1.

APV-Forum Feuchtemesstechnik
28.11. und 29.11.2006 Dresden

Online Moisture-Measurement in
Fluidised-Bed
Granulate- and Dryingprocess
Design of a Sensor to meet pharma-requirements
including first expieriences in a
Glatt Fluidised-Bed Granulator
Dr.-Ing. Claas Dscher
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Company
1994: Dscher & Dscher GmbH
Distributor of Industrial MoistureMeasurement-Devices

2001: Foundation of AMS GmbH

[Advanced Microwave Systems]
Development and Manufacturing of
Measurement-Systems to verify Moistureand Density by Microwave-Technology
Co-operation with Prof. Knchel, CAU
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Project - Team
Mikrowave - Moisture - Measurement
Prof. Dr. Jrg Breitkreutz:University of Dsseldorf
Caroline Buschmller:

University of Dsseldorf

Dr. Wolfgang Wiedey:

Pharbil Waltrop GmbH

Dr. Jochen A. Dressler:

Glatt GmbH

Dr. Claas Dscher:

Dscher&Dscher GmbH

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Structure

Physical Basics of Microwave-Technology

Measurement-Principle
Advantages
Design of Sensor
Materials of the Trial
Equipment
Results
Advantages for the Granulate-Process

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Physical Basics

Water
Molecule
Wassermolekl

Carrier Material
Trgermaterial

Water
Molecule
Wassermolekl

Trgermaterial
Carrier Material
Water
in im
Product
Wasser
Produkt

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Electro-Magnetic
Field

Physical Basics
Two MeasurementSignals will be needed
for measuring the
Moisture.

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2-Parameter Microwave
Resonance Principle

Physical Basics
same relative Moisture

Number of watermolecules is
determined by
Moisture and Density

low density

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high density

Physical Basics
Energy-Carryover from
field to product

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Change of velocity of
propagation

Measurement-Principle
Electric-flux-lines of a
scatter field sensor

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Measurement-Principle
Spectrum of
resonances of
various densities

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Measurement-Principle

Loss of energy and

frequency-shift of
various densities

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Advantages
Microwaves penetrate
material

Moisture will be measured on

surface as well as in kernel

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Advantages

density-independent moisture-measurement
no influence of any contamination
fast, ca. 1/500 sec
independent from color and structure
measures on surface as well as in kernel
long-term and stable calibration
large independency from carrier material

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Design of Sensor
Includes Reference-Resonator:

Patent EP 1331 476

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Design of Sensor
Conventionel Design

Improved Design
Titan

Keramik
Ceramic

22-Component-Glue
K Kleber

Ceramic Ring
Keramikring

Dielectrical Plastic
Material including
Keramik
mit
Circuit
Path
Leiterbahn

Titan

Stainless Steel
Edelstahl

Patent EP1437588

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The Task
Continuous Moisture Measurement in the
Fluidised-Bed-Process of a Pharmaceutical Production
Requirements to the Measurement:
density-independent
no influence of temperature-variations
detects moisture on surface as well
as in kernel
independent from structure of product
(powder => granulate)
ATEX 20 dust-explosion-protection
sensor-sided
pressure-resistant up to 15 bar
pharma-appropriate materials

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high density

low density

Streaming

Materials of the Trial

Dehydration Glatt
Microcrystal Cellulose
Lactose 200 mesh
10 % Kollidon(R) 90F

2 kg
4 kg
1,7 kg

Granulation Glatt
Microcrystal Cellulose
Lactose 200 mesh
6 % Kollidon(R) 90F

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2 kg
4 kg
10 kg

Materials of the Trial

Streaming Glatt
Microcrystal Cellulose
Lactose 200 mesh
6 % Kollidon(R) 90F

2 kg
4 kg
10 kg

Granulation Pharbil
80 % Microcrystal Cellulose
20 % Active Ingredient
Granulate-Liquid: watery Kollidon(R) Solution

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Equipment
Plant
GPCG 15
(Glatt)
WSG 60
(Glatt)
MoistureScan (Dscher&Dscher)

Processes
Dehydration in Fluidised Bed
Spray Granulation in Fluidised Bed

Calibration
Karl Fischer Titration
LOD 70C

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Equipment

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Equipment

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Equipment

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Results
Dehydration-Diagram
Trocknungskurve 27-09-II GPCG 15 (Glatt)
70

Temperatur
Temperature

12

50

10

40

30

20

10

10:48

10:55

11:02

11:09
Zeit
Time

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11:16

11:24

11:31

prozentuale Feuchte
relative
Moisture

14
60

LOD

Results
70

15

60

13
11

50

40

7
30
5
20

10
0
14:52

15:00

15:07

15:14

15:21

Datum
Date und
andUhrzeit
Time

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relative Moisture
prozentuale
Feuchte

Product-Temperature
Produkttemperatur

Trocknungskurve 26-09-II GPCG 15 (Glatt)

Dehydration-Diagram

15:28

15:36

-1
15:43

LOD

Results
Dehydration-Diagram
Granulierungskurve 27-09- VI GPCG 15 (Glatt)
50

6
5

40
35

30
25

20
2

15
10

5
0
14:52

15:07

15:21

15:36

15:50

Time
Uhrzeit

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prozentuale
Feuchte
relative Moisture

Product-Temperature
Produkttemperatur

45

16:04

16:19

0
16:33

LOD

Results
Granulierungskurve 27-09- V GPCG 15 (Glatt)
Granulation-Diagram
60

4,5
4
3,5

40

3
2,5

30
2
20

1,5

relative Moisture
prozentuale
Feuchte

Product-Temperature
Produkttemperatur

50

1
10
0,5
Sprhluft
ausgefallen
->
Klumpenbildung
Breakdown
of Spraying
Formation of Lump
0
14:16

14:24

14:31

Time
Uhrzeit

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14:38

0
14:45

Results
Streaming
variable (Glatt) (Glatt)
variable
Durchstrmung
3

prozentuale
Feuchte
relative Moisture

2,5
0 m/h

500 m/h
1000 m/h

1,5
1
0,5
0
0:00:00

Granulat
wird
leicht nachgetrocknet
Granulate
slightly
dehydrated
Starke
Fluidisierung
Strongnderung
Variationder
of Fluidising
keinen
no Influence
Measurement
->
Einflusstoauf
die Messung
0:02:53

0:05:46

0:08:38
Zeit
Time

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0:11:31

0:14:24

1500 m/h
1700 m/h
LOD 70 C

Results
45

2006-07-21
Make-Up
2006-07-21
Ansatz22 (Granulation
(GranulierungPharbil)
Pharbil)

8,00
7,00
6,00
5,00

35

4,00
30

3,00
2,00

25

1,00
20
00:00

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00:28

00:57
Time
[hh:mm]
Zeit[hh:mm]

01:26

0,00
01:55

Feuchte [%]
Moisture
[%]

Temperature
[C]
Temperatur [C]

40

Results
8,00
7,00

40

6,00
5,00

35

4,00
30

3,00
2,00

25
20
00:00

1,00
00:28

00:57

01:26

0,00
01:55

Time
[hh:mm]
Zeit[hh:mm]
Karl Fischer

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Moisture
Feuchte [%]

Temperature
[C]
Temperatur [C]

45

2006-07-21
Make-Up
(Granulation Pharbil)
Pharbil)
2006-07-21
Ansatz 2 (Granulierung

Results
kalibr.Microwave-Measurement
Mikrowellenmessung
Calibrated

Korrelation
Pharbil)
Correlation(Granulierung
(Granulation Pharbil)
7,50
7,00
6,50
6,00
5,50
5,00
4,50
4,00
3,50
3,50

4,00

4,50

5,00

5,50

6,50

Karl-Fischer
Messung
Karl-Fischer
Measurement
Messungen
07-2006
Meas. 07-2006

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6,00

Messungen
09-2006
Meas. 07-2006

7,00
7,50
R2 = 0,9696

Advantages for the Granulate-Process when

Verifying Moisture
Aim:

Prevention of Over-Dehydration

Pelleting: Tablets partly are flaking

Prevention of Under-Dehydration
Pelleting: Granulate or Powder is gluing onto Punching Tool

Accurate achieve to the target-moisture

Prevention of repeated make-up of Dehydration-Process, Quality of Granulate

Reproducable target-moisture

even when climate is changing when drying with ambient air.

Proper Validation of Process

Information about Homogenity of Product

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Advantages for the Granulate-Process when

Verifying Moisture

Time saving due to Online-Validation of the

Process
Automated Control of air-supplytemperature to aim for a constant of
dehydration-rate
Gentle dehydration possible

Control of Product-Moisture to optimising

granulate, grading is starting with productspecific, ideal moistures

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