BUCHI E-816 SOX User Manual

Operation Manual
Extraction Unit
E�812/816 SOX
093169
en
Table of contents
1 About this manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5
1.1 Reference documents. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5
1.2 Abbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
2 Safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6
2.1 User qualification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2.2 Proper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2.3 Improper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2.4 Safety warnings and safety signs used in this manual . . . . . . . . . . . . . . . . . . 7
2.5 Product safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9
2.5.1 General hazards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9
2.5.2 Warning labels on housing and assemblies . . . . . . . . . . . . . . . . . . . . . . 10
2.5.3 Personal protective equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
2.5.4 Safety elements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.6 General safety rules . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
3 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
3.1 Scope of delivery . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
3.1.1 Standard instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
3.1.2 Standard accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
3.1.3 Optional accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
3.2 Technical data overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
3.3 Materials used. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
4 Description of function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
4.1 Overview over the instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
4.2 Functional principle of a Soxhlet extraction . . . . . . . . . . . . . . . . . . . . . . 19
4.2.1 Step 1 - extraction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
4.2.2 Step 2 - rinsing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
4.2.3 Step 3 - drying . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
4.2.4 Solvent collection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
4.3 Controls of the Extraction Unit. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
5 Putting into operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
5.1 Installation site. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
5.2 Electrical connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
5.3 Condensers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
5.4 Soxhlet extractor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
5.5 Water supply connections. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
5.6 Cooling water connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
5.7 Cooling medium connection. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
5.7.1 Recirculating Chiller B-740/41 or equivalent model . . . . . . . . . . . . . . . . . . 25
5.7.2 Recirculating Chiller F-1xx . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
5.8 Solvent hose connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
3 E-812/816 Soxhlet Operation Manual, Version B
Table of contents
6 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
6.1 Main screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
6.2 General information on buttons . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
6.3 Description of the menu functions . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
6.3.1 Starting up the instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
6.3.2 Instrument settings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
6.3.3 Occupying the positions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
6.3.4 Defining a method. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
6.3.5 Saving a method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
6.3.6 Opening a method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
6.3.7 Deleting a method. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
6.3.8 Abort function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
6.3.9 Skip function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
6.3.10 Service functions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
6.4 Example of an extraction process . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
6.4.1 Material and equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
6.4.2 Preparing an extraction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
6.4.3 After the extraction process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
6.4.4 Emptying the solvent tank . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
6.4.5 Reusing the solvent . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
7 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
7.1 Daily maintenance. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
7.1.1 Housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
7.1.2 Hoses and hose connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
7.1.3 Glass parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
7.1.4 Solvent tank. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
7.2 Weekly maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
7.2.1 Heating elements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
7.3 Monthly maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
7.3.1 Cleaning the seals. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
7.3.2 Replacing the seals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
7.3.3 Condenser . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
7.3.4 Flushing the tank valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
7.4 Customer service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
8 Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
8.1 Malfunctions and their remedy. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
8.2 Error messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
8.3 Too high/too low results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48
9 Shutdown, storage, transport and disposal . . . . . . . . . . . . . . . . . . . . . . . . 49
9.1 Preparing the instrument for storage and transport . . . . . . . . . . . . . . . . . . 49
9.2 Storage and transport . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
9.3 Disposal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
10 Spare parts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
11 Declarations and requirements. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
11.1 FCC requirements (for USA and Canada) . . . . . . . . . . . . . . . . . . . . . . . 52
11.2 Declaration of conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53
4 E-812/816 Soxhlet Operation Manual, Version B
1 About this manual
This manual describes the Extraction Unit E-812/816 SOX and provides all information required for its safe operation and to maintain it in good working order.
It is addressed to laboratory personnel and operators in particular.
Read this manual carefully before installing and running your system and note the safety precautions in section 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. Technical data are subject to change without notice.
NOTE
The symbols pertaining to safety are explained in section 2.

1 About this manual

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.
The English manual is the original language version and serves as basis for all translations into other languages. If you need another language version of this manual, you can download available versions at www.buchi.com.

1.1 Reference documents

For information on the Extraction Unit E-812/816 Hot Extraction, please refer to the corresponding manuals as PDF on CD available in English, German, French, Italian and Spanish
• Extraction Unit E-812/816 Hot Extraction, Operation Manual number 93164 - 93168

1.2 Abbreviations

FEP: Fluorinated Ethylene Propylene FPM: Fluorpolymer rubber PMMA: Polymethyl methacrylate PP: Polypropylene PTFE: Ethylenetetrafluoroethylene PVDF: Polyvinylidene difluoride
5 E-812/816 Soxhlet Operation Manual, Version B

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 Safety

2.2 Proper use

The instrument has been designed and built for laboratories. It serves for activities associated with fat extraction.
It is used for:
• Soxhlet extraction with diethyl ether, hexane, petroleum ether and chloroform.

2.3 Improper use

Applications not mentioned above are improper. Also, applications, which do not comply with the technical data, are considered improper. 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.
• Determination of samples, which can explode or inflame (example: explosives, etc.) due to shock,
friction, heat or spark formation.
• Use in overpressure situations.
• Use with other glassware than the original from BUCHI.
• Use with other solvents than diethyl ether, hexane, petroleum ether or chloroform.
• Use with more than the allowed maximum solvent amount (max. 150 ml).
• Use with samples that react with solvent.
6 E-812/816 Soxhlet Operation Manual, Version B

2.4 Safety warnings and safety signs used in this manual

DANGER, WARNING, CAUTION and NOTICE are standardized signal words for identifying levels of hazard seriousness of risks related to personal injury and property damage. All signal words, which are related to personal injury are accompanied by the general safety sign.
For your safety it is important to read and fully understand the table below with the different signal words and their definitions!
Sign Signal word Definition Risk level
!
DANGER
Indicates a hazardous situation which, if not avoided, will result in death or serious injury.
2 Safety
★★★★
WARNING
!
CAUTION
!
NOTICE
no
Supplementary safety information symbols may be placed in a rectangular panel on the left to the signal word and the supplementary text (see below example).
Space for
supplementary
safety
information
symbols.
Table of supplementary safety information symbols The reference list below incorporates all safety information symbols used in this manual and their
meaning.
Indicates a hazardous situation which, if not avoided, could result in death or serious injury.
Indicates a hazardous situation which, if not avoided, may result in minor or moderate injury.
Indicates possible property damage, but no practices related to personal injury.
!
SIGNAL WORD
Supplementary text, describing the kind and level of hazard / risk seriousness.
• List of measures to avoid the herein described, hazard or hazardous situation.
• ...
• ...
(property damage only)
★★★☆
★★☆☆
★☆☆☆
Symbol Meaning
General warning
Electrical hazard
Heavy weight, avoid overexertion
7 E-812/816 Soxhlet Operation Manual, Version B
Symbol Meaning
Harmful to life-forms
Pinch point, mechanical hazards
Fire hazard
Hot item, hot surface
2 Safety
Device damage
Inhalation of substances
Chemical burns by corrosives
Wear laboratory coat
Wear protective goggles
Wear protective gloves
Heavy weight, lifting requires more than one person
Additional user information Paragraphs starting with Note transport helpful information for working with the device / software or its
supplementaries. Notes are not related to any kind of hazard or damage (see following example).
8 E-812/816 Soxhlet Operation Manual, Version B
NOTE
Useful tips for the easy operation of the instrument / software.

2.5 Product safety

The Extraction Unit is designed and built in accordance with 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 General hazards

Pay attention to the following safety notices:
!
WARNING
Death or serious injuries by formation of explosive atmospheres inside the instrument.
• Before operation, check all tube connections for correct installation
• Check for proper system tightness
2 Safety
!
DANGER
Death or serious injuries by use in explosive environments.
• Do not store or operate the instrument in explosive environments
• Provide sufficient ventilation and make sure to directly withdraw fumes
!
WARNING
Death or serious burns by flammable vapors.
• Remove all sources of flammable vapors
• Do not store flammable chemicals in the vicinity of the device
!
CAUTION
Risk of burns by hot heating glass plate (up to 250°C).
• Do not touch hot parts or surfaces
• Let the system and inserted extraction cells cool down safely
• Do not move the instrument or parts of it when hot
Risk of instrument damage by liquids or mechanical shocks.
• Do not spill liquids over the instrument or its components
• Do not move the instrument when it is loaded with sample liquid
• Do not drop the instrument or its components
• Keep external vibrations away from the instrument
• Safely attach the instrument to the bench in earthquake prone regions
• Do not operate the instrument without the safety shield installed
NOTICE
9 E-812/816 Soxhlet Operation Manual, Version B
2 Safety
Risk of instrument damage by wrong mains supply.
• External mains supply must meet the voltage given on the type plate
• Check for sufficient grounding

2.5.2 Warning labels on housing and assemblies

The following warning sticker(s) can be found on the housing or assemblies of the instrument:
Symbol Meaning Location
Hot item, hot surface Sticker / label, located at the heating block

2.5.3 Personal protective equipment

Always wear personal protective equipment such as protective eye goggles, protective clothing and gloves. The personal protective equipment must meet all requirements of the supplementary data sheets for the chemicals used.
NOTICE
!
WARNING
Serious chemical burns by corrosives.
• Observe supplementary data sheets of all used chemicals.
• Handle corrosives in well ventilated environments only.
• Always wear protective goggles.
• Always wear protective gloves.
• Always wear protective clothes.
• Do not use damaged glassware.
10 E-812/816 Soxhlet Operation Manual, Version B

2.5.4 Safety elements

Electronics
• The heating element is equipped with an electronic over-temperature protection.
• If no cooling water is detected at the cooling water output (for example, due to a leak in the
condenser), the electronic over-protection will stop all processes.
• To start a program at least one extraction position must be activated in the software.
• Safety shield: The protective shield protects operators from broken glass, solvent splashes and
prevents burns from the hot plates.
• Safety shield sensor: To start an extraction the protective shield must be closed.
Optional
• The protective shield (optional accessory) for the condenser protects operators from broken glass in case of an accident or explosion.

2.6 General safety rules

2 Safety
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.
11 E-812/816 Soxhlet Operation Manual, Version B
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

3 Technical data

Table 3-1: Standard instrument
Product Order number
Extraction Unit E-816 Soxhlet (6 place; 100 - 120 VAC / 200 - 240 VAC; 50/60 Hz; 1950/1200 W)
Extraction Unit E-812 Soxhlet (2 place; 100 - 120 VAC / 200 - 240 VAC; 50/60 Hz; 700/1200 W)
47581
49111
12 E-812/816 Soxhlet Operation Manual, Version B

3.1.2 Standard accessories

2
3
3 Technical data
Table 3-2: Standard accessories
1
E-812 E-816 Product Order number
1 1 Beaker pliers, 50 mm a 02004
1 1 Pliers for glass sample tubes with frit
4
b
47609
1 1 Turix wrench c 44349
5 5 Hose clamp, Ø 10.1 mm d 28737
- 1 Holder for 6 beakers (for E-816) 47643
1 3 Set of glass sample tubes, 2 pieces 49430
1 1 Set of holders for glass sample tubes
49432
with frits, set of 6 pieces
1 3 Set of beakers Soxhlet, 2 pieces 49427
1 3 Set of Soxhlet glass chamber, 2 pieces 49452
13 E-812/816 Soxhlet Operation Manual, Version B
3 Technical data
Table 3-2: Standard accessories (cont.)
E-812 E-816 Product Order number
2 2 Paper thimbles 25 x 100 mm,
41882
set of 6 pieces
2 2 Paper thimbles 33 x 94 mm,
41883
set of 6 pieces
1 1 Set of holders for paper thimbles
49428
25 x 100 mm, 6 pieces
1 1 Set of holders for paper thimbles
49429
33 x 94 mm, 6 pieces
1 1 Boiling stones, 10 g 42864
1 1 Plastic funnel 51167
1 1 Hose adapter for cooling media input 49151
1 1 Cooling water hose complete,
37780
G3/4”, G1/2”, L = 1.5 m
1 1 Solvent hose, Tygon SE 200, 1 m a 49450
1 1 PTFE hose, 500 mm b 25315
2
1
14 E-812/816 Soxhlet Operation Manual, Version B
3 Technical data
Table 3-2: Standard accessories (cont.)
E-812 E-816 Product Order number
3
1
5
2 2 Knurled screw (for solvent hose) a 43237
2 2 Clamping ring (for solvent hose) a 43238
4
2
5 5 Hose clamp, Ø 9.6 mm b 27738
2 2 Hose, silicone, Ø 6/9
43940
L = 1.5 m c
2 2 Condenser connection hose, silicone,
49161
L = 0.35 m, mounted
1 5 Condenser hose, silicone, L = 0.20 m
49163
d
2 2 Hose coupling (wide and small) e 43565
2 6 Set of seals, Viton, 2 pieces 49431
2 6 Seal PVDF holder 47610
1 1 Set of seals PTFE 49433
1 1 Sound absorber 15641
2 6 Glass valve unit complete 47590
1 1 Power cable
Type CH 10010
Type Schuko 10016
Type GB 17835
Type USA 10020
Type AUS 17836
1 1 Operation Manual E-812/816 SOX
English 93169
German 93170
French 93171
Italian 93172
Spanish 93173
15 E-812/816 Soxhlet Operation Manual, Version B

3.1.3 Optional accessories

3 Technical data
Table 3-3: Optional accessories
Product Order number
Holder for glass sample tubes, micro­wavable (6 positions), PTFE
Holder for glass sample tubes, (4 positions), PP
Condenser complete, including connector, straight
49424
37462
47604
Protective shield E-816 SOX 51923
Protective shield E-812 SOX 51968
Expansion element 51957
16 E-812/816 Soxhlet Operation Manual, Version B

3.2 Technical data overview

Table 3-4: Technical data
Dimensions (L x H x D) 275 x 776 x 456 mm 635 x 776 x 456 mm
Connection voltage 100 - 120 VAC / 200 - 240 VAC
Power consumption max. 700/1200 W max. 1950/1200 W
Weight 21 kg 36 kg
Overvoltage category II II
Pollution degree 2 2
Environmental conditions Temperature Altitude Humidity
3 Technical data
Extraction Unit E-812 Soxhlet Extraction Unit E-816 Soxhlet
100 - 120 VAC / 200 - 240 VAC
± 10%, 50/60 Hz
for indoor use only 5 – 40 °C up to 2000 m above sea level maximum relative humidity 80% for temperatures up to 31 °C, and then linearly decreasing to 50% at 40 °C
± 10%, 50/60 Hz
for indoor use only 5 – 40 °C up to 2000 m above sea level maximum relative humidity 80% for temperatures up to 31 °C, and then linearly decreasing to 50% at 40 °C

3.3 Materials used

Table 3-5: Materials used
Component Material designation Material code
Housing Stainless steel
Glass parts Borosilicate glass 3.3
Axial seal FPM 80-Shore A 170-A
Solvent hose inside instrument FEP DN 3.18/2.18; FEP DN 8/6
Solvent hose Tygon with FEP veneer
Solvent tank Borosilicate glass 3.3
Solvent valve and valve piston Body: Al Mg Si Sn Bi (Stanal-32)
Cooling media hoses Silicone
Condenser holder PVDF
Heating plate Ceran-Hightrans
Protective shield PMMA transparent green 777
Membrane glass valve Fluorez
Surface: Ematal, plane, high corro­sive-compressed
®
17 E-812/816 Soxhlet Operation Manual, Version B
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