Thermo Scientific HAAKE User manual

002-7585 Version 2.4 March 2020
Thermo Scientific
HAAKE Falling Ball Viscometer
TypeC
Instruction Manual

© 2020 Thermo Fisher Scientific Inc. All rights reserved.
Thermo Fisher Scientific Inc. provides this document to its customers with a product purchase to use in the
product operation. This document is copyright protected and any reproduction of the whole or any part of this
document is strictly prohibited, except with the written authorization of Thermo Fisher Scientific Inc.
The contents of this document are subject to change without notice. All technical information in this
document is for reference purposes only. System configurations and specifications in this document supersede
all previous information received by the purchaser.
This document is not part of any sales contract between Thermo Fisher Scientific Inc. and a purchaser. This
document shall in no way govern or modify any Terms and Conditions of Sale, which Terms and Conditions of
Sale shall govern all conflicting information between the two documents.

Table of Contents
1
1. Quality Assurance 3..........................
2. Your Contacts at Thermo Fisher Scientific 3....
3. Key to Symbols 4.............................
4. Safety Notes and Warnings 4..................
5. Unpacking 6..................................
5.1 Transportation damage? 6.................
5.2 Before return delivery: 6...................
5.3 Contents of Delivery 6.....................
5.4 Material for use 7.........................
5.5 Spare parts 7.............................
5.6 Waste disposal 7..........................
5.7 WEEE Compliance 7......................
6. Setting Up 8..................................
6.1 Assembly 8..............................
7. Unit Description 9............................
7.1 Principle of the measurement 9.............
7.2 Description of the instrument 9..............
8. Functional Elements 10........................
9. Measuring 11..................................
9.1 Preparation for a test 11....................
9.1.1 Temperature control 11...............
9.1.2 Loading the sample 11................
9.1.3 Selection of the balls 12...............
9.2 Measurement of the falling times 13..........
9.3 Evaluation of the test results 14..............
9.3.1 Reproducibility 15....................
9.3.2 Comparability 15....................
9.4 Viscosity determination of gases 16...........
10. Cleaning the Measuring Tube 17................
11. Calibration of the Falling Ball Viscometer 18.....
12. Maintenance by the User 20....................
12.1 Exchange of the measuring tube and
the jacket tube 20..........................
12.2 Order numbers 21..........................
13. Spare Parts 22.................................
13.1 Recommended spare parts for
a period of 3 years 22.......................
13.2 Single parts 23.............................
13.3 High--resolution thermometer 24.............
13.3.1 The use of a thermometer with
wetting expansion liquid 24............
13.4 Contents of the ball box 26..................

Table of Contents
2
14. Appendix 27...................................
14.1 Example: Evaluation 27.....................
14.2 Example: Calibration of ball 1 27.............

Quality Assurance/Contacts at Thermo Fisher Scientific
3
1. Quality Assurance
Dear customer,
Thermo Fisher Scientific implements a Quality Manage-
ment System certified according to ISO 9001:2008.
This guarantees the presence of organizational structures
which are necessary to ensure that our products are deve-
loped, manufactured and managed according to our cu-
stomers expectations. Internal and external audits are car-
ried out on a regular basis to ensure that our QMS is fully
functional.
We also check our products during the manufacturing pro-
cess to certify that they are produced according to the
specifications as well as to monitor correct functioning and
to confirm that they are safe. The results are recorded for
future reference.
The “Final Test” label on the product is a sign that this unit
has fulfilled all requirements at the time of final manufacturing.
Please inform us if, despite our precautionary measures,
you should find any product defects. You can thus help us
to avoid such faults in future.
2. Your Contacts at Thermo Fisher Scientific
Please get in contact with us or the authorized agent who
supplied you with the unit if you have any further questions.
Thermo Electron (Karlsruhe) GmbH
Part of Thermo Fisher Scientific
Dieselstraße 4
D-76227 Karlsruhe, Germany
Tel. [phone]
Fax [phone]
[e-mail]
www.thermofisher.com
The following specifications should be given when product
enquiries are made:
Unit name printed on the front of the unit and specified on
the name plate.
Type: Order No. 356--0001
Serial number:
____________ 12 digit number
(e.g. 201625085062)
____ Manufacturing year
4 digit number (e.g. 2016)
_____ Production order no..
5 digit number (e.g. 25085)
___ Serial no.
3 digit number (e.g. 062)
If you have any questions regarding installation or technical
issues, please contact the helpdesk. You will find the contact
form at:
https://tfs-3.secure.force.com/materialcharacterization/

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Safety Notes and Warnings
4
3. Key to Symbols
Warns the user of possible damage to the unit, draws
attention to the risk of injury or contains safety notes
and warnings.
Denotes an important remark.
1Indicates the next operating step to be carried out and
what happens as a result thereof.
Warns the user of possible damage to the unit.
4. Safety Notes and Warnings
These notes are intended to draw your attention to risks
which only YOU can recognize and avoid or overcome. They
are intended to enhance your own safety consciousness.
We have set the highest quality standards for ourselves and
this unit during development and production. Every unit
meets relevant safety regulations. The correct unit usage
and proper handling is however solely your responsibility.
The following notes must be observed:
This instruction manual must be carefully studied!
It contains important information on the connec-
tion to the local mains supply, correct unit usage
and safe handling.
Check for transportation damage during unpack-
ing. Get in contact with supplier and/or carrier for
settlement of damage claims. Do not try to start up
a damaged unit before the damage has been re-
paired or you have ascertained the effect of the da-
mage.
Ensure that this manual is always at hand for every
unit operator.
Only use this unit solely for the intended applica-
tion.
Repairs, alterations or modifications must only be
carried out only by a professional trained by
Thermo Fisher Scientific to handle this equipment.
Considerable damage can be caused by improper
repairs. The Thermo Fisher Scientific-service de-
partment is at your disposal for repair work.

!
!
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Safety Notes and Warnings
5
Thermo Fisher Scientific does not assume respon-
sibility for independent repairs and consequences
of improper use.
Do not clean the unit with solvents (fire risk!) --
a wet cloth soaked in household detergent is nor-
mally sufficient.
Only use the heat transfer liquids recommended by
Thermo Fisher Scientific. Please refer to the respec-
tive EC -- Safety Data Sheet.
Severe skin burns can be caused by contact with
hot unit parts!
The Falling Ball Viscometer can be operated using a suita-
ble circulator and appropriate bath liquid in the temperature
range up to +150 C which even considering cooling and in-
sulation may heat up parts of the Falling Ball Viscometer
enough to cause serious skin burns if contact is made.
Thermo Fisher Scientific recommends the use of personal
protective equipment (gloves, safety glasses, laboratory
coat, and safety shoes) when operating with the Falling Ball
Viscometer. When working at high temperatures wear use
temperature--resistant gloves.
We do not know what substance you will be ex-
amining with this device. Many substances are:
flammable or explosive
unhealthy
dangerous for the environnent
You alone are responsible for the handling of these sub-
stances!
Our advice:
If in doubt, consult a safety specialist.
Read the safety data sheet valid for your country the
product manufacturer’s or supplier’s
Read relevant regulations concerning dangerous
materials
Observe relevant guidelines for laboratories in your
country

Unpacking / Setting Up
6
5. Unpacking
5.1 Transportation damage?
Notify carrier (forwarding merchant, railroad,
post office etc.),
Compile a damage report.
5.2 Before return delivery:
Inform dealer or manufacturer
(Small problems can often be dealt with on the spot).
5.3 Contents of Delivery
The following standard accessory is delivered together
with the falling ball viscometer:
Order-No. Description
002-7580 Falling ball viscometer, ready for testing
800-0182 Set of balls 1--6 (see chapter 10.3)
800-0012 Hollow stopper
800-0013 Stopper
800-0119 Ball tweezers
800-0125 Cleaning piston
800-0131 Cleaning brush
800-0014 Cover plate
800-0027 Stopper gasket =15.6mm
002-5176 Thermometer gasket =10mm
003-2110 Socket wrench (see chapter 10.2)
LEERER MERKER Instruction manual
089--2094 Calibration certifikate

Unpacking / Setting Up
7
5.4 Material for use
No other material except for cleaning material (800-0125
cleaning piston, 800-0131 cleaning brush) is necessary at
normal use.
5.5 Spare parts
See chapter 13.
5.6 Waste disposal
The transportation packing is made out of paper and can be
recycled.
5.7 WEEE Compliance
This product is required to comply with the European Union’s
Waste Electrical & Electronic Equipment (WEEE) Directive
2012/19/EU. It is marked with the following symbol:
Thermo Fisher Scientific has contracted with one or more re-
cycling/disposal companies in each EU Member State, and
this product should be disposed of or recycled through them.

Unpacking / Setting Up
8
6. Setting Up
6.1 Assembly
Insert the measuring tube into the stand and fasten it with the
knurled nut.

a
b
A
C
B
Thermometer
2
1
3
Unit Description
9
7. Unit Description
7.1 Principle of the measurement
The HAAKE Falling Ball Viscometer measures the viscosity
of transparent newtonian liquids. This viscosity is correlated
to the time a ball requires to fall a defined distance. The rol-
ling and sliding movement of the ball through the sample
filled into a slightly inclined cylindrical measuring tube is de-
scribed by means of the fall time. The test results are given
as the dynamic viscosity using the internationally standard-
ized absolute unit of ”milli Pascal seconds” (mPa¡s).
Note: 1 mPa¡s = 1 cP (centi Poise)
The Falling Ball Viscometer corresponds to the require-
ments of many international standards, i.e. ISO 12058 and
the german standard DIN 53 015.
7.2 Description of the instrument
The heart of the instrument is the measuring tube made of
glass 1and a ball 2. This tube carries two ring marks A and
B, which are spaced 100 mm apart and which limit the mea-
suring distance. The ring mark C is in the middle between A
and B. The measuring tube is jacketed by means of an outer
glass tube, which encloses a room 3to be filled with a tem-
perature controlled liquid. The measuring tube is fastened to
the stand in such a way that its axis is inclined with respect
to the vertical by 10during the measurement.
The measuring tube together with the jacket may be pivoted
in order to turn the tube upside down again to let the ball re-
turn to the initial position before a measurement. The mea-
suring tube is closed on both sides by two stoppers, one of
which 13 contains a capillary and a small reservoir. This
stopper prevents undesirable changes of pressure in the liq-
uid sample and has a passage for air bubbles when the tem-
perature is being changed. The viscometer incloses all sam-
ples completely to prevent volatization and film forming. The
stand may be levelled by means of its water level aand the
levelling screws b. Ein Thermometer, welches auswechsel-
bar ist, ermöglicht das genaue Ablesen in dem Temperatur-
bereich der geplanten Messung.
As standard, the Falling Ball Viscometer is supplied with a
thermometer in the range of --1 Cto+26C. Optionally
other thermometers are available, which are listed in section
13.2.

Functional Elements
10
8. Functional Elements
4
12
11
2
3
1
4
17
14
18
7
8
8
9
17
15
13 16
18
20
1Falling tube 12 Jacket tube
2Ball 13 Hollow stopper
3Tempering room 14 Stopper
4Screw 15 Capillary
7Set screw 16 Closing plate
8Gasket 17 Gasket for falling tube
9Cover 18 Threaded bush
11 Brace 20 Connecting rod

13
15
2
1
Measuring
11
9. Measuring
9.1 Preparation for a test
9.1.1 Temperature control
The HAAKE Falling Ball Viscometer may be temperature
controlled in a temperature range from --20 C up to +150C
using liquid circulators.
Ensure that the sample to be measured is homogeneously
tempered. For this purpose a sufficient tempering time must
be provided, at least 30 minutes. Ideally, the sample was pre-
heated to the measurement temperature.
The temperature in the jacket around the measuring tube
must be maintained within a temperature tolerance of
0.03C for test temperatures between 10 up to 80C.
For test temperatures beyond these limits the tolerances
may be increased to 0.05C.
The tempering room 3must be free of air bubbles.
Severe skin burns can be caused by contact with
hot unit parts!
9.1.2 Loading the sample
All parts of the viscometer being in direct contact with the
sample must be kept clean and dry.
A sample volume of approximately 45 cm3is poured into the
measuring tube 1up to 20 mm below the rim of the tube.
Then the ball 2is placed into the tube and the hollow stopper
13 is introduced. The liquid should reach a level just beyond
the capillary 15. The sample in the tube must be free of air
bubbles.
Only then does the measurement begin.

Measuring
12
9.1.3 Selection of the balls
The standard ball set contains 6 balls, which pass through
the measuring tube of an inner diameter of approximately
15.94 0.01 mm.
Order-
No.
Ball
No.
Made of Density
(standard
values)
g/cm3
Diameter
of the ball
mm
Constant K
(approx.)
mPascm3/gs
Recomm.
measuring
range mPas
800--0002 1boron silica glass 2.2 15.81 0.01 0.007 0.6 -- 10
800--0003 2boron silica glass 2.2 15.6 0.05 0.09 9 -- 140
800--0004 3nickel iron alloy 18.1 15.6 0.05 0.09 40 -- 700
800--0005 4nickel iron alloy 18.1 15.2 10.7 150 -- 5000
800--0006 5nickel iron alloy 18.1 14.0 0.5 71500 -- 50 000
800--0007 6nickel iron alloy 18.1 11.0 135 >7500
1W.-No. 1.3912
Additionally the following balls are deliverable:
Order-
No.
Ball Made of Density
(standard
values)
g/cm3
Diameter
of the ball
mm
Constant K
(approx.)
mPascm3/gs
Recomm.
measuring
range mPas
800--0009 Gboron silica glass 2.2 15.91 0.02 -- gases
800--0010 G3 boron silica glass 2.2 15.30 0.4 20 to 200
800--0011 G4 boron silica glass 2.2 14.40 3.5 150 to 1500
The measuring ranges for viscosity indicated are related to
DIN 53015 (as of February 2001).

Measuring
13
9.2 Measurement of the falling times
The jacket tube snaps into a defined 10-position at the bot-
tom of the instrument.
By turning over the jacket tube, the ball is set to the measu-
ring position.
The falling time of the ball moving from the ring mark A to ring
mark B is determined by using a stop watch. The time period
starts when the lower periphery of the ball touches the ring
mark A, which must appear as a straight line. The falling time
ends when the lower periphery of the ball touches the ring
mark B, which again must appear as a straight line. If one
uses the distance AC or CB to reduce very long falling times
for high viscous liquids the double of the measuring time pe-
riod must be taken into account.
Turning the jacket tube 180again the ball returns to its start
position. It is good practice to take the mean value out of sev-
eral falling time values (3 to 5).
When testing dark liquids it is usually very difficult to see the
lower part of the ball. In this case we advise to take the ball
equator when it passes through the ring marks.

Measuring
14
9.3 Evaluation of the test results
The dynamic viscosity (in mPas) is calculated using the
following equation:
=K(1-- 2)¡t
where:
K = ball constant in mPascm3/gs (see chapter 11)
1= density of the ball in g/cm3(see chapter 11)
2= density of the liquid to be measured at the measuring
temperature in g/cm3
t = falling time of the ball in seconds.
Test results:
The dynamic viscosity is given in units of mPas(cP)and
must be completed by stating the sample temperature.
The dynamic viscosity may be converted to the kinematic
viscosity by using the following equation:
=

= kinematic viscosity [mm2/s] [1 mm2/s = 1 cSt]
= dynamic viscosity [mPas]
= density of the liquid sample [g/cm3]

Measuring
15
To evaluate the reliability of the results the following criteria
may be used:
9.3.1 Reproducibility (one person, one instrument)
If one person determines two test results under identical test
conditions, these results are supposed to be acceptable if
they do not vary more than the figures stated in the table
below from the average value.
9.3.2 Comparability (several persons, several different
instruments)
If two sets of test results are reached in two different labora-
tories under comparable conditions, these results are sup-
posed to be acceptable if they do not vary more than the fig-
ures stated in the table below from the average value.
Ball-No. Reproducibility % Comparability %
DIN 53015 ISO 12058
11.0 2 2
2, 3, 4 0.5 1 2
50.7 1.5 1
61.5 3 3
The falling ball viscometer is suitable only for measure-
ments on Newtonian fluids and is calibrated.

Measuring
16
9.4 Viscosity determination of gases
The viscosity determination of gases has to be done with ball
G which is made out of glass.
1The measuring tube must be closed with rubber stop-
pers fitted with glass stopcocks.
Measuring tube, glass ball and gas must be clean and
dry.
2The tube is flushed several times with the gas to be
tested to push out any remains of air. Then the tube fil-
led with the gas sample is closed with the stopcocks
and raised to the test temperature.
The calculation of the gas viscosity is based on the compari-
son with the viscosity of air at 20 C(= 181510-- 5 mPas):
gas =FG
F
A
1815 10-- 5 (mPa s)
where:
gas: viscosity of the gas at the temperature T
FG: falling time of the ball in the gas at the temperature T
FA: falling time of the ball in air at a temperature of +20C
Viscosity of the air at a temperature of +20C:
1815 10-- 5 (mPa s)

Cleaning the Measuring Tube
17
10. Cleaning the Measuring Tube
1Usually the tube is cleaned by rinsing it with a suitable
solvent.
2High viscous liquids (glue and heavy oils, etc.) have to
be removed with the cleaning piston which is supplied
with the instrument. Push this piston slowly through the
tube.
After this, there will be only a thin film of the liquid left
on the walls of the tube which then can be removed with
a solvent.
If the plug is removed during cleaning, it can
subsequently be inserted into the downpipe more
easily if it is moistened.

Calibration
18
11. Calibration of the Falling Ball Viscometer
The falling ball viscometer is checked according to the
HAAKE regulations before delivery. The geometry relates
strictly on the DIN 53015/ISO 12058 and therefore the listed
ball constants can be used.
The calibration of the instrument can be done using nation-
ally recyclable calibration fluids. This procedure is also rec-
ommended for new balls or after repairs and for falling ball
viscometers integrated into a measuring procedure accord-
ing to ISO 9000.
Testing ...
periodically: to be defined by the user or to be read in the QC-hand book.
with nationally recyclable
standards: Calibration fluids acknowledged in the corresponding user
country, e.g. Europe: DKD/PTB calibration fluids, in Japan:
JIS fluids or in the USA: Cannon calibration fluids.
The calibration excludes the influence of allowed tolerances
when measuring balls and falling tubes.
The following Thermo Fisher Scientific products can be used
for testing the instrument:
Order-No. Type (mPas)
at 20C
for balls
082--5042 E7 5 1
082--5043 E200 120 2, 3
082--5044 E2000 1900 4
082--5046 E6000 6000 5
082--5336 E15000 15000 6
For calibration of the falling ball viscometer the following cal-
ibration fluids (recyclable in Europe) are recommended:
Order-No. Type (mPas)
at 20C
for balls
082--5303 100 BW 100 2, 3
082--5304 2000 AW 2000 4, 5
082--5305 10000 B 10000 5, 6