Roadshow Mikrofluidik 2013 Automatized Execution of Multivariate Experiments

Roadshow Mikrofluidik 2013 Automatized Execution of Multivariate Experiments in Microstructured Reactors (Automatisierte Durchführung multivariater Experimente in mikrostrukturierten Reaktoren) Hi. Tec Zang Gmb. H

Micro Technology Motivation for Laboratory Automation Acceleration of development processes (time-to-market) Advanced reproducibility Increased reliability Increased safety Advanced process control Inline analytics Improvement of quality Cost savings: Unattended operation (overnight, weekend, . . . ) Automated data evaluation Resource savings: Chemicals Energy Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 2

Micro Technology Laboratory Automation Special conditions for automation in R&D labs Constraint Resultant claim Tight deadlines Flexible, modular experimental setup with standardised components and connectors Rare space Compact technology High cost pressure Cost effective technique, low engineering costs For lack of qualified personnel: Adaptation of changing tasks and operation of automation technology by laboratory personnel, as far as compatible with the safety regulations Easy to use technology for basic functions (like connection of sensors, actuators and standardised components …) Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 3

Micro Technology Laboratory Automation General requirements to Process Control Systems in R&D Very easy handling High flexibility Modular construction of hardware and software PC-based user interface Low system costs compared to automation of production Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 4

Micro Technology Laboratory Automation Special hardware requirements for R&D Compact installation direct at the process plant Flexible, standardised and potential-free interfaces (EMI robust) Trouble-free interfacing with sensors, actuators and laboratory apparatuses High precision (20/24 bit resolution, absolute measurement uncertainty <0. 1% / <0. 01%) Integrated universal and specialized closed loop process controllers with autotune functionality Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 5

Micro Technology Laboratory Automation Special software requirements for R&D Drag and drop programming of the recipe schedule e. g. according to IEC unit operation concept Online configuration and parameterisation during plant operation Large depth of processing data by using integrated control and analysis programming language Data export for external programs (. xls, . csv, . txt, …) Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 6

Micro Technology Accelerating the development process Previous methods: Parallelisation of experiments in Batch Reactors Typical Volume 0. 1 to 5 Liter Advantages Proven technology Simplified scale-up Disadvantages Relatively large space required Possibly high safety expenses Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 7

Micro Technology Accelerating the development process Previous methods: Parallelisation of experiments in Synthesis Robots Typical Volume 1 ml to 100 ml Advantages Proven technology Highest throughput by massively parallel operation Disadvantages Restricted in unit operations Possibly high safety expenses Very complicated for pressure or vacuum No simple scale-up Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 8

Micro Technology Accelerating the development process New paradigm in micro reaction plants: Sequencing of experiments in Continuous Reactors instead of parallelisation experiments in batch reactors Advantages Only one single reaction system needed Fewer restrictions in terms of pressure and temperature compatible to continous production Relatively high throughput Best reproducibility due to automated operation Disadvantages Not yet adopted everywhere Not suitable for all syntheses Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 9

Micro Technology Experimental setup PI flowsheet (example) 2 reaction steps 4 individualy controlled feeds 5 individually controlled temperatures Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 10

Micro Technology Experimental setup Fully automated Lab. Box process-interface Lab. Vision® software with Easy. Batch Auot. Sam autosampler TM TM TM Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 11

Micro Technology Instrumentation components Liquid conveyors Gear pumps Annular gear pumps Syringe pumps Gravimetric control units Balances Mass flow meters and controllers Autosamplers, Liquid handling systems and multi port valves Upstream and downstream processing Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 12

Micro Technology Instrumentation components Standard sensors and actuators T, p, p. H, . . . / valves, heaters, . . . Tempering systems Electrical heaters Constant temperature circulators Fourfold tempering System, only one chiller required Cryogenic system down to - 180 ° C Inline analytical instruments ATR-FTIR, NIR, UV spectr. Liquid phase detector (organic/anorganic) Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 13

Micro Technology Automation system hardware Lab. Manager® (or Lab. Box ) process interface TM Standardised NAMUR connectors for sensors, actuators, laboratory equipment and analytic instruments Integrated closed loop controllers and power supplies Extremly compact (a small box instead of a bulky cabinet) Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 14

Micro Technology Automation system interfaces Analogue inputs and outputs Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 15

Micro Technology Automation system interfaces Analogue inputs Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 16

Micro Technology Automation system interfaces Digital inputs and outputs Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 17

Micro Technology Automation system interfaces Heater drivers and serial interfaces Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 18

Micro Technology Interface Example Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 19

Micro Technology Automation system software Lab. Vision® Standard in laboratory automation software Real NAMUR compliant R&D process control system End to end data chain from experiment design to ELN/LIMS database User-friendly operation Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 20

Micro Technology Lab. Vision™ Project Modules Automation project design via drag and drop Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 21

Micro Technology Easy connection of sensors, actuators and laboratory instruments Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 22

Micro Technology Application oriented function blocks Operations (excerpt): Surge doser Batch amount doser Batch rate doser Conti doser Refill device Vacuum controller Temperature cascade controller Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 23

Micro Technology Application oriented function blocks Example: Gravimetric flow control Balance and pump Autotuning Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 24

Micro Technology Easy. Batch. TM sequential control Spreadsheet based programming of test procedures Self-explanatory Interactive operation and changes during runtime are possible Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 25

Micro Technology Hi. Text. TM universal programming language Control Online evaluation Communication Special procedures for Easy. Batch TM Multitasking Easy to use Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 26

Micro Technology Laboratory Notebook and automatically generated documentation Functionality Standardised automated evaluation Consistent presentation of parameters, measured values, analytic data and results Transfer of data to a LIMS Export as. pdf file (manipulation-proof) Export as. rtf file (for post-processing) WYSIWYG form designer Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 27

Micro Technology Event report Complete report of the course of events Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 28

Micro Technology Event report Complete report of measured data and set points Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 29

Micro Technology Laboratory Information Management System Functionality Planning and organising Administration and documentation of recipe, batch-, educt-, product- and sample-data Search and retrieval Comparison and analysis of data Coupling devices Advantages Support of daily laboratory work Increases productivity Error prevention Protects sensitive information Makes knowledge available to the user Prevents information manipulation Easy utilisation of information Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 30

Micro Technology Syr. Dos™ - syringe pump for mixing and continuous operation All-purpose use Resistant to aggressive media Wetted materials: glass, PTFE, KEL-F or PPF, opt. ceramics Compact high grade steel casing Syringes from 10µl up to 50 ml Optional pressure up to 90 bar 48. 000 steps, max. 10. 000 steps/s Optional continuous conveyance Calibration in mg/min and ml/min Interfaces (RS 232, RS 485, MODBus, 4 -20 m. A, 0 -10 V) Comfortable Dosi. Master™ software for dosing profiles, dispensing and mixing purposes Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 31

Micro Technology Auto. Sam. TM liquid handling system Applications Sampling of specimens Provision of reactants Quenching, mixing and diluting Liquid/Liquid extraction Properties and Procedures Sample tubes with diaphragms are easily processed Bottling under inert gas possible Exchangeable sample tray Separate, large waste vessel Programmable handling methods Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 32

Micro Technology Gravi. Dos® - gravimetric controlled dosage High performance Low-cost Compact and robust Large dosing range Refilling without dosing interruption Increased control accuracy compared to balances Resistant to aggressive media Easy to clean Available as platform- or overhead-balance Optionally stirring and heating Applicable as massflow and filling quantity meter Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 33

Micro Technology Phase detection and separation Detection of anorganic and organic liquid (and gaseous) phase Automated separation of anorganic and organic liquid phase Thermal measuring principle or Capacitive measuring principle Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 34

Micro Technology Customised Solutions Mixed assembly applications micro-mixers and glas components Continuous as well as batch operation Totally integrated Automation Unattended operation Mobile Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 35

Micro Technology Thanks a lot for your attention! Fully Automated Execution of Multivariate Experiments on the example of Microstructured Reactors info@hitec-zang. de www. hitec-zang. com Automatized execution of multivariate experiments in microstructured reaction plants Hi. Tec Zang Gmb. H 36