공정형 실시간 입도 및 안정성 영상 분석장치-독일 S&E GmbH 사 제품-Insitu Particle Size Analyzer

관리자

Optical back Reflection Measurement (ORM) 기술에 기초하여 국제 특허를 획득한

신개념의 온-라인  입도 및  영상 화상 분석 장치로써 파이프라인 및 Reactor 반응조등에

직접 설치하여 24시간 실시간으로 입도 변화, 안정도 변화 및 Coalescense 과정을

직접 모니터링 할수 있게하는 차세대 기술에 기초한 획기적인 장치:

 

현재 SHELL, SIEMENS 및 BASF 등에서 현장에 직접 설치하여 사용중인 기종 입니다.

 

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

Sequip PAT- Sensor Series provide:

  • Highest selectivity and sensitivity under original production conditions
  • Optimisation of quality and purity of solids
  • Increase of productivity with the formulation of new products
  • Increase of production safety
  • High saving of time wihtin product development
  • Production quality control 24h/365 days a year
  • Ex-protection versions for operational application

Insitu PAT-Sensors measure all particles and droplets with optical back reflection properties. 

 

Absolutely transparent products cannot be measured yet!

Clear products without large diffraction differences like CO2 in CH4 or polystyrol can be measured with special laser components!

 

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 of the Particle SYSTEM Analysis 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. Furthermore, the roughness of the examined Particle SYSTEMS can be determined by Multi Capture Technique.

 

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.

 


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 1 – 300 sec
  • Temperatures from minus 120°C to 300°C
  • Even the laboratory PAT-Sensors are insutu sterilizable up to 165° when switched-off


Presentation of results

The following presentation demonstrates a measurement of  PVC 100-125 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 increases. After reducing the rotation speed fof 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. 

 

ECA - Emulsion Characterisation Analyser


Droplet sizes in emulsions 

Migration– and stability analysis of high concentrated disperse phased emulsion and suspension with insitu sensors in lab and pilot plant



ECA Application


ECA- Sensor allows measuring of size changing in original formulas of suspension

and emulsion under insitu conditions with a minimum distance of 1 µsec between

two droplets.



Therefore the formulation can be detected in streaming dispersed phase in real

time.


Particle size was measured the with an ECA . In parallel, we prepared freeze fractured replicas of the samples and examined the specimens by TEM.

The results are shown in fig. 02 to 04:

For this experiment the ECA Sensor will directly insitu placed in undilluted original concentrated dispersed phase. For instance in a beaker or mini reactor for formulation of new products

Emulsions with 20 % oil phase revealed the most shallow size distribution. By increasing the oil content the spread broadens and the mode of the distribution moves towards smaller values. 80 % emulsions gave almost the same particle size distribution as the 60 % emulsions. Only a small but reproducible peak in the size range from 50 to 80 µm indicated the inhomogenity of this preparation. However, this is not sufficient for a quantitative characterization of the system.

The measurement enables to monitor coalescence in 60 % emulsions as well as Ostwaldt ripening which occurs in 20 % emulsions.

 From these results, we conclude that 3D ORM technology is able to in situ characterize emulsions with up to 60 % oil content. The method is sufficiently sensitive to monitor severe changes due to coalescence as well as to trace small changes produced by Ostwaldt ripening. Emulsions with 80 % oil could not quantitatively be characterized.


However, we must bear in mind that these emulsions are susceptible to dilution.

Thus, reliable results can only be expected when the samples can be analyzed without extensive dilution. Thus, this challenging problem cannot be solved by currently existing methods. The results of the ORM-Measurement, however, can be taken as a fingerprint which is characteristic for this sample and allows to identify changes which occur during manufacturing or storing.  

 

Detecting with ECA - Sensor :
 

  • Agglomeration of  products,
  • Stability of dispesphased systems,
  • Dissolution processes  of substances.

No sample taking and preparation needed.

 

 

Mode of Operation


ECA-Sensor–technology  based on Time of Flight Technology (TOF) and Optical back Reflection Measurement (ORM)  and  is a further development of the well known 3D ORM technology. 

Particles and droplets and their structures were detected and measured by a laser beam  with higher energy as 3D ORM  and with <10mW.  At crossing the particles and droplets the laser beam detected  their geometric expansion. This time periods in µs will displayed in a statistic of all counted events.   

 

The patented measuring method of the optical visibility of the particles works in a band of wave length of 680 nm. So 300 nm will be the deepest detection limit  for diffuse dispersphased  systems. Clear dispersphased systems  can also be detected with a laser power more than 10 mW.  




Dynamic insitu ECA - Sensor



Elektronic


cabinet IP 44; optionally IP69

Data connection RJ 45 Bus

voltage 230V , when required 110 V


Optical fiber


2 m cable between sensor and electronic 

 

Automation



Software



SeQuip ORM–Software ist Bestandteil des Lieferumfanges

Microsoft Windows 2000 and XP compatible without PC


 

Installation and conditions



Installation and

Training


1 day at the customer


Documentation


Manual in English available


Requirements 


Fitting of the in situ ECA Sensor:



Inline Sensor configuration for lab reactors



100 – 240 Volt AC; 5 Amai PS,  earth cable needed

Electrical connection



Dust free environments with controlled temperature for the PC

 

ECA - Sensors



Type


Measuring range in µm


Max. concentration Cv in %


40 ECA

60 ECA

125 ECA


< 0,5 – < 40

< 0,8 – < 60

<1 - <125


80

75

70


Sensor dimensions:


diameter 10 mm; length: 200 mm

diameter 14 mm; length 300 mm

diameter 18 mm; length 255/ 478 mm


Conditions:


Pressure: optionally vacuum up to 6 bar



Temperature: optionally 5 up to 85°C

Out of action insitu sterilizable up to 165°C! 

 

 

Hardware Specifications



Material of the

Sensors:


1,4571 (SS 316) for all parts which are in contact with the

medium –other materials as required



Electrochemical polished sapphire window at the sensor

head optical grade: MIL– PRF-1383B 10-5



Sealing: Hifluor – O-rings  (other materials as required)


Max. operating

pressure:


Vacuum up to 3 bar, Optional 16 bar


Working temperature


Plus 5°C - 85°C, optional minus 20 - 165°C 


Installation


300 m – max. distance between measuring device and PC 

Max. 4 sensors, which can be connected with the PC   


Validation


Option: Validation and 21 CFR Part 11


Software


Sequip ORM


Weight


15 kg (Sensor + Electronic)