Insitu PAT-Sensors for detection of particulate changes under process conditions

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1 Sequip Live Particle Sizer PAT- Series provide: Highest selectivity and sensitivity under original production conditions Optimisation of quality and purity of solids Increase of productivity Increase of production safety High saving of time within product development Production quality control 24h/365 days a year Ex-protection versions for operational application

2 Your benefits: We realise your wishes directly and provide customized solutions for your products. We offer you an optimal price/performance ratio as we reduce cost intensive marketing and administrative work to a necessary minimum by: direct communication per and Internet all relevant information are available in the Internet from price to installation suggestions no unnecessary visits of sales representatives specialists only on demand provision of usage licences even over short periods - for project measurements of your products on site by your personal - with an easy to use Sequip software accounting periods of usage licences as requested Sequip customers decide about handling of all internal data

3 We invite you - continuously monitor your particulate indices rapidly, accurately and under original production conditions The patented PAT-Sensor Technology quantifies, based on optical back reflexion, size as well as the number of particles in original concentrated dispersions. You can identify quickly and effectively the influences of process parameters on your product Insitu PAT-Sensor Systems with microscopic acquisition and counting of droplet and particle sizes by continuous adjustment of the focus depth over the measurement time within disperse phase systems and also in original concentrations from laboratory to the scale up for production.

4 Your benefit at a glance: The Insitu PAT-sensor continuously determines the particulate Fingerprint of your particle systems in situ under process conditions and you increase your product quality by continuous quality control over 24 hours. TOR + ORM - Technology The unique dynamic focussing provides a broad measurement range from <0.5 to 4000 µm because of continuous changes of the focus depth. By continuous acquisition of the particulate changes, deviations of size, number and shape can be detected at once, representing a major advantage for production control. The Laser Time of Reflection analysis (TOR) added by Sequip in combination with the Sequip Software allows permanent monitoring of possible production variations. The hereby achieved constancy of your products serves the safety of your company 365 days a year. Application in process Insitu PAT-sensors are mounted directly in the production plant and measure the product in its original state and in real time. Thus, processes like e.g. crystallization processes, flocculation processes, granulation and polymerisation can be monitored and controlled accurately. A timeconsuming sample taking is not necessary. Return of The ROI normally is a few weeks per PAT-Sensor Investment (ROI) Time saving in product development The Insitu PAT-sensor measure in original concentrations and in real time. So, the influence of changes in particle size can be evaluated at each step of development. If in beaker or pipeline - you always get an "undiluted information" under insitu conditions to reach your target.

5 Insitu PAT-Sensors measure all particles and droplets with optical back reflection properties. Absolutely transparent products cannot be measured yet! As the particles tend to agglomerate with concentrations from 1 Vol%, the particle collectives are normally present as Particle Systems(PSyA). Therefore, the resultant particulate Fingerprints represent reproducible indices for PAT control. Conditional to acquisition properties of agglomeration structures you can evaluate broader particulate distributions than with laser diffraction spectrometres (PSD) and get displayed the total spectrum as size index over the time. Therefore, the measurements with PAT-Sensors in original concentrated products show fingerprints of the actual Particle System Distributions under process conditions. The changes are detected and displayed by the PAT-Sensors under original conditions at any time during production. When the products to be measured are diluted, the sensors detect the size distribution of discrete present particles continuously as under laboratory conditions. Thus, an optical shading is impossible.

6 We provide two measurement techniques for your applications: - undiluted measurement in original concentrations - diluted measurement PAT-Sensor Live Particle Sizer insitu PAT-Sensors provide size distributions from diluted and original concentrated suspensions and emulsions as well as measurement results from disperse present dry products. We supply you with the Live Particle Sizer insitu PAT-Sensor Systems in line with usage licences, completely configurated with hard- and software. The easy handling allows you an autonomous usage. If required, our consulting service is also available.

7 PAT - Sensor Benefits: All particles are counted and presented as trend value over time, based on counting results in the fraction sizes, as quantity distribution, length distribution, surface distribution or volume distribution Measuring periods from sec Temperatures from minus 90 C to 300 C Even the laboratory PAT-Sensors are insitu sterilizable up to 165 when switched-off

8 Presentation of results The following presentation demonstrates a measurement of PVC µm (sieved on validated Rhewum sieving machine) in dependance of the concentration. Within the area from 10:05 to 13:37 the picture shows the addition of 5g PVC each time to the total source of 10 g to 400 g water at start. Then, the mixer was turned of twice and reactivated after a short break. The measurement very quickly shows the sedimentation of the particles. At the second mixing process the rotational speed was shortly doubled, by what the count rate in counts/sec strongly. After reducing the rotation speed for the mixer to an experimental value of 450 rpm, the decreasing count rate demonstrates the presence of a light sedimentation effect. The measurement results still remain within the limits and are reproducable.

9 Patented PAT-Sensor Technology - measures only particles in the focus Multiple scatterings are not detected by the opto-mechanical construction design. Through an only 4 µm sized single mode fiber a laser beam is dynamically focussed through a measurement probe and the inner optics into the product to be analyzed. An optical system rotating with 2 m/s inserts the laser beam spirally. The patented dynamical focus is to be synchronized and moved with the same speed into the medium to be measured. Thus, measuring of particles in the focus only and blinding out of the surrounding area is warranted. The spiral dynamical focus is the decisive advantage to conventional turbidity measurement and FBRM!(*TM by Mettler Toledo Lasentec) You wonder, what, for example, is measurable of particulate product properties?

10 Measurable Products from A to Z A limited selection from measured products: state 2007 aluminium oxide baby lotion bio flocks Bio-ointment <10µm bitter salt bitter salt / magnesium sulphate bitumen emulsion 5-125µm breadcrumbs brewer's yeast butter calcium chloride precipitation crystals cat litter cellulose cellulose slurry cement < 45µm ceramic slurries < 2µm cereals chocolate coal slurry after the grinding coarse meal granulate coating paint cocoa coffee colour pigments <2µm coolant emulsions copper slurries cream crystals in emulsions <125µm defrothing agent deodorant lotion dextrose dextrose monohydrate diamond slurry emulsions + micro capsules eye drops feed fermentation fertilizer fodder gas bubbles in vegetable fat Gas pockets in margarine (PIA) glucose and other saccharine recognition margarine mayonnaise megapearls metal powder MgCl 2 6 H 2 O micro capsules 2-15µm milk of lime multi-material emulsions natural cosmetics <20µm paper additives <3µm PCC peeling lotion penta-erythrite phosphate gravel µm photo emulsion pigments: yellow, red, black < 4µm polyethylene (PE) Polymer + defrothing agent polymer granulate shape recognition polystyrene polyvinyl chloride (PVC) potassium chloride powdered paint precipitated gypsum primary matter for washing agent gold overburden granulates µm gypsum hair dying products hand lotion high speed granulating µm Hostaformpowder <2 25µm ice creme Inert-gas distribution in O/W ink ink jet slurry <4µm insuline keto-glucol acid <500µm kidney stone lactose <50-500µm printing colour latex paste<2µm latex paint raw gypsum magnesium chloride road metal precipitation crystals salt µm Malt products with shape

11 seeds sewer mud 0,5-250µm shampoo silica gel silicic gel / 2-250µm silicone emulsions silver pigment paste <1µm skin lotion soda sorbic acid ß-carotene eye drops steel / water in a counterflow styrene sugar sugar <800 µm sulphur (polymer) Sus-emulsions <5µm Terephthalaldehyde Titandioxid 0,5 to 5 µm titanium dioxide in emulsions Toothpaste Uranium particles vaccination sugar <150 µm vitamin flocks w o w emulsion washing liquid washing powder washing powder pearls water lacquer 15 Vol. % waxes / < 4µm wood shavings yeast yoghurt o-w-o emulsion

12 Process flow in practice Practice Particle Change Result 1 Droplet formation Droplets of different compunds are homogenized Distinct distribution shift 2 Distribution of Blending of pigments in pigments in the emulsions emulsion After the emulsion is homogen, the emulsion raw data are substracted from the pigments+emulsion data 3 Distribution of droplet formation during polymerisation Droplets get larger and stabilize Fine fraction is reduced in favour of coarse fraction 4 Dry or wet grinding Particles getting smaller Distribution change - higher fine fraction 5 Nucleation at precipitation Particles grow out of nano scale Distribution change - higher fine fraction increasing 6 Particle breakage or splitting Particles getting smaller Distribution change - higher fine fraction - lower coarse fraction 7 Growth of particles Particles getting larger Distribution change - higher coarse fraction 8 Agglomeration and flocculation processes Particles form particle systems Distribution change - higher coarse fraction - lower fine fraction 9 Deaggregation Particles dissolve Particles dissolve

13 10 Change of shape at crystallisation Particles deformate hange of distribution function Information on applications beyond the Sequip measurement ranges you'll possibly find at Configuration of the system: The system consists of a patented Sensor, which is manufactured for Sequip in Hasteloy C 276 by default and the modified Sequip evaluation software TOR), which is connected with a single mode fibre optic RJ 45 Hub cable to the Computer and the Sequip Trend Software. Standard models and options: Diameter of sensor at measurement window Total length of the sensor at site of measurement window 18 mm laboratory model or 25 mm process model 240 mm medium touched site Total length of the sensor 500 mm in standard version; extendable up to max. 3 metres Measurement speed Number of measurement channels Up to 30 m/s with adding of particle velocity into evaluation software 1024 internal and 128 external Particle sizes In measurement ranges from <0.5 µm to 4000 µm Pressure range Up to 6 bar standard, optional up to 16 bar Temperature range From +5 C to 125 C or 165 C Optimal physical requirements possible on demand Measurement period per measurement 1 second to 300 seconds

14 Long time evaluation 6 trends as particulate ratios over elapsed time over 24 hours Distribution Modelling / Validation Calibration: Output alternative Internal sieving curve as base for trend display possible PVC and CaOH calibration standards 6x 4-20 ma; 6 x digital outputs PAT Analysis of particulate systems - from beaker to tube line and the reactor, inside of the process The Insitu PAT-Sensor is placed in the product, this may be within a laboratory beaker or directly within a supply line in pilot plant stations or process. The PAT- Sensor System is started and the distribution is presented on screen within seconds. Changes during measurement phases are continuously displayed. The data are displayed as trend graph over time. Changes in production process can be detected at once and appropriate action can be taken accordingly. The Insitu PAT-Sensor Systems provide the opportunity to transmit data digitally and/or analogically. Insitu PAT-Sensor Systems - Measuring Ranges and Concentration Possible measuring ranges <0.5 to 4000 µm Volume concentration in Vol% Measurement of < 5% Particle Distributions 5 -> 40% Particle System Distributions above 60% Fingerprints Applications Homogenization Polymerisation under EX-conditions

15 Dispersion Granulation Fermentation Disaggregation Flocculation Particle and droplet size dependent crystallization Installation examples in practice The installation of Live Particle Sizer insitu PAT-Sensors in industrial instruments, tanks or pipelines is carried out with appropriate mounting sockets. The following figures show two typical inline installation configurations of the sensor. Due to the existing flow conditions, certain installation guidelines have to be observed to achieve optimal measurement conditions.

16 Installation in a by pass Optimisation of milling processes By continuous monitoring of the milling process a deviation of the milling material from the set-point parameters is detected directly. Then, you can interfere immediately with the milling process. The Insitu PAT-Sensor detects smallest changes. Thus, the milling time is optimised and the quantity of milling cycles is reduced. Example of use in mill works Pneumatic conveyor pipe line Filler neck PAT-Sensor Mill work PAT-Sensor Flow direction

17 Application areas of Live Particle Sizer insitu PAT Sensor Systems System Application areas Diameter Lab Process of sensor tip Pilot Plant Length of sensor tip Pressur e range (bar) Temp. range media ( C) of Total length PAT- Sensor Max. Measure ment range (µm) , , , <2-500 All dimensions in mm (unless otherwise noted). Equipment Fibre optic cable SM connection between sensor and control unit (m) Sensor material Series Hasteloy C 276 Hasteloy C 276 Hasteloy C 276 Hasteloy C 276 Hasteloy C 276 ATEX-Certification standard Flange connection optional optional ANSI/DIN ANSI/DIN ANSI/DIN *** Other configurations are available on request and customer wish.

18 What are the features of Sequip? You want to optimise your process or product development with PAT? We provide opportunities with an optimum cost/benefit ratio. The Live Particle Sizer insitu PAT-Sensor Systems are manufactured under quality control by Sequip consultants, based on their international experiences, through introduction of. By standardization of the Sequip PAT-Sensors, we reach a coverage of more than 85% of the known application areas and, therefore, a cost effective production for the benefit of you and all. What are the features of the Sequip Service: 1. As interested customer you have informed yourself about Insitu PAT-Sensor Systems in the Internet and like to evaluate your products process analytically under particulate conditions with a PAT-Sensor System. 2. You create a Login with your personal data on our website and request a quotation by filling in the requirement profile. 3. Please send the completed requirement profile with your specifications via to Sequip. 4. We respond to your inquiry within 3 work days. 5. You receive an offer for a usage licence for testing the system and the option for extension. You decide about the usage licence period (minimum usage one week). 6. The price for the usage licence includes delivery and collection, by request, setting-up operation and service if required. 7. After expiration of the usage licence you decide whether you wish an extension of the usage licence.

19 8. Based on this, Sequip will check, if the employed PAT-Sensors are not scheduled elsewhere and make a proposal accordingly. 9. Please send your questions and problems also via to Sequip and you'll receive a qualified response from our engineers and consultants within 3 work days. Terms and Conditions: Insurance: Transport insurance is borne by Sequip. Insurance on site is for customer's account. Functioning: S & E ensures a proper functioning of the ordered configuration based on the measurements with the provided service reticle. Summary of customer benefits with use of PAT-Sensor Technology compared to other technologies: Selective Multi Focus Reflection Measurement, as a consequence extremely high resolution of the signal level detected by the sensor optics, which are automatically adapted to the resolution area of the electronics to the present measurement ranges from < 0.5 to 4000 micron Measurements in 1024 internal fractions, based on this, a resolution of 0,5 µm is achieved, which is the base an exact measurement and its reproducibility Analysis of signals, based on shape changes of your particles via the optional additional software Highly sensitive optical receiver, which defines the run time of the focus above the particles and is not affected by colour influences. The signal range and not the signal height is used for evaluation. The high count rate garantees a high statistical reliablility above of Sigma 4

20 Contact: Insitu PAT-Sensors for detection of particulate Automatic point zero alignment of the optic in media free of particles Highest sensitivity for finest crystals and their surface morphology 10 times higher signal rates High performance electronics 100 KC/sec Best cost / performance ratio with ROI times of a few weeks Quality and Development made in Germany Leading world technology state of the art 2007 S & E GmbH Sequip Sensor & Equipment Rahmer Str. 30b D Düsseldorf Fax: ++49 (0)203 / haase@sequip.de