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Ian Haley

Outline of Modules 1

The Basics

Part 1 - What is Particle Size

Part 2 - Presentation Method and Weighting Part 3 The Importance of Shape Part 4 Count-based Measurement

Part 5 FBRM and The Chord Length Distribution Part 6 Chord Length and Particle Shape Part 7 - An Outline of Different Particle Characterisation Methods and the

Effect of Particle Shape

Outline of Modules

Statistics and Data Handling

Part 8 - Understanding the Mean, Median and Mode of a Particle System

Part 9 Precision and Accuracy Part 10 Correlating FBRM to Other Data Part 11 - Channel Grouping and Statistics Part 12 Signal Aliasing

Part 13 - Probe Location and Orientation Part 14 Standard Procedures

Ian Haley

Particle Size

Many particles are complex Three-dimensional objects. Yet we want to represent their size by just one number.

Particle size = 326 m But how was it calculated? And what does this tell us about the particle and others like it?

Size

What is the size of this particle?

10mm

Size

But what is the size of this particle?

50mm

10mm

7

There is no single definition of particle size In this (document), particle size is defined as the diameter of a sphere having the same physical properties; this is known as the spherical equivalent diameter.

(Source: International Standards Organization (ISO 9276-1:1998))

By volume

By surface area

By settling velocity

By sieve analysis

Ian Haley

There is no single definition of particle size In this (document), particle size is defined as the diameter of a sphere having the same physical property; this is known as the spherical equivalent diameter.

(Source: International Standards Organization (ISO 9276-1:1998))

By volume

By surface area

By settling velocity

By sieve analysis

The physical property we use has a major effect on the way in which particle size is calculated. 10

What is the average size of this two-particle system? In other words, What does my PSA lab tell me?

11

These numbers are all the correct average size. There are a large number of other methods of calculation that would be correct

as well.

Mean diameter

Number-based dist. = 55.0 m Area-based dist. = 99.1 m

Diameter: 10m

Diameter: 100m

12

Equal Volumes

Number-based dist. = 10.1 m Area-based dist. = 18.2 m

13

One 100 m particle

(A) contains the same quantity of material as onethousand 10 m particles (B)

A Total number Diameter Surface area Total volume 1 particle 100 m 31,400 m2 524,000 m3

14

Number Distribution

12 10

Number

8 6 4 2 0 10 100 1 1

Diameter (m)

1E+06 1E+06

Volume Distribution

Volume (m3)

10m

Diameter: 100m

Diameter (m)

15

Number Distribution

12 10 10

Number

8 6 4 2 0 10 1000 1

Diameter (m)

1E+06 1E+06

10m

522,025

Volume (m3)

Diameter: 100m

5,220

0E+00 10 100

Diameter (m)

16

Number Distribution

1200 1000 1000

Number

1000

10m

1

200

0 10 100

Diameter (m)

1E+06 1E+06

Volume Distribution

Volume (m3)

100m

10

100

Diameter (m)

17

Number Distribution

1200 1000 1000

Number

1000

10m

Diameter (m)

1E+06 1E+06

Volume Distribution

1044050

Volume (m3)

100m

100m

Diameter (m)

18

into 1000 small particles

Initial particle system Total number Total surface area Total volume Number mean diameter Volume moment mean diameter 27 particles 847,000 m2 14,140,000 m3 100.0 m 100.0 m

After breakage of one particle 1026 particles 1,161,800 m3 14,140,000 m3 12.3 m 96.7 m

Relative change 3700% increase 37% increase 0% 87.7% decrease 3.3% decrease

19

Probability (%)

All three distributions have the same mean but significantly different distributions!

What is the mean of this distribution?

21

Which distribution is the most sensitive in your application?

Mean = 7.1 m Mean = 9.2 m

Mean = 12.2 m

Mean = 15.2 m

The size distribution is presented as: a) Total number b) Total length (based on projected area) c) Total surface area d) Total volume of particles within each size classification

Presentation method determines sensitivity to different regions of the population. (Example: Population of Cubes)

Number Distribution

Length Distribution

Area Distribution

Volume Distribution

23

The statistic choice/presentation method determines the sensitivity to different regions of the population.

Example: A population of cubes

FBRM No Weight

Emphasizes changes to the fine (small) end of the distribution

Emphasizes changes to the coarse (large) end of the distribution

25

No Weighted Distribution

Time=0 min

Time=0 min

Time=90 min

Time=180 min

Time=90 min

Time=180 min

distributions at 3 time points show a decrease in count and an increase in dimension

Unweighted distribution is sensitive to

fine particles population

distribution for same 3 time points show enhanced resolution to growth in coarse particle dimension

Square weighted distributions is

sensitive to coarse particle dimension

26

Unweighted Distribution #/s <50 m

Time=0 min Time=90 min Time=180 min

#/s 50-1000 m

Time=0 min Time=90 min Time=180 min

27

Distribution weighting (by

number, length, area, or volume) can significantly enhance or reduce the resolution to change.

weighting function will enhance the changes that directly relate to the application goal.

In this example, the squareweighted distribution does not detect small changes in the concentration of fine material.

distribution is very sensitive to the amount of fine material present.

28

Distribution weighting (by

number, length, area, or volume) can significantly enhance or reduce the resolution to change.

weighting function will enhance the changes that directly relate to the application goal.

However, the squareweighted distribution is very sensitive to the amount of coarse material.

unweighted distribution does not detect small changes in the concentration of coarse material.

29

Our descriptions of fine and coarse

material are relative

smallest and largest particles in a given system

Fines

Coarse

30

Reporting of particle size must include definitions of:

The physical property selected to characterize size of the particles, for example:

Diameter Chord length Projected area Surface area Volume Settling rate Response of electrical, optical, or acoustical field Number-based distribution Length-based distribution Area-based distribution Volume-based distribution Scale (log vs. linear) Channel grouping Count vs. normalized

- Shape - Refractive index - Coincidence effects

31

calculation used to characterize the particle distribution.

- Property

Sphere having the same settling rate Sphere fitting through the same-size sieve aperture Sphere producing a similar diffraction pattern No shape assumption - Chord length distribution Calculation Number Length Area Volume

fundamentally wrong, they just measure different properties of the particles.

32

Ian Haley

10 m

24.7 m

100 m

The surface area of the needle is 60% greater than that of the sphere.

34

Simplicity: A sphere is the only shape that can be described by

one unique number (the diameter), regardless of the particles orientation.

35

5 m 18 m

50 m

Calculate the diameter of a sphere with the same volume as the cylinder

A spherical equivalent diameter based on volume (VSED)

How does the VSED relate to the length and width of this particle? The surface area of the cylinder is 73% greater than the sphere! A needle will handle and flow differently to a sphere!

36

5 m

24 m

100 m

Calculate the diameter of a sphere with the same volume as the cylinder

A spherical equivalent diameter based on volume (VSED)

The cylinder has doubled in length; but the diameter of the equivalent

sphere has only increased by 33%

37

YES!

NO!

38

Run 3

Very different morphologies for three batches of the same process

Run 5

Run 5

Run 6

information about the process?

39

behave the same way?

particles?

40

Most instruments will assume that the signal is derived from a spherical

particle, and in turn derive a spherical equivalent diameter based on this incorrect assumption.

software (excluding some image analysis packages) that account for non-spherical shapes. Most will generally track growth or reduction of shaped particles, but not in an absolute sense.

The further particle shape moves away from a sphere, the less accurate

instruments based on a spherical equivalent model become.

41

Ian Haley

Instruments and techniques used to measure particle size fall into

A measurement is made on a cloud or ensemble of particles simultaneously.

Particles are not measured individually The distribution is expressed as size vs percentage or distribution density These are normalised techniques

Conversely.

Some instruments derive their data by measuring particles individually The data is sensitive to changes in population The distribution is expressed as size vs number These are count-based techniques

43

In this example, particle dimension is

held constant as the concentration of the dispersed phase increases.

chords increases, the normalized distribution shows that the size and shape of the particles remain relatively unchanged.

changes in particle dimension and/or changes in the numberbased particle concentration.

population information from the data.

44

Each channel in a count-based

distribution is independent of change occurring in other ranges of the distribution.

distribution is dependent on changes occurring in other regions of the distribution.

distribution indicates dramatic relative change in this size region.

shows that the actual number of particles measured in this range did not change.

45

Allows you to measure particle population You can track changes in particle concentration

Track absolute changes in isolated size regions, independent of other

size regions

Hide the effect of concentration

Only relative changes in concentration can be tracked

46

Ian Haley

Cutaway view of FBRM In-process Probe PVM image illustrating the view from the FBRM Probe Window

Probe installed in process stream

Focused beam

48

Enlarged view

PVM image illustrating the view from the FBRM Probe Window

Probe detects pulses of Backscattered light And records measured Chord Lengths

This core patented technology is called Focused Beam Reflectance Measurement [FBRM]

49

Enlarged view Typical FBRM applications include: -Crystallization -Formulations -Precipitation Path of -Polymerization Focused -Emulsification Beam -Microencapsulation -Dissolution and disintegration -Flocculation -Fermentation Thousands of Chord Lengths are measured each second to produce the FBRM Chord Length Distribution :

51

Standard Focal Position - -0.02 mm (20m inside the

window) measured from outside surface of probe window.

excellent sensitivity to realtime change in count and dimensions of particle population. - Minimizes noise from properties of the system that are not under investigation.

52

Outbound:

Return:

degraded by

- Absorption by the carrying fluid. - Attenuation due to particles between

the window and measuring zone.

the measuring zone.

Note: Particles between the window and the measuring zone will reflect light that will be detected as background signal. This will significantly degrade the signalto-noise ratio.

53

54

10 9 8 7 6 5 4 3 2 1

Counts

1 2 3 4 5 6 7 8 9 10 Chordlength [a.u.]

55

Ian Haley

Chords are Measured from every Aspect

57

A chord length distribution is a function of average shape and dimension of particles and particle structures as they actually exist in process.

Sphere

Sphere

measurement is known. In most cases the affect of shape on measurement can be filtered out or enhanced to track the change.

Needle Needle

Platelet

Platelet

58

59

60

61

62

growth of a needle

Ruf, A., Worlitschek, J, Mazzotti, M. Modeling and Experimental Analysis of PSD Measurements through FBRM. Part & Part Syst Characterization. 17 (4), 167-179, 2001.

63

growth of a needle

Ruf, A., Worlitschek, J, Mazzotti, M. Modeling and Experimental Analysis of PSD Measurements through FBRM. Part & Part Syst Characterization. 17 (4), 167-179, 2001.

64

growth of a needle

Ruf, A., Worlitschek, J, Mazzotti, M. Modeling and Experimental Analysis of PSD Measurements through FBRM. Part & Part Syst Characterization. 17 (4), 167-179, 2001.

65

Distributions

How do we define a collection of particles of differing size and/or shape?

66

Presentation method determines sensitivity to different regions of the population. (Example: Population of Cubes)

No Wt

600

500

400

Count/sec

300

200

100

0

1 3 5 7 15 Dimension 25 40 65

67

Part 7: An Outline of Different Particle Characterisation Methods and the Effect of Particle Shape

Ian Haley

Focused Beam Reflectance Measurement Track real-time changes in particles and droplets as they naturally exist in the process

PVM Technology

Particle Video Microscope Microscope quality images, in-process and in real time

to 3mm

to 1mm

69

METTLER TOLEDO PVM enables qualitative and quantitative particle

system characterization

70

The following schematic represents the change in morphology. Long Needles Short cubic/diamond crystals

PVM images show metastable seeds

are long needle shaped crystals

t=10mins

72

At 25mins - polymorphic transformation

occurs

t=25mins

73

After 45mins the transformation is

complete

tighter

t=45mins

74

Dilute sample (0.01% wt or lower) of particles

added to Laser Diffraction bench top system

(particles can break, dissolve, etc during this step)

transmission.

Laser Dilute Particles Detector

the light scatter on the detector is collected (diffraction pattern)

Fraunhofer theory) is used to fit a diffraction pattern of spheres with the measured diffraction pattern

Volume Based Distribution

Normalized distribution

Distribution Assuming all

particles are spheres

77

78

Laser Diffraction

79

80

81

Sieving will size based on the 2nd largest particle dimension Particles of the same width will be sized the same Particles of different shapes but the same width will be sized the same

82

What is the process or product parameter of concern? Critical

parameters may include:

Filtration Milling Drying Flow properties Product yield and purity Bulk Product quality properties Dissolution Bulk density Formulation properties

parameters?

What instrument permits us to monitor this critical parameter? Is sampling or safety an issue?

83

Understand how the mean, median and mode are calculated Study how particle system changes impact the mean and median Understand the best statistic to choose for a given objective

85

9m

25m

50m

25m

32m

Mean

= 28m (9+25+25+32+50)/5

Median = 25m (50% greater than this size; 50% smaller than this size) Mode = 25m (most common occurrence)

86

9m

25m

50m

25m

80m

32m

120m

Mean = 49m (9+25+25+34+50+80+120)/7 Median = 32m (50% greater than this size;50% smaller than this size) Mode = 25m (most common occurrence)

87

9m

25m

50m

25m

32m

5m 5m

5m

5m

Mean

= 18m (5+5+5+5+9+25+25+34+50)/9

Median = 9m (50% greater this size;50% smaller than this size) Mode = 5m (most common occurrence)

88

Mean: +75%

Median: +22% 89

Mean: -35%

Median: -64%

Mean: -40%

PVM

Median: -67%

90

Mean: -40%

Median: -67%

91

Conclusions

The mean, median and mode are all averages used to characterize

particle systems

very small) particles; for example large boulders during milling

the fine end of the distribution; for example secondary nucleation

study

92

Ian Haley

Precision

- The ability of the instrument to yield the same

response to repeated measurements of the same unchanging sample.

Accuracy

- The ability of an instrument to yield results that are as

close as possible to the absolute properties possessed by a sample.

close as possible to a recognized Reference or Standard Method

94

Accuracy

When discussing accuracy it is important to specify:

- The absolute property in question. (e.g. absolute chord length, true

diameter, etc)

independently determined.

95

A. Both Precise and Accurate. B. Measurement capable of monitoring

and control: Precise measurement with a consistent offset (bias). Good sensitivity to change.

monitoring and control. Poor sensitivity to change. Average (x) of all measurements will approach the true value.

and offset.

96

Two goals of FBRM instrument

design:

instrument repeatability, so instruments are repeatable and can be validated across sites and during scale up (lab to plant).

instrument to itself, so measurements of the same system will always measure the same distribution and provide opportunity for control, quality by design, and process optimization.

97

Case A (Ideal):

Accurate and Precise

100% 80% 60% 40% 20% 0% 0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0

4.0

95% Confidence

Interval = +/-5.0%

8.0

Measured Value

0.0 1.0 2.0 3.0 4.0 5.0

98

Case C: Accurate Measurement, poor precision

25% 20% 15% 10% 5% 0% 0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0

True Mean = 4.0 Measured Mean = 4.0 95% Confidence Interval = +/50%

8.0

Measured Value

0.0 1.0 2.0 3.0 4.0 5.0

Time (minutes)

99

Case B: Precise Measurement with an Offset

100% 80% 60% 40% 20% 0% 0.0

8.0

True Mean = 4.0 Measured Mean = 6.0 95% Confidence Interval = +/5.0%

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

Measured Value

0.0 1.0 2.0 3.0 4.0 5.0

100

Why is this true? Any given statistic is primarily the function some specific region of the chord length distribution. Some regions may have more or less counts depending on the particle system.

101

Sensitivity Defined

The ability to of the instrument to respond to a real change in the process parameter of interest. The higher the sensitivity, the smaller the real change in process the instrument is able to detect.

102

Is this noise?

Or is there insufficient information to provide a signal of sufficient stability (precision)?

8.0

Measured Value

0.0 1.0 2.0 3.0 4.0 5.0

103

A 0.1% increase in the solids concentration resulted in a corresponding 0.1% increase in the output signal.

104

Increasing single measurement duration improves measurement precision.

2 sec.

5 sec.

10 sec. 1 min.

5 min.

Increasing number of measurements to average (navg) improves measurement precision.

1000

10.0%

100

10

1.0%

0.1% 1000

107

Increasing the Measurement Duration (with no averaging) provides more stable data, but will increase the minimum response time.

1450 1400 1350 1300 1250 1200 -1.0 0.0 1.0 2.0 3.0 4.0 + 1.0 % by weight, SMD = 1 sec Step Change in Concentration

1500

1500 1450 1400 1350 1300 1250 1200 -1.0 0.0 1.0 2.0 3.0 4.0 + 1.0 % by weight, SMD = 10 sec Step Change in Concentration

1500 1450 1400 1350 1300 1250 1200 -1.0 0.0 1.0 2.0 3.0 4.0 + 1.0 % by weight, SMD = 60 sec Step Change in Concentration

1500 1450 1400 1350 1300 1250 1200 -1.0 0.0 1.0 2.0 3.0 4.0 + 1.0 % by weight, SMD = 120 sec Step Change in Concentration

108

Increasing the number of measurements to average (navg) improves precision. However, response is dampened with increased averaging.

1450 1400 1350 1300 1250 1200 -1.0 0.0 1.0 2.0 3.0 4.0 + 1.0 % by weight, Average = 10 Step Change in Concentration

1500

1500 1450 1400 1350 1300 1250 1200 -1.0 0.0 1.0 2.0 3.0 4.0 + 1.0 % by weight, Average = 30 Step Change in Concentration

1450 1400 1350 1300 1250 1200 -1.0 0.0 1.0 2.0 3.0 4.0 + 1.0 % by weight, Average = 60 Step Change in Concentration

1500

1500 1450 1400 1350 1300 1250 1200 -1.0 0.0 1.0 2.0 3.0 4.0 + 1.0 % by weight, Average = 120 Step Change in Concentration

109

Provide a precise measurement that reflects the smallest

change of interest to the process or product parameter of concern.

110

Ian Haley

112

240

220

200

180

160

140

120

113

114

350

Extrapolating LD data

300

250

Mean (D 4,3)

200

150

100

50

Time (s)

115

116

117

118

How close does the FBRM instrument response come to the measurement of product quality or process efficiency

119

1) A correlation is made between specific cake resistance (filterability) and both the dimension and number of particles 2) One can measuring the in-situ particle dimension and count with FBRM and predict downstream filtration rates. 3) FBRM is highly successful in predicting filtration because of its high sensitivity to changes in the number of fine particles

Optimization of Pharmaceutical Batch Crystallization for Filtration and scale-up Brian K. Johnson, Carol Szeto, Omar Davidson and Art Andrews AIChE Annual Meeting, Los Angeles, CA, November 1997

AJ Parker CRC for Hydrometallurgy

25

20

15

200 rpm

10

100 rpm

5

121

The Use of FBRM in the Study of Flocculation Processes Phil Fawell, CSIRO

SPSC 01 (Ge et al 2004)

peak (flocs) biomass

122

FBRM peak (bubbles) and ethanol production

Ian Haley

How to Choose the Right Channel Grouping for Your Work & the Affect of the Chosen Grouping on Statistics

Channel Grouping*

124

Channel A Definition

A bin with a specific upper and lower limit in microns. Counts with a chord length measured between those limits are put in that specific channel.

125

The FBRM hardware is based on 4096 linear 0.25 micron channels,

so the primary x-axis is this linear scale.

channels.

FBRM logarithmic scales are calculated from the linear scale channel

data.

The choice between linear and log scales will change your statistics

Many other particle size instruments use hardware based on a log

scale. They do not provide statistics based on a linear scale.

126

Logarithmic Grouping

Each channel width is progressively wider than the

preceding channel width.

proportionate to their logarithms.

of the distribution.

channels) is provided on the large-particle side of the distribution.

127

Linear Grouping

All channels have equal width. The distance between the channel midpoints is also equal. Equal resolution is provided throughout the distribution. Each channel has an equal probability of a count being

placed in it.

128

Logarithmic Grouping

100-Channel Log Grouping (same data set as linear):

129

Linear Grouping

100-Channel Linear Grouping (same data set as log):

130

Comparison of statistics (linear vs. logarithmic channel grouping for the same data set):

Statistic #/sec #/meas Median Mean Mode 10th Percentile 100 Linear, 0-1000 m 501,000 1,002,000 500.00 m 500.00 m 495.00 m 223.28 m 100 Log, 1-1000 m 500,998 1,001,996 499.96 m 500.12 m 520.79 m 223.17 m % Difference 0.0004% 0.0004% 0.008% 0.024% 5.21% 0.05%

50th Percentile

90th Percentile

12.525th Percentile

500.00 m

776.72 m 250.00 m 12.525% 87.475% 204.35 m

499.96 m

778.21 m 249.96 m 12.53% 87.47% 204.72 m

0.008%

0.2% 0.016% 0.04% 0.006% 0.18%

131

The more counts per channel, the better the statistical stability.

The fewer channels chosen, the more counts there will be per channel.

change and the more counts required for statistical stability.

change and the less counts required for statistical stability.

132

Channel Grouping

Rules of Thumb:

encompasses all the data.

133

Exp. 1: Mostly Fine - Linear Scale

70

60 50 Count 40 30 20 10 0 0 200 400 600 Dimension (m) 800 1000 Count t = 5mins t = 10mins

70

60 50 40 30 20 10 0 1 10 Dimension (m) 100 1000 t = 5mins t = 10mins

In this example most of the particle counts are less than 100m with an

increase in the number of particles in this range over time

Using a linear scale one-tenth of the channels are for particles less than

100m not very sensitive to change in this region

Using a logarithmic scale two-thirds of the channels are for particles less than

100m much more sensitive to change in this region*

*NOTE: The caveat is for channels narrower than the actual data (0.25 um), the data is interpolated 134

Internal usage only

Exp 2: Mostly Coarse - Linear Scale

100 90 80 70 60 50 40 30 20 10 0

0 t = 5mins t = 10mins

100 90 80 70 60 50 40 30 20 10 0

1 t = 5mins t = 10mins

Count

200

800

1000

Count

10 Dimension (m)

100

1000

In this example most of the particle counts are greater than 100m with an

increase in the number of particles in this range over time

Using a linear scale nine-tenths of the channels are for particles greater than

100m very sensitive to change in this region

Using a logarithmic scale one-third of the channels are for particles greater

than 100m much less sensitive to change in this region

135

Log scale

136

Linear scale

linear scale

137

Linear scale

linear scale

138

Ian Haley

Signal Aliasing

aliasing can be important.

oscillation time, instrument response time, data lag and averaging can conspire to present a misleading result

Case A (measurement interval = 30 sec)

process variable.

Process Variable Measured Data Points Instrument Output Reconstructed Signal

Process Variable

Time (minutes)

141

lag is increased and the amplitude of the oscillations is dampened.

Process Variable

b) Averaging = 5 measurements

Time (minutes)

142

Case C (measurement interval = 120 sec)

lag is increased and the amplitude of the oscillations is dampened.

b) Measurement Duration = 120 sec

Process Variable

Time (minutes)

143

Case D (measurement interval = 240 sec)

measurement interval greater than 175 seconds (half the period of the process oscillations).

c) Measurement Interval = 240 sec

Process Variable

0.0

5.0

10.0

15.0

20.0

25.0

30.0

Time (minutes)

144

duration approaches the period of the process.

no dynamics.

Process Variable

c) Averaging = 10 measurements

10.0

15.0

20.0

25.0

30.0

35.0

40.0

Time (minutes)

145

Part 13: Practical Aspects of Using FBRM: Probe Location and Orientation

Ian Haley

FLANGE WELDED TO DIP PIPE BY CUSTOMER EXHAUST TUBE RETAINING FLANGES

REACTOR TOP

LENGTH

375MM 14.75IN

147

representative of the process for process changes to be tracked.

Probe insertion: 30-60

angle to the flow

fresh slurry - Maintains a clean probe window

149

Probe Orientation

- Extremes in individual particle density (very low or very high in relation to the carrying solution). Lower solids concentration. Lower carrying solution viscosity. A larger median particle size. A wider particle size distribution. Greater particle shape deviation from a sphere.

Probe Orientation

Smaller differences between particle density and carrying solution density. Higher solids concentration (dispersed-phase liquid). A smaller median particle size. A narrower particle size distribution. Smaller differences between average particle shape and a sphere.

Probe installed in a vertical, up-flow pipe,

three to five pipe diameters from the top of the last elbow:

6

5 7

pipe upstream of the probe - Offers the most uniformly random and representative presentation of the dispersed phase to the measurement zone - Keeps the probe window residue-free

2 4 FLOW 3

152

153

FLANGE HELD IN PLACE ON THE PROBE WITH SCREWED-ON FLANGE ADAPTOR EXTENDED PROBE HOUSING

well-mixed, representative sample to the probe

that will present the material of interest to the probe tip

MIXER

PROBE TIP

BAFFLE

154

Avoid areas that are not

completely homogeneous

Leading Side of Baffle Mixer Rotation

top of the reactor, locate it near the leading side of the baffle

baffle, as this is where there are dead areas and eddies where particles may settle or segregate

155

Location of the probe within the

vessel must take into account the vertical direction of the flow. (Is the flow upward or downward at the vessel wall?)

Mixer Rotation

inserted from the top of the vessel, the probe must be installed in a location where the flow is in a generally upward direction.

156

Ian Haley

Instrument Repeatability Assurance

Assessment of instrument measurement performance

Initial instrument OQ

Uses PVC Reference Standard & Fixed Beaker Stand Unique PVC Standard prepared and measured on new instrument in

Lasentec factory

Standard delivered with instrument to customer Standard measured and compared with factory reference data

Continued instrument PQ

Uses PVC Reference Standard & Fixed Beaker Stand Measure Standard at regular intervals and compare with factory reference

data

158

PVC Measurement:

at the Factory at startup (IQ/OQ) after 3 months (PQ)

159

Reproducibility Best quality data

Minimises effect of light scattering or refractive difference changes on

quality of data

Procedure for locating correct Window Reference Position

Precision micrometer used to adjust focus position

160

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