Engineering for Success:

The Aqueous Film Coating Process

A Special Presentation for:

The International Society of Pharmaceutical Engineers, Los Angeles Chapter
May 12, 2005
Fred A. Rowley
Director, Corporate Manufacturing Technical Support
Watson Labs., Inc.
1

Where Aqueous Coating Fits Into The Big

Picture
The Aqueous Film Coating Unit Operation

Weigh and Screen Materials

Wet or Dry Granulate as

Required

Add Lubricant

Blend Materials

Compress Tablets

Aqueous Film Coating

Tablet Printing
(Optional)

Popular Myths About Tablet Coating

It is more art than
science.
Coating pan operators
are prima donnas.
Water based coating is
tricky.
Coating solutions are just
dyes in water and you can
mix them anywhere.
3

Aqueous Coating Is Not Like

Granulating and Tablet Compressing
Aqueous film coating
demands:
Consistent tablet
hardness
Controlled spray rates
Controlled operating
temperature
Controlled air flow
rates for drying
Bad things can happen
in seconds.
(Or you could end up
with this)

Popcorn ball
4

Our Topics For Today

Introduction to Aqueous Film Coating

The Coating Room Systems
A Review of Coating Installations Around The World
Types of Common Pumping Systems
Typical Coating Suspension: Component Parts
Suspension Preparation
How The Coating Process Works
Spray Guns: Anatomy and Function
The Eight Critical Operating Parameters
Common Coating Defects Seen on the Production Floor

Introduction To The Coating

Room
Basics of The Coating Area

View of a Typical Coating Operation:

What The Operator Sees
Coating Pan
Suspension
vessel
Pumping System
Spraying System

What the Operator Doesnt See

Inlet side of the pan:

Inlet air turbine
Inlet air filtration with paper and HEPA filters
Air treatment packages:
Air heating system
Steam, high pressure hot water, electricity (not recommended)
Humidification and dehumidification systems
Outlet side of the pan:
Solvent recovery system (refrigeration, torch)
Bag house (or scrubber)
Outlet air turbine

The Entire Operation Then Looks Like This

The Entire Process Also Showing The Suspension

Spraying System

10

A Side Vented Pan Showing Most of

the System Parts Assembled at the
Factory

11

Two Basic Types of Perforated Coating

Pans
Side vented (100% perforated):
OHara
Accela Cota
others

Front vented (Partially perforated):

Vector
Freund
others
12

A Comparison of Front and Side Vented Pans

Side Vented Pan

Front Vented Pan

13

Examples of Coating Installations Around The

World

14

Examples of Front Vented Coating Installations

in the Pharmaceutical and Nutritional
Supplement Industries

Pan
Pumping system
Control panel
Ducts

15

An Example of a Side Vented 48 Pan in

The Manufacturers Testing Room

16

Fully Automated Aqueous Film Coater

Pliva Pharmaceuticals (Poland)

17

Types of Common Pumping

Systems

18

Common Pumping Systems, Coupled

with a Magnetic Flow Meter, Used to
Deliver Coating Suspensions
Gear Pumps
Peristaltic Pumps
Rotary Lobe Pumps
Used with a:
Magnetic flow meter
19

Gear Pumps
Advantages
*Inexpensive
*Solvent Friendly
*High Pressure

Disadvantages
*Not used for
Suspensions
*Difficult to Clean
*Difficult to Service

20

Peristaltic Pumps
Advantages
*Good for
suspensions
*Easy to clean
*Easy to service

Disadvantages
*Pulses
*Not for sugar
coating
*May or may not
work for solvent
coating
21

Rotary Lobe Pumps

Advantages

*Good for
suspensions
*High pressure
*Low suction

Disadvantages

*Require high flow

rates
*Expensive
*Seals may fail

22

Magnetic Flow Meters

Advantages
*Inexpensive
*Cleanable

Disadvantages
*Solutions must be
conductive
*Not a direct mass reading

23

A Typical Coating Suspension

Formulation:
Component Parts

24

Aqueous Film Coating

Formulation
Typical Film Coating Composition

Film-forming polymer
Plasticizer
Pigment/Colorant

7.0-18.0%
0.5-2.0%
2.5-8.0%

25

Aqueous Film Coating

Formulation
Water Soluble Polymers

Hydroxypropyl methylcellulose (HPMC)

Methylcellulose (MC)
Hydroxypropyl cellulose (HPC)
Polyvinylpyrrolidone (PVP)
Food starch (modified)
26

Aqueous Film Coating

Formulation
Common Film Forming Materials in
Sustained Release Products
Sustained Release
Ethylcellulose (EC)
Methacrylic acid copolymers ( Eudragit types)
Enteric Release
Cellulose acetate phthalate (CAP)
Hydroxypropyl methylcellulose phthalate (HPMCP)
Polyvinyl acetate phthalate (PVAP)
27

Aqueous Film Coating

Formulation
Common Plasticizers
Water soluble
Polyethylene glycol (PEG)
Propylene glycol (PG)

Water insoluble
Tributyl citrate (TBC)
Acetylated monoglyceride (AMG)
Dibutyl sebacate (DBS)
Castor oil

28

Suspension Preparation
Critical for Success. Frequently taken for granted!
Check for:
Even distribution of powders.
Lumps and fish eyes should not be allowed.
Screen suspension through an 80 mesh s/s screen.

Mix during preparation but Stir during actual use.

Be very careful of your terminology used on the batch record.
Note: FDA is sensitive to the improper use of the two terms.

Suspensions vs Solutions:
Note that terms are commonly used interchangeably.

29

Example of An Optimized Suspension

Preparation Process

High shear material addition.

Guarantees the best possible suspension.
Little chance for lumps, fish eyes, paste.
30

Optimized Suspension Preparation Vessel:

Engineered for Success
Used to prepare the
suspension.
May also be used for
transportation and as
a holding tank.
Turn off homogenizer.
Low shear/speed
stirring.
Coating suspension

31

Suspension Holding Tank:

Suboptimized Suspension Preparation
Should be used for
holding after
manufacturing.
Stir vs Mix.
Portable.
Unfortunately, commonly
used with a mixer to
prepare and hold the
suspension.
32

Moving forward:
How The Coating Process Works

33

How the Coating Process Works

34

An Internal View of the Coating Pan

When Viewed Head On

35

Spray Guns

Nomenclature and Process

36

Spray Pattern From an Aqueous

Coating System

Outside of the pattern is slower than the inside.

This may require some degree of overlapping of
spray patterns.
37

Air Cap

Solution
nozzle

Gun Nomenclature
Air cap supplies atomizing
and pattern air.
Solution nozzle supplies
coating suspension.
Needle closes the
suspension port.
Manual setting adjusts
both needle thrust and
percent solution port
opening.
Note: Air cap/suspension
nozzle and needle come in
Needle
matched sets.
38

Critical Operating Parameters

for Optimized Aqueous Coating
How We Achieve Success on The Coating Floor

39

Time Out!
Freds Little Check List
When I am asked to teach solid dosage or film coating, I
perform my on line two minute audit to determine how
professional the coating organization is:
Does the operator have a flashlight, ruler and small brushes?
Is there a range for gun to bed distance on the worksheet?
Got a set of spare needles handy?
Is there dried coating material stuck anywhere in the pan?
Do the guns have drip cups?
(Are there newspapers/magazines in the room?)

40

A Late Addition Side of A Vector HC-130:

And Why Do You Think They Installed This
Old Light On a New Coating Pan?

Patheon, Monza, Italy

41

The Eight Critical Parameters For

Aqueous Coating
Gun Geometry
Atomizing/Pattern Air
Pan Pressure
Pan Speed
Spray Rate
Inlet/Outlet Air temperature
Total Air Volume
Adhesion of particles to the gun surface
42

(1) Gun Geometry & Calibration:

Our First Optimization Opportunity

Gun to bed
Boom placement

Gun to Gun
Gun to side of pan
Cocked guns
Position of the guns
in relation to the
tablet bed.
43

Boom Placement and Boom Type

Varies between manufacturers and pan models.

May be fixed or variable.
Taken for granted and often overlooked as a variable during scale up or product transfer.
Notice the photograph to the right. At the end of a 2.5 hour coating run we see beautiful yellow
tablets with absolutely no adhesion of coating material anywhere in the pan. This should be
our goal; we should not allow any other conditions.

44

Cocked Guns
Guns become cocked from
movement in/out of the pan,
mechanical adjustment or
operator abuse.
Cocked side to side: over wet
condition.
Cocked up or down: solution
sticks to the pan.
Check guns by looking
straight down the boom.
Guns can also become
cocked by loose fittings due
to heat/cold expansion and
contraction.

45

Gun To Bed Distance

Well understood and reported in the literature.

Usually stated as a specification on the worksheet.
Most common settings for aqueous coating are 8 or 10
from the bed, depending on the spray rate used.
Always fixed, never use a range.
46

Gun To Gun Distance

Widely accepted or assumed to be fixed..but this is false.

Not recognized as a variable in the literature.
Usually not stated as a specification or set point on a worksheet.
Setting is 5.5 or 6.0 gun tip to gun tip between guns.
47

Gun to Side of the Pan

Measure tip of last gun on either side of the boom to either the front
side of the pan or the back of the drum.
Three possible problems may result:
solution on the window (right) or solution on the side or back of
the pan or both.
Setting is widely understood but not recognized as a possible variable
to be checked.
Check the setting with placebos, then fix the gun.
48

Periodically, Check Your Operation!

Use a flashlight.
Look for problems.
Pause, if necessary.
Optimize!

49

Examples of Two Bad Pan Set Ups

Pan speed is too fast,

tablets are too active
Back gun is too close to the
rear of the pan (just barely).
50

Guns in Relation to Bed Height

Tablet beds differ due to pan charge, size and shape of the tablet.
Guns should be set at the bottom of the waterfall in the upper 1/3 of the
bed.
Recheck at the beginning of each campaign or when pan charge changes.
51

Three Pans Good, One Pan Bad

52

Gun Calibration
Standardized Suspension Delivery

53

Gun Calibration is Important

Variation in solution rates between guns is common.

A variance of not more than +/- 10 ml. between guns is acceptable.
What do you do if the variation exceeds recommended spread?
Adjust the needle stroke from the back of the gun.

54

(2) Atomizing and Pattern Air

55

Atomizing and Pattern Air

One of the 8 critical
parameters for success.
Converts a stream of
suspension into a mist.
Too much/too little
atomizing air is bad.
Fixed vs variable pattern
air.
Too much/too little
pattern air is also bad.

56

A Visual Comparison of The Roles of

Atomizing and Pattern Air
Atomizing air joins
suspension here

Pattern air:
flattens spray
cone
57

Fixed Vs Variable Pattern Air

Pattern air shapes the solution cone. The
more air the flatter the cone.
In some systems the pattern air is fixed.
In some systems the pattern air is variable
and is set by the operator.

58

Too Much or Too Little Pattern Air

Too much pattern air flattens the cone and
may create an over spray condition.
Result: Over wetting that causes picking.

Too little pattern air concentrates the cone

in an insufficient area of the tablet bed.
Result: Tablet erosion and or picking.

59

(3) Pan Pressure

60

Pan Pressure
One of the 8 critical parameters
for success.
Never positive
Usually between -0.1 H20 and
-0.50 H20.
Never more than
-1.0H2O.
(Excessive pressure causes
unusual defects incorrectly
attributed to other causes.)

61

Pan Pressure and Pan Seals

Pan pressure is seriously reduced when the seals used to maintain

pressure in the pan weaken and then break.
In this picture we see an Accela Cota 48 pan with a broken seal.
This should be replaced immediately.
62

(4) Pan Speed

63

Pan Speed:
A Frequently Overlooked Optimization Opportunity
One of the 8 critical
parameters for success.
There is no single specific
setting. This is a relative
setting based on tablet size,
shape and load.
Experience and observation
are the initial basis of good
science.
Two basic pan speeds for
each product:
1) Initial speed to achieve
a basic covering and
then
2) steady state speed.

64

Anti-Slide Bars and Pan Baffles

65

Anti-Slide Bars and Baffles

Anti-Slide Bars (Blue):
Used to center the
tablet bed in front of the
outlet air plenum.
Not a mixing device.
Almost mandatory.

Baffles (Red):
Mixing device.
More than one kind.

66

(5) Spray Rate

67

Spray Rate
One of the 8 critical
parameters for
success.
Usually between 80150 ml/min./gun.
Recommend 80
ml/min/gun with gun to
bed distance of 8.
Recommend 120
ml/min/gun with gun to
bed distance of 10.
68

(6) Inlet and Outlet

Temperatures

69

Inlet/Outlet Air Temperature

One of the 8 critical
parameters for
success.
An alert organization
keys on an outlet air
temperature target
and let the inlet vary
within a range.
Outlet air target is
usually between 45
and 55 Deg. C.

70

Important Distinction!
Inlet air temperature is a set point, whereas
outlet air temperature is a function

Inlet air CFM + Inlet air Temp + Spray Rate+ Atomizing air = Outlet Temp.

Inlet temp is a set point, outlet temp

is a function
Monitoring outlet air temperature helps us determine if any
of the other factors have changed or shifted.

71

(7) Air Volume (CFM)

Drying Capacity

72

Total Air Volume (CFM or cubic feet per minute)

Means Total Drying Capacity

The Coating process is usually somewhat tolerant to

variations in total air volume.
However it becomes a critical parameter for products
sensitive to heat or moisture
Total CFM Is a factor in coating efficiency.

73

(8) Adhesion of Particles To

The Spray Guns

74

Adhesion of Coating Material to the Gun

Assembly
One of 8 critical
parameters for success.
Serious problem when
left unattended.
Solution:
Leave atomizing air
on, then:
Stop spraying
Leave atomizing air
on
Brush residue off
Resume coating.

75

Use a Brush To Remove The Dry Particles

Stop spraying.
Keep atomizing air
on.
Brush the guns &
assembly.
Resume spraying

76

Putting It All Together and Summary

Aqueous film coating is a controllable
process with eight critical operating
parameters.
It cannot be fully controlled by a computer.
Fully trained and knowledgeable operators
are required for success in this unit
operation.

77

You know youre in trouble in the coating

room if you hear:
So what if the gun drips a bit
Let me check with the mechanic
The nozzles are fixed at the factory
What do I need a ruler for?
Flashlights arent allowed in the coating
room
A little coating material at the back of the pan is
normal
Needles bend a little, doesnt matter
Pan pressure is the pressure of the tablets pressing up
against the drum, the more the better

78

Common Coating Defects &

Causes

79

Rough/Orange Peel Appearance

Problem:
Spray drying of
membrane

Causes:
Not enough vehicle
High CFM/inlet temp.
High atomization air.

80

Picking
Problem:
Tablets are too wet.

Possible Causes:
Spray rate too high
Guns too close together
Insufficient atomizing
air
Pan speed too low

81

Film Cracking
Problem:
Small cracks appear in
the coating.

Causes:
Wrong plasticizer.
Insufficient plasticizer.
Solution too
concentrated (Thick).
Insufficient atomizing
air.
82

Film Chipping
Problem:
Coating gone from the
tablet edge.

Causes:
High pan rpm
Low spray rate
Both together
Sharp tablet edges

83

Bridging of the Logo

Problem:
The letters and numbers
fill in with dried
suspension.

Causes:
High spray rate coupled
with high CFM (drying
capacity).
Inadequate atomizing
air
Poor tooling design.
84

Film Peeling
Problem:
Tablets are baking and
the coating ruptures.

Causes:
Very high spray rate
Low CFM
Tacky coating material
Lack of adhesion
(nothing to stick to, the
tablet is too hard)
85

Twins or Twinning
Problem:
Tablets stick together:

Twinning

Causes:
High spray rate
Inadequate drying
capacity
Tablet shape/design
Belly band too thick
Tablet too long
One or more factors

86

Logo Erosion
Problem:
Tablet erodes before coating
can adhere to the surface.

Causes:

Spray rate too slow

Pan speed too fast
Both
Soft tablets/combined
with items shown
above.

87

Film Cracking
Rather rare defect.
Not seen often
Happens when
solution evaporates
or is mixed too
thick.

88

Stability Issues:
Physical Changes in Tablet Appearance
Problem:
Off color with (maybe) off
odor tablets
Causes:
Microbial contamination
Moisture sensitivity.
Heat sensitivity.
Incompatibility:
Film to tablet
Excipients to API.
Both factors combined.
89

Grand Summary:
Film coating is unforgiving.
Coating is easily optimized.
You may avoid errors If You
understand the critical operating
parameters

90

Thank You For Listening!

Comments are always

welcomed:
Fred Rowley
frowley@watsonpharm.com

91