extraction and scrubber neutralization of acid fumes and reaction gases

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B-414 Scrubber Operation Manual 96701 en

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Scrubber Extraction and neutralization of acid fumes and reaction gases

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B-414ScrubberOperation Manual

96701 en

Table of contents

3 B-414 Operation Manual, Version D

Table of contents

1 About this manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51.1 Reference documents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51.2 Abbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

2 Safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62.1 User qualifi cation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62.2 Proper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62.3 Improper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62.4 Warning notices used in this manual . . . . . . . . . . . . . . . . . . . . . . . . . . 72.5 Product safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72.5.1 Instrument-related hazards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72.5.2 Other hazards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82.5.3 Safety measures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82.5.4 Safety elements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82.6 General safety rules . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

3 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103.1 Scope of delivery . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103.1.1 Standard instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103.1.2 Scrubber with condenser . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103.1.3 Scrubber with cold trap . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 113.1.4 Scrubber complete with condenser and reaction stage . . . . . . . . . . . . . . . . 113.1.5 Standard accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 123.1.6 Optional accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 123.1.7 Upgrade. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 133.2 Technical data overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 133.3 Materials used. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 133.4 Recommended consumables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

4 Description of function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 154.1 Functional principle of the Scrubber . . . . . . . . . . . . . . . . . . . . . . . . . . 154.2 Scrubber capacity. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 164.3 Condenser . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 174.4 Cold trap . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 174.5 External receiving vessel (option) . . . . . . . . . . . . . . . . . . . . . . . . . . . 18

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 modifi cations may be made to the instrument without the prior written agreement of Buchi. Unauthorized modifi cations may affect the system safety or result in accidents. This manual is copyright. Information from it may not be reproduced, distributed, or used for competi-tive 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.

Table of contents

4 B-414 Operation Manual, Version D

5 Putting into operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 195.1 Installation site. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 195.2 General commissioning procedure for all Scrubber models . . . . . . . . . . . . . . 195.3 Commissioning the Scrubber with condenser / cold trap and reaction vessel . . . . . 205.4 External receiving vessel (optional). . . . . . . . . . . . . . . . . . . . . . . . . . . 215.5 Hose connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 215.5.1 Hose connections of the basic model . . . . . . . . . . . . . . . . . . . . . . . . . 215.5.2 Hose connections for Scrubber with condenser / cold trap . . . . . . . . . . . . . . 235.5.3 Hose connections for Scrubber with condenser / cold trap and reaction vessel . . . . 245.6 Electrical connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 255.7 Preparing washing solutions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 255.7.1 Washing solutions for acidic vapors and gases . . . . . . . . . . . . . . . . . . . . 255.7.2 Washing solutions for alkaline vapors and gases . . . . . . . . . . . . . . . . . . . 255.7.3 Color indicator. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 255.8 Filling up the prepared washing solution . . . . . . . . . . . . . . . . . . . . . . . . 26

6 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 276.1 Typical applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 276.2 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

7 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 297.1 Housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 297.2 Glass parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 297.3 Tubes / tube connectors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 297.4 Sealing system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 297.4.1 Cleaning the seals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 307.4.2 Replacing the seals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 307.5 Washing insert . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 307.6 Washing solution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 317.7 Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 317.8 Power supply fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 327.9 Silencer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 327.10 Functional test. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 327.11 Customer service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32

8 Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 338.1 Malfunctions and their remedy . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33

9 Shutdown, storage, transport and disposal . . . . . . . . . . . . . . . . . . . . . . . . 349.1 Storage and transport . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 349.2 Disposal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34

10 Spare parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3510.1 Spare parts on the exploded instrument view . . . . . . . . . . . . . . . . . . . . . 3510.2 Miscellaneous . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36

11 Declarations and requirements. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3711.1 FCC requirements (for USA and Canada) . . . . . . . . . . . . . . . . . . . . . . . 3711.2 Declaration of conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38

1 About this manual

5 B-414 Operation Manual, Version D

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.

NOTEThe 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 - 96764Digest Automat K-438, Operation Manual numbers 96765 - 96769Digestion Unit K-424, Operation Manual numbers 96710 - 96714Digestion Unit K-435, Operation Manual numbers 96720 - 96724

1.2 Abbreviations

CR: Chloroprene Rubber EPDM: Ethylene Propylene DimonomerFEP: Fluorinated Ethylene Propylene FPM: Fluoroelastomer pa: pro analysisPA: Polyamides PMMA: PolymethylmethacrylatePOM: PolyoxymethylenePP: Polypropylene PPS: Polyphenylenesulfi de PTFE: Polytetrafl uoroethylene (Tefl on)PUR: Polyurethanes

••••

2 Safety

6 B-414 Operation Manual, Version D

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 safety-related 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 qualifi cation

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 infl ame (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.

••

•••••

2 Safety

7 B-414 Operation Manual, Version D

2.4 Warning notices used in this manual

WARNINGGenerally, the triangular warning symbol indicates the possibility of personal injury or even loss of life if the instructions are not followed.

WARNINGHot surface.

WARNINGElectrical hazard.

WARNINGBiohazard.

ATTENTIONWith the general “Read this” symbol, ATTENTIONs indicate the possibility of equipment damage, malfunctions or incorrect process results, if instructions are not followed.

NOTEUseful 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. Neverthe-less, 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 insuffi ciently 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:

WARNINGPotential implosion risk if used with damaged glassware.

Beware of damaged or cracked glass parts.

WARNINGPotential 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 fi re hazard.

••

•••

2 Safety

8 B-414 Operation Manual, Version D

2.5.2 Other hazards

WARNINGCertain solvents in or in the vicinity of the Scrubber can form peroxides and/or are highly infl am-mable.

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.

WARNINGRisk 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.

WARNINGRisk 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.

••

2 Safety

9 B-414 Operation Manual, Version D

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 autho-rized 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 modifi cations to the spare parts used are only allowed with the prior written permission of the manufacturer.

Modifi cations

Modifi cations to the instrument are only permitted after prior consultation with and with the written approval of the manufacturer. Modifi cations and upgrades shall only be carried out by an authorized Buchi technical engineer. The manufacturer will decline any claim resulting from unauthorized modifi -cations.

3 Technical data

10 B-414 Operation Manual, Version D

3 Technical data

This chapter introduces the reader to the instrument specifi cations. 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.

NOTEFor detailed information on the listed products, see www.buchi.com or contact your local dealer.

3.1.1 Standard instrument

Table 3-1: Standard instrumentProduct Order number

B-414 Scrubber, standard

230 V / 50 Hz 37876

120 V / 60 Hz 37877

100 V / 50/60 Hz 37878

1 adsorption vessel, complete 38128

1 hose, adsorption / pump 37885

3.1.2 Scrubber with condenser

Table 3-2: Scrubber with condenserProduct Order number

230 V / 50 Hz 37882

120 V / 50 Hz 37883

100 V / 60 Hz 37884

1 condenser unit 37775

3 tube connectors, bent with screw cap 32885

1 silicone hose Ø 6/9 04133

1 spring ring 37872

1 holder ring for receiving vessel 36709

1 seal for receiving vessel 37873

1 receiving vessel 1.2 l 37776

1 hose, condenser / lye 37888

1 adsorption vessel, complete 38128

1 hose, adsorption / pump 37885

3 Technical data

11 B-414 Operation Manual, Version D

3.1.3 Scrubber with cold trap

Table 3-3: Scrubber with cold trapProduct Order number

230 V / 50 Hz 37879

120 V / 50 Hz 37880

100 V / 50/60 Hz 37881

1 cold trap complete 38083

3 tube connectors, bent with screw cap 32885

1 receiving vessel 1.2 l 37776

1 spring ring 37872

1 holder ring for receiving vessel 36709

1 seal for receiving vessel 37873

1 hose, condenser / lye 37888

1 adsorption vessel, complete 38128

1 hose, adsorption / pump 37885

3.1.4 Scrubber complete with condenser and reaction stage

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

230 V / 50 Hz 37988

120 V / 50 Hz 37989

100 V / 50/60 Hz 37990

1 condenser unit 37775

3 hose connections bent with screw caps 32885

1 silicone hose Ø 6/9 04133

1 spring ring 37872

1 holder ring for receiving vessel 36709

1 seal for receiving vessel 37873

1 receiving vessel 1.2 l 37776

1 hose, condenser / lye 37888

1 adsorption vessel, complete 38128

1 hose, adsorption / reaction 37887

1 reaction stage 37956

3 Technical data

12 B-414 Operation Manual, Version D

3.1.5 Standard accessories

Table 3-5: Standard accessoriesProduct Order number

1 neoprene hose 10021

1 power cable

Type CH 10010

Type Schuko / Japan 10016

Type GB 17835

Type USA 33763

Type AUS 17836

Operation Manual:

English 96701

German 96700

French 96702

Italian 96703

Spanish 96704

3.1.6 Optional accessories

Table 3-6: Optional accessoriesProduct Order number

1 condenser unit 37775

1 cold trap complete 38083

1 condensate drain 37785

1 reaction vessel 37797

1 lip gasket, acid-resistant 38064

1 hose, adsorption / pump 37885

1 hose, reaction / pump 37886

1 hose, adsorption / reaction 37887

1 hose, condenser / washing solution 37888

1 connection cable B-414 / Digestion Units, Control Unit

14738

Set large receiving vessel 4 l 48668

3 Technical data

13 B-414 Operation Manual, Version D

3.1.7 Upgrade

Table 3-7: Upgrade possibilitiesProduct Order number

1 condenser with receiving vessel 1.2 l, complete

37954

Cold trap with receiving vessel 1.2 l, complete

37955

1 reaction stage, complete 37956

3.2 Technical data overview

Table 3-8: Technical dataScrubber Unit B-414

Dimensions (L x H x D) 260 x 450 x 480 mm

Weight 13 kg

Power system voltage / frequency 230 V ± 10 % / 50 Hz 120 V ± 10 % / 60 Hz 100 V ± 10 % / 50/60 Hz

140 W100 W100 W

Ambient temperature For indoor use only, altitude up to 2000 m above seal level, maximum relative humidity 80 %, 5 - 40 °C

Pump suction capacity 34 l/min

Overvoltage category II

Pollution degree 2

Power consumption 200 W

Current consumption (230 V) 1.5 A

3.3 Materials used

Table 3-9: Materials usedComponent Material designation

Housing PUR

Minor hardware PP, PA, POM

Lip gasket acid- / lye-resistant FPM, EPDM

Gasket PTFE, CR

Protective disc PMMA

Glass parts Borosilicate 3.3

Pump PPS, CR, FPM

Hoses CR, FEP

3 Technical data

14 B-414 Operation Manual, Version D

3.4 Recommended consumables

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

Fluka, purum p.a. 4 - 8 mm 05110

Merck, granulated 102518

Table 3-11: Color indicator for washing solutionProduct Order number Merck

Bromothymol blue, Merck 3026

4 Description of function

15 B-414 Operation Manual, Version D

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 neutraliza tion 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 specifi c 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

24

3

1

5

� Receiving vessel� Condenser (or cold trap)� Reaction tubelet

� Adsorption vessel� Neutralization vessel

Fig. 4.1: Overview over the Scrubber

4 Description of function

16 B-414 Operation Manual, Version D

P U M P

Reaction stageNeutralisation

Adsorption

Condensation

1

2

3

4

5

6

� Condenser or cold trap� Receiving vessel� Neutralization vessel with washing solution

� Adsorption vessel with adsorbents� Reaction stage� Fume exhaust pump

Fig. 4.2: Functional principle of the Scrubber

Condensation stage

Condensation of vapors Condensation of water steam (prevention of warming or an increase in volume of the washing solu-tion)Condensation of the liquids carried along

Neutralization stage

Neutralization of acid or alkaline gases

Adsorption stage

Specifi c adsorptions and retention of particles (using granules of activated charcoal or a universal adsorption granulate)Recondensation of aerosols

Reaction stage

Specifi c 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)

••

••••

4 Description of function

17 B-414 Operation Manual, Version D

4.3 Condenser

123

4

� Cooling water out� Connection to neutralization stage

� Emission in (connection to emission source)� Cooling water in

Fig. 4.3: Connections of the condenser

4.4 Cold trap

1

2

� Emission in (connection to emission source) � Connection to neutralization stage

Fig. 4.4: Connections of the cold trap

4 Description of function

18 B-414 Operation Manual, Version D

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

5 Putting into operation

19 B-414 Operation Manual, Version D

5 Putting into operation

This chapter describes how the instrument is installed and gives instructions on initial startup.

NOTEInspect the instrument for damages during unpacking. If necessary, prepare a status report immedia-tely 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, fl at and stable base.

ATTENTIONTo ensure the instrument safety do not place any object on top of it.

ATTENTIONPlace 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 fi lled with cotton wool and install it. Check the glass for fl aws 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.

NOTEWhen you carry out Kjeldahl digestions, the suction capacity might become too high. Therefore we recommend to fi ll 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

••••

5 Putting into operation

20 B-414 Operation Manual, Version D

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 fi ts 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.

1

2

3

� Spring ring� Holder ring� Gasket PTFE

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.

••

••

5 Putting into operation

21 B-414 Operation Manual, Version D

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

ATTENTIONDo 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

NOTEUse 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.

5 Putting into operation

22 B-414 Operation Manual, Version D

3

2

1

45

� Neutralization stage� Connection of the neutralization vessel� Adsorption vessel

� Distribution head� Silencer

Fig. 5.4: Hose connections of the basic model

5 Putting into operation

23 B-414 Operation Manual, Version D

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.

12

3

4

5

6 78

9

10

� 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

••••

5 Putting into operation

24 B-414 Operation Manual, Version D

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

3

2 1

6 7

45

98

10

� 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

•••••

5 Putting into operation

25 B-414 Operation Manual, Version D

5.6 Electrical connections

ATTENTIONMake 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 connec-tion cable.

5.7 Preparing washing solutions

ATTENTIONAlways 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, ordissolve 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 concen-trations. 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 stan dard 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.

••

––

••

5 Putting into operation

26 B-414 Operation Manual, Version D

5.8 Filling up the prepared washing solution

To fi ll 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 fi ll up to the wavy maximum fi lling mark.Reassemble the instrument in the reverse order.

1

2

3

45

� Adsorption vessel� Nut GL-14� Protective cover with protective shield

� Washing insert� ON/OFF switch

Fig. 5.7: Filling up the washing solution

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

•••••

6 Operation

27 B-414 Operation Manual, Version D

6 Operation

This chapter gives examples of typical instrument applications and instructions on how to operate the instrument properly and safely.

WARNINGRisk of injury.

Never operate the instrument when glassware is damaged.

ATTENTIONSwitch on the B-414 before a connected instrument produces gases.

6.1 Typical applications

Table 6-1: Typical applicationsGases and vapors Chemical formula Neutralization (stage 2) Specifi c reactins (stage 4)

Kjeldahl digestions SO2, H2SO4 saturated soda / NaOH 8 - 10 % (max. 20 %)

Sulfur dioxide SO2 saturated soda / NaOH 8 - 10 % (max. 20 %)

Sulfuryl chloride SO2Cl2 NaOH 8 - 10 % (max. 20 %)

Hydrochloric or hydro-bromic acids

HCI, HBr NaOH 8 - 10 % (max. 20 %)

Thionyl chloride SOCl2 NaOH 8 - 10 % (max. 20 %)

Cyanuric chloride C3N3Cl3 NaOH 8 - 10 % (max. 20 %)

Carbonic acid chloride R-COCI NaOH 8 - 10 % (max. 20 %)

Phosgene COCI2 NaOH 8 - 10 % (max. 20 %)

Ammonia NH3 HCI max. 15 % / H2SO4 max. 20 %

Nitrous oxides (nitrous gases)Nitric acid / aqua regia

NOX NaOH 20 % FESO4 saturated

Chlorine, bromine, iodine Cl2, Br2, J2 NaOH 8 - 10 % (max. 20 %) FESO4 saturated

Thiophenols Ar-SH NaOH 8 - 10 % (max. 20 %) KMnO4 saturated

Thioalcohols, mercaptan R-SH NaOH / javelle water KMnO4 saturated

Hydrogen sulphide H2S NaOH 8 - 10 % (max. 20 %) KMnO4 saturated

Carbon disulphide CS2 NaOH 8 - 10 % (max. 20 %) KMnO4 saturated

Prussic acid HCN NaOH 8 - 10 % (max. 20 %) KMnO4 saturated

6 Operation

28 B-414 Operation Manual, Version D

6.2 Operation

1

2

Switch on the power switch �. Make sure that the cooling water fl ow 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.

••

Fig. 6.1.: Operation

7 Maintenance and repairs

29 B-414 Operation Manual, Version D

7 Maintenance

This chapter gives instructions on all maintenance work to be performed in order to keep the instru-ment in good working condition.

WARNINGElectrical hazard:

Prior to all maintenance work on the instrument switch off the power supply and remove all sources of fl ammable vapor.

ATTENTIONAlways 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.

ATTENTIONNever 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

ATTENTIONWhen 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.

7 Maintenance and repairs

30 B-414 Operation Manual, Version D

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 neces-sary, 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 remedyPosition in Fig. 9.1 Order no. Description Replacing interval

-- 40029 Set of seals EPDM for tube connectors once a year

8 37928 O-ring to adapter (37777) once a year

13 03575 Gasket SVL 42 x 30 PTFE once a year

17 03576 Gasket SVL 22 x 16 PTFE once a year

19 38225 Hose seal once a year

23 37873 Seal for receiving vessel once a year

34 37925 Gasket ring once a year

38 37871 Silencer unit 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.

12

3

2

4

5

6 7

� Nut M20� Swirl disc� Spacer tube� Swirl disc holder

� Lip gasket� Protective disc� Tube connector adapter M20 GL-14

Fig. 7.1. Exploded view of the washing insert

7 Maintenance and repairs

31 B-414 Operation Manual, Version D

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 fi rst 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 neutra lization 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 pre vents the possibility of the pump getting damaged. For a discription of how to prepare and fi ll up the washing solution, see chapter 5.7.

NOTEMake sure to dispose of the used washing solution according to your laboratory guidelines.

7.7 Pump

4 3

2

1

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

Fig. 7.2: Flushing the pump

••••••••••

7 Maintenance and repairs

32 B-414 Operation Manual, Version D

7.8 Power supply fuses

1

2

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 V120 V: T 1 A L 250 V230 V: T 1 A L 250 V

Put the fuse holder back.

•••

–––

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 fi nger 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 instru-ment 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 offi cial Buchi customer service offi ces are given on the Buchi website under: www.buchi.com. If malfunctions occur on your instrument or you have technical questions or applica-tion problems, contact one of these offi ces.

The customer service offers the following:

Spare part deliveryRepairsTechnical advice

•••

8 Troubleshooting

33 B-414 Operation Manual, Version D

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 offi cial 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 remedyMalfunction Possible cause Corrective measure

B-414 does not work No mains connectionFuses defective

Mains switch defective

Check whether the instrument is connected to the mainsReplace the defective fusesContact the Buchi customer service

Pump does not work Wiring defectivePump defective

Contact the Buchi customer service

Fumes are not exhausted during extraction (Scrubber suction capacity too weak)

Suction system leakingHose bentAdsorption vessel cloggedWashing solution dirtyAdsorbents cloggedPump dirtySilencer unit cloggedOverpressure valve dirty

Tighten the tube connectionsCheck the hosesCheck the adsorption vesselExchange the washing solutionRenew the adsorbentsClean the pumpReplace the silencer unitContact the Buchi customer service

Fumes are exhausted too fast during extraction (Scrubber suction capacity too strong)

Suction system clogged

Adsorbents cloggedSilencer unit defectiveOverpressure valve defective

Check all stages and the connected digestion unit as wellExchange the adsorbentsReplace the silencer unitContact the Buchi customer service

Washing solution turns yellow Washing solution dirty Exchange the washing solution

9 Shutdown, storage, transport and disposal

34 B-414 Operation Manual, Version D

9 Shutdown, storage, transport and disposal

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

9.1 Storage and transport

WARNINGBiohazard:

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.

10 Spare parts

35 B-414 Operation Manual, Version D

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 modifi cations 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

4

3

1

2

6

7

25

12

38

32

29

34

33

36

35

26

17

19

9

10119

30

39

161514

13

22

2324

28

21

5

27

8

18

31

20

37

Fig. 10.1: Spare parts on the exploded instrument view

10 Spare parts

36 B-414 Operation Manual, Version D

Table 10-1: Spare parts on the exploded instrument view

Position Product Order

number

Position Product Order number

1 Protective shield 37820 20 Hose adsorption / pump 37885

2 Neutralization vessel 37786 21 Condenser complete, including: 38022

3 Lip gasket lye-resistant EPDM 37874 22 - Spring ring 37872

4 Lip gasket acid-resistant FPM 38064 23 - Gasket 37873

5 Swirl disc 37821 24 - Holder ring 36709

6 Set of 4 tube connectors with cap bent FPM

40295 25 Receiving vessel, 1.2 l 37776

7 Adapter for GL-14 37777 26 Hose condenser / washing solution 37888

8 O-ring to adapter (37777) 37928 27 Cold trap 37781

9 Screw cap GL-14 (set of 10) 41956 28 O-ring FPM for cold trap 38067

- Set of seals EPDM for tube connectors (set of 10)

40029 29 Trap unit for cold trap 37782

10 Hose seal 38225 30 Connector GL-14 straight 37642

11 Screw cap GL-14 40624 31 Introduction tube assembly 37778

12 Adsorption vessel 37774 32 Reaction vessel, 1.0 l 37797

13 Gasket SVL 42 x 30 PTFE 03575 33 Screw cap SVL 42 03551

14 Adapter complete for adsorption vessel

37971 34 Gasket ring 37925

15 O-ring 47.2 for adsorption vessel 37857 35 Hose adsorption / reaction 37887

16 O-ring 39.7 for adsorption vessel 38068 36 Hose reaction / pump 37886

17 Gasket SVL 22 x 16 PTFE 03576 37 Condensate drain 37785

18 Adapter SVL 22 / GL14, complete 37972 38 Silencer unit 37871

19 Seal for FEP tube 38225 39 Distribution head, complete 37952

10.2 Miscellaneous

Table 10-2: MiscellaneousProduct Order number

Set of sealings FPM (10 pieces) 40040

Axial fl ow fan B-414 38026

11 Declarations and requirements

37 B-414 Operation Manual, Version D

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 protec-tion 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.

11 Declarations and requirements

38 B-414 Operation Manual, Version D

11.2 Declaration of conformity

We BÜCHI Labortechnik AGdo hereby declare on our responsibility that the product:

Scrubber B-414

which is the object of this certifi cation, is in accordance with the following norms:

EN 61010-1:2001 (~ IEC 61010-1) Safety requirements for electrical equipment for measurement, control, and laboratory usePart 1: General requirements

EN 55011:1998 + A1:1999 (IEC/CISPR 11:1997, modifi ed + A1:1999) Industrial, scientifi c 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 fl uctuations and fl icker

In accordance with the regulations of the EU guidelines

73/23/EEC (electrical operating equipment/low-voltage guidelines)89/336/EEC (electromagnetic compatibility)

Flawil, 12.01.06BÜCHI Labortechnik AGMeierseggstrasse 40PostfachCH-9230 Flawil 1Switzerland Tel.: +41 (0)71 394 63 63 Guido Worch Fax: +41 (0)71 394 65 65 Quality [email protected]

BÜCHI Labortechnik AGCH-9230 Flawil 1 / SwitzerlandT +41 71 394 63 63 F +41 71 394 65 65 096701

www.buchi.com Quality in your hands