 Aromatic Acid Chlorides 1544.8.1.2 Dansylchloride 1554.8.1.3 Ninhydrin Reaction 1554.8.1.4 FMOC Derivatization 1554.8.2 For GC and GC-MS 1564.8.2.1 Silylation 1564.8.2.2 Acetylation 1574.8.2.3 Methylation 1574.8.2.4 Methoxyamination 1584.8.2.5 Fluorinating Reagents 1584.8.3 For GC and GC-MS In-Port Derivatization 1594.9 Temperature Control 1634.9.1 Heating 1634.9.1.1 Incubation Overlapping 1634.9.2 Cooling 1644.10 Mixing 1664.10.1 Vortexing 1664.10.2 Agitation 1674.10.3 Spinning 1694.10.4 Mixing with Syringes 1694.10.5 Cycloidal Mixing 169References 1715 Integration into Analysis Techniques 1915.1 GC Volatiles Analysis 1915.1.1 Static Headspace Analysis 1925.1.1.1 Overcoming Matrix Effects 1945.1.1.2 Measures to Increase Analyte Sensitivity 1955.1.1.3 Static Headspace Injection Technique 1955.1.2 Multiple Headspace Quantification 1975.1.3 Dynamic Headspace Analysis 2015.1.3.1 Purge and Trap 2025.1.3.2 Dynamic Headspace Analysis with In-Tube Extraction 2045.1.3.3 Dynamic Headspace Analysis Using Sorbent Tubes 2075.1.3.4 Needle Trap Microextraction 2085.1.4 Tube Adsorption 2105.2 GC Liquid Injection 2225.2.1 Sandwich Injection 2225.2.2 Hot Needle Injection 2225.2.3 Liquid Band Injection 2245.2.4 Automated Liner Exchange 2265.3 LC–GC Online Injection 2305.4 LC Injection 2335.4.1 Dynamic Load and Wash 2345.4.2 Using LC Injection Ports with a Pipette Tool 235References 2376 Solutions for Automated Analyses 247First About Safety 2486.1 Dilution 2486.1.1 Geometric Dilution of Reference Standards 2486.1.2 Dilution for Calibration Curves 2516.1.3 Preparation of Working Standards 2566.2 Derivatization 2596.2.1 Silylation 2606.2.2 SPME On-Fiber Derivatization 2626.2.3 Metabolite Profiling by Methoximation and Silylation 2666.3 Taste and Odor Compounds Trace Analysis 2716.4 Sulfur Compounds in Tropical Fruits 2766.5 Ethanol Residues in Halal Food 2846.6 Volatile Organic Compounds in Drinking Water 2896.7 Geosmin and 2-MIB 2956.8 Solvent Elution from Charcoal 3016.9 Semivolatile Organic Compounds in Water 3046.10 Polyaromatic Hydrocarbons in Drinking Water 3156.11 Fatty Acid Methylester 3216.11.1 Application 3216.12 MCPD and Glycidol in Vegetable Oils 3286.13 Mineral Oil Hydrocarbons MOSH/MOAH 3396.14 Pesticides Analysis – QuEChERS Extract Clean-Up 3476.15 Glyphosate, AMPA, and Glufosinate by Online SPE-LC-MS 3626.16 Pesticides, PPCPs, and PAHs by Online-SPE Water Analysis 3686.17 Residual Solvents 3756.18 Chemical Warfare Agents in Water and Soil 3826.19 Shale Aldehydes in Beer 3906.20 Phthalates in Polymers 394References 400A Appendix 413A.1 Robotic System Control 413A.1.1 Maestro Software 413A.1.2 Chronos Software 414A.1.3 Graphical Workflow Programming 415A.1.4 Sample Control Software 416A.1.5 Local System Control 417A.1.6 Script Control Language 418A.2 System Maintenance 418A.2.1 Syringes 418A.2.1.1 Manual Syringe Handling 418A.2.1.2 Syringe Cleaning 418A.2.1.3 Plunger Cleaning 419A.2.1.4 Needle Cleaning 419A.2.1.5 Confirming the Dispensed Volume of a Syringe 420A.2.1.6 Sterilization 420A.2.2 Pipettes 421A.2.2.1 Calibration 421A.2.2.2 Pipette Parts Maintenance 421A.2.3 System Hardware Maintenance Schedule 422A.3 Syringe Needle Gauge 423A.4 Pressure Units Conversion 425A.5 Solvents 425A.5.1 Solvent Miscibility 425A.5.2 Solvent Stability 428A.5.2.1 Halogenated Solvents 428A.5.2.2 Ethers 429A.5.3 Solvent Viscosity 429A.6 Material Resistance 429A.6.1 Glass 432A.6.2 Polymers 432A.6.3 Stainless Steel 433References 437Glossary 441References 451Index 453

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Hans-Joachim Hübschmann graduated as Certified Food Chemist from the Technical University in Berlin, Germany, working on residue analysis of anabolic agents and pesticides in foods. He started his career in diagnostics, medical analytical instruments and application development working for a number of German companies in chromatography, mass spectrometry and in biotechnology. He joined Thermo Fisher Scientific in Bremen, Germany, and held several international positions covering inorganic and isotope ratio mass spectrometry specializing in food safety, forensic and dioxin analysis. In 2015 he established the independent consulting agency HANS Analytical Solutions for the development of automated sample preparation workflows. In his current capacity he is located in Osaka, Japan, as the Vice President Sales of CTC Analytics for the emerging Asia/Pacific region.

• Foreword xiiiPreface xv1 Introduction 11.1 A Perspective on Human Performance 2References 52 The Analytical Process 72.1 Laboratory Logistics 72.1.1 Analytical Benefits of Instrumental Workflows 92.1.1.1 Data Quality 112.1.1.2 Turnkey Operation 112.1.1.3 Green Analytical Chemistry 112.1.1.4 Productivity 122.1.2 Standard Operation Procedure 132.1.3 Economical Aspects 15References 163 Workflow Concepts 193.1 Sample Preparation Workflow Design 193.1.1 Transfer of Standard Methods to Automated Workflows 203.1.2 Method Translation 213.1.2.1 Sketching the Automated Workflow 223.1.2.2 Robotic System Configuration 223.1.3 Online or Offline Configuration 253.2 Instrumental Concepts 253.2.1 Workstations 253.2.2 Revolving Tray Autosamplers 263.2.3 Selective Compliance Articulated Robots 283.2.4 Cartesian Robots 283.2.5 Multiple Axis Robots 323.2.6 Collaborative Robots 333.3 Sample Processing 353.3.1 Sequential Sample Preparation 353.3.2 Prep-ahead Mode 353.3.3 Incubation Overlapping 363.3.4 Batch Processing 363.3.5 Parallel Processing Workflows 383.3.6 Sample Identification 383.3.6.1 Barcodes 383.3.6.2 Radio-Frequency Identification Chips 403.4 Tool Change 413.4.1 Manual Tool Change 413.4.2 Automated Tool Change 423.4.3 Tool Identification 443.5 Object Transport 463.5.1 Magnetic Transport 463.5.2 Gripper Transport 483.5.3 Needle Transport 503.6 Vial Decapping 50References 524 Analytical Aspects 554.1 Liquid Handling 554.1.1 About Drops and Droplets 554.1.2 Syringes 564.1.2.1 Precision and Accuracy 574.1.2.2 Syringe Needles 584.1.2.3 Syringe Needle Point Styles 594.1.2.4 Syringe Plunger Types 604.1.2.5 Syringe Termination 614.1.2.6 Operational Parameters 624.1.3 Vial Bottom Sensing 664.1.4 Pipetting 674.1.4.1 Air Displacement Pipettes 684.1.4.2 Positive Displacement Pipets 694.1.4.3 Pipetting Modes 694.1.4.4 Aspiration 714.1.4.5 Dispensing 734.1.4.6 Liquid-Level Detection 744.1.4.7 Liquid Classes 754.1.4.8 Pipet Tips 754.1.4.9 Functional Pipet Tips 784.1.4.10 Pipet Tip Materials 814.1.5 Dilutor/Dispenser Operation 824.1.6 Flow Cell Sampling 844.2 Solid Materials Handling 854.2.1 Workflows with Solid Materials 864.2.2 Automated Solids Dosing by Powder Dispensing 864.3 Weighing 884.4 Extraction 904.4.1 Liquid Extraction 914.4.2 Pressurized Fluid Extraction 924.4.2.1 Solvents and Extraction 934.4.2.2 Miniaturization and Automation 944.4.2.3 In-Cell Clean-Up 964.4.2.4 International Standard Methods 974.4.3 Liquid/Liquid Extraction 974.4.4 Dispersive Liquid/Liquid Micro-Extraction 1004.4.4.1 Automated DLLME Workflows 1034.4.4.2 DLLME for Soil and Urine 1034.4.4.3 DLLME for Pesticides in Food 1044.4.4.4 DLLME Hyphenation with LC 1044.4.5 Sorptive Sample Preparation 1044.4.5.1 Solid-Phase Micro-Extraction 1054.4.5.2 SPME Fiber 1094.4.5.3 SPME Arrow 1124.4.5.4 Solid-Phase Micro-Extraction with Derivatization 1164.4.5.5 Direct Solid-Phase Micro-Extraction Mass Spectrometry 1194.4.5.6 Stir Bar Sorptive Extraction 1214.4.5.7 Thin-Film Micro-Extraction 1234.5 Clean-Up Procedures 1244.5.1 Filtration 1244.5.1.1 Filter Materials 1254.5.1.2 Syringe Filter 1264.5.1.3 Filter Vials 1274.5.2 Solid-Phase Extraction 1294.5.2.1 The General SPE Clean-Up Procedure 1334.5.2.2 On-Line SPE 1344.5.2.3 Micro-SPE Clean-Up 1374.5.2.4 Syringe-Based Micro-SPE 1414.5.3 Gel Permeation Chromatography 1434.5.3.1 Standardized Methods 1454.5.3.2 Workflow and Instrument Configuration 1454.5.3.3 GPC-GC Online Coupling 1464.5.3.4 Micro-GPC-GC Online Coupling 1474.6 Centrifugation 1484.7 Evaporation 1504.8 Derivatization 1534.8.1 For LC and LC-MS 1544.8.1.1 Aromatic Acid Chlorides 1544.8.1.2 Dansylchloride 1554.8.1.3 Ninhydrin Reaction 1554.8.1.4 FMOC Derivatization 1554.8.2 For GC and GC-MS 1564.8.2.1 Silylation 1564.8.2.2 Acetylation 1574.8.2.3 Methylation 1574.8.2.4 Methoxyamination 1584.8.2.5 Fluorinating Reagents 1584.8.3 For GC and GC-MS In-Port Derivatization 1594.9 Temperature Control 1634.9.1 Heating 1634.9.1.1 Incubation Overlapping 1634.9.2 Cooling 1644.10 Mixing 1664.10.1 Vortexing 1664.10.2 Agitation 1674.10.3 Spinning 1694.10.4 Mixing with Syringes 1694.10.5 Cycloidal Mixing 169References 1715 Integration into Analysis Techniques 1915.1 GC Volatiles Analysis 1915.1.1 Static Headspace Analysis 1925.1.1.1 Overcoming Matrix Effects 1945.1.1.2 Measures to Increase Analyte Sensitivity 1955.1.1.3 Static Headspace Injection Technique 1955.1.2 Multiple Headspace Quantification 1975.1.3 Dynamic Headspace Analysis 2015.1.3.1 Purge and Trap 2025.1.3.2 Dynamic Headspace Analysis with In-Tube Extraction 2045.1.3.3 Dynamic Headspace Analysis Using Sorbent Tubes 2075.1.3.4 Needle Trap Microextraction 2085.1.4 Tube Adsorption 2105.2 GC Liquid Injection 2225.2.1 Sandwich Injection 2225.2.2 Hot Needle Injection 2225.2.3 Liquid Band Injection 2245.2.4 Automated Liner Exchange 2265.3 LC–GC Online Injection 2305.4 LC Injection 2335.4.1 Dynamic Load and Wash 2345.4.2 Using LC Injection Ports with a Pipette Tool 235References 2376 Solutions for Automated Analyses 247First About Safety 2486.1 Dilution 2486.1.1 Geometric Dilution of Reference Standards 2486.1.2 Dilution for Calibration Curves 2516.1.3 Preparation of Working Standards 2566.2 Derivatization 2596.2.1 Silylation 2606.2.2 SPME On-Fiber Derivatization 2626.2.3 Metabolite Profiling by Methoximation and Silylation 2666.3 Taste and Odor Compounds Trace Analysis 2716.4 Sulfur Compounds in Tropical Fruits 2766.5 Ethanol Residues in Halal Food 2846.6 Volatile Organic Compounds in Drinking Water 2896.7 Geosmin and 2-MIB 2956.8 Solvent Elution from Charcoal 3016.9 Semivolatile Organic Compounds in Water 3046.10 Polyaromatic Hydrocarbons in Drinking Water 3156.11 Fatty Acid Methylester 3216.11.1 Application 3216.12 MCPD and Glycidol in Vegetable Oils 3286.13 Mineral Oil Hydrocarbons MOSH/MOAH 3396.14 Pesticides Analysis – QuEChERS Extract Clean-Up 3476.15 Glyphosate, AMPA, and Glufosinate by Online SPE-LC-MS 3626.16 Pesticides, PPCPs, and PAHs by Online-SPE Water Analysis 3686.17 Residual Solvents 3756.18 Chemical Warfare Agents in Water and Soil 3826.19 Shale Aldehydes in Beer 3906.20 Phthalates in Polymers 394References 400A Appendix 413A.1 Robotic System Control 413A.1.1 Maestro Software 413A.1.2 Chronos Software 414A.1.3 Graphical Workflow Programming 415A.1.4 Sample Control Software 416A.1.5 Local System Control 417A.1.6 Script Control Language 418A.2 System Maintenance 418A.2.1 Syringes 418A.2.1.1 Manual Syringe Handling 418A.2.1.2 Syringe Cleaning 418A.2.1.3 Plunger Cleaning 419A.2.1.4 Needle Cleaning 419A.2.1.5 Confirming the Dispensed Volume of a Syringe 420A.2.1.6 Sterilization 420A.2.2 Pipettes 421A.2.2.1 Calibration 421A.2.2.2 Pipette Parts Maintenance 421A.2.3 System Hardware Maintenance Schedule 422A.3 Syringe Needle Gauge 423A.4 Pressure Units Conversion 425A.5 Solvents 425A.5.1 Solvent Miscibility 425A.5.2 Solvent Stability 428A.5.2.1 Halogenated Solvents 428A.5.2.2 Ethers 429A.5.3 Solvent Viscosity 429A.6 Material Resistance 429A.6.1 Glass 432A.6.2 Polymers 432A.6.3 Stainless Steel 433References 437Glossary 441References 451Index 453

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