BUCHI B-811 LSV User Manual

Operation Manual

Extraction System

B 811

096675 en

Table of contents

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	Warning notices used in this manual . . . . . . . . . . . . . . . .	.	7
	2.5	Product safety		7
	2.5.1	Instrument-related hazards . . . . . . . . . . . . . . . . . . . .		. 7
	2.5.2	Other hazards		8
	2.5.3	Safety measures . . . . . . . . . . . . . . . . . . . . . . .	.	8
	2.5.4	Safety elements		8
	2.6	General safety rules . . . . . . . . . . . . . . . . . . . . . .	.	9
3	Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .		.	10
	3.1	Scope of delivery . . . . . . . . . . . . . . . . . . . . . . .	. 10
	3.1.1	Standard instrument		10
	3.1.2	Standard accessories . . . . . . . . . . . . . . . . . . . . . .		11
	3.1.3	Optional accessories . . . . . . . . . . . . . . . . . . . . . .		14
	3.2	Technical data overview		16
	3.3	Materials used		17
4	Description of function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .		.	18
	4.1	Instrument function . . . . . . . . . . . . . . . . . . . . . .	.	18
	4.2	Overview of the instrument . . . . . . . . . . . . . . . . . . . .		19
	4.3	The three steps in general		20
	4.3.1	Extraction . . . . . . . . . . . . . . . . . . . . . . . . . .		20
	4.3.2	Rinsing . . . . . . . . . . . . . . . . . . . . . . . . . .	.	20
	4.3.3	Drying		21
	4.4	The three steps in detail		21
	4.4.1	Extraction - Step 1 . . . . . . . . . . . . . . . . . . . . . .	.	21
	4.4.2	Rinsing - Step 2		24
	4.4.3	Drying - Step 3 (to 9) . . . . . . . . . . . . . . . . . . . . . .		25
	4.5	Programming . . . . . . . . . . . . . . . . . . . . . . . .	.	25
	4.5.1	Extractions without rinsing and without drying		25
	4.5.2	Extractions with rinsing and without drying . . . . . . . . . . . . . .	.	26
	4.5.3	Extractions without rinsing and with drying . . . . . . . . . . . . . .	.	26
	4.5.4	Extractions with rinsing and with drying . . . . . . . . . . . . . . . .		27
	4.6	Control panel of the Extraction System B-811		28

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Table of contents

5	Putting into operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .		.	29
	5.1	Installation site		29
	5.2	Electrical connections		29
	5.3	Mounting the glass parts . . . . . . . . . . . . . . . . . . . .	.	30
	5.4	Fastening the optical sensor		30
	5.5	Connecting to tap water		31
	5.6	Inert gas connections . . . . . . . . . . . . . . . . . . . . . .		31
	5.7	Connecting to a recirculating chiller . . . . . . . . . . . . . . . . .		. 32

5.7.1When is it recommended to work with a recirculating chiller? . . . . . . . . . 32

	5.7.2 Connection to the cooling water sensor			33
	5.7.3	Rear connections . . . . . . . . . . . . . . . . . . . . . .	.	. 33
	5.7.4	Connection to the condensers . . . . . . . . . . . . . . . . . .	.	34
6	Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .		. .	35

6.1Description of the function keys . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35

	6.2	Preparing for an extraction . . . . . . . . . . . . . . . . . . . .		36
	6.3	Soxhlet Standard Mode - programming example . . . . . . . . . . . .	.	36
	6.4	Soxhlet Warm Mode - programming example		37
	6.5	Hot Extraction Mode - programming example		38
	6.6	Continuous Mode - programming example . . . . . . . . . . . . . .	.	39
	6.7	Storing / deleting a program		40
	6.8	Printing . . . . . . . . . . . . . . . . . . . . . . . . . .	.	41
	6.9	Optical sensor		42
	6.10 Handling the sample/sample holder			42
	6.11	Choosing the heating parameters . . . . . . . . . . . . . . . . . .		43
	6.12 Solvent addition during extraction			43
7	Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .		.	44
	7.1	Housing		44
	7.2	Hoses and hose connections . . . . . . . . . . . . . . . . . . .		. 44
	7.3	Glass parts . . . . . . . . . . . . . . . . . . . . . . . . .		. 44
	7.4	Magnetic glass valve . . . . . . . . . . . . . . . . . . . . . .		45
	7.5	Membrane assembly . . . . . . . . . . . . . . . . . . . . . .		45
	7.6	Heating elements . . . . . . . . . . . . . . . . . . . . . . .		. 45
	7.7	Holder ring with seal		46
	7.8	Glass sample tubes . . . . . . . . . . . . . . . . . . . . . .	.	46
	7.9	Solvent beakers		46
	7.10	Emergency release mechanism . . . . . . . . . . . . . . . . . .	.	46
	7.11	Customer service . . . . . . . . . . . . . . . . . . . . . . .		. 47
8	Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .		.	48
	8.1	Malfunctions and their remedy		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		49
10	Spare parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .		.	50

11 Declarations and requirements . . . . . . . . . . . .			. . . . .	. . . . . . . . .	. . .	. .	51
11.1	FCC requirements (for USA and Canada) . .	.	. . .	. . . . . .	. .	.	. 51
11.2	Declaration of conformity . . . . . . . .		. . . .	. . . . . .	. .	.	52

4	B-811 Operation Manual, Version G

1  About this manual

1 About this manual

This manual describes the Extraction System B-811 and provides all information required for its safe operation and to maintain it in good working order.

It is addressed to laboratory personnel 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 (WARNINGS and ATTENTIONS) are explained in section 2.

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 Hydrolysis Unit B-411/E-416, the Recirculating Chiller B-740 and the Mixer B-400, please refer to the corresponding manuals available in English, German, French, Italian and Spanish

•Hydrolysis Unit B-411/E-416, Operation Manual numbers 96684 - 96688

•Recirculating Chiller B-740, Operation Manual numbers 96690 - 96694

•Mixer B-400, Operation Manual numbers 96540 - 96544

1..2 Abbreviations

LSV: Large sample volumes

PTFE: Polytetrafluoroethylene

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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 extraction (solid-liquid extraction) of samples with known solvents or solvent mixtures and the reduction or drying of the extract. Solvents with boiling points between 30 °C and 150 °C as well as inert gas may be used.

It is used for:

•Soxhlet Standard

•Soxhlet Warm

•Hot Extraction

•Continuous

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 with samples that react with solvent.

•Use in conjunction with solvents containing peroxides.

•Use in overpressure situations.

•Use with other glassware than the original from Buchi.

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2  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.

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 Extraction System B-811 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 Instrument-related hazards

Pay attention to the following safety notices:

WARNING

Potentially hot surfaces during operation, especially at the heating elements (up to 250 °C).

• Always be aware of the risk of being burned.

WARNING

Potentially lethal voltage inside the instrument.

•Do not remove covers and other parts protecting from electricity.

•Always keep the areas of electric parts, such as power supply plug, mains switch, etc. dry.

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 damaged seals.

•Beware of incorrect installed or damaged glass valve.

•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 Extraction System B-811 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.

2..5..3 Safety measures

In case a safe operation of the instrument no longer appears possible, the instrument must be shut down and secured against unintentional operation.

It must be assumed that safe operation is no longer possible:

•if there is visible instrument damage,

•following a long period of storage under unfavorable conditions,

•following transport under difficult conditions.

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

2..5..4 Safety elements

Electrics:

The main power switch automatically turns to the zero position (off) if the power supply is overloaded or a short circuit occurs.

Electronics

•The heating elements are 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 will stop all processes.

•The protective shield protects operators from broken glass in case of an accident or explosion.

•An extraction position is only activated if a beaker is in contact with the lower heating element. In order to start a program, at least one extraction position must have been activated. If one of the glass beakers break, the program closes the glass valves and terminates the processing of all activated heating elements.

•If one of the solvent beakers gets dry (e.g. due to a defective seal or an open cooling unit), the software turns off the corresponding heating element.

•It is possible to release solvent and/or open the gas valve at any time during operation (only applicable for activated extraction positions).

•Only high quality borosilicate 3.3 glass is used. In order to prevent glass breakage, the cooling supply connections are threaded and can therefore be screwed on and off.

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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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3  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
Extraction System B-811, 230 V	36680
Extraction System B-811, 115 V	36681
Extraction System B-811, 100 V	40550

Table 3-2: LSV instrument

Product	Order number
Extraction System B-811 LSV, 230 V	37900
Extraction System B-811 LSV, 115 V	37901
Extraction System B-811 LSV, 100 V	40549

Table 3-3: Mixed instrument

Product	Order number
Extraction System B-811 Standard/LSV	11056621
(two positions of each), 230 V

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3  Technical data

3..1..2 Standard accessories

Table 3-4: Standard/LSV accessories

Product		Order number	Order number
		B-811 Standard	B-811 LSV
4	Extraction chambers	36710	37902
4	Condensation tubes	37482	37903
4	Sample holders	36559	37904
1	Set of solvent beakers (4 pieces)	37276	38597

1 Set of glass sample tubes	37281	37563
(4 pieces)
Pack of paper thimbles 33 x 94 mm	41883
(6 pieces)
Pack of paper thimbles 43 x 123 mm		41884
(6 pieces)
Set thimble holders 33 x 94 mm	37279	-
(4 pieces)

8 Holder rings (black ring already

36709

mounted to the extraction chambers with the seals)

2 Sets of seals for extraction chambers

37388

(4 pieces per set, already mounted to the extraction chambers with the holder rings)

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3  Technical data

Table 3-4: Standard/LSV accessories (cont.)

Product	Order number	Order number
	B-811 Standard	B-811 LSV
4 Condensers	36711

1 Set of blank plugs (4 pieces)	37368

4 Magnetic valves complete	36687

Membrane with anchor for valve unit	37534
(included in magnetic valve complete
(36687))
1 Inert gas supply	37496

1	Cooling water hose, Nyflex	04113
1 Water connection complete		37780
2	Hose clamps	22352
1	Silicon hose water drain	04134
4	Conducts (already mounted to the	36530
condenser)
PTFE band		08607
1	Silicon hose for condenser, 250 mm,	04133

premounted

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3  Technical data

Table 3-5: Mixed instrument accessories

Product		Order number
4	Condensers	36711
2	Extraction chambers	36710
2	Extraction chambers LSV	37902
2	Condensation tubes	37482
2	Condensation tubes LSV	37903
2	Sample holders	36559
2	Sample holders LSV	37904
1	Set of solvent beakers, 4 pieces	37276
1	Set of solvent beakers LSV, 4 pieces	38597
1	Set of glass sample tubes	37281
1	Set of glass sample tubes LSV	37563
2 Thimble holders 33 x 94 mm (part of		-
set thimble holders 37279)
2	Holder baskets for thimbles	37905
43 x 123 mm
1	Pack of paper thimbles 33 x 94 mm,	41883
6 pieces
1	Pack of paper thimbles	41884
43 x 123 mm, 6 pieces
8	Holder rings	36709
2	Sets of seals	37388
1	Set of blank plugs, 4 pieces	37368
4	Magnetic valves complete	36687
1	Inert gas supply	37496
Cooling water hose		04113
Water connection complete		37780
2	Hose clamps	22352
1	Silicon hose water drain	04134
4	Conducts	36530
PTFE band		08607
1	Silicon hose for condenser, 250 mm	04133

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			3  Technical data
		Table 3-6: Standard/LSV/mixed instrument accessories
		Product	Order number
		1 Power cable
		Type CH	10010
		Type Schuko	10016
		Type GB	17835
		Type USA	10020
		Type AUS	17836
		1 Operation Manual B-811
		English	96675
		German	96674
		French	96676
		Italian	96677
		Spanish	96678
3..1..3	Optional accessories
		Table 3-7: Optional accessories
		Product	Order number	Order number
			B-811 Standard	B-811 LSV
		Set of solvent beakers (4 pieces)	37276	38597
		Set of glass sample tubes	37281	37563
		(4 pieces)
		Holder basket for thimbles; to be used	-	37905
		with holder, order no. 37904, LSV
		(1 piece)
		Holder for glass sample tubes, PTFE,	51903	-
		microwavable (6 pos.)

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3  Technical data

Table 3-7: Optional accessories (cont.)

Product	Order number	Order number
	B-811 Standard	B-811 LSV
Holder for glass sample tubes	37462	-
Set thimble holders 43 x 123 mm	37280	-
(4 pieces)
Set thimble holders 33 x 94 mm	37279	-
(4 pieces)
Set thimble holders 22 x 80 mm	37278	-
(4 pieces)
Set thimble holders 25 x 100 mm	37277	-
(4 pieces)
Pack of paper thimbles 33 x 94 mm	41883	-
(6 pieces)
Pack of paper thimbles 43 x 123 mm	41884
(6 pieces)
Pack of paper thimbles 25 x 100 mm	41882	-
(6 pieces)
Pack of paper thimbles 22 x 80 mm	41881	-
(6 pieces)
Star printer 512 serial, complete	48258
Printer cable IDP-460	28468
Adapter for printer cable IDP-460	31411
Ink ribbon for printer IDP-460	38683
Ink ribbon for Star printer 512	44306

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3  Technical data

Table 3-7: Optional accessories (cont.)

Product	Order number	Order number
	B-811 Standard	B-811 LSV
Paper roll for Star printer 512	38684
Set of fluororubber seals (4 pieces)	42654

Quartz sand (0.3 - 0.9 mm), 2.5 kg	37689

Paper thimbles 25 x 100 mm		18105
(25 pieces)
Paper thimbles 43 x 123 mm		18106
(25 pieces)
Silicone tubes 6/9		04133
Silicone tube 12/14, 2 cm		04134
Angle		01992
LSV upgrade kit (Standard to LSV)	37910	-

3..2 Technical data overview

Table 3-8: Technical data

Extraction System B-811

Extraction System B-811 LSV variant

Dimensions (L x H x D)	600 x 980 x 290 mm
	with extended condenser holder
	600 x 700 x 290 mm during opera-
	tion

600 x 980 x 290 mm

with extended condenser holder 600 x 700 x 290 mm during operation

Connection voltage	100 - 120 VAC / 200 - 240 VAC	100 - 120 VAC / 200 - 240 VAC
	± 10%, 50/60 Hz	± 10%, 50/60 Hz
Power consumption	max. 1250 W	max. 1250 W
Weight	32 kg	32.5 kg
Overvoltage category	II	II
Pollution degree	2	2
Environmental conditions	for indoor use only	for indoor use only
Temperature	5 – 40 °C	5 – 40 °C
Altitude	up to 2000 m above sea level	up to 2000 m above sea level
Humidity	maximum relative humidity 80% for	maximum relative humidity 80% for
	temperatures up to 31 °C, and then	temperatures up to 31 °C, and then
	linearly decreasing to 50% at 40 °C	linearly decreasing to 50% at 40 °C

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3  Technical data

Table 3-8: Technical data (cont.)

			Extraction System B-811	Extraction System B-811 LSV variant
		Cooling water consumption	60 l / h	60 l / h
		Max. water pressure	6 bar	6 bar
		Interface	RS 232	RS 232
3..3	Materials used
		Table 3-9: Materials used
		Component	Material designation	Material code
		Housing	Coated tin, stainless steel
		Remote controller	Acrylonitrile-butadiene-styrol	ABS
		Hoses	Polytetrafluorethylene, Silicone	PTFE, Si
		Protective shield	Polycarbonate	PC
		Cable	Polyurethane	PUR
		Valve body	Aluminium	Al
		Valve threads	Polyoxymethylene	POM
		Valve membrane	Fluorez
		Seals	Polytetrafluorethylene,	PTFE
			glass fiber reinforced polyether-	PEEK 30 GF
			etherketon, fluororubber
		Seal holders	Polyethylenterephtalate	PETP 30 GF
		Holder ring for extraction chamber	Glass fiber reinforced polyamid 6.6	PA 66 GF
		Materials in contact with media	Borosilicate glass 3.3, PTFE
		Sample, condenser holders and	PTFE, Glass fiber reinforced	UP-GFK
		extraction chamber holder	synthetics

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