Extraction and Scrubber Neutralization of Acid Fumes and Reaction Gases | Electromagnetic Interference | Sodium Hydroxide

B-414

Scrubber

Operation Manual

96701 en

Table of contents

Table of contents
1 About this manual . . . . . . . . . . . . . . . . . . . . . . 1.1 Reference documents . . . . . . . . . . . . . . . . . 1.2 Abbreviations . . . . . . . . . . . . . . . . . . . . . Safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.1 User qualification . . . . . . . . . . . . . . . . . . . 2.2 Proper use . . . . . . . . . . . . . . . . . . . . . . 2.3 Improper use . . . . . . . . . . . . . . . . . . . . . 2.4 Warning notices used in this manual . . . . . . . . . 2.5 Product safety. . . . . . . . . . . . . . . . . . . . . 2.5.1 Instrument-related hazards . . . . . . . . . . . . . . 2.5.2 Other hazards . . . . . . . . . . . . . . . . . . . . . 2.5.3 Safety measures . . . . . . . . . . . . . . . . . . . 2.5.4 Safety elements . . . . . . . . . . . . . . . . . . . . 2.6 General safety rules . . . . . . . . . . . . . . . . . . Technical data . . . . . . . . . . . . . . . . . . . . . . . . 3.1 Scope of delivery . . . . . . . . . . . . . . . . . . . 3.1.1 Standard instrument. . . . . . . . . . . . . . . . . . 3.1.2 Scrubber with condenser . . . . . . . . . . . . . . . 3.1.3 Scrubber with cold trap . . . . . . . . . . . . . . . . 3.1.4 Scrubber complete with condenser and reaction stage 3.1.5 Standard accessories . . . . . . . . . . . . . . . . . 3.1.6 Optional accessories . . . . . . . . . . . . . . . . . 3.1.7 Upgrade. . . . . . . . . . . . . . . . . . . . . . . . 3.2 Technical data overview . . . . . . . . . . . . . . . . 3.3 Materials used. . . . . . . . . . . . . . . . . . . . . 3.4 Recommended consumables . . . . . . . . . . . . . Description of function . . . . . . . . . . . . . . . . . . . 4.1 Functional principle of the Scrubber . . . . . . . . . . 4.2 Scrubber capacity. . . . . . . . . . . . . . . . . . . 4.3 Condenser . . . . . . . . . . . . . . . . . . . . . . 4.4 Cold trap . . . . . . . . . . . . . . . . . . . . . . . 4.5 External receiving vessel (option) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5 .5 .5 .6 .6 .6 .6 .7 .7 .7 .8 .8 .8 .9 10 10 10 10 11 11 12 12 13 13 13 14 15 15 16 17 17 18

2

3

4

Read this manual carefully before installing and running your system and note the safety precautions in chapter 2 in particular. Store the manual in the immediate vicinity of the instrument, so that it can be consulted at any time. No technical modifications may be made to the instrument without the prior written agreement of Buchi. Unauthorized modifications may affect the system safety or result in accidents. This manual is copyright. Information from it may not be reproduced, distributed, or used for competitive purposes, nor made available to third parties. The manufacture of any component with the aid of this manual without prior written agreement is also prohibited. If you need another language version of this manual, you can download it at www.buchi.com.

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B-414 Operation Manual, Version D

Table of contents

5

6

7

8 9

10

11

Putting into operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5.1 Installation site. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5.2 General commissioning procedure for all Scrubber models . . . . . . . . . . . 5.3 Commissioning the Scrubber with condenser / cold trap and reaction vessel . . 5.4 External receiving vessel (optional). . . . . . . . . . . . . . . . . . . . . . . . 5.5 Hose connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5.5.1 Hose connections of the basic model . . . . . . . . . . . . . . . . . . . . . . 5.5.2 Hose connections for Scrubber with condenser / cold trap . . . . . . . . . . . 5.5.3 Hose connections for Scrubber with condenser / cold trap and reaction vessel . 5.6 Electrical connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5.7 Preparing washing solutions. . . . . . . . . . . . . . . . . . . . . . . . . . . 5.7.1 Washing solutions for acidic vapors and gases . . . . . . . . . . . . . . . . . 5.7.2 Washing solutions for alkaline vapors and gases . . . . . . . . . . . . . . . . 5.7.3 Color indicator. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5.8 Filling up the prepared washing solution . . . . . . . . . . . . . . . . . . . . . Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6.1 Typical applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6.2 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7.1 Housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7.2 Glass parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7.3 Tubes / tube connectors . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7.4 Sealing system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7.4.1 Cleaning the seals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7.4.2 Replacing the seals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7.5 Washing insert . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7.6 Washing solution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7.7 Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7.8 Power supply fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7.9 Silencer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7.10 Functional test. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7.11 Customer service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8.1 Malfunctions and their remedy . . . . . . . . . . . . . . . . . . . . . . . . . Shutdown, storage, transport and disposal . . . . . . . . . . . . . . . . . . . . . 9.1 Storage and transport . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9.2 Disposal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Spare parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10.1 Spare parts on the exploded instrument view . . . . . . . . . . . . . . . . . . 10.2 Miscellaneous . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Declarations and requirements. . . . . . . . . . . . . . . . . . . . . . . . . . . . 11.1 FCC requirements (for USA and Canada) . . . . . . . . . . . . . . . . . . . . 11.2 Declaration of conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . .

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19 19 19 20 21 21 21 23 24 25 25 25 25 25 26 27 27 28 29 29 29 29 29 30 30 30 31 31 32 32 32 32 33 33 34 34 34 35 35 36 37 37 38

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B-414 Operation Manual, Version D

1

About this manual

1

About this manual
This manual describes the Scrubber and provides all information required for its safe operation and to maintain it in good working order. It is adressed to laboratory personnel in particular. NOTE The symbols pertaining to safety (WARNINGS and ATTENTIONS) are explained in chapter 2.

1.1

Reference documents
For information on the Digest System, the Digest Automat, and the Digest Unit, please refer to the corresponding manuals available in English, German, French, Italian and Spanish • • • • Digest System K-437, Operation Manual numbers 96760 - 96764 Digest Automat K-438, Operation Manual numbers 96765 - 96769 Digestion Unit K-424, Operation Manual numbers 96710 - 96714 Digestion Unit K-435, Operation Manual numbers 96720 - 96724

1.2

Abbreviations
CR: Chloroprene Rubber EPDM: Ethylene Propylene Dimonomer FEP: Fluorinated Ethylene Propylene FPM: Fluoroelastomer pa: pro analysis PA: Polyamides PMMA: Polymethylmethacrylate POM: Polyoxymethylene PP: Polypropylene PPS: Polyphenylenesulfide PTFE: Polytetrafluoroethylene (Teflon) PUR: Polyurethanes

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2

Safety

2

Safety
This chapter points out the safety concept of the instrument and contains general rules of behavior and warnings from hazards concerning the use of the product. The safety of users and personnel can only be ensured if these safety instructions and the safetyrelated warnings in the individual chapters are strictly observed and followed. Therefore, the manual must always be available to all persons performing the tasks described herein.

2.1

User qualification
The instrument may only be used by laboratory personnel and other persons who on account of training or professional experience have an overview of the dangers which can develop when operating the instrument. Personnel without this training or persons who are currently being trained require careful instruction. The present Operation Manual serves as the basis for this.

2.2

Proper use
The instrument has been designed and built for laboratories. It serves for the neutralization and adsorption of gases that arise during chemical reactions and syntheses. Only gases with known chemical composition may be drawn off.

2.3

Improper use
Applications not mentioned above are improper. Also, applications, which do not comply with the technical data, are considered improper. In particular no gases with unknown chemical composition may be drawn off. The operator bears the sole risk for any damages caused by such improper use. The following uses are expressly forbidden: • Use of the instrument in rooms which require ex-protected instruments. • Use on samples, which can explode or inflame (example: explosives, etc.) due to shock, friction, heat or spark formation. • Use in overpressure situations. • Drawing off liquids. • Drawing off solvents. • Drawing off vapors of organic solvents. • Use for cleaning of room air.

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Safety

2.4

Warning notices used in this manual
WARNING Generally, the triangular warning symbol indicates the possibility of personal injury or even loss of life if the instructions are not followed. WARNING Hot surface. WARNING Electrical hazard. WARNING Biohazard. ATTENTION With the general “Read this” symbol, ATTENTIONs indicate the possibility of equipment damage, malfunctions or incorrect process results, if instructions are not followed. NOTE Useful tips for the easy operation of the instrument.

2.5

Product safety
The Scrubber is designed and built in accordance with current state-of-the-art technology. Nevertheless, risks to users, property, and the environment can arise when the instrument is used carelessly or improperly. The manufacturer has determined residual dangers emanating from the instrument • if the instrument is operated by insufficiently trained personnel. • if the instrument is not operated according to its proper use. Appropriate warnings in this manual serve to make the user alert to these residual dangers.

2.5.1

Instrument-related hazards Pay attention to the following safety notices: WARNING Potential implosion risk if used with damaged glassware. • Beware of damaged or cracked glass parts. WARNING Potential explosion risk if solvent vapors accumulate within the instrument housing. • Always use the instrument in a well ventilated area. • Beware of damaged or cracked glass parts. • Beware of the fire hazard.

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2

Safety

2.5.2

Other hazards WARNING Certain solvents in or in the vicinity of the Scrubber can form peroxides and/or are highly inflammable. • Always be aware of the explosion risk when working with hazardous substances or with substances of unknown composition. • Always provide a good ventilation within or in the vicinity of the system. WARNING Risk of implosion when operating the instrument with an external pump and excess pressure on the overpressure valve. • Always operated the instrument with the build-in pump and do not use an external pump. WARNING Risk of acidic vapors forming in the vicinity of the instrument when the washing solution is not exchanged regularly. • Always use a color indicator to judge the state of the washing solution and exchange the solution as soon as the color indicator undergoes a color change.

2.5.3

Safety measures Always wear personal protective equipment such as protective eye goggles, protective clothing and gloves when working with the instrument.

2.5.4

Safety elements • Overpressure valve • The protective disc on top of the washing insert and the protective cover with the protective shield to be mounted at the neutralization vessel protects operators from broken glass and solvent splashes.

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2

Safety

2.6

General safety rules
Responsibility of the operator The head of laboratory is responsible for training his personnel. The operator shall inform the manufacturer without delay of any safety-related incidents which might occur during operation of the instrument. Legal regulations, such as local, state and federal laws applying to the instrument must be strictly followed. Duty of maintenance and care The operator is responsible for ensuring that the instrument is operated in proper condition only, and that maintenance, service, and repair jobs are performed with care and on schedule, and by authorized personnel only. Spare parts to be used Use only genuine consumables and genuine spare parts for maintenance to assure good system performance and reliability. Any modifications to the spare parts used are only allowed with the prior written permission of the manufacturer. Modifications Modifications to the instrument are only permitted after prior consultation with and with the written approval of the manufacturer. Modifications and upgrades shall only be carried out by an authorized Buchi technical engineer. The manufacturer will decline any claim resulting from unauthorized modifications.

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Technical data

3

Technical data
This chapter introduces the reader to the instrument specifications. It contains the scope of delivery, technical data, requirements and performance data.

3.1

Scope of delivery
Check the scope of delivery according to the order number. NOTE For detailed information on the listed products, see www.buchi.com or contact your local dealer.

3.1.1

Standard instrument Table 3-1: Standard instrument
Product Order number

B-414 Scrubber, standard 230 V / 50 Hz 120 V / 60 Hz 100 V / 50/60 Hz 1 adsorption vessel, complete 1 hose, adsorption / pump 3.1.2 Scrubber with condenser Table 3-2: Scrubber with condenser
Product Order number

37876 37877 37878 38128 37885

230 V / 50 Hz 120 V / 50 Hz 100 V / 60 Hz 1 condenser unit 3 tube connectors, bent with screw cap 1 silicone hose Ø 6/9 1 spring ring 1 holder ring for receiving vessel 1 seal for receiving vessel 1 receiving vessel 1.2 l 1 hose, condenser / lye 1 adsorption vessel, complete 1 hose, adsorption / pump

37882 37883 37884 37775 32885 04133 37872 36709 37873 37776 37888 38128 37885

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Technical data

3.1.3

Scrubber with cold trap Table 3-3: Scrubber with cold trap
Product Order number

230 V / 50 Hz 120 V / 50 Hz 100 V / 50/60 Hz 1 cold trap complete 3 tube connectors, bent with screw cap 1 receiving vessel 1.2 l 1 spring ring 1 holder ring for receiving vessel 1 seal for receiving vessel 1 hose, condenser / lye 1 adsorption vessel, complete 1 hose, adsorption / pump 3.1.4 Scrubber complete with condenser and reaction stage

37879 37880 37881 38083 32885 37776 37872 36709 37873 37888 38128 37885

Table 3-4: Scrubber complete with condenser and reaction stage
Product Order number

230 V / 50 Hz 120 V / 50 Hz 100 V / 50/60 Hz 1 condenser unit 1 silicone hose Ø 6/9 1 spring ring 1 holder ring for receiving vessel 1 seal for receiving vessel 1 receiving vessel 1.2 l 1 hose, condenser / lye 1 adsorption vessel, complete 1 hose, adsorption / reaction 1 reaction stage

37988 37989 37990 37775 04133 37872 36709 37873 37776 37888 38128 37887 37956

3 hose connections bent with screw caps 32885

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Technical data

3.1.5

Standard accessories Table 3-5: Standard accessories
Product Order number

1 neoprene hose 1 power cable Type CH Type Schuko / Japan Type GB Type USA Type AUS Operation Manual: English German French Italian Spanish 3.1.6 Optional accessories Table 3-6: Optional accessories
Product

10021 10010 10016 17835 33763 17836 96701 96700 96702 96703 96704

Order number

1 condenser unit 1 cold trap complete 1 condensate drain 1 reaction vessel 1 lip gasket, acid-resistant 1 hose, adsorption / pump 1 hose, reaction / pump 1 hose, adsorption / reaction 1 hose, condenser / washing solution 1 connection cable B-414 / Digestion Units, Control Unit Set large receiving vessel 4 l

37775 38083 37785 37797 38064 37885 37886 37887 37888 14738 48668

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Technical data

3.1.7

Upgrade Table 3-7: Upgrade possibilities
Product Order number

1 condenser with receiving vessel 1.2 l, complete Cold trap with receiving vessel 1.2 l, complete 1 reaction stage, complete

37954 37955 37956

3.2

Technical data overview
Table 3-8: Technical data
Scrubber Unit B-414

Dimensions (L x H x D) Weight Power system voltage / frequency

260 x 450 x 480 mm 13 kg 230 V ± 10 % / 50 Hz 120 V ± 10 % / 60 Hz 100 V ± 10 % / 50/60 Hz 140 W 100 W 100 W

Ambient temperature Pump suction capacity Overvoltage category Pollution degree Power consumption Current consumption (230 V)

For indoor use only, altitude up to 2000 m above seal level, maximum relative humidity 80 %, 5 - 40 °C 34 l/min II 2 200 W 1.5 A

3.3

Materials used
Table 3-9: Materials used
Component Material designation

Housing Minor hardware Lip gasket acid- / lye-resistant Gasket Protective disc Glass parts Pump Hoses

PUR PP, PA, POM FPM, EPDM PTFE, CR PMMA Borosilicate 3.3 PPS, CR, FPM CR, FEP

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Technical data

3.4

Recommended consumables
Table 3-10: Active charcoal for adsorption vessel
Product Order number Fluka / Merck

Fluka, purum p.a. 4 - 8 mm Merck, granulated Table 3-11: Color indicator for washing solution
Product

05110 102518

Order number Merck

Bromothymol blue, Merck

3026

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Description of function

4

Description of function
This chapter explains the basic principle of the instrument, shows how it is structured and gives a functional description of the assemblies. The pump draws off the gases and vapors produced in chemical reactions via a condenser or a cold trap providing a receiving vessel underneath. The condensation stage is used as a preliminary extractor for vapors, water steam (to prevent warming or an increase in volume of the washing solution) and for the liquids carried along with them, thus extending the service life of the neutralization stage. The acid or alkaline gases are washed and neutralized in the neutralization stage. The next stage, the adsorption stage, holds back most of the undesired particles by means of granules of activated charcoal or a universal adsorption granulate. It also enables the aerosols to recondensate. In the reaction stage that follows specific redox reactions are accomplished. The built-in overpressure valve makes sure that a certain pressure limit is not exceeded. The used air is directly lead into an exhaust or into the open air through a silencer.

4.1

Functional principle of the Scrubber

2 3

4

1 5

Receiving vessel Condenser (or cold trap) Reaction tubelet Fig. 4.1: Overview over the Scrubber

Adsorption vessel Neutralization vessel

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Description of function

Adsorption

4 1
PUMP

6 3 2 5

Condensation

Neutralisation

Reaction stage

Condenser or cold trap Receiving vessel Neutralization vessel with washing solution Fig. 4.2: Functional principle of the Scrubber

Adsorption vessel with adsorbents Reaction stage Fume exhaust pump

Condensation stage • Condensation of vapors • Condensation of water steam (prevention of warming or an increase in volume of the washing solution) • Condensation of the liquids carried along Neutralization stage • Neutralization of acid or alkaline gases Adsorption stage • Specific adsorptions and retention of particles (using granules of activated charcoal or a universal adsorption granulate) • Recondensation of aerosols Reaction stage • Specific reactions (e.g., redox reactions)

4.2

Scrubber capacity
The suction capacity of the Scrubber B-414 is designed for Digestion Units with a maximum of 20 sample tubes. Connection examples: • • • • Connection of up to two Digestion Units K-424 (6 places each) Connection of one Digestion Unit K-435 (12 places) Connection of one Digest Automat K-438 (20 places) Connection of one Digest System K-437 (20 places)

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Description of function

4.3

Condenser

3

2

1

4

Cooling water out Connection to neutralization stage Fig. 4.3: Connections of the condenser

Emission in (connection to emission source) Cooling water in

4.4

Cold trap

2 1

Emission in (connection to emission source) Fig. 4.4: Connections of the cold trap

Connection to neutralization stage

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Description of function

4.5

External receiving vessel (option)
A large receiving vessel for up to 4 l is optionally available. It serves for the digestion of high volumes of water samples.

Fig. 4.5: External receiving vessel

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Putting into operation

5

Putting into operation
This chapter describes how the instrument is installed and gives instructions on initial startup. NOTE Inspect the instrument for damages during unpacking. If necessary, prepare a status report immediately to inform the postal company, railway company or transportation company. Remove the transprotation lock at the bottom of the instrument. Keep the original packaging for future transportation.

5.1

Installation site
Install the instrument on a clean, flat and stable base. ATTENTION To ensure the instrument safety do not place any object on top of it. ATTENTION Place the Scrubber B-414 on the left side of a digestion unit (e.g. Digestion Unit K-424, K-435, Digest System K-437 or Digest Automat K438). The Scrubber ventilation is located on the left side. In case the Scrubber is placed on the right side of another unit, cool air will hit the digestion sample and cool it down, so that no digestion can take place.

5.2

General commissioning procedure for all Scrubber models
To commission the Scrubber B-414, proceed as follows: • Apply the protective cover and shield to the neutralization vessel. • Make sure that the silencer is filled with cotton wool and install it. • Check the glass for flaws and cracks. • Check the seals and gaskets (embrittlement, scratches). If they are not OK, take them out and replace them (see also chapter 7). • Carefully insert the glass parts using a clamping ring (without pressure from above). Otherwise there is a risk of damaging the glassware. NOTE When you carry out Kjeldahl digestions, the suction capacity might become too high. Therefore we recommend to fill activated charcoal into the adsorption vessel and to add glass wool at both ends. The glass wool prevents charcoal from being drawn into the vacuum pump. The activated charcoal should be grainy with a particle size of 2 to 6 mm.

Fig. 5.1: Adsorption vessel with activated charcoal and glass wool

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Putting into operation

5.3

Commissioning the Scrubber with condenser / cold trap and reaction vessel
To prepare the complete Scrubber model for operation, proceed as follows: • Insert the white PTFE gasket into the holder ring for the receiving vessel, so that it fits properly into it on both sides. • Press the holder ring into the gap provided for condenser / cold trap and receiving vessel. • Apply the spring ring to the bottom of the condenser / cold trap (the cooling water / contaminated air inlet must be at the bottom) and introduce the condenser into the holder ring. • Screw the receiving vessel counterclockwise into the holder ring underneath the condenser. Spring ring Holder ring Gasket PTFE

3

1 2

Fig.5.2: Connection between condenser and receiving vessel

• Insert the reaction vessel into the housing from below. • Insert the introduction tube of the reaction tubelet into the reaction vessel and screw it in tightly.

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Putting into operation

5.4

External receiving vessel (optional)
To commission the optional external receiving vessel, proceed as follows: • Connect the one end of the adapter (FEP hose) to the bottom of the condenser. • Connect other side of the adapter to the external receiving vessel and fasten the connection with the black screw caps.

Fig.5.3: Connecting the external receiving vessel

ATTENTION Do not use plastic tanks for the collection of condensate but only original glass vessels from Buchi. • The diameter of the connection between the outlet and the receiving vessel must not be less than 10 mm. • The materials used must be resistant to the condensate and must withstand a vacuum of 100 mbar.

5.5

Hose connections
NOTE Use clips and cable ties where necessary to secure the cables in place.

5.5.1

Hose connections of the basic model The basic model consists of the neutralization and the adsorption vessel. To establish the hose connections, proceed as follows: • Connect the adsorption vessel to the distribution head and secure with tube connectors GL-14 at both ends. • Connect the emission source via a Woulff bottle to the neutralization vessel.

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Putting into operation

3 2

1

4 5
Neutralization stage Connection of the neutralization vessel Adsorption vessel Fig. 5.4: Hose connections of the basic model Distribution head Silencer

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Putting into operation

5.5.2

Hose connections for Scrubber with condenser / cold trap To establish the hose connections, proceed as follows: • • • • Put tube connectors GL-14 on all PTFE hoses. Connect the emission source to the condenser / cold trap inlet (position in Fig. 5.2 ). Connect the condenser / cold trap outlet (position in Fig. 5.2) to the neutralization vessel. Connect the adsorption vessel to the distribution head.

2

1

10 3

6

7

9 8

4 5
Neutralization stage Adsorption vessel Reaction stage Distribution head Silencer Inlet from emission source Outlet to neutralization vessel Cooling water inlet (bottom) Cooling water outlet (top) Condenser

Fig. 5.5: Hose connections for Scrubber with condenser / cold trap

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Putting into operation

5.5.3

Hose connections for Scrubber with condenser / cold trap and reaction vessel To establish the hose connections, proceed as follows: • • • • • Put tube connectors GL-14 on all PTFE hoses. Connect the emission source to the condenser / cold trap inlet (position in Fig. 5.3 ). Connect the condenser / cold trap outlet (position in Fig. 5.3) to the neutralization vessel. Connect the adsorption vessel to the top of the reaction tubelet. Connect the reaction tubelet (connection at the front) to the distribution head

2

1

10

3 6

7

9 8

4 5
Neutralization stage Adsorption vessel Reaction stage Distribution head Silencer Inlet from emission source Outlet to neutralization vessel Cooling water inlet (bottom) Cooling water outlet (top) Condenser

Fig. 5.6: Hose connections for Scrubber with condenser / cold trap and reaction vessel

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Putting into operation

5.6

Electrical connections
ATTENTION Make sure that the voltage on the socket corresponds to the voltage given on the type plate of the instrument. Always connect the instrument to an earthed socket. External connections and extension cables must be provided with an earthed conductor lead (3-pole couplings, cable or plug equipment) as the mains lead has a molded plug, thus avoiding risks due to inadvertent defective wiring. Make sure that no electric sparks form in the instrument or its surroundings as they might damage the instrument. Connect the Scubber B-414 to the mains with the power cord contained in the scope of delivery. To start the Scrubber automatically at the same time the digestion process starts, connect it to the Control Unit B-436, to a Digest System K-437 or to a Digest Automat K-438 with the optional connection cable.

5.7

Preparing washing solutions
ATTENTION Always wear personal protective equipment such as protective eye goggles, protective clothing and gloves when working with washing solutions.

5.7.1

Washing solutions for acidic vapors and gases • Sodium hydroxide 8-10 %, max. 20 % • Sodium carbonate – dissolve 600 g Na2CO3 in 3 l distilled warm water, or – dissolve 1.7 kg Na2CO3 · 10H2O in 3 l distilled warm water

5.7.2

Washing solutions for alkaline vapors and gases • Hydrochloric acid, max. 15% • Sulphuric acid, max. 20% Depending on the area of application, it is recommended to use different washing solutions or concentrations. The B-414 Scrubber is supplied ex works with a lye-resistant lip gasket. For operating with acid washing solutions, an acid-resistant lip gasket should be used.

5.7.3

Color indicator A color indicator is added to the washing solution to assess its washing power visually as well. We recommend to use 100 mg of color indicator for 3 l of washing solution. Bromothymol blue serves as a standard indicator. The transition area here is between pH 6.0 to 7.6. Thus the fresh solution has a blue color while the neutralized or acidic solution has an orange yellowish color. Depending on the application purpose, other suitable color indicators should be used.

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Putting into operation

5.8

Filling up the prepared washing solution
To fill up the washing solution, proceed as follows: • • • • • Remove the adsorption vessel by gently pulling it upwards. Loosen the tube connector GL-14 at the neutralization vessel and pull off the hose. Remove the protective cover with the protective shield. Remove the protective disc with the washing insert from the neutralization vessel. Carefully pour the washing solution into the washing vessel and fill up to the wavy maximum filling mark. • Reassemble the instrument in the reverse order.

1

2 3

5 4

Adsorption vessel Nut GL-14 Protective cover with protective shield Fig. 5.7: Filling up the washing solution

Washing insert ON/OFF switch

NOTE For information on how and when to exchange the washing solution, see chapter 7.6

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6

Operation

6

Operation
This chapter gives examples of typical instrument applications and instructions on how to operate the instrument properly and safely. WARNING Risk of injury. • Never operate the instrument when glassware is damaged. ATTENTION Switch on the B-414 before a connected instrument produces gases.

6.1

Typical applications
Table 6-1: Typical applications
Gases and vapors Chemical formula Neutralization (stage 2) Specific reactins (stage 4)

Kjeldahl digestions Sulfur dioxide Sulfuryl chloride Hydrochloric or hydrobromic acids Thionyl chloride Cyanuric chloride Carbonic acid chloride Phosgene Ammonia Nitrous oxides (nitrous gases) Nitric acid / aqua regia Chlorine, bromine, iodine Thiophenols Thioalcohols, mercaptan Hydrogen sulphide Carbon disulphide Prussic acid

SO2, H2SO4 SO2 SO2Cl2 HCI, HBr SOCl2 C3N3Cl3 R-COCI COCI2 NH3 NOX

saturated soda / NaOH 8 - 10 % (max. 20 %) saturated soda / NaOH 8 - 10 % (max. 20 %) NaOH 8 - 10 % (max. 20 %) NaOH 8 - 10 % (max. 20 %) NaOH 8 - 10 % (max. 20 %) NaOH 8 - 10 % (max. 20 %) NaOH 8 - 10 % (max. 20 %) NaOH 8 - 10 % (max. 20 %) HCI max. 15 % / H2SO4 max. 20 % NaOH 20 % FESO4 saturated

Cl2, Br2, J2 Ar-SH R-SH H 2S CS2 HCN

NaOH 8 - 10 % (max. 20 %) NaOH 8 - 10 % (max. 20 %) NaOH / javelle water NaOH 8 - 10 % (max. 20 %) NaOH 8 - 10 % (max. 20 %) NaOH 8 - 10 % (max. 20 %)

FESO4 saturated KMnO4 saturated KMnO4 saturated KMnO4 saturated KMnO4 saturated KMnO4 saturated

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6

Operation

6.2

Operation
• Switch on the power switch . • Make sure that the cooling water flow rate does not exceed 60 l/h. • The suction performance can be regulated during operation by drilling a 0.1 - 0.3 mm wide hole in the screw cap GL-14 (e.g. when samples are getting dry). • Carry out a functional test as described in chapter 7.10.

2

1
Fig. 6.1.: Operation

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7

Maintenance and repairs

7

Maintenance
This chapter gives instructions on all maintenance work to be performed in order to keep the instrument in good working condition. WARNING Electrical hazard: • Prior to all maintenance work on the instrument switch off the power supply and remove all sources of flammable vapor. ATTENTION Always wear personal protective equipment such as protective eye goggles, protective clothing and gloves when maintaining the instrument.

7.1

Housing
Check the housing for defects (switches, plugs) and clean it regularly with a damp cloth. ATTENTION Never use solvents as cleaning agents as these might damage the instrument.

7.2

Glass parts
The glass parts can be taken out and cleaned with commercially available cleaning agents or in an ultrasonic bath. After the glass parts have been cleaned and fully dried, check each part visually for cracks, scratches and for any parts or sections that might have splintered off. Take out and replace any damaged glass parts.

7.3

Tubes / tube connectors
Visually examine the tube connections regularly. When tubes become cracked and brittle, replace them with new tubes. Grease all joints on the condenser side regularly to achieve optimum tightness of the system. Flush out the tubes regularly with water or ethanol.

7.4

Sealing system
ATTENTION When removing and reinstalling the seals and gaskets, make sure not to damage them. Always move them perpendicularly to the axis of the glass parts and ensure no damage occurs to the sealing lip. Never apply grease to the seals and never touch them with sharp object, otherwise they will get damaged.

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7

Maintenance and repairs

7.4.1

Cleaning the seals To prolong the lifetime of the seals, rinse them regularly with water, especially if working with crystalline products. Afterwards, dry them with a solft cloth. To remove the seals, see Fig. 7.1.

7.4.2

Replacing the seals Seals are subject to wear and tear, thus you should check them regularly and replace them, if necessary, e.g. if they do not pass the functional test described in chapter 7.8 anymore. We recommend to replace the seals as follows: Table 8-1: General malfunction and their remedy
Position in Fig. 9.1 Order no. Description Replacing interval

-8 13 17 19 23 34 38

40029 37928 03575 03576 38225 37873 37925 37871

Set of seals EPDM for tube connectors O-ring to adapter (37777) Gasket SVL 42 x 30 PTFE Gasket SVL 22 x 16 PTFE Hose seal Seal for receiving vessel Gasket ring Silencer unit

once a year once a year once a year once a year once a year once a year once a year once a year

7.5

Washing insert
The washing insert must be cleaned from time to time and the lip gasket must be replaced when brittle.

6

7

5 4

2 3

2 1
Nut M20 Swirl disc Spacer tube Swirl disc holder Fig. 7.1. Exploded view of the washing insert Lip gasket Protective disc Tube connector adapter M20 GL-14

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Maintenance and repairs

To (re)assemble the washing insert, proceed as follows: • • • • • • • • • • Insert the lip gasket into the protective disc . Place the protective disc on the swirl disc holder . Screw on the adapter and tighten it. Insert the first swirl disc . Insert the spacer tube . Insert the second swirl disc . Screw the washing insert into the adapter . Introduce the washing insert into the neutralisation vessel. Put on the protective disc. Put on the protective cover with shield and center the neutralization vessel.

7.6

Washing solution
Used washing solutions may impair the functionality of the B-414 Scrubber especially in the range of the neutralization point as a result of strong foaming. Changing the washing solution in appropriate time (when the color indicator ongoes a color change) keeps the adsorption stage and/or reaction stage from getting soiled and prevents the possibility of the pump getting damaged. For a discription of how to prepare and fill up the washing solution, see chapter 5.7. NOTE Make sure to dispose of the used washing solution according to your laboratory guidelines.

7.7

Pump
To flush the pump, proceed as follows: and flush out the • Take off the silencer pump with distilled water through the secondary air valve . • Switch on the instrument and collect the waste water in a suitable vessel .

2

1

4

3

Fig. 7.2: Flushing the pump

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Maintenance and repairs

7.8

Power supply fuses
To replace the power supply fuses, proceed as follows: • Pull out the power supply cable. • Remove the fuse holder . • Replace the defective fuse with a new fuse of the same type: – 100 V: T 2.0 A L 250 V – 120 V: T 1 A L 250 V – 230 V: T 1 A L 250 V • Put the fuse holder back.

2 1

Fig. 7.3: Replacing the power supply fuses

7.9

Silencer
Replace the silencer once a year.

7.10

Functional test
To check whether the overpressure valve functions properly, screw off the left tube connector at the distribution head and put a finger on the opening. After the overpressure valve has switched, a change of sound is audible. The system is tight, when the washing solution in the neutralization vessel bubbles when the instrument is switched on.

7.11

Customer service
Only authorised service personnel are allowed to perform repair work on the instrument. These persons have a comprehensive technical training and knowledge of possible dangers which might arise from the instrument. Addresses of official Buchi customer service offices are given on the Buchi website under: www.buchi.com. If malfunctions occur on your instrument or you have technical questions or application problems, contact one of these offices. The customer service offers the following: • Spare part delivery • Repairs • Technical advice

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8

Troubleshooting

8

Troubleshooting
This chapter helps to resume operation after a minor problem has occurred with the instrument. It lists possible occurrences, their probable cause and suggests how to remedy the problem. The troubleshooting table below lists possible malfunctions and errors of the instrument. The operator is enabled to correct some of those problems or errors by him/herself. For this, appropriate corrective measures are listed in the column “Corrective measure”. The elimination of more complicated malfunctions or errors is usually performed by a Buchi technical engineer who has access to the official service manuals. In this case, please refer to your local Buchi customer service agent.

8.1

Malfunctions and their remedy
Table 8-1: General malfunction and their remedy
Malfunction Possible cause Corrective measure

B-414 does not work

No mains connection Fuses defective Mains switch defective

Check whether the instrument is connected to the mains Replace the defective fuses Contact the Buchi customer service Contact the Buchi customer service Tighten the tube connections Check the hoses Check the adsorption vessel Exchange the washing solution Renew the adsorbents Clean the pump Replace the silencer unit Contact the Buchi customer service Check all stages and the connected digestion unit as well Exchange the adsorbents Replace the silencer unit Contact the Buchi customer service Exchange the washing solution

Pump does not work

Wiring defective Pump defective

Fumes are not exhausted during Suction system leaking extraction (Scrubber suction capacity Hose bent too weak) Adsorption vessel clogged Washing solution dirty Adsorbents clogged Pump dirty Silencer unit clogged Overpressure valve dirty Fumes are exhausted too fast during Suction system clogged extraction (Scrubber suction capacity too strong) Adsorbents clogged Silencer unit defective Overpressure valve defective Washing solution turns yellow Washing solution dirty

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9

Shutdown, storage, transport and disposal

9

Shutdown, storage, transport and disposal
This chapter instructs how to shut down the instrument, how to pack it for storage or transport, and specifies the storage and shipping conditions.

9.1

Storage and transport
WARNING Biohazard: • Remove all dangerous substances from the instrument and clean it thoroughly. Store and transport the instrument in its original packaging.

9.2

Disposal
To dispose of the instrument in an environmentally friendly manner, a list of materials is given in chapter 3. This helps to ensure that the components are separated and recycled correctly. Make especially sure to dispose of the gas springs appropriately. Please follow valid regional and local laws concerning disposal.

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10

Spare parts

10

Spare parts
This chapter lists spare parts, accessories, and options including their ordering information. Order the spare parts from Buchi. Always state the product designation and the part number when ordering spare parts. Use only genuine Buchi consumables and genuine spare parts for maintenance and repair to assure good system performance and reliability. Any modifications to the spare parts used are only allowed with the prior written permission of the manufacturer.

10.1

Spare parts on the exploded instrument view

29

21

26

28 23 30 27

22 24

18 19 17 12 9

20

35 36

25 37 14 16 6

13 15

38

11 10 9

39 7 8

31

33 5 4 3 34

32 2

1

Fig. 10.1: Spare parts on the exploded instrument view

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Spare parts

Table 10-1: Spare parts on the exploded instrument view
Position Product Order number Position Product Order number

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19

Protective shield Neutralization vessel Lip gasket lye-resistant EPDM Lip gasket acid-resistant FPM Swirl disc Set of 4 tube connectors with cap bent FPM Adapter for GL-14 O-ring to adapter (37777) Screw cap GL-14 (set of 10) Set of seals EPDM for tube connectors (set of 10) Hose seal Screw cap GL-14 Adsorption vessel Gasket SVL 42 x 30 PTFE Adapter complete for adsorption vessel O-ring 47.2 for adsorption vessel O-ring 39.7 for adsorption vessel Gasket SVL 22 x 16 PTFE Adapter SVL 22 / GL14, complete Seal for FEP tube

37820 37786 37874 38064 37821 40295 37777 37928 41956 40029 38225 40624 37774 03575 37971 37857 38068 03576 37972 38225

20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39

Hose adsorption / pump Condenser complete, including: - Spring ring - Gasket - Holder ring Receiving vessel, 1.2 l

37885 38022 37872 37873 36709 37776

Hose condenser / washing solution 37888 Cold trap O-ring FPM for cold trap Trap unit for cold trap Connector GL-14 straight Introduction tube assembly Reaction vessel, 1.0 l Screw cap SVL 42 Gasket ring Hose adsorption / reaction Hose reaction / pump Condensate drain Silencer unit Distribution head, complete 37781 38067 37782 37642 37778 37797 03551 37925 37887 37886 37785 37871 37952

10.2

Miscellaneous
Table 10-2: Miscellaneous
Product Order number

Set of sealings FPM (10 pieces) Axial flow fan B-414

40040 38026

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Declarations and requirements

11

Declarations and requirements

11.1

FCC requirements (for USA and Canada)
English: This equipment has been tested and found to comply with the limits for a Class A digital device, pursuant to both Part 15 of the FCC Rules and the radio interference regulations of the Canadian Department of Communications. These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment. This equipment generates, uses and can radiate radio frequency energy and, if not installed and used in accordance with the instruction manual, may cause harmful interference to radio communications. Operation of this equipment in a residential area is likely to cause harmful interference in which case the user will be required to correct the interference at his own expense. Français: Cet appareil a été testé et s'est avéré conforme aux limites prévues pour les appareils numériques de classe A et à la partie 15 des réglementations FCC ainsi qu’à la réglementation des interférences radio du Canadian Department of Communications. Ces limites sont destinées à fournir une protection adéquate contre les interférences néfastes lorsque l’appareil est utilisé dans un environnement commercial. Cet appareil génère, utilise et peut irradier une énergie à fréquence radioélectrique, il est en outre susceptible d’engendrer des interférences avec les communications radio, s’il n’est pas installé et utilisé conformément aux instructions du mode d’emploi. L’utilisation de cet appareil dans les zones résidentielles peut causer des interférences néfastes, auquel cas l’exploitant sera amené à prendre les dispositions utiles pour palier aux interférences à ses propres frais.

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Declarations and requirements

11.2

Declaration of conformity
We BÜCHI Labortechnik AG do hereby declare on our responsibility that the product: Scrubber B-414 which is the object of this certification, is in accordance with the following norms: EN 61010-1:2001 (~ IEC 61010-1) Safety requirements for electrical equipment for measurement, control, and laboratory use Part 1: General requirements EN 55011:1998 + A1:1999 (IEC/CISPR 11:1997, modified + A1:1999) Industrial, scientific and medical (ISM) radio-frequency equipment - Radio disturbance characteristics - Limits and methods of measurement EN 60335-1:2002: Household and similar electrical appliances - Safety Part 1: General requirements EN 6100-3-2:2000 Limits for harmonic current emissions EN 6100-3-3:2000 Limitations of voltage fluctuations and flicker In accordance with the regulations of the EU guidelines 73/23/EEC (electrical operating equipment/low-voltage guidelines) 89/336/EEC (electromagnetic compatibility) Flawil, 12.01.06 BÜCHI Labortechnik AG Meierseggstrasse 40 Postfach CH-9230 Flawil 1 Switzerland Tel.: +41 (0)71 394 63 63 Fax: +41 (0)71 394 65 65 buchi@buchi.com www.buchi.com

Guido Worch Quality Manager

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B-414 Operation Manual, Version D

BÜCHI Labortechnik AG CH-9230 Flawil 1 / Switzerland T +41 71 394 63 63 F +41 71 394 65 65

096701

www.buchi.com

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