Roadshow Mikrofluidik 2013 Automatized Execution of Multivariate Experiments in Microstructured...

Roadshow Mikrofluidik 2013

Automatized Execution of Multivariate Experiments in Microstructured Reactors

(Automatisierte Durchführung multivariater Experimente in mikrostrukturierten Reaktoren)

Prof. Dr.-Ing. Werner ZangCTO of HiTec Zang GmbH

Automatized execution of multivariate experiments in microstructured reaction plants 2HiTec Zang GmbH

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


Micro Technology

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 …)

Laboratory Automation

Special conditions for automation in R&D labs


Micro Technology


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 toautomation of production


Micro Technology


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


Micro Technology


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, …)


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


Micro Technology

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



Micro Technology

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



Micro Technology

Experimental setup

PI flowsheet (example) 2 reaction steps 4 individualy controlled

feeds 5 individually controlled

temperatures


Micro Technology

Experimental setup

Fully automated LabBox

TM

process-interface LabVision® software with EasyBatch

TM

AuotSamTM

autosampler


Micro Technology

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

Instrumentation components


Micro Technology

Standard sensors and actuators T, p, pH,... / 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)

Instrumentation components


Micro Technology

Automation system hardware

LabManager® (or LabBoxTM) process interface 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)


Micro Technology

Automation system interfaces

Analogue inputsand outputs


Micro Technology


Analogue inputs


Micro Technology


Digital inputs and outputs


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Heater drivers and serial interfaces


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Interface Example


Micro Technology

Automation system software

LabVision® 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


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LabVision™ Project Modules

Automation project design via drag and drop


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Easy connection of sensors, actuators and laboratory instruments


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Application oriented function blocks

Operations (excerpt): Surge doser Batch amount doser Batch rate doser Conti doser Refill device Vacuum controller Temperature

cascade controller


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Application oriented function blocks

Example: Gravimetric flow control Balance and pump Autotuning


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EasyBatchTM sequential control

Spreadsheet based programming of test procedures

Self-explanatory

Interactive operation and changes during runtime are possible


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HiTextTM universal programming language

Control

Online evaluation

Communication Special procedures

for EasyBatchTM

Multitasking

Easy to use


Micro Technology

Laboratory Notebook and automatically generated documentation

Functionality Standardised

automated evaluation

Consistent presen-tation 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


Micro Technology

Event report

Complete report of the course of events


Micro Technology

Event report

Complete report of measured data and set points


Micro Technology

Laboratory Information Management System

Functionality Planning and organising Administration and documen-

tation 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


Micro Technology

SyrDos™ - 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 (RS232, RS485, MODBus,

4-20mA, 0-10V) Comfortable DosiMaster™ software

for dosing profiles, dispensing and mixing purposes


Micro Technology

AutoSamTM 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


Micro Technology

GraviDos® - gravimetric controlled dosage

High performance

Low-cost

Compact and robust

Large dosing range

Refilling without dosing interruption

Increased control accuracycompared 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


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


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Customised Solutions

Mixed assembly applications micro-mixers and glas

components Continuous as well as

batch operation

Totally integrated Automation

Unattended operation

Mobile


Micro Technology

Fully Automated Execution of

Multivariate Experiments

on the example of

Microstructured Reactors

[email protected]

www.hitec-zang.com

Thanks a lot for your attention!

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