Fritsch Laser Particle Sizer ANALYSETTE 22 NT Operating instructions

ANALYSETTE 22

LASER-PARTICLE SIZER

Operang instrucons

FRITSCH NanoTec

Valid starng with: 22.8000/0001

Read the instrucons prior to performing any task!

Translaon of the original operang instrucons

Version 02/2020 Index 004

Fritsch GmbH

Milling and Sizing

Industriestraße 8

D - 55743 Idar-Oberstein

Telephone: +49 (0) 6784/ 70-0

Fax: +49 (0) 6784/ 70-11

Email: inf[email protected]

Internet: www.fritsch-sizing.de

Cercaons and CE conformity

Fritsch GmbH has been cered by the SGS-TÜV Saar GmbH.

An audit cered that Fritsch GmbH conforms to the requirements of the

DIN EN ISO 9001:2015.

The enclosed Conformity Declaraon lists the guidelines the FRITSCH

instrument conforms to, to be able to bear the CE mark.

Cercaon

CE Conformity

Cercaons and CE conformity

- 3 -

Table of contents

1Safety informaon and use........................................................... 8

1.1 Requirements for the user..................................................... 8

1.2 Scope of applicaon............................................................... 8

1.3 Obligaons of the operator.................................................... 9

1.4 Informaon on hazards and symbols used in this manual..... 9

1.5 Informaon on hazards at the instrument........................... 12

1.6 Device safety informaon.................................................... 12

1.6.1 Laser.................................................................................. 13

1.6.2 Ultrasound........................................................................ 14

1.7 Protecve equipment.......................................................... 15

1.8 Electrical safety.................................................................... 15

2 Technical data.............................................................................. 16

2.1 Dimensions.......................................................................... 16

2.2 Weight.................................................................................. 16

2.3 Operang noise.................................................................... 16

2.4 Voltage................................................................................. 16

2.5 Current consumpon........................................................... 16

2.6 Power consumpon............................................................. 17

2.7 Electrical fuses..................................................................... 17

2.8 Measuring ranges................................................................. 17

3Installaon................................................................................... 18

3.1 Transport.............................................................................. 18

3.2 Unpacking............................................................................ 18

3.3 Seng up............................................................................. 20

3.4 Removing the transport securing device of the measuring

device................................................................................... 22

3.5 Accessory case..................................................................... 23

3.5.1 Accessory case 1 - wet / dry dispersion unit..................... 23

3.5.2 Accessory case 2 - dry dispersion unit.............................. 23

3.5.3 Accessory case 3 - powder funnels................................... 23

3.6 Electrical connecon............................................................ 24

3.6.1 Electrical fuses.................................................................. 24

3.6.2 Stability of the mains voltage............................................ 24

3.6.3 Adapng to the mains....................................................... 24

4Inial start-up.............................................................................. 25

4.1 Connecons for measuring unit........................................... 25

4.2 Connecons for supply units................................................ 26

4.2.1 Wet dispersion unit........................................................... 26

4.2.2 Small volume wet dispersion unit SVA.............................. 28

4.2.3 Small volume wet dispersion unit SVM............................. 30

4.2.4 Dry dispersion unit............................................................ 31

Table of contents

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4.2.4.1 Technical data for compressed air.................................. 32

4.2.4.2 Compressed air connecon........................................... 32

4.2.4.3 Technical data for vacuum cleaner................................. 33

4.2.4.4 Connecng the exhaust................................................. 33

4.2.4.5 Mounng and posioning the vibratory feeder............. 35

4.2.4.6 Connecng the vibratory feeder.................................... 36

4.2.4.7 Connecng the measuring cell inseron....................... 37

4.2.5 Falling chute...................................................................... 39

4.2.5.1 Technical data for vacuum cleaner................................. 40

4.2.5.2 Connecng the exhaust................................................. 41

4.2.5.3 Mounng and posioning the vibratory feeder............. 42

4.2.5.4 Connecng the vibratory feeder.................................... 43

4.2.5.5 Connecng the measuring cell inseron....................... 44

4.3 Preparaon of the computer............................................... 45

4.4 Checking communicaon..................................................... 47

5 Supply units................................................................................. 48

5.1 Wet dispersion unit.............................................................. 48

5.1.1 Design of wet dispersion unit............................................ 48

5.1.2 Selecng the liquids.......................................................... 48

5.1.3 Filling the measuring circuit.............................................. 50

5.1.4 Sample addion................................................................ 51

5.2 Small volume wet dispersion unit SVA................................. 52

5.2.1 Design of small volume wet dispersion unit SVA.............. 52

5.2.2 Selecng the liquids for the SVA....................................... 52

5.2.3 Filling the measuring circuit.............................................. 54

5.2.4 Sample addion................................................................ 55

5.3 Small volume wet dispersion unit SVM................................ 56

5.3.1 Design of small volume wet dispersion unit SVM............. 56

5.3.2 Selecng the liquids for the SVM...................................... 56

5.3.3 Filling the SVM measuring circuit...................................... 58

5.3.4 Sample addion................................................................ 60

5.4 Dry dispersion unit............................................................... 61

5.4.1 Design of dry dispersion unit............................................ 61

5.4.2 Seng the pressure.......................................................... 62

5.4.3 Sample addion................................................................ 62

5.4.4 Seng the vibratory feeder.............................................. 62

5.4.4.1 Opmising the vibraon of the feeder.......................... 64

5.5 Falling chute......................................................................... 65

5.5.1 Design of falling chute....................................................... 65

5.5.2 Sample addion................................................................ 65

5.5.3 Seng the vibratory feeder.............................................. 66

5.5.3.1 Opmising the vibraon of the feeder.......................... 67

Table of contents

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6 Using the device........................................................................... 68

6.1 Replacing the measuring cell............................................... 68

6.2 Wet dispersion units............................................................ 69

6.2.1 Fritsch test powder F500.................................................. 69

6.2.2 Dispersion of barely weable samples............................. 71

6.2.3 Measurement of hardly soluble samples.......................... 71

6.3 Dry dispersion unit and falling chute................................... 72

6.3.1 Selecng the vibratory feeder........................................... 72

6.3.2 Fritsch test powder F70.................................................... 72

7 Accessories................................................................................... 75

7.1 Converng the dry dispersion unit to a falling chute........... 75

7.2 AutoSampler dry dispersion unit......................................... 76

7.2.1 Funconal principle of AutoSampler................................ 76

7.2.2 AutoSampler connecons................................................. 76

7.2.3 Installaon of AutoSampler.............................................. 76

7.2.4 Control panel.................................................................... 77

7.2.5 Using the AutoSampler..................................................... 78

7.2.6 AutoSampler standard operang procedure (MaS con-

trol)................................................................................... 78

7.3 Extended conversion kit for the small volume wet disper-

sion unit SVA........................................................................ 81

7.4 Immersion pump set............................................................ 81

8 Cleaning........................................................................................ 82

8.1 Cleaning the devices............................................................ 82

8.2 Cleaning the hoses............................................................... 82

8.3 Cleaning the wet measuring cell.......................................... 82

8.3.1 Design of wet measuring cell............................................ 83

8.3.2 Preparaon....................................................................... 83

8.3.3 Emptying the system......................................................... 84

8.3.4 Removing the wet measuring cell..................................... 85

8.3.5 Cleaning the measuring cell glasses.................................. 87

8.3.5.1 Front measuring cell glass.............................................. 87

8.3.5.2 Fixed measuring cell glass.............................................. 87

8.3.6 Flow plate.......................................................................... 88

8.3.7 Sealing rings...................................................................... 88

8.3.8 Mounng the wet measuring cell..................................... 89

8.3.9 Check the wet measuring cell for impermeability............ 90

8.4 Cleaning the dry dispersion unit and falling chute............... 90

8.5 Cleaning the dry measuring cell........................................... 91

8.5.1 Design of dry measuring cell............................................. 91

8.5.2 Removing the dry measuring cell...................................... 92

8.5.3 Cleaning the measuring cell glasses.................................. 92

8.5.3.1 Front measuring cell glass.............................................. 93

Table of contents

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8.5.3.2 Back measuring cell glass............................................... 93

8.5.4 Base body.......................................................................... 93

8.5.5 Mounng the dry measuring cell...................................... 94

9 Maintenance................................................................................ 95

9.1 Replacing hoses in wet dispersion units.............................. 96

10 Checklist for troubleshoong...................................................... 97

11 Disposal........................................................................................ 98

12 Guarantee terms.......................................................................... 99

13 Exclusion of liability................................................................... 101

14 Safety logbook........................................................................... 103

15 Index........................................................................................... 105

Table of contents

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1 Safety informaon and use

1.1 Requirements for the user

This operang manual is intended for persons assigned with operang

and monitoring the Fritsch ANALYSETTE 22. The operang manual and

especially its safety instrucons are to be observed by all persons

working on or with this device. In addion, the applicable rules and regu-

laons for accident prevenon at the installaon site are to be observed.

Always keep the operang manual at the installaon site of the ANALY-

SETTE 22.

People with health problems or under the inuence of medicaon,

drugs, alcohol or exhauson must not operate this device.

The ANALYSETTE 22 may only be operated by authorised persons and

serviced or repaired by trained specialists. All commissioning, mainte-

nance and repair work may only be carried out by technically qualied

personnel. Qualied personnel are persons who, because of their educa-

on, experience and training as well as their knowledge of relevant

standards, regulaons, accident prevenon guidelines and operang

condions, are authorised by those responsible for the safety of the

machine to carry out the required work and are able to recognize and

avoid possible hazards as dened for skilled workers in IEC 364.

In order to prevent hazards to users, follow the instrucons in this

manual.

Malfuncons that impair the safety of persons, the ANALYSETTE 22 or

other material property must be reced immediately. The following

informaon serves both the personal safety of operang personnel as

well as the safety of the products described and any devices connected

to them: All maintenance and repair work may only be performed by

technically qualied personnel.

This operang manual is not a complete technical descripon. Only the

details required for operaon and maintaining usability are described.

Fritsch has prepared and reviewed this operang manual with the

greatest care. However, no guarantee is made for its completeness or

accuracy.

Subject to technical modicaons.

1.2 Scope of applicaon

The ANALYSETTE 22 can be universally used to determine the parcle

size distribuon of suspensions, emulsions and solids. It is mainly used in

research and development and in quality and process control.

The ANALYSETTE 22 uses the FRITSCH patent with a measuring cell which

can be posioned in the convergent laser beam to determine parcle

size distribuon.

Safety informaon and use

- 8 -

The laser parcle sizer described here is an operaons resource for use in

industrial environments. This operaons resource possesses hazardous

live components and laser radiaon sources during operaon. Therefore

serious health hazards or material damage can result, e.g., aer the

impermissible removal of the required covers or insucient mainte-

nance.

1.3 Obligaons of the operator

Before using the ANALYSETTE 22, this manual is to be carefully read and

understood. The use of the ANALYSETTE 22 requires technical knowl-

edge; only commercial use is permied.

The operang personnel must be familiar with the content of the oper-

ang manual. For this reason, it is very important that these persons

actually receive the present operang manual. Ensure that the operang

manual is always near the device.

The ANALYSETTE 22 may exclusively be used within the scope of applica-

ons set down in this manual and within the framework of guidelines put

forth in this manual. In case of non-compliance or improper use, the cus-

tomer assumes full liability for the funconal capability of the ANALY-

SETTE 22 and for any damage or injury arising from failure to full this

obligaon.

By using the ANALYSETTE 22 the customer agrees with this and recog-

nizes that defects, malfuncons or errors cannot be completely excluded.

To prevent risk of damage to persons or property or of other direct or

indirect damage, resulng from this or other causes, the customer must

implement sucient and comprehensive safety measures for working

with the ANALYSETTE 22.

Neither compliance with this manual nor the condions and methods

used during installaon, operaon, use and maintenance of the ANALY-

SETTE 22 can be monitored by Fritsch GmbH. Improper execuon of the

installaon can result in property damage and thus endanger persons.

Therefore, we assume absolutely no responsibility or liability for loss,

damage or costs that result from errors at installaon, improper opera-

on or improper use or improper maintenance or are in any way con-

nected to these.

The applicable accident prevenon guidelines must be complied with.

Generally applicable legal and other obligatory regulaons regarding

environmental protecon must be observed.

1.4 Informaon on hazards and symbols used in this manual

Safety informaon in this manual is designated by symbols. Safety infor-

maon is introduced by keywords that express the extent of the hazard.

Safety informaon

Safety informaon and use

- 9 -

DANGER!

This symbol and keyword combinaon points out a

directly hazardous situaon that can result in death or

serious injury if not avoided.

WARNING!

This symbol and keyword combinaon points out a pos-

sibly hazardous situaon that can result in death or

serious injury if not avoided.

CAUTION!

This symbol and keyword combinaon points out a pos-

sibly hazardous situaon that can result in slight or

minor injury if not avoided.

NOTICE!

This symbol and keyword combinaon points out a pos-

sibly hazardous situaon that can result in property

damage if not avoided.

To call aenon to specic hazards, the following symbols are used in the

safety informaon:

DANGER!

This symbol and keyword combinaon points out a

directly hazardous situaon due to electrical current.

Ignoring informaon with this designaon will result in

serious or fatal injury.

DANGER!

This symbol and keyword combinaon designates con-

tents and instrucons for proper use of the machine in

explosive areas or with explosive substances. Ignoring

informaon with this designaon will result in serious

or fatal injury.

DANGER!

This symbol and keyword combinaon designates con-

tents and instrucons for proper use of the machine

with combusble substances. Ignoring informaon with

this designaon will result in serious or fatal injury.

Special safety informaon

Safety informaon and use

- 10 -

WARNING!

This symbol and keyword combinaon points out a

directly hazardous situaon due to movable parts.

Ignoring informaon with this designaon can result in

hand injuries.

WARNING!

This symbol and keyword combinaon points out a

directly hazardous situaon due to hot surfaces.

Ignoring informaon with this designaon can result in

serious burn injuries due to skin contact with hot sur-

faces.

Safety informaon can refer to specic, individual procedure instrucons.

Such safety informaon is embedded in the procedure instrucons so

that the text can be read without interrupon as the procedure is being

carried out. The keywords described above are used.

Example:

1. Loosen screw.

2.

CAUTION!

Risk of entrapment at the lid.

Close the lid carefully.

3. Tighten screw.

This symbol emphasises useful ps and recommenda-

ons as wells as informaon for ecient operaon

without malfuncon.

To emphasise procedure instrucons, results, lists, references and other

elements, the following designaons are used in this manual:

Designaon Explanaon

1., 2., 3. ...

Step-by-step procedure instrucons

ðResults of steps in the procedure

Safety informaon in the procedure

instrucons

Tips and recommendaons

Further designaons

Safety informaon and use

- 11 -

Designaon Explanaon

References to secons in this manual and rele-

vant documentaon

Lists without a specic order

[Buon] Operang elements (e.g. push buon, switch),

display elements (e.g. signal lamps)

‘Display’ Screen elements (e.g. buons, funcon key

assignment)

1.5 Informaon on hazards at the instrument

There is a laser radiaon hazard warning on the back of the device.

It is explained below.

Do not remove the informaon and warning signs.

Cauon! Beware of laser beam

1.6 Device safety informaon

nThe laser parcle sizer has been designed from the viewpoint of

safety to users; nevertheless, residual hazards cannot be ruled out.

nThe device may only be used for the purpose described in

Ä

Chapter

1 ‘Safety informaon and use’ on page 8.

nOnly use original accessories and original spare parts. Failure to

observe this instrucon can compromise the funconing of the

machine.

nSafe conduct must be strictly observed during all work.

Safety informaon and use

- 12 -

DANGER!

Explosion hazard!

– When measuring oxidisable substances, e.g. metal,

organic material, wood, coal, plascs etc. there is a

risk of spontaneous combuson (dust explosion) if

the proporon of ne parcles exceeds a certain

percentage. Therefore special safety measures (e.g.

measurement in suspension) must be taken and

the work must be supervised by a specialist.

– The device is not explosion-protected and is not

suitable for measuring explosive, ammable or oxi-

dising substances.

– The device must not be used in electrically conduc-

ve, dusty or damp environments.

– Do not use highly ammable and ammable liquids

such as alcohols, ketones and benzines etc.

DANGER!

Mains voltage

– Do not allow any liquids to run inside the device.

WARNING!

The maximum accepted concentraon (MAC) levels of

the valid safety regulaons must be observed. If neces-

sary, venlaon must be provided or the machine must

be operated under an extractor hood.

nUnauthorised alteraon of the device will void Fritsch's declaraon

of conformity to European direcves and void the guarantee.

nIf, aer reading the operang manual, there are sll quesons or

problems, please do not hesitate to contact our specialised per-

sonnel.

1.6.1 Laser

NanoTec

2 semiconductor lasers

Laser 1: Wavelength 532 nm, power 10 mW

Laser 2: Wavelength 850 nm, power 20 mW

Safety informaon and use

- 13 -

The lasers are classied in Class 3b EN 60825-1/11.2001 and with regard

to the laser emier may only be operated in the valid range of the safety

regulaons of the German Labour Inspectorate in accordance with the

corresponding safety instrucons in EN 60825 Part 1 and 2. The user

must inform himself about the dangers of handling laser beams before

use.

WARNING!

Laser radiaon!

Laser devices of laser class 3B and 4 are dangerous for

the human eye, so that even an exposure me of 0.25

sec is sucient to cause permanent damage to the

rena. Therefore it is mandatory for every person who

is operang the device with the housing open during

repairs or maintenance to wear suitable safety goggles.

The safety goggles must be suitable for the wavelength

of the laser being used.

WARNING!

Laser radiaon!

– Never look directly into the laser beam.

– Always avoid placing any reecve objects in the

laser beam.

– Wear suitable safety goggles during maintenance

and adjustment work on the open laser emier. (<

10 mW, 532 and 940 nm).

It is not necessary to appoint a laser safety ocer for the ANALYSETTE 22

as the laser radiaon sources are fully enclosed and not accessible.

The ANALYSETTE 22 is classied in laser protecon class 1 according to

EN 60825.

The laser is automacally switched o when the meas-

uring cell inseron is removed.

1.6.2 Ultrasound

NOTICE!

– Do not operate the sample bath without liquids.

–Do not reach into the liquid during irradiaon.

Safety informaon and use

- 14 -

The ultrasonic emier installed in the wet dispersion unit has a power of

up to 120 was and a frequency of 40 kHz. It converts electrical energy

into ultrasound waves, which disperse in the liquid and result in so-called

cavitaon. Cavitaon both destructs agglomerates and degasses the

liquid.

During degassing the cavitaon noise changes, loud degassing noises are

eliminated at the end of the degassing procedure and the device appears

to work more quietly. Lower noise levels do not imply reduced ultra-

sound power but rather the end of the degassing procedure.

DANGER!

Explosion hazard, combusble substances

– Do not use highly ammable and ammable liquids

such as alcohols, ketones and benzines etc. or any

chemicals, which contain or could break down into

chloride ions (some disinfectants, household deter-

gents and washing-up liquids), in the dispersion

unit. See

Ä

Chapter 5.1.2 ‘Selecng the liquids’

on page 48.

–Aer prolonged use the liquid warms up, therefore

check the temperature.

– Do not use aggressive liquids (e.g. strong acids,

concentrated salt soluons).

1.7 Protecve equipment

Protecve equipment, such as covers, must be used as intended and may

not be disabled or removed.

1.8 Electrical safety

Connect the measuring unit and supply units to a mains line protected

with a residual current circuit breaker.

The mains switches separate the devices from the mains on two poles.

The mains fuse provides overload protecon.

Safety informaon and use

- 15 -

2 Technical data

2.1 Dimensions

Measuring units:

nNanoTec: 53 x 65 x 35 cm (w x d x h)

Supply units:

nWet dispersion units: 32 x 65 x 44 cm (w x d x h)

nSmall volume wet dispersion unit SVA: 32 x 65 x 44 cm (w x d x h)

nSmall volume wet dispersion unit SVM: 14 x 33 cm (Ø x h)

nDry dispersion unit: 36 x 65 x 75 cm (w x d x h)

nFalling chute: 36 x 65 x 75 cm (w x d x h)

Accessories:

nAutoSampler: 31 x 58 x 22 cm (w x d x h)

2.2 Weight

Measuring unit:

nNanoTec 39 kg net!

Supply units:

nWet dispersion unit 30.8 kg

nSmall volume wet dispersion unit SVA 35.8 kg

nSmall volume wet dispersion unit SVM 8 kg

nDry dispersion unit 25 kg

nFalling chute 24.6 kg

Accessories:

nAutoSampler 9.4 kg

2.3 Operang noise

The workplace-specic emission value is LpA<70 dB(A).

2.4 Voltage

Single phase alternang current 100-120 V / 200-240 V ± 10%.

2.5 Current consumpon

The maximum current consumpon is 0.2 A for the measuring unit and

0.4 A for the dispersion units.

Technical data

- 16 -

2.6 Power consumpon

The maximum power consumpon is 50 W (measuring unit), 100 W

(supply unit).

2.7 Electrical fuses

2 x 2 A fuses each in the measuring unit and dry dispersion unit;

2 x 4 A fuses in the wet dispersion unit.

2.8 Measuring ranges

ANALYSETTE 22 NanoTec

Wet dispersion: 0,01-2100 µm Dry dispersion: 0,1 - 2100 µm

Selectable measuring ranges:

0,01 - 45 µm / 15 - 2100 µm / 0,01 - 2100 µm

Technical data

- 17 -

3 Installaon

3.1 Transport

DANGER!

Do not step under the transport pallet during transport.

WARNING!

Improper liing can lead to personal injury or property

damage. The machine is only to be lied with suitable

equipment and by qualied personnel.

Fritsch laser parcle sizers are delivered in wooden cases on pallets. Do

not lt or stack these crates. The laser parcle sizers must be transported

and stored in their packaging and protected from weather and outside

inuences.

Transport over larger distances only in the original Fritsch packaging.

The guarantee excludes all claims for damage due to improper transport.

3.2 Unpacking

The measuring unit and a dispersion unit are packed

together in one box. If two or more supply units were

ordered these are packed in separate boxes. To remove

proceed as follows.

Please check the delivery against your order! If the delivery is incomplete

or damaged, inform the shipping agent immediately and inform FRITSCH

GmbH within 24 hours. Any claims received later cannot be considered.

Installaon

- 18 -

Only open the box with the arrows poinng upwards! Remove the trans-

port packaging as shown in the following illustraons.

1. Pull out the nails that fasten the upper lid and then remove the lid.

2. The accessory case is under the lid. Take out the case.

3. Remove the upper foam parts.

4.

NOTICE!

The upper handles are not transport handles but

are used to li out the measuring cell inseron.

Installaon

- 19 -

CAUTION!

Crushing hazard!

Always li with 2 persons.

5. Li the measuring unit and the dispersion unit out of the foam

mouldings with two persons as shown in the image.

Thanks to the grooves in the foam mouldings you

can hold the device by the base plate and li it

out.

Separately packed supply units are removed from the

box in the same way!

3.3 Seng up

The supply units of the ANALYSETTE 22 must be placed

directly beside the measuring unit.

Place the device indoors on a at, stable surface. It does not have to be

fastened to the surface.

Please avoid excessive heat build-up (from sunlight, heaters or similar), a

dusty environment and its eect on the interior of the measuring unit as

well as extreme humidity (>85%).

The permissible ambient temperature during operaon of the device is

10°C to 35°C. Storage is possible from 1°C to 40°C. If it is ancipated that

the temperature range e.g. for a scheduled transport is lower than the

permied range, the enre suspension circuit (dispersion unit, hoses and

measuring cell in the measuring unit) must be thoroughly rinsed rst

with pure ethanol and then the ushing liquid must be completely

removed.

Installaon

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Fritsch Laser Particle Sizer ANALYSETTE 22 NT Operating instructions

Fritsch Laser Particle Sizer ANALYSETTE 22 NT Operating instructions

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