Buchi B-820, B-821 User Manual

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BÜCHI Fat Determination B-820/B-821

Contents

5 Operation 28

5.1 Control, operating and display elements 28

5.2 Operating the unit 31

5.2.1 User configuration 34

5.2.2 Printer configuration 35

5.2.3 System configuration 36

5.2.4 Autosampler configuration 37

5.2.5 Preheating/Separation column conditioning 38

5.2.6 Gas flow rate setup 39

5.2.7 Sample weight and mode adjustment 43

5.2.8 Determination 45

5.2.9 Data output 49

5.2.10 Statistics 51

5.2.11 Clearing data 54

6 Maintenance 55

6.1 Control checks 55

6.2 Replacing the septum in the injection head 55

6.3 Cleaning the FID 56

6.4 Replacing the ignition coil 56

6.5 Checking the formic acid 57

6.6 Installing a new separation column 57

6.7 Changing the printer paper roll 57

6.8 Changing the ribbon 58

6.9 Checking for fractures and cracks 58

6.10 Customer service 58

6.11 Maintenance of the Autosampler 59

6.11.1 General 59

6.11.2 Syringe and syringe needle 59

6.11.3 Replacing the main power fuse 59

7 Taking out of operation 60

7.1 Switching off the unit 60

7.2 Storage/Transport 60

7.3 Disposal 60

8 Replacement parts 61

9 Appendix 62

9.1 Technical data 62

9.2 Error messages 63

9.3 Materials used 64

9.4 FCC requirements (for USA and Canada) 65

9.5 Declaration of conformity 66

1 Scope of delivery 3

2 Safety 7

2.1 Symbols 7

2.2 Requirements for the customer 7

2.3 Proper use 7

2.4 Improper use 8

2.5 General hazards 8

2.6 Safety measures 9

2.7 Handling of gas cylinders in the laboratory 10

2.8 Modifications 10

2.9 Responsibility of the operator 10

3 Function 11

3.1 Operational principles 12

3.2 System description Autosampler B-821 14

3.2.1 Introduction 14

3.2.2 Carousel support 14

3.2.3 Carousel 14

3.2.4 Turntable 14

4 Putting into operation 15

4.1 Accessories 15

4.2 Location of unit 15

4.3 Power connections 16

4.4 Connecting periphery devices 16

4.5 Filling the formic acid 18

4.6 Gas connections 18

4.7 Checking supply lines for leaks 20

4.8 Installing the separation column 21

4.9 Setting the correct gas flow rate 22

4.10 FID ignition 22

4.11 Installation of Autosampler B-821 22

4.11.1 Unpacking and inspection 22

4.11.2 Retrofitting a manual basic system with an Autosampler 23

4.11.3 Installing the mounting plate 23

4.11.4 Mounting the Autosampler on the B-820 unit 23

4.11.5 Removing the transportation belt 23

4.11.6 Installing the syringe/needle assembly 24

4.11.7 Connecting the signal cable to the B-820 unit 24

4.11.8 Connecting power to the Autosampler B-821 24

4.11.9 Aligning the syringe needle with the injection head of the B-820 unit 25

4.11.10 Connecting the pneumatics to the Autosampler 26

4.11.11 Installing the solvent reservoir bracket 26

4.11.12 Routing and securing the solvent lines and the waste line 26

en, Version H (66 pages) Order no. B-820/B-821 Instructions 96571

BÜCHI Fat Determination B-820/B-821

Please read these instructions thoroughly before using the Fat Determination Unit B-820/B-821. These instructions should be kept near the unit for general reference.

Section 2 contains important notes on safety, which must be observed if the Fat Determination Unit is to be operated safely.

Due to continuous improvement and updating, technical specifications may be altered without prior notice. No part of this document may be reproduced, copied or transmitted in any way nor by using electronic or optical systems without prior agreement and written permission of Büchi Labortechnik AG. All rights reserved. © Büchi Labortechnik AG, 1996, 1999

BÜCHI Fat Determination B-820/B-821

1 Scope of delivery

Figure 1: Complete view of B-820/B-821 Figure 2: Complete view of B-820, Manual

Manual basic system

incl. individual

Version B-815 B-820 B-821 Total fat order no. fatty acids order no.

230V 230V 230V - 36925 37628 200V 120V 200V - 37109 37627 120V 120V 230V - 36924 37626

Automatic basic system

incl. individual

Version B-815 B-820 B-821 Total fat order no. fatty acids order no.

230V 230V 230V 230V 36923 37631 200V 120V 200V 230V 37108 37630 120V 120V 230V 230V 36922 37629

System prepared for Autosampler

incl. individual

Version B-815 B-820 B-821 Total fat order no. fatty acids order no.

230V 230V 230V - 37601 37634 200V 120V 200V - 37602 37633 120V 120V 230V - 37603 37632

Autosampler Retrofit 36926 Retrofit Fatty Acids manual 37635 Retrofit Fatty Acids automatic 37636

Table 1: Appliance models

BÜCHI Fat Determination B-820/B-821

Figure 3: Accessories

햳햲햴햵 햶햹햺

햷햻햾햿햸

1 Scope of delivery

Accessories Manual Basic System

Accessories B-815 (refer to Manual B-815)

Accessories B-820 Manual (refer to Table 2)

Accessories Automatic Basic System

Accessories B-815 (refer to Manual B-815)

Accessories B-820 Automatic (refer to Table 3)

Accessories Autosampler B-821 (refer to Table 4)

Accessories Autosampler Retrofit

Accessories Autosampler B-821 (refer to Table 4)

Accessories retrofit kit (refer to Table 5)

EPROM Set B-821

Accessories Individual Fatty Acids

Separation Column Fatty Acids 37620 Calibration Set Fatty Acids 37622

EPROM Set manual or automatic

Accessories B-820 Manual

1 Soap bubble meter, compl. 햶 34878 1 Separation column "Total Fat" 햻 34916

1 Supply line H2 햳 36134 1 Supply line Air 햲 36135 1 Syringe 10µl 햾 34258 1 High temperature septum (50 off) 햿 34382 4 Vespel seals 햹 34229 2 Threaded column joints 1/4" 햸 34228 2 Fork spanners w.a. flats 8 햵 16522 1 Fork spanner w.a. flats 17 x 19 햴 19831

1 Power cable (PNE, 2.5 m)

available in the following versions: 햷 Type CH 10010 Type Grounded (shock-proof) 10016 Type GB 17835 Type AUS 17836 Type USA, 230 V 33763

1 Instruction manual available in the following languages:

German 96570 English 96571 French 96572 Italian 96573 Spanish 96574

1 Packaging 34560

Table 2: Accessories B-820 Manual

BÜCHI Fat Determination B-820/B-821

Accessories B-820 Automatic

1 Soap bubble meter, compl. 햶 34878 1 Seperation column "Total Fat" 햻 34916

1 Supply line H2 햳 36134 1 Supply line Air 햲 36135 1 High temperature septum (50 pcs) 햿 34382 4 Vespel seals 햹 34229 2 Threaded column joints 1/4" 햸 34228 2 Fork spanners w.a. flats 8 햵 16522 1 Fork spanner w.a. flats 17 x 19 햴 19831 1 T piece D1/8“ 36845 1 Jumper cord W VDE 30983

1 Power cable (PNE, 2.5 m)

available in the following versions 햷 Type CH 10010 Type Grounded (shock-proof) 10016 Type GB 17835 Type AUS 17836 Type USA, 230 V 33763

1 Instruction manual

available in the following languages: German 96570 English 96571 French 96572 Italian 96573 Spanish 96574

1 Packaging 34560

Table 3: Accessories B-820 Automatic

1 Scope of delivery

BÜCHI Fat Determination B-820/B-821

Accessories B-821 Automatic

1 Septum * 1 Cylinder (reservoir) holder *

2 Glass cylinders for rinsing solvent and

waste 37069 1 Carousel 37085 1 Serial number label for carousel 37103 1 Mounting plate * 1 Sample vessel 2ml, compl. (100 ) 37068 4 Washers 16 mm * 2 Fuses 240V, 0.2A * 1 Fuse 250V, 0.5A * 1 Hamilton syringe 37066 1 Needle for Hamilton syringe 37067 1 Tubing PUR 1/8“ L = 3000 * 1 Foam rubber of neoprene length 100mm *

Table 4: Accessories Autosampler B-821

* Compare with spare parts list of the original operating instructions for

the 8200 CX.

Accessories Retrofit Kit

1 Cover for Autosampler 36758 1 Plate for Autosampler 36726 4 Spacers 36727 1 FID cap 34124 1 T piece D1/8“ 36845 2 LZS-K M4*10 10355 3 LZS-K M3*6 20390 3 FAE-SCH M3 10717 3 U-SCH M3 10571 4 SS-K M4*10 20909 1 Jumper cord W VDE 30983 5 Cable binders 2.6*200MM WS 03572 1 LZS-K M5*10 19645

Table 5: Accessories retrofit kit

1 Scope of delivery

BÜCHI Fat Determination B-820/B-821

2 Safety

This unit has been built in accordance with the state of engineering and the recognized rules of safety. Nevertheless, it can still be a source of risks and hazards:

• if used by persons with insufficient training

• if used for purposes other than that for which it is intended.

2.1 Symbols

Stop

Information about hazards which can lead to serious material damage or cause serious or potentially fatal injury.

Warning

Information about hazards which can be harmful to the user’s health or lead to material damage.

Please note

Information about technical requirements which if not observed can lead to malfunctions, inefficiency and production loss.

2.2 Requirements for the customer

The device must only be operated by persons who have the training or professional experience to comprehend the hazards that can arise when using the unit.

Personnel without such training or persons currently undergoing a course of training should be trained thoroughly. This Instruction Manual should be the basis for this training.

2.3 Proper use

The unit is designed and built for use in laboratories. It is intended to be used for determining the fat content based on fatty acids or the butyric acid. Its function depends on the Büchi Extraction Unit B-815: Some microliters of the upper extracted phase which contains the fatty acids and the internal standard are injected either manually into the Fat Determination Unit B-820, or automatically into the Fat Determination Unit with Autosampler B-821. The detection occurs with a flame ionization detector (FID). The subsequent evaluation is made by integrating the total peak areas.

Only original Büchi replacement parts and accessories may be used. Any modifications to the device or accessories shall be permitted only upon consultation with and obtaining a written authorization from the manufacturer.

2 Safety

BÜCHI Fat Determination B-820/B-821

2 Safety

2.4 Improper use

Any use other than those already listed, and any application that does not conform with the technical data is deemed to be improper use. The customer shall bear sole responsibility for any damage resulting from improper use.

Use of this instrument is strictly prohibited in:

• explosion-proof environments,

• rooms where gas cylinders cannot be stored.

2.5 General hazards

General hazards arise from:

• covering the ventilation slots

• an insufficient distance from the back of the unit to the

wall (see Section 4 "Putting into operation“).

• touching the injection head and the FID (risk of burning).

• improper storage of gas cylinders.

• inadequate installation of connections to gas cylinders.

Apart from authorized maintenance personnel, no one is allowed to remove any safety devices and covers. Touching live parts may result in fatal injury!

Electrical danger

Before connecting the unit to power make sure that the operating voltage shown on the serial plate agrees with the mains voltage.

The power plug may only be inserted into a socket with grounded contact. Its protective effect may not be suppressed by an extension line not having a ground wire.

Warning:

a) Any interruption of the ground wire inside or outside of the

unit or a disconnection of the ground wire may cause

potential problems. Deliberate tampering is prohibited.

b) When opening covers or removing parts, unless this can

be done by hand, live parts may be exposed. Bear in mind

that connecting parts may also be live.

BÜCHI Fat Determination B-820/B-821

c) Before an alignment, maintenance, repair or replacement

of parts, the unit must be disconnected from all sources of electric current, whenever it becomes necessary to open the unit.

If any of the services above must be performed on a powered on unit, it should only be done by a specialist who is famlilar with the dangers involved.

d) It should be ensured that only fuses of the type and rated

amperage as indicated are used for replacement. The use of repaired fuses or short-circuiting the fuse block is prohibited.

e) If an operation free from danger cannot be ensured, the

unit must be put out of operation and protected from any unauthorized use.

It can be assumed that an operation free from danger cannot be ensured any more if:

• the unit shows visible damages,

• the unit does not work any more,

• after long-term storage under inadequate circumstances,

• after having been exposed to considerable strain during transport.

2.6 Safety measures

The steel lines for hydrogen and synthetic air supplied with the equipment have different connections to the unit preventing improper connections.

Please make sure that connections at reduction valves are correct.

If, due to a lack of gas pressure in the system, the electronic valves will close preventing any hydrogen or synthetic air leaks.

Personal protective garments must be worn, such as goggles, gloves and a laboratory coat.

The Instruction Manual is a component of the Fat Determination Unit B-820/B-821 and should remain with the unit for easy reference by any user. This also applies to the additional language variants of these instructions, which can be ordered separately.

2 Safety

BÜCHI Fat Determination B-820/B-821

2.7 Handling of gas cylinders in the laboratory

Gas cylinders should be handled according to the pertinent local regulations and provisions. The following are general safety measures.

1. Protect gas cylinders from excessive heat, mechanical damage and corrosive substances.

2. Gas cylinders should not be stored or connected in areas with a major risk of fire.

3. Gas cylinders should be easily accessible at all times.

4. Full and empty gas cylinders should be stored separately according to the type of gas.

5. Gas cylinders should only be stored and transported with the protective cap screwed on.

6. Gas cylinders should be protected from falling down and rolling away.

7. In case of leak and fire: Close cylinder valves immediately. Cool any overheated cylinder with plenty of water.

8. Only keep as many replacement cylinders in the laboratory as are necessary for continuous operation.

9. Open cylinder valves slowly.

10. Cylinder valves must neither be oiled nor greased.

11. Close cylinder valves when switching the unit off.

12. Close valves of empty cylinders.

2.8 Modifications

Modifications on the unit or on replacement parts or accessories as well as the use of any other replacement parts or accessories as those indicated in this Manual are only permitted after consulting with Büchi Labortechnik AG and obtaining written consent.

2.9 Responsibility of the operator

The operator is responsible for instructing personnel. For manuals in other languages refer to Table 2, Section 1.

The operator should inform the manufacturer about events relevant to safety which occur with operating the Fat Determination Unit.

2 Safety

BÜCHI Fat Determination B-820/B-821

3 Function

The Fat Determination Unit B-820, which can be completed with the Autosampler B-821 (refer to Figure 5) is an instrument which determines total fat on the basis of fatty acids or individual fatty acids in organic matrices using a gas-chromatographic technique.

It is designed to function with the Büchi Extraction Unit B-

815. The temperature program and the evaluation function are preprogrammed and have an extremely short analysis run time, enabling the user to carry out the fat determination process quickly and easily. The appliance is not a universal gas-chromatograph.

3 Function

Figure 5: Fat Determination Unit B-820, Automatic

Figure 4: Fat Determination Unit B-820, Manual

BÜCHI Fat Determination B-820/B-821

3 Function

3.1 Operational principles

Figure 6: Diagram

햲

햳

햴 햵

햷

햶

헀

햿

햸

햾

햹

햽

햺

햻

헁

헂

햲 Synthetic air 햳 Hydrogen (percentage purity 5.0) 햴 Pressure reducing valve for synthetic air 햵 Pressure reducing valve for hydrogen 햶 Electronic valve for synthetic air 햷 Electronic valve for hydrogen 햸 Damping tube for synthetic air 햹 Damping tube for hydrogen 햺 Absorption tube 햻 Gas saturation vessel (formic acid 85 %) 햽 Forced-air oven 햾 Separation column 햿 Injection head 헀 Flame ionization detector (FID) 헁 Electronic 헂 Output

Main principle

1. Switch on the unit (the switch is located on the back of

the unit). Perform the input steps as described in Section 5 «Operation».

2. Using a syringe, extract some solution from the upper phase

of the extracted and saponified sample (see operating instructions for Extraction Unit B-815) and inject into the Fat Determination Unit.

3. A temperature program is performed automatically accor-

ding to the selected method. The fatty acids are separated from the solvent and internal standard and detected by the flame ionization detector.

4. An evaluation program, specifically developed for this unit,

calculates the content of total fat of individual fatty acids.

BÜCHI Fat Determination B-820/B-821

3 Function

Depending on the determination parameters, nine different determination modes can be selected:

Mode Abbreviat. Description Factor General Fact.gen Determines the factor that will be necessary for the determination of the

total fat content.

General correction Gen.corr. Determines the fat content of all products. It will still determine milk or

dairy products though, but it is not appropriate for products with a significant butyric acid content. In this case use "Spec.corr."

Special correction Spec.corr. Determines the fat content for milk or dairy products, or products with a

significant butyric acid content.

Blank value for butyric acid Bl.butyr. Determines the blank value for the butyric acid determination. Butyric acid factor Fact.b.a. Determines the factor that will be necessary for the determination of the

butyric acid content.

Butyric acid But.acid Simultaneous determination of the butyric acid content, the milk fat

content (optional), and the overall fat content (optional) in all products.

Fatty acid calibration FA-calib. Determines the retention period for six saturated fatty acids (calibration

set “Fatty Acids”).

Fatty acid factor FA-factor Determines the factor that will be necessary for the determination of the

fatty acids

Fatty acids FA-det. Identification and determination of the contents of the individual fatty

acids and calculation of the sum parameter of the saturated, monoand polyunsaturated fatty acids in all products.

Table 6: Overview of the determination modes

Application Column (Order No.) Start temperature /Analysis time Mode Total fat 34916 130 °C / 8 min. Gen.fact.

130 °C / 8 min. Gen.corr.

90 °C / 10 min. Spec.corr.

90 °C / 10 min. Butyr.con.

Butyric acid 34916 90 °C / 10 min. Bl.butyr.

90 °C / 10 min. Butyr.fact.

90 °C / 10 min. Butyr.con.

Individual fatty acids 37620 150 °C / 41 min. FA-calib.

150 °C / 41 min. FA-fact.

150 °C / 41 min. FA-det.

Table 7: Overview of the determination parameters

The analysis time is calculated from the start of the determination to the re-start of the next determination. The analysis time therefore contains the following time sectors:

• Separation time for the separation of the fatty acids

• Preheating of the separation column at 260 °C at the end

of the separation

• Conditioning of the column for the next analysis depending on the mode of determination.

BÜCHI Fat Determination B-820/B-821

3.2 System description Autosampler B-821

3.2.1 Introduction

The Autosampler is comprised of essentially three modules: the storage module, the injection tower module, and the pneumatics module. It is mounted on the Büchi Fat Determination Unit B-820 above the injection head. The Autosampler is operated through the keypad of the B-820.

The Autosampler is powered through the B-820 via a connection cable. The power entry module as well as the power on/off switch and the voltage selector module are located at the rear of the Autosampler. If you want to connect the Autosampler directly to the mains, you can adjust voltages of 100, 120, 230, and 240 Volts and frequencies of 50/60 Hz at the voltage selector module. Refer to paragraph 4.11.8 (Mains voltage connection to Autosampler B-821) to adjust your own country’s voltage.

햲 Turntable 햳 Pneumatics module 햴 Power on/off switch 햵 Power entry module 햶 Carousel support 햷 Carousel 햸 Injection tower module

3.2.2 Carousel support

The carrousel support comprises a carousel, a position sensor, a vial sensor, and the turntable. It is secured to a rotating hinge on the injection tower. An indicator (LED) is located on the front side of the carousel support; the LED lights when the unit is ON.

3.2.3 Carousel

The carousel can hold up to forty-eight sampling vials of 2 ml. It may be removed for placing the vials. The serial number label which is lettered from 1 through 48 may be glued on the carousel. A small raised indicator at the center knob marks the correct position.

3.2.4 Turntable

The turntable is driven by two motors, one to rotate the turntable (clockwise) and another to move the turntable forward or backward. The carousel mounts on the turntable and is fixed by a vertical pin.

Figure 7: Autosampler B-821

3 Function

햲

햳

햴

햵

햶

햷

햸

BÜCHI Fat Determination B-820/B-821

4 Putting into operation

Unpacking and checking the B-820 unit

Open the carton carefully in order to avoid breaking the glass of the enclosed separation column, soap bubble meter and syringe. Unpack the unit with care and check for any possible damage. It is important that any damage incurred during transit is determined and reported immediately. If this is the case, a full statement of facts must be immediately reported to the shipping agent.

Autosampler B-821

For unpacking and checking refer to Section 4.11.1.

It is advisable to keep the packaging for future transport.

4.1 Accessories

The following accessories necessary to operate the unit are not included in delivery and cannot be ordered from the manufacturer:

• Hydrogen (percentage purity 5.0, gas cylinder or central supply)

• Synthetic air (gas cylinder or central supply)

• 2 pressure reducing valves for gas cylinders

• Two G 1/8” connections to the reducing valves (oxygen and synthetic air)

• Formic acid (85%)

• Stopwatch

• Soap solution

• When using the Autosampler: n-butanol (pure) (for rinsing the syringe)

4.2 Location of unit

The unit must only be operated in ventilated rooms (window or artificial ventilation). It must be installed on a stable, clean and even surface.

For safety reasons and to ensure sufficient cooling of the oven, the back and side walls of the unit must be placed at least 13 cm (5.2 inch) away from the walls or any other object. No containers or chemicals should be placed behind the unit (due to outflow of the hot air).

4 Putting into operation

BÜCHI Fat Determination B-820/B-821

4.3 Power connections

Check that the voltage of the socket is identical to the voltage specified on the serial plate. Only connect the unit to a plug which is grounded. External couplings and extension cables must be grounded (3-contact couplings, cables and connectors). The ground wire must not be tampered with in any way. Risks caused by possible internal defects are thus prevented.

Check the frequency of the power supply and adjust the unit accordingly (see Section 5.2.3, "System configuration“).

4.4 Connecting periphery devices

The unit has three serial and one parallel interface (RS-232C). This enables connection of a computer, a balance, an external printer and the Autosampler B-821 to the rear of the unit. If a balance or printer is connected, the proper balance or printer type must be entered in the initialization menu under system configuration or printer configuration (see Section 5.2.3, "System configuration" or Section 5.2.2, "Printer configuration“).

Any IBM or IBM compatible PC may be used for data output to a PC. The computer connection cable is available as an accessory (cable length: 10 meters):

B-820 Computer cable 29502

Balance

The following types can be connected:

Mettler: All AT balances, as well as AE types with

upgraded interface option 012 and hand key or foot pedal.

Sartorius: All analytical balances of the type MC1 as well

as balances with interface MP8-4.

A&D: FR and HA series.

The interface parameters in B-820 are preset and cannot be modified.

The balance parameters are as follows:

• 2400 baud

• even parity

•7 bit

• 1 stop bit

• Software handshake

Figure 8: Connection of periphery devices to back of unit

4 Putting into operation

BÜCHI Fat Determination B-820/B-821

The balance connection cables are available as accessories (cable length: 9 meters):

B-820 Mettler AE 30699 B-820 Mettler AT 30498 B-820 Sartorius 30760 B-820 A&D 30699

Please consult the balance operating instructions before making adjustments!

Printer

The following printers can be connected*, whereby the printer languages (PCL: Printer Control Language; LQ: Epson Emulation) are supported:

• Epson

• Canon

• HP DeskJet

• HP LaserJet

* The following printers have been tested at Büchi:

• Epson Stylus Color 440

• Canon Bubble Jet BJC-600, BJ-200 EX (DIP switch setting LQ)

• HP DeskJet 550C/690C

• HP LaserJet 4L

The printer connection cable is available as accessories (cable length: 3 meters, type: Centronics):

B-820 Printer cable 30754

The B-820 supports the IBM character set. Please consult printer operating instructions before making adjustments!

Autosampler B-821

Installation of the Autosampler is described in Section 4.11.

4 Putting into operation

BÜCHI Fat Determination B-820/B-821

Figure 9: Gas saturation bottle with formic acid, 85%

4.5 Filling the formic acid

A small gas saturation bottle is located at the back of the unit, which must be filled with max. 20 ml of formic acid (85%). The gas saturation bottle must always contain some formic acid (85%); do not exced arms of vessel. In this way, it is ensured that the hydrogen is saturated with formic acid vapor.

The gas saturation bottle must be kept tightly closed in order to ensure that the hydrogen system is hermetically sealed.

Caution: The bottle is under pressure

- Do not open when the B-820 is in operation/hot

- Do not fill up while the B-820 is in operation/hot

- Do not overfill, max. 20 ml or less 1 cm below the vessel's arms!

- Only fill when the unit is turned off and is at room temperature

- Filling under any other circumstances may lead to system contamination!

4.6 Gas connections

Gases used:

Gas function Gas type Setting pressure

Combustible + hydrogen 5.0 5 bar (72.5 psi) separating gas

Auxiliary gas synthetic air 5 bar (72.5 psi)

Autosampler synthetic air 5 bar (72.5 psi) Operating gas

Only use synthetic air, and not compressor air generated and filtered on-site.

General

Synthetic air and hydrogen from gas cylinders must be equipped with a two-stage pressure reducing valve. The exit ports of this valve should be threaded. To enable a precise adjustment of the output pressures, use a pressure reducing valve with a measuring capacity of 0 to 10 bar (0 to 150 psi). The output pressures at the valves to the B-820 unit should be 5.0 bar (72.5 psi) both for synthetic air and for hydrogen.

4 Putting into operation

Newer instrument models see mark "-MAX-"

BÜCHI Fat Determination B-820/B-821

4 Putting into operation

Gas supply connection to the B-820

1/8” copper capillaries 햴 with pre-fitted quick-lock couplings are included in the delivery. To connect the gas supply, the quick-lock couplings are fitted to the corresponding couplings (labelled with “H2” and “Synth. Air”) on the back of the B-820. (See Figure 10: Gas connection layout, Page 19)

Ensure the correct connection of the gas cylinder to the unit.

The following are included in the Büchi delivery:

H2 connection 햲 inc. copper capillary 36134 Air connection 햳 inc. copper capillary 36135

To be supplier by the user:

햵 Hydrogen 5.0 햶 Synthetic air

햷 Cylinder pressure 햸 pressure reducing valve (two- 햹 Required pilot pressure stage) for hydrogen and syn-

thetic air in the range from 0-10 bar ( 0-150 psig)

햺 Connecting parts to the pressure reducing valve

Figure 10: Gas connection layout

}

BÜCHI Fat Determination B-820/B-821

4 Putting into operation

4.7 Checking supply lines for leaks

After connecting the pressure lines to the unit, open both cylinder valves before switching on the unit, and then close them again once the pressure is achieved. The pressure indicator on the pressure reducing valve should remain constant for approx. 10 minutes. The cylinder valves can be reopened once this check is completed.

The primary pressure, the tightness of the supply lines and the gas flow (see Section 4.9, "Setting the correct gas flow rate“) must be rechecked every time a gas cylinder is changed.

Check the separation column for possible fractures and cracks before each use. The unit must not be operated if the separation column is damaged (hydrogen leak).

BÜCHI Fat Determination B-820/B-821

4.8 Installing the separation column

1. Open the oven door

2. Position the seals, screws and nuts as shown in Figure 11.

3. Figure 12 shows how to fit the separation column. Push both sides of the column up as far as they will go, hold in place and tighten nuts by hand.

4. The two nuts must be tightened by ¼ to ½ turn using the supplied spanner (17”).

Take care not to overtighten nuts as this could break the glass.

Figure 11: Positioning seals and

screw nuts

Separation column installedInstalling the separation column

4 Putting into operation

The procedure is the same for

the "Fatty Acid column"

Figure 12: Installing the colums

The column should be heated only when gas (H2) is flowing. Prior to operation, always ensure that the gas supply is opened.

When fitting a new column, always ensure that there is a septum in the injection head.

After a long period of use (approx. 1,000 injections), the injection zone of the separation column can become soiled, which can impair the reproducibility of the individual measurements.

A new column must be conditioned before doing any opera- tions. This requires a preheating period of 120 min. (see Section 5.2.5, "Preheating/Separation column conditioning“).

The results of the first two injections using a new column can vary greatly. Therefore, these values should be ignored.

BÜCHI Fat Determination B-820/B-821

4.9 Setting the correct gas flow rate

The gas pressures are electronically controlled, digitally displayed and preset to a basic value by the manufacturer. However, this basic value does not ensure the correct gas flow rate and must be adjusted after preheating. Therefore, measure the gas flow rate of the hydrogen and synthetic air after first commissioning the unit, and adjust the set value if necessary. The correct gas flow rate should be checked periodically at minimume when:

• replacing the gas cylinder

• replacing the separation column

• carrying out service work

(see Section 5.2.6, "Gas flow setup“).

4.10 FID ignition

The ignition of the FID is carried out automatically. If required, it can also be carried out manually by pressing key combination «SHIFT» / «i».From the top of the FID look for red heating coil.

If the heating coil is defective, use a lighter to ignite the FID flame.

4.11 Installation of Autosampler B-821

4.11.1 Unpacking and inspection

Autosampler B-821:

Your Autosampler B-821 is shipped and delivered to you in a carton. To unpack proceed as follows:

1. Place the carton in a way to make sure the top side is up (arrows).

2. Open and lift the top cover.

3. Use the two hand holes to lift the inner liner from the carton.

4. Do not overlook the syringe which is packed in a separate small container.

5. Remove the transport protection (See Chapter 4.11.5).

Do not lift the Autosampler by the carousel support to avoid damaging the hinge of the carousel support (see Figure 16). Latch of carousel support). Lift only at the lower left and upper right corners of the Autosampler.

4 Putting into operation

BÜCHI Fat Determination B-820/B-821

4.11.2 Retrofitting a manual basic system with an Autosampler

The system may only be retrofitted by authorized service technicians. They have had a thorough professional and technical training and are aware of the risks which may ensue from noncompliance with the Safety Regulations.

4.11.3 Installing the mounting plate

The mounting plate and both washers are supplied together with the Autosampler B-821. For mounting the mounting plate, proceed as follows:

1. Place the mounting plate on the baseplate to ensure that

all holes align.

2. Secure the mounting plate with both enclosed M4x10

screws and both washers which have an extra large diameter. The screws go through the holes of the mounting plate and reach the baseplate.

4.11.4 Mounting the Autosampler on the B-820 unit

In order to mount the Autosampler on the B-820 unit proceed as follows:

1. Place the Autosampler on the mounting plate 햲 just

mounted . Push the Autosampler carefully to cover the position holes until the threaded bolts with the knurled screws engage in the holes of the mounting plate 햲.

2. Tighten the quick-lock screws 햳 riveted to the bottom of

the baseplate (refer to Figure 13: Securing the Autosampler).

4.11.5 Removing the transportation belt

In order to protect the syringe carriage from transport damage, it is secured to the upper stop using a transport security belt. The transport security belt can be seen if you look at the Autosampler from above. Cut the transport security belt. The syringe carriage will fall down slightly. Now remove the transport security belt carefully from the Autosampler B-821.

Before any subsequent transportation, a transport security belt must again be used to secure the syringe.

4 Putting into operation

Figure 13: Securing the Autosampler with quick-lock screws

햳

햲

BÜCHI Fat Determination B-820/B-821

Syringe mount assembly

Side locking tabs

Solvent line connection

Syringe carriage

Figure 14: Syringe/needle mounting hardware

Side locking tabs

Syringe carriage bracket

Red indicator tab

4.11.6 Installing the syringe/needle assembly

Goggles should be worn during installation

To install the syringe/needle in the Autosampler proceed as follows:

1. Open syringe mounting assembly by firmly lifting the side

locking tabs simultaneously and raising them to the upper position. As this may require slight force, hold the syringe mounting assembly down with the forefingers and press the tabs simultaneously up with the thumbs. A red indicator tab shows at the syringe mounting assembly when the mounting is unlocked.

2. Refer to Figure 14a: Syringe/needle mounting: Guide the syringe needle through the hole of the needle guide. Then let the syringe rest on the lower bracket and press the upper part of the plunger into the top slot.

3. Close the syringe mounting by holding the mounting with one hand and pressing the side locking tabs down with the other hand. Check that the mounting is fully closed before pushing the side locking tabs down. It is closed when the red signal tab is not visible.

4. Connect the solvent line laterally to the syringe (refer to Figure 14b: Syringe/needle mounting). Slide the knurled nut back from the end of the line. Push the line onto the side connection of the syringe. Then tighten the knurled nut at the syringe only by hand (do not use a tool).

5. Refer to paragraph 4.11.9 to align the syringe needle with the injection head of the B-820 unit.

If the solvent line has not been connected correctly or not at all, solvent may spray from the line.

4.11.7 Connecting the signal cable to the B-820

unit

A data cable is fitted to the Autosampler B-821 which emerges at the rear of the unit. Insert the cable at the rear of the B-820 unit into the corresponding interface (refer to Figure 8: Connection of periphery units at the rear of the unit).

4.11.8 Connecting power to the Autosampler

B-821

Before connecting the Autosampler to the mains check that the power switch is OFF (0). Then check the voltage rating (230 V) on the serial number label and the position of the white pin in the power entry module at the rear of the unit. If they agree, go to Step 5.

4 Putting into operation

BÜCHI Fat Determination B-820/B-821

If they do NOT agree, proceed as follows:

1. Remove the cover of the fuse block 햲 .

2. Pull the voltage selector card carefully out of the fuse block with a needle-nosed pliers.

3. Orient the selector card so that the voltage that is to be used can be inserted into the fuse block in the direction of the arrow. Turn the printed side (plastic part on the selector card) to face forward.

4. Replace the cover on the fuse block and check that the pin is showing in the hole of the desired operating voltage.

5. Connect the power cable to the rear of the Autosampler and to the B-820 unit (refer to Figure 8: "Connection of periphery units at the rear of the unit“)

•

4.11.9 Aligning the syringe needle with the

injection head of the B-820 unit

At this stage, the Autosampler has been installed on the B820 unit, the syringe/needle has been fitted and the data cable has been connected to the B-820 unit. The voltage has been correctly set and the Autosampler is connected to power.

햲 Latch 햳 Hinge

In order to align the syringe/needle with the injection head of the B-820 unit proceed as follows:

1. Check that the Autosampler is OFF (0). Press down the latch (refer to Figure 16: Carousel support) of the carousel support 5 and swing out the support.

2. Switch the Autosampler ON (I). Lift the syringe cariage slowly by hand until a click can be heard. Now lower the carriage until the needle is just a little above the injection head.

3. Loosen the screws of the mounting plate sufficiently to shift it by hand together with the Autosampler.

4. Align the needle accurately with the injection head. Then retighten the screws of the mounting plate, so the Autosampler cannot be moved.

5. Lower the syringe carriage two or three times until the syringe needle punctures the injection head septum. You can now check that the syringe and the syringe needle are properly aligned with one another. Repeat this procedure each time you replace the syringe/needle.

6. To return the syringe carrier to its rest position, raise the syringe carrier until a click can be heard. Then lower the carriage again by a fraction of an inch to rest on the stop.

4 Putting into operation

Figure 15: Power entry module

햲

Figure 16: Latch of carousel support

햲

햳

BÜCHI Fat Determination B-820/B-821

Figure 17: Gas connection with Autosampler

4.11.10 Connecting the pneumatics to the Autosampler

Compressed air (approx. 3 bar/40 – 60 psig) is required for the Autosampler to operate correctly. Use the same synthetic air which is required for the B-820 unit. For the pneumatic connection, the T-screw connection 햲 supplied with the Autosampler is installed additionally into the feeding line for connecting the pneumatics. The 1/8" tubing of polyurethane supplied with the Autosampler is connected to the T-screw connection and to the hose nipple located at the rear panel of the Autosampler.

Before connecting or disconnecting the tubing make sure that the feeder valves are closed.

This tubing must not be put in front of the oven flap. Affix it to the top of the B-820.

4.11.11 Installing the solvent reservoir bracket

The bracket holds two solvent bottles of 180 ml each and is secured on the lower left side of the B-820 unit by means of an M5*12 screw. For a more secure fix we recommend to cut the self-adhesive foam rubber part (included in the standard accessory kit of the Autosampler) into halves and to attach them to the rear of the bracket (on the left and right side).

4.11.12 Routing and securing the solvent lines and the waste line

Two solvent lines for rinsing the syringe and one waste line are already fitted to the Autosampler. To operate the Autosampler, you will only need the line marked with «Sol A», since only one solvent is used for rinsing the syringe. The bracket for both solvent reservoirs (included in the standard accessory kit) takes up the solvent reservoir for rinsing the syringe and the reservoir for the waste solvent.

4 Putting into operation

햲

B-821

Air

B-820

BÜCHI Fat Determination B-820/B-821

4 Putting into operation

To install and secure the lines proceed as follows:

1. All PTFE lines which emerge from the bottom of the Autosampler are pushed between the cover and the housing of the B-820 unit and are secured with a cable binder on the pre-assembled binder base to the rear panel of the B-820 unit.

Check that the PTFE lines are not routed in front of the air flap of the oven in the back of the unit.

2. The lines are routed along the bottom of the B-821 unit up to the solvent reservoirs.

3. Fill a bottle of „n-pure butanol“ or rinsing the syringe.

The reservoirs should be labeled to avoid later confusion.

4. Connect the line marked with «Sol A» to the reservoir labeled accordingly which contains the solvent for rinsing the syringe.

5. Connect the waste line to the second reservoir.

Check that the reservoir removing the waste is positioned below the level of the Autosampler B-821.

Avoid any kinks of the lines.

BÜCHI Fat Determination B-820/B-821

Ensure that the unit has been commissioned according to the instructions in Section 4, Putting into operation.

5.1 Control, operating and display elements

The main power switch is located at the back of the unit.

If, in the case of a failure, the current requirement of the unit increases to more than 12 A, a bimetallic switch interrupts the circuit, which automatically turns the main power switch off. After the fault has been rectified, the unit can be operated by turning it on once again.

The operating panel shows:

햲 Display

햳

Lamp lights up when the unit is ready for an injection or a gas flow measurement.

햴

Lamp lights up when the determination or preheating process is running.

햵

Lamp lights up when a failure has occurred.

햶

Each menu command has its own help text which can be called up via the display.

햷

Pressing this key moves the application one step up on the menu hierarchy. Exceptions are the sample weight/mode, the elimination table and the data output table, where pressing the <ESCAPE> key will return you to the main menu.

햸

Moves the cursor up within a menu.

5 Operation

Figure 18: Control, operating and display elements

5 Operation

BÜCHI Fat Determination B-820/B-821

햹

Moves the cursor down within a menu.

햺

Confirms position of cursor and performs menu command.

햻

Allows selection of a variety of options (e.g. balances, print system, frequency etc.). In the sample weight table, pressing the OPTION key copies a field into the next row.

햽

These keys enable input of numeric values and this key enables you

to cancel input.

햾

Darkens display.

햿

Lightens display.

헀

Manual paper feed.

5 Operation

BÜCHI Fat Determination B-820/B-821

Use the keyboard to enter sample identification and report titles and press this key

to cancel.

The key

has the same function as this key, "ENTER".

5 Operation

헂

BÜCHI Fat Determination B-820/B-821

5.2 Operating the unit

The following flow chart shows the operating structure. This is followed by a systematic description of all the options provided by this unit.

The unit contains a help program which can be accessed by pressing the HELP button.

5 Operation

BÜCHI Fat Determination B-820/B-821

Version: 3.00af Gas supply on? User: C.Heiter Press <ENTER> to cont.

C13 : 285 C20 : 1095 C16 : 516 C22 : 1408 C18 : 768 C24 : 1687

SWITZERLAND

Preheating p H2 55kPa

Sample weight/Mode p air 50kPa Determination T oven 130°C Data manager T inj. 220°C Setup T FID 260°C

Sample no: 5 p H2 55kPa

Vial no: 5 p air 50kPa Switch off: yes T oven 140°C Start after 62s T inj. 220°C Main menu T FID 260°C

gen.corr.

Name: coconut oil

Manual sample weight

Automatic sample weight Factors

Main menu

Stop p H2 55kPa

Main menu p air 50kPa

T oven 260°C T inj. 220°C T FID 260°C

Remaining time 1215s

Time: 2400s p H2 55kPa

Start preheating p air 50kPa Main menu T oven 130°C

T inj. 220°C T FID 260°C

Determination with autosampler

Determination without autosampler

Sample no: 5 p H2 55kPa

Next number p air: p air 50kPa

T oven 130°C T inj. 220°C

Main menu T FID 260°C

Ready injection 2 gen.corr. Name: coconut oil

5 Operation

Manual sample weight

Automatic sample weight Factors Calibration

Main menu

Determination "Fatty Acids"

Determination "Total fat"

No Mode Weihgt Weight Weight Conc.

[g] C13[g] C5[g] [%] 1 fact.gen. 0.7055 0.2115 99.8 Name: Factor 2 fact.b.a. 0.055 0.054 99.5 Name: Factor C4 3 but. acid 0.8550 0.2134 0.056 Name: butter 4 gen.corr. 4.3575 0.1245 Name: wheat 5 spec.corr

. 2.3654 0.2056

Name: cheese

"Table of factors"

Factor Fat: 0.953 Factor butyric acid: 1.123 CF: 28.570 Blank value but.acid 0.0031g

Main menu

No Mode Weight Weight Conc.

[g] C13[g] [%] 1 FA-calib. Name: Calibration 2 FA-factor 0.7133 0.2078 99.7 Name: Factor 3 FA-det. 2.1351 0.2132 Name: milk powder

Factor fatty acids: 1.053

Main menu

BÜCHI Fat Determination B-820/B-821

Press. system: air p H2 55kPa Air-pressure: 50kPa p air 50kPa

Main menu T oven 130°C

T inj. 220°C Wait until ready T FID 260°C Req. flow H2 + air: 20 ml/2.5s

Printer: HP-Deskjet

Title: Online intern: no Online extern: yes Main menu

Language: English

User: Carmen Heiter Unit: [%] Beep: off Areas: off Main menu

First sample: 1 Last sample: 25

Clear data

Main menu

Device: Display

First sample: 5 Last sample: 6 Eliminate Start output Main menu

Device: Printer int.

First sample: 1 Last sample: 25 Start output Main menu

Press. system: H2 p H2 55kPa

H2-pressure: 55kPa p air 0kPa Main menu T oven 130°C

T inj. 220°C Wait until ready T FID 260°C Req. flow H2: 10 ml/7s

Gas flow setup

User configuration Printer configuration System configuration Autosampler Main menu

"Gas flow setup for H2" short column

User configuration

Printer configuration

System configuration

Baudrate: 9600

Data Bits: 8 Stop Bits: 1 Parity: none Protocol: none Main menu

PC-Interface

Autosampler: yes

Injections: 2

Main menu

Autosampler

Balance: Mettler AE Frequency: 50Hz Column: Total Fat Time/Date:

PC-Interface

Main menu

5 Operation

Date: 01.17.03

Time: 17:18 Main menu

Data output p H2 55kPa

Statistic p air 50kPa Clear data T oven 130°C Main menu T inj. 220°C

T FID 260°C

Press.system: H2 p H2 250kPa

H2-pressure: 280kPa p air 0kPa Main menu T oven 150°C

T inj. 220°C Wait until ready T FID 260°C Req. flow H2: 10 ml/10s

long column

short column

"Gas flow setup for air" short column

Press. system: air p H2 280kPa

Air-pressure: 50kPa p air 50kPa Main menu T oven 150°C

T inj. 220°C Wait until ready T FID 260°C Req. flow H2 + air: 20 ml/2.7s

"Data output"

"Statistic"

"Clear Data"

BÜCHI Fat Determination B-820/B-821

Preheating p H2 55kPa Sample weight/Mode p air 50kPa Determination T oven 130°C Data manager T inj. 220°C

Setup T FID 260°C

5.2.1 User configuration

Position cursor on <Setup>.

Position cursor on <User configuration> command.

Language: English

User: Carmen Heiter Unit: % Beep: off Areas: off Main menu

Position cursor on <Language>. Use the OPTION key to select from one of the following languages: English, German, French, Italian or Spanish.

Position cursor on <User>. The user name can be entered. Position cursor on <Unit>. The following parameters may be chosen: [g/100g], [g/kg], [mg/kg], [%], [ppm]. Only the [g/100g] unit is activated for the “Fatty Acids” option.

Position cursor on <Beep>. Use the OPTION key to activate (on) or deactivate (off) signal buzzer which sounds at end of a chromatogram.

Position cursor on <Areas>. Use the OPTION key to activate (on) or deactivate (off) the printing of peak areas at the end of a chromatogram.

Position cursor on <Main menu>.

Gas flow setup

User configuration

Printer configuration System configuration Autosampler Main menu

5 Operation

BÜCHI Fat Determination B-820/B-821

Printer: HP Deskjet

Title: Online intern: no Online extern: yes Main menu

5.2.2 Printer configuration

Position cursor on <Setup> .

Position cursor on <Printer configuration>.

Position cursor on <Printer>.

Use the OPTION key to select the following printers:

HP-Deskjet, HP-Laserjet, Canon, EPSON LX-850, None.

Position cursor on <Title>. An alphanumeric designation can be entered which will subsequently be printed on each report.

Position cursor on <Online intern>. Use the OPTION key to activate (yes) or deactivate (no) the internal printer to print the result after determination.

Position cursor on <Online extern>. Use the OPTION key to activate (yes) or deactivate (no) the external printer to print the result after determination.

Position the cursor on <Main menu>.

Gas flow setup

User configuration

Printer configuration

System configuration Autosampler Main menu

Preheating p H2 55kPa Sample weight/Mode p air 50kPa Determination T oven 130°C Data manager T inj. 220°C

Setup T FID 260°C

5 Operation

BÜCHI Fat Determination B-820/B-821

5.2.3 System configuration

Position the cursor on <Setup>.

The cursor is positioned on <Gas flow setup>. Position the cursor on <System configuration>.

Balance

The cursor is positioned on < Balance>.Use the OPTION key to select parameters for the following balances: Sartorius (MC1 types as well as balances with interface MP8-4), Mettler AE, Mettler AT, A & D (FR, HA series) or none.

Frequency

The cursor is positioned on <Frequency>. Use the OPTION key to select the network frequency (50 Hz or 60 Hz).

Column

The cursor is positioned on <Column>. Use the OPTION key to select between the fast "total fat" determination with the short column and the "fatty acid" determination with the long column.

The cursor is positioned on <Time/Date>.

• The date can be entered (German: DD.MM.YY; English: MM.DD.YY).

• The correct time can be entered (hours, minutes).

Position the cursor on <PC interface>.

Gas flow setup User configuration Printer configuration

System configuration

Autosampler Main menu

Preheating p H2 55kPa Sample weight/Mode p air 50kPa Determination T oven 130°C Data manager T inj. 220°C

Setup T FID 260°C

Balance: Mettler AE Frequency: 50Hz Column: Total Fat Time/Date

PC-Interface

Main menu

5 Operation

BÜCHI Fat Determination B-820/B-821

Gas flow setup User configuration Printer configuration System configuration

Autosampler

Main menu

Autosampler: yes

Injections: 2

Main menu

Preheating p H2 55kPa Sample weight/Mode p air 50kPa Determination T oven 130°C Data manager T inj. 220°C

Setup T FID 260°C

5 Operation

Baudrate: 9600

Data Bits: 8 Stop Bits: 1 Parity: None Protocol: None Main menu

PC-Interface

This menu is meant for the setup of interface parameters for the PC interface. The cursor is positioned on Baudrate.The Baudrate cannot be changed. Position cursor on Data bits. Press the OPTION key to select the number of bits for the transmission.

Position cursor on Stop bits. Press the OPTION key to select <1> or <2>. Press the OPTION key to position parity even/ odd or none.

Position protocol on Software Handshake none or Hardware Handshake RTS/CTS or none.

Position cursor on <Main menu>.

5.2.4 Autosampler configuration

Position cursor on <Setup>.

The cursor is positioned on <Gas flow setup>. Position cursor on <Autosampler>.

The cursor is positioned on <Autosampler>. Press OPTION key to select <Manual injection> (no) or <Autosampler> (yes). Position cursor on <Injections>. The number of injections per sample weight may be selected from 1 to 9. «Total fat» option: max. 9 injections per sample weight. «Fatty acids» option: max. 6 injections per sample weight.

Position cursor on <Main menu>.

BÜCHI Fat Determination B-820/B-821

5.2.5 Preheating/Separation column conditioning

If the unit has been turned off for longer than 30 minutes, the unit must be preheated for 30 minutes before a determination or gas flow setup procedure is performed. If a new column has been installed, the preheating period is 2 hours (separation column conditioning).

Carry out the following steps:

Turn on the gas

Turn on the main power switch to activate the unit. The Büchi logo appears for approx. 2-3 secs. This is followed by the user menu.

Enter user name and check the output pressure (5 bar +/-

0.5 bar or 72.5 psi +/- 0.7 psi).

The venting flap closes, the main menu appears and the pressures build up. As soon as the set pressure values are reached, the heating elements begin to heat up. The cursor is positioned on <Preheating>.

The actual temperature and pressure values are displayed on the right.

pH2: Actual pressure for hydrogen p

air

: Actual pressure for synthetic air

Oven

: Actual temperature for oven

inj.

: Actual temperature for injection heating

FID

: Actual temperature for the flame ionization detector (FID)

Enter the preheating time of 1800 secs (or 7200 secs if the column needs conditioning). The preheating procedure cannot be started until the entered set pressure values and set temperatures have been reached. (Ready LED must be permanently lit). If this is not the case, an error message will appear.

Preheating p H2 55kPa

Sample weight/Mode p air 50kPa Determination T oven 130°C Data manager T inj. 220°C Setup T FID 260°C

SWITZERLAND

Version: 3.00af Gas supply on?

User: C.Heiter Press <ENTER> to cont.

SWITZERLAND

5 Operation

BÜCHI Fat Determination B-820/B-821

Time: 2400s p H2 55kPa

Start preheating p air 50kPa Main menu T oven 130°C

T inj. 220°C T FID 260°C

Position the cursor on <Start preheating>.

The preheating procedure is in operation (running LED is lit up). <Remaining time> shows the remaining preheat time.

If the cursor is positioned on <Stop> and confirmed by pressing the <ENTER> key, the preheat procedure is interrupted and the main menu reappears.

The main menu also reappears when the preheating period is finished. To return directly to the main menu without interrupting the preheating procedure, press the <ESCAPE> key.

5.2.6 Gas flow rate setup

If the unit has been turned off for longer than 30 minutes, the unit must be preheated for 30 minutes before the gas flow rate setup procedure can be performed (see chapter 5.2.5, "Preheating/Separation“ column conditioning).

The flow rate measurement takes place at an oven temperature of 130 °C.

Proceed as follows:

Position the cursor on <Setup>.

The cursor is positioned on <Gas flow setup>.

Stop p H2 55kPa

Main menu p air 50kPa

T oven 260°C T inj. 220°C T FID 260°C

Remaining time 1215s

Gas flow setup

User configuration Printer configuration System configuration Autosampler Main menu

Preheating p H2 55kPa Sample weight/Mode p air 50kPa Determination T oven 130°C Data manager T inj. 220°C

Setup T FID 260°C

5 Operation

BÜCHI Fat Determination B-820/B-821

1. In order to check the hydrogen flow rate, the cursor is positioned on <Press. system: H2> and the air pressure is switched off internally (p air: 0 kPa). Connect the soap bubble meter, containing approx. 2 ml soap solution, to the FID (see figure 19) and wait until the Ready LED lights up.

2. Press the bulb to release a soap bubble. Use a stopwatch to time how long the bubble takes from marker 1 to marker 2 (see figure 20). When using the short column, the time should be 7 ±

0.1 sec (flow rate: 10 ml/7 ± 0.1 sec). When using the long column, the time should be 10 ±

0.1 sec (flow rate: 10 ml/10 ± 0.1 sec).

3. If the stopped time deviates from the set time, the hydrogen pressure must be adjusted accordingly, Position the cursor on H2 pressure and enter new value. Once the ready LED lights up, the flow rate can be remeasured. This procedure should be repeated until the set value has been achieved.

4. Reposition cursor on <Press. system: H2> and press <Option>. The display now reads <Press. system: Air>.

The pressure values “55 kPa” and “250 kPa” are standard values, for total fat and fatty acid modes respectively, and can vary depending on the unit.

Press. system: H2 p H2 55kPa

H2-pressure: 55kPa p air 0kPa Main menu T oven 130°C

T inj. 220°C Wait until ready T FID 260°C Req. flow H2: 10 ml/7 s

Figure 19: Installing the soap bubble meter

5 Operation

Determination "Total Fat" (short column)

Press. system: H2 p H2 280kPa

H2-pressure: 280kPa p air 0kPa Main menu T oven 150°C

T inj. 220°C Wait until ready T FID 260°C Req. flow H2: 10 ml/10 s

Determination "Fatty Acid" (long column)

BÜCHI Fat Determination B-820/B-821

Press. system: air p H2 55kPa Air-pressure: 50kPa p air 50kPa

Main menu T oven 130°C

T inj. 220°C Wait until ready T FID 260°C Req. flow H2+air 20 ml/2.5 s

Press. system: air p H2 55kPa Air-pressure: 50kPa p air 50kPa

Main menu T oven 130°C

T inj. 220°C

T FID 260°C Req-flow H2+air: 20 ml/2.5 s

5. To check the air flow rate, the cursor is positioned on

<Press. system: Air> during which the air pressure is built up. Wait until the actual pressure value is identical to the set pressure value on display (Ready LED lights up).

6. Press the bulb to release a soap bubble. Use a stopwatch to time how long the bubble takes from marker 1 to marker 3 (see figure 20). When using the short column, the time should be 2.5 ±

0.1 sec (flow rate: 20 ml/2.5 ± 0.1 sec). When using the long column, the time should be 2.7 ±

0.1 sec (flow rate: 20 ml/2.7 ± 0.1 sec).

7. If the stopped time deviates from the set time, the air pressure value must be adjusted accordingly (position the cursor on air pressure and enter new value). Once the Ready LED lights up, the gas flow should be remeasured.

8. Dismantle the soap bubble meter from the FID.

Wear gloves or use a small towel for dismantling as the screw is very hot.

Ensure that the soap bubble meter is removed from the FID before returning to the main menu.

9. Position the cursor on <Main menu>.

While switching to the main menu the FID ignites automatically. The oven temperature is set again according to the adjusted mode.

Preheating p H2 55kPa Sample weight/Mode p air 50kPa

Determination T oven 130°C

Data manager T inj. 220°C Setup T FID 260°C

5 Operation

Determination "Total Fat" (short column)

Press. system: air p H2 280kPa

Air-pressure: 50kPa p air 50kPa Main menu T oven 150°C

T inj. 220°C Wait until ready T FID 260°C Req. flow H2+air: 20 ml/2.7 s

Determination "Fatty Acid" (long column)

BÜCHI Fat Determination B-820/B-821

Figure 20: Measuring the gas flow rate with a digital stop watch, counting in 1/

100

th of a second interval.

10 ml

Marker 3

20 ml

Marker 2

Marker 1

5 Operation

Re-check the gas flow rate and the supply lines for leakages (see Section 4.7, Checking supply lines for leaks) each time the gas cylinder or column is changed as well as after service interventions.

BÜCHI Fat Determination B-820/B-821

5.2.7 Sample weight and mode adjustment

Position the cursor on <Sample weight/Mode>.

Manual sample weight

If no balance is connected to the B-820, the sample weights must be entered manually in the sample weight table using the keypad. Confirm “Manual sample weight” with “ENTER”. The sample weight table appears.

Automatic sample weight

For this option, a balance must be connected as described in Chapter 4.4. Confirm “Automatic sample weight” with “ENTER”. The sample weight table appears. After selecting the mode, move the cursor to the next field (Weight [g] with “ENTER”. When the weight has been transferred, the cursor moves to the next field in a similar way to the “Manual sample weight”.

Factors

The current factors are entered here. These valves are incaporated in the final result. Confirm with “ENTER”. The factor table will then appear.

Manual sample weight

When the sample weight table appears, the cursor will be located at the first free sample number (No.). After selecting the mode, enter the weight (in grams) for each sample and the internal standards. Confirm each entry with “ENTER”. Depending on the mode selected, the cursor will automatically move to the next available field.

Automatic sample weight

When the sample weight table appears, the cursor will be located at the first free sample number (No.). After selecting the mode, transfer the weight (in grams) for each sample and the internal standards for the connected balance type. Depending on the mode selected, the cursor will automatically move to the next available field.

Preheating p H2 55kPa

Sample weight/Mode p air 50kPa

Determination T oven 130°C Data manager T inj. 220°C Setup T FID 260°C

Manual sample weight

Automatic sample weight Factors

Main menu

5 Operation

No. Mode Weight Weight Weight Conc.

[g] C13 [g] C5 [g] [%] 1 fact.gen. 0.7055 0.2115 99.8 Name: Factor 2 Fact.b.a. 0.055 0.054 99.5 Name: Factor C4 3 But.acid 0.8550 0.2134 0.056 Name: Butter 4 gen.corr. 4.3575 0.1245 Name: Wheat 5 spec.corr. 2.3654 0.2056

Name: Cheese

Sample weight table

No. Number of the sample in the sample weight table. Mode Determination mode used, which is selected dependent on the sample type ((See Chapter 3, Table 6). Select the mode with “OPTION” and

confirm with “ENTER”. Weight [g] Weight of the sample, which is entered in g. Confirm the weight with “ENTER”. Weight C13 [g] Weight of the internal standard (tridecanoic acid), which is entered in g. Confirm the weight with “ENTER”. Weight C5 [g] Weight of the internal standard (valeric acid), which is entered in g. Confirm the weight with “ENTER”. Conc. [%] Concentration of the fat standard (e.g., pork fat, 99.8% or concentration, depending on the standard used) and/or the butyric acid (e.g.,

butyric acid, 99.5% or according to purity used) that will be necessary for the determination of the factor. This column is only selected in the

modes “Gen.fact.”, “FA-fact.” and “Butyr.fact”. It is skipped over in all other modes. Name Sample identification (sample name) entered from the keypad and confirmed with “ENTER”.

Key for Sample weight table:

BÜCHI Fat Determination B-820/B-821

Manual sample weight

Automatic sample weight Factors

Main menu

5 Operation

After the sample identification (Name) has been entered and been confirmed with “ENTER”, the cursor automatically moves to the next free cell. In doing this, the mode of the previous sample will also be transferred, and must be changed - where required - using the “OPTION” key. The fields “Weight [g]”, “Weight C13 [g]”, “Weight C5 [g]”, “Conc. [%]” and “Name” fields of the previous row can be copied into the current row one after the other by pressing the “OPTION” key.

Within the column, you can move between the fields of each sample number with “SELECT”.

You can move to the first sample number (No. 1) with the key combination “SHIFT” + “SELECT” (upward arrow), and to the last sample number with the key combination “SHIFT” + “SELECT” (downward arrow). For the “Total Fat” option, the sample memory contains 75 samples (No. 75), and 48 samples (No. 48) for the “Fatty acids” option.

After completing the entries, press “ESCAPE” to exit the Sample Weight table. To switch to the Main Menu, place the cursor on “Main Menu” with “SELECT” and confirm with “ENTER”. Or press “ESCAPE” twice after completing the entries to move directly to the Main Menu.

Select the “Factors” menu with “SELECT”, and confirm with “ENTER”. The Factors table then appears.

BÜCHI Fat Determination B-820/B-821

5 Operation

Factors table

Fat factor

Entry of the factor that will be used for the determination in the “gen.corr.” and “spec.corr.” modes.

Butyric acid factor

Entry of the factor that will be used for the butyric acid determination in the “but.acid” mode.

Entry of the correlation factor. This factor is required in the “but.acid” mode for the conversion of the butyric acid content to the milk fat.

Blank value of the butyric acid

Entry of the blank value in g, which will be required for the determination of the butyric acid. (“Fact.b.a.” mode).

After completing the entries, press “ESCAPE” to exit the Factors table. To switch to the Main Menu, place the cursor on “Main Menu” with “SELECT” and confirm with “ENTER”. Or press “ESCAPE” twice after completing the entries to move directly to the Main Menu.

All the inputs made in “Factors” must be updated by the user himself. A factor will not be automatically overwritten or changed. The calculation of the results takes place on the basis of the stored factors. If one of the factors is changed after the start of the determination, the calculation will always be carried out with the factors stored at the time of the evaluation (= end of the analysis run).

5.2.8 Determination

Once the sample weights have been entered, the determination can be started.

Factor Fat: 0.953 Factor butyric acid: 1.023 CF: 28.570 Blank value but. acid 0.0031 g

Main menu

Factors table

Preheating p H2 55kPa Sample weight/Mode p air 50kPa

Determination T oven 130°C

Data manager T inj. 220°C Setup T FID 260°C

BÜCHI Fat Determination B-820/B-821

5 Operation

Determination with the Autosampler

Sample No.

Enter the sample number (from the sample weight table) with which the determination should be started. Confirm it with “ENTER”; the cursor moves to the next row. The corresponding sample identification (Name), the injection number (here the second injection) and the sample-specific determination mode (“spec.corr.”) will be shown in the display.

Vial No.

Position of the sample (sample vial) in the sample carousel of the Autosampler, in which the sample (Sample No.) that is to be determined is located.

It must be ensured that the sample number corresponds to the content of the sample vial. To facilitate the overview, sample numbers are selected to be the same as the vial numbers.

Switching off

Can be set to “YES” or “NO” with “OPTION”. “YES” means that the temperature will be reduced to room temperature after the end of the last determination, and that the gas feed for the hydrogen and synthetic air will then be switched off via the valves. These settings are equivalent to a “STAND-BY” mode (energy-saving mode). If the system finds itself in “STANDBY” after the last determination, the display will indicate “The determination finished correctly”.

“The determination finished correctly” Here, the system will be in a pressure-free condition. The following work can be carried out: – Column change – Septum change in the injector – Refilling of the gas saturation vessel with formic acid, 85%

(purity)

“NO” means that all temperatures and the gas feed take on the settings of the “READY” mode after the end of the last determination (see Chapter 5.1). The “READY” LED indicates that the system is ready to carry out measurements.

Start

The determination is started with the “START” function (the cursor must be on “START”) and “ENTER”. This automatically initiates the rinsing of the syringe and the selection of the corresponding sample vial. If a “Preheating” should be carried out, or the system is carrying out a conditioning (“Running” LED illuminated), the number of seconds remaining before the first injection can take place will be indicated in the “Start” line (in this case, 62 seconds).

Sample no: 5 p H2 55 kPa Vial no: 5 p air 50 kPa Switch off: yes T oven 140°C Start after 62s T inj. 220°C Main menu T FID 260°C

spec.corr

Name: cream cheese

BÜCHI Fat Determination B-820/B-821

5 Operation

Procedure

The sample will be injected automatically. The corresponding temperature program runs automatically in the background according to the determination mode (see Chapter 3, Table

7). At the end of the determination, the venting flap opens; the oven area will be conditioned in order to prepare the system for the next determination. The evaluation takes place automatically, and will be printed out depending on the printer configuration (see Chapter 5.2.2). The next injection takes place as soon as “Ready for Injection” appears in the display (the “READY” LED lights up). This procedure will continue until there are either no more sample vials in the carousel or no more sample weights in the sample weight table.

The number of injections per sample will be entered under “Autosampler” in the “Setup” menu (see Chapter 5.2.4). A maximum of 9 injections per sample vial are provided for the “Total fat” option and a maximum of 6 injections per sample vial for the “Fatty acids” option.

“Memory full” appears if the maximum number of injections has been exceeded. The determination series will be terminated prematurely in this case.

A determination series can be interrupted with the key combination “SHIFT S”. The determination that is currently running will be ended, the syringe will be rinsed and the sample carousel will be moved to its home position (Position 1).

The sample carousel may not be moved or be swung to the side during a determination series. This will lead to a termination of the series. Additional sample vials can be added at any time, however, whereby the sample weight and/or factors must also be added in the respective tables.

Figure 21a: Factor determination report (short column) with printout of the bottles; internal printout

BÜCHI Fat Determination B-820/B-821

5 Operation

Sample no: 5 p H2 55kPa Next number p air 50kPa

T oven 89°C T inj. 220°C

Main menu T FID 260°C

Wait until ready spec.corr. Name: cream cheese

Sample no: 5 p H2 55kPa Next number p air 50kPa

T oven 90°C T inj. 220°C

Main menu T FID 260°C

Ready injection 2 spec.corr. Name: cream cheese

Figure 21b: Fat determination report (short column) without printout of the vials; internal printout

Figure 21c: Factor determination report (long column) without printout of the vials; internal printout

Determination with manual syringe

Sample No.

Entry of the sample number (from the sample weight table) that should be determined as the next sample. is Confirm this with “ENTER”; the cursor moves to the next row. The corresponding sample identification (Name), the injection number (here the second injection) and the sample-specific determination mode (“spec.corr.”) will be shown in the display.

If the set temperatures and pressures have not been reached, or as long as “Preheating” is running, the message “Wait until ready” will be shown on the display. In this case, no LED will be illuminated, or the “Running” LED will be on.

Procedure

If the set values are reached, the “READY” LED lights up, and the message “ready injection” appears in the display (in this case, the second injection). After carefully rinsing the syringe with n-butanol, 2 ml of extract (upper phase) are now injected into the injector port using the microliter syringe. The temperature program starts automatically after the injection. The corresponding temperature program runs automatically in the background according to the determination mode (see Chapter 3, Table 7). At the end of the determination, the venting flap opens; the oven area will be conditioned in order to prepare the system for the next determination. The evaluation takes place automatically, and will be printed out depending on the printer configuration (see Chapter 5.2.2). The next manual injection can take place as soon as “Ready for Injection” appears in the display (the “READY” LED lights up).

BÜCHI Fat Determination B-820/B-821

Device: Printer int.

First sample: 1 Last sample: 25 Start output Main menu

Data output p H2 55kPa

Statistic p air 50kPa Clear data T oven 130°C Main menu T inj. 220°C

T FID 260°C

5 Operation

5.2.9 Data output

Set the cursor on “Data manager” and confirm with “ENTER”.

Device

The desired type of output can be selected with “OPTION” in this row.

Possible selections for the device

•“display”: Display of the data on the display; “Display” is

the default setting.

•“internal printer”: printout of the data on the internal

printer.

•“external printer”: printout of the data on an external

printer (see Chap 5.2.2).

First sample

Entry of the first sample number of wich the report shall begin. Confirm entry with “ENTER”.

Last sample

Entry of the last sample number of the report. Confirm entry with “ENTER”.

Start output

Start the output. Move the cursor to the “Start Output” row and start the output with “ENTER”.

Once the results have been output to the display, you can jump back to the previous menu with “ESCAPE”.

The subsequent data output (Fig. 21d) includes the data of the sample identification, the sample weights, the user, and the result(s) of each injection. The chromatograph will not be printed out here. The ON-line mode (see Chapter 5.2.2) has to be activated for a printout of the chromatogram.

Preheating p H2 55kPa Sample weight/Mode p air 50kPa Determination T oven 130°C

Data manager T inj. 220°C

Setup T FID 260°C

Figure 21d:

Data output of the results (total fat)

BÜCHI Fat Determination B-820/B-821

5 Operation

Place the cursor on “Main Menu” and confirm with “ENTER”.

What will be printed out?

Data output “Display”

For all modes, only the data of the “first sample” (inc. all injections) will be shown in the display. The “last sample” field is not active in the “Display” data output mode. In the above example, only the data of sample number 5 will be displayed, including all injections. In the “fatty acids” option, all the user data and the results for total fat, the sum parameters and the contents for FA/TG (Fatty Acid/Trigylceride) of each injection will be displayed. In all other modes, the sample and user data and the results of each injection will be displayed.

Data output “internal printer”

The data from the “first sample” to the “last sample” will be output to the internal printer. With the “Fatty acid” option, the user data and the results for total fat, the sum parameters and the contents for FA/TG (Fatty Acid/Trigylceride) of each injection will be printed out (see Fig. 21e). In all other modes, the sample and user data and the results of each injection will be printed out (see Fig. 21d).

Data output “external printer”

The data from the “first sample” to the “last sample” will be output to the external printer. With the “Fatty acid” option, the user data and the results for total fat, the sum parameters and the contents for FA/TG (Fatty Acid/Trigylceride) of each injection will be printed out (see Fig. 21f). In all other modes, the sample and user data and the results of each injection will be printed out.

Once the output is completed, press “ESCAPE” once to exit the data output area. To switch to the Main Menu, place the cursor on “Main Menu” with “SELECT” and confirm with “ENTER”. Or press “ESCAPE” twice after completing the entries to move directly to the Main Menu.

Device: Printer int. First sample: 1 Last sample: 25 Start output

Main menu

Figure 21e: Data output of the results (fatty acids) to the internal printer

Figure 21f: Data output of the results (fatty acids) to the external printer

BÜCHI Fat Determination B-820/B-821

5 Operation

Content value x

Figure 22a: Sample statistics

Sample 1 Sample 2 Sample M

Figure 22b: Group statistics

CONTENT VALUE X

→→

→

→→

→

5.2.10 Statistics

Sample statistics

Up to 9 injections can be carried out with the same sample. The following characteristics are obtained from these values :

• Average sample value:

• Standard sample deviation:

• Sample variation coefficient:

Group statistics

Several samples can be grouped together to form a sample group. The following characteristics are obtained from these values :

• Average group value:

• Standard group deviation:

• Group varation coefficient:

S =

n i=1

(x – x )

n–l

v =

100.

(x )

v =

100.

i: N

umber of the sample

”Total fat” option:

i= 1, 2, ... m with m= 1, 2, ... 75

”Fatty acids” option:

i= 1, 2, ... m with m= 1, 2, ... 48

Number of injections carried out per sample ”Total fat” option:

n= 1, 2, ... 9

”Fatty acids” option:

n= 1, 2, ... 6

Number of samples that should be statistically evaluated; has the same significance as the number of tests of the same sample ”Total fat” option:

m= 1, 2, ... 75

”Fatty acids” option:

m= 1, 2, ... 48

xi:

Mean sample value from the values (e.g., fat content) of the i

sample

xg:

Group mean value from mean sample values (xi) of all m samples

Sg:

Group standard deviation of the sample relative to a random sample.

Group variation coefficient of the sample (= relative standard deviation)

Key to the group statistics:

Key to the sample statistics:

i: Number of the injection

”Total fat” option: i= 1, 2, ... n with n= 1, 2, ... 9 ”Fatty acids” option: i= 1, 2, ... n with n= 1, 2, ... 6

n: Number of injections carried out per sample

”Total fat” option: n= 1, 2, ... 9

”Fatty acids” option: n= 1, 2, ... 6 xi: Result (e.g., fat content) of the ith injection xP: Mean value from values (xi) of a sample Sg: Standard deviation of the sample relative to a random sample : Variation coefficient of the sample (= relative standard

deviation)

BÜCHI Fat Determination B-820/B-821

Data output p H2 55kPa

Statistic p air 50kPa

Clear data T oven 130°C Main menu T inj. 220°C

T FID 260°C

5 Operation

Set the cursor on “Data manager” and confirm with “ENTER”.

Set the cursor on “Statistic” and confirm with “ENTER”.

The Statistics function is only activated for the “Total fat” option (total fat, butyric acid, factors, blank value butyric acid). For the “fatty acids” option, the Statistics function is only activated for software version V3.0 and higher. In this way, statistics for the total fat content and the factor can be calculated.

Device

In this row, the desired type of output unit can be selected with “OPTION”.

Possible selections

(“OPTION”) for the device (Device)

•“Display”: Display of the data on the display; “Display” is

the default setting.

•“internal printer”: printout of the data on the internal

printer

•“external printer”: printout of the data on an external

printer (see Chap 5.2.2)

First/Last sample

Entry of the first/last sample number for the statistic interval. Confirm each entry with “ENTER”. If the first and last sample numbers are the same, the sample statistics will be calculated; otherwise the calculation of the group statistics will be carried out.

Preheating p H2 55kPa Sample weight/Mode p air 50kPa Determination T oven 130°C

Data manager T inj. 220°C

Setup T FID 260°C

Device: Display First sample: 5 Last sample: 6

Eliminate

Start output Main menu

BÜCHI Fat Determination B-820/B-821

5 Operation

Figure 23a: “Total fat” statistics report, internal printer (“Total fat”/”fatty acids” option)

Figure 23b: “Total fat” statistics report, external printer (“Total fat”/”fatty acids” option)

No Name Result Elim

5. 1 Cereal 1 7.23g/100g yes

5. 2 Cereal 2 7.26g/100g no

5. 3 Cereal 3 7.28g/100g no

6. 1 Cereal 4 7.32g/100g no

6. 2 Cereal 5 7.30g/100g no

6. 3 Cereal 6 7.28g/100g no

Elimination

The elimination of individual measurements. Place the cursor on the “Eliminate” row and confirm with “ENTER”. A table of the available measurements will appear; each measurement is specified by its sample number (e.g., 5.1, 6.1), the number of the injection (e.g., 5.1, 6.1) and the sample name. The cursor can be moved to the desired sample name/ measurement using the “SELECT” key. In the “Elim” column, a measurement can be selected with “YES” and be deselected with “NO” by pressing the “OPTION” key. If the measurement is selected, it will not be included in the statistics. The cursor is moved to the next sample with “SELECT”. With “ESCAPE”, you arrive in the Statistics menu, where you can start the calculation of the statistics with “Start output”.

Start output

Start the output. Move the cursor to the “Start Output” row and start the output with “ENTER”.

When using an Autosampler, the current status of the determination series can be called up via the “Eliminate” function. All samples that have already been determined will be listed in the table (“Eliminate”).

BÜCHI Fat Determination B-820/B-821

5 Operation

5.2.11 Clearing data

Place cursor on “Data manager” and confirm with “ENTER”.

Place the cursor on “Clear data” and confirm with “ENTER”.

First/last sample

Entry of the first/last sample number, which determine the sample interval to be cleared. Confirm each entry with “ENTER”.

Clear data

Clear the sample identification and the result in the defined interval (first to last sample number). After placing the cursor on “Clear data”, confirm the function with “ENTER”. Sample data will be actively cleared, and the message “Data has been cleared” appears.

Place the cursor on “Main Menu” and confirm with “ENTER”.

First sample: 1 Last sample: 25

Clear data

Main menu

First sample: 1 Last sample: 25 Clear data

Main menu

Preheating p H2 55kPa Sample weight/Mode p air 50kPa Determination T oven 130°C

Data manager T inj. 220°C

Setup T FID 260°C

Dat output p H2 55 kPa Statistic p air 50 kPa

Clear data T oven 130°C

Main menu T inj. 220°C

T FID 260°C

BÜCHI Fat Determination B-820/B-821

6 Maintenance

6.1 Control checks

All regulations designed to ensure that the Fat Determination Unit is kept in proper working order must be complied with. These include periodic cleaning and inspections to check for possible damage.

6.2 Replacing the septum in the injection head

The septum needs replacing after approx. 100 injections. These can be ordered from Büchi.

When a column is replaced a new septum must be installed. Only replace the septum when the unit is turned off. The unit must be in a room temperature, pressure -free state.

To replace the septum in the injection head, proceed as follows:

1. Open top cover of unit

Switch off the unit and allow to cool down.

2. Unscrew the injection head ring

3. Remove old septum

4. Insert new septum

5. Screw injection head ring back in place

6. Close top cover of unit

Figure 24: Replacing the septum in the injection head

6 Maintenance

BÜCHI Fat Determination B-820/B-821

6.3 Cleaning the FID

1. Switch off unit

Allow unit to cool down

2. Disconnect detector cable (= signal cable )

3. Disconnect ignition cable

4. Loosen main arm of FID's top body

5. Remove FID's top body

6. Unscrew the jet with the wrench (Order No. 036678); jet sits inside the FID's base body

7. Clean jet with fine wire and clean the collector, if necessary

8. Reinstall FID (ensure that all sealings are reinstalled)

6.4 Replacing the ignition coil

1. Switch off unit

Allow unit to cool down

2. Disconnect ignition cable 햲

3. Loosen threaded joint and remove 햳

4. Insert new ignition coil and retighten threaded joint

5. Reconnect ignition cable

Figure 26: Replacing the ignition coil

Figure 25: Cleaning the FID

6 Maintenance

햳

햲

햳

햴

햵

햴

햶

BÜCHI Fat Determination B-820/B-821

6.5 Checking the formic acid

The volume of formic acid shown on the back of the unit must be checked at regular intervals, e.g. each time the gas cylinder is changed. If the formic acid is replaced or added, wait approx. 10 minutes after filling before starting the unit. The unit must be preheated for 40 minutes after filling before a determination procedure is carried out.

Caution: the container is under pressure

• Do not open if the B-820 is warm or is in operation

• Do not refill if the B-820 is warm or is in operation

• Do not overfill, max. 20 ml or at less 1 cm below the vessel's arms!

• Only fill when the unit is turned off and is at room temperature

• Filling under any other circumstances may lead to system contamination!

6.6 Installing a new separation column

Loosen the threaded column joint and carefully remove the old column. The new column can then be fitted as described in Section 4.8, "Installing the separation column“.

When installing a new separation column, ensure that there is used a new septum in the injection head, and use new vespel seals for the new column as well. If a new column is installed, it must be preheated for 120 minutes before any injections can be done (see Section 5.2.5 "Preheating/Conditioning of separation column“).

6.7 Changing the printer paper roll

Place the paper roll in the holder and feed the end of the paper through the upper slit.

Press the «Paper» key until the paper reappears through the front opening.

Figure 27: Changing the printer paper roll

6 Maintenance

BÜCHI Fat Determination B-820/B-821

6.8 Changing the ribbon

Press lightly on the left hand side of the ribbon (<Push>) - this enables the ribbon to be lifted out. Feed the paper into the slit of the new ribbon, insert the new ribbon and press down lightly.

6.9 Checking for fractures and cracks

Check the gas connections and separation column for possible fractures and cracks before each use. The unit must not be operated if the separation column is damaged.

6.10 Customer service

Work on or in the unit must only be carried out by authorized service personnel, i.e. skilled technicians who are familiar with the operating instructions and current safety regulations and accident prevention.

Büchi service centers have instrument specific service manuals which are only available to authorized personnel.

There is a list of the Büchi customer service centers on the last page of this instruction manual. For any application or technical question as well as unit malfunctions, please contact one of these centers.

Büchi customer service representatives are pleased to provide the following services:

• Replacement parts service (when placing an order, please use the article numbers printed in this manual)

• Repair service

• Maintenance service

• Technical hotline

6 Maintenance

BÜCHI Fat Determination B-820/B-821

6.11 Maintenance of the Autosampler

6.11.1 General

Optimum performance of the Autosampler is ensured by routine and preventive maintenance procedures. The procedures described below should reflect the frequency and duration with which the Autosampler is used.

6.11.2 Syringe and syringe needle

Dangerous chemicals, use eye and skin protection measures.

Cleaning

Remove the needle from the syringe before attempting the cleaning procedures described below.

As only clear solvent is used, cleaning is only necessary occasionally. If, however, the inner surfaces of the syringe are soiled or discoloured, the syringe must be rinsed once again using a suitable solvent.

Needle replacement

To replace the needle, proceed as follows:

• Loosen the knurled nut

• Remove the old needle from the syringe

• Fit the new needle

• Retighten the knurled nut

• Mount the syringe on the syringe mounting bracket

• Check that the needle is positioned correctly

• Rinse out the syringe several times (press “Start”, “Shift S” and repeat, see Chapter 5.28)

6.11.3 Replacing the main power fuse

To replace the main power fuse, proceed as follows:

• Pull the power plug at the rear of the Autosampler

• Open the cover of the fuse module (refer to Figure 15, paragraph 4.11.8 power voltage connection at the Autosampler B-821) with a narrow screwdriver

• Snap out the defective fuse

• Insert a fuse of the same voltage and amperage

• Replace the cover

6 Maintenance

BÜCHI Fat Determination B-820/B-821

7 Taking out of operation

7.1 Switching off the unit

Before the unit is switched off, it is recommended to complete the running analysis. Once the analysis has ended, the LED display changes from “RUNNING” to “READY”. The unit can now be switched off using the main switch on the back of the unit. The unit can also be switched off directly from the “Energysaving mode” (see Chapter 5.2.8 Determination with Autosampler). When “The determination finished correctly” appears on the display, the unit can be switched off using the main switch on the back of the unit.

7.2 Storage/Transport

The units should be stored and transported in their original packaging and in clean condition.

Ensure that the separation column has been removed from the oven of the B-820 unit and farmic acid vessel emptied before moving the unit.

7.3 Disposal

To ensure that disposal of the B-820 and B-821 units is as environmentally friendly as possible, a list of the materials used, some of which are marked with material codes, is provided in Section 9.3, "Materials used". This ensures that components can be separated and, where appropriate, recycled.

Care must be taken that regulations are complied with, when disposing of electrical components. Furthermore, all methods of disposal should comply with regional and local legislations.

7 Taking out of operation

BÜCHI Fat Determination B-820/B-821

8 Replacement parts

Only original Büchi accessories and replacement parts guarantee the operational safety and reliability of this unit. Use of any replacement parts or accessories other than Büchi is only permitted with the express permission of the manufacturer. For assembly and dismantling purposes, replacement parts should only be used as described in Section 6 "Maintenance"of this instruction manual. Inspection by or assignment to an unofficial third party is prohibited. The reproduction or manufacture of any parts found in this manual is also prohibited.

Replacement parts detection unit B-820 Order no.

Paper roll 26341 Printer ribbon 26400 FID ignition coil 27275 Syringe 10 µl 34258 Needle D5/0.18 36654 Gas saturation vessel 34361 Soap bubble meter, compl. 34878 High-temperature septum (50 off) 34382 Threaded column joint 1/4" 34228 Vespel seal 34229 Separation column "Total fat" 34916 Key for FID nozzle 36678 Separation column "Fatty Acid" 37620 Calibration Set "Fatty Acid" 37622

Table 8: Replacement parts B-820

Replacement parts Autosampler B-821 Order no.

Hamilton syringe 37066 Needle for Hamilton syringe 37067 Sample vessels 2mL, compl. (100 off) 37068 Glass bottle for rinsing solvent and waste 37069 Carousel 37085 Serial number label for carousel 37103

Table 9: Replacement parts B-821

BÜCHI Fat Determination B-820/B-821

9 Appendix

9.1 Technical data

B-820

Unit dimensions, 470 x 370 x 430 mm (width x height x depth)

Packaging dimensions ••• (width x height x depth)

Weight (net) 30.4 kg

Line voltage 230 V/50/60 Hz

200 V/50/60 Hz

Power input* max. 2 kW

Current consumption max. 9A

Ambient temperature 5 – 40°C

Table 10: Technical data B-820

B-821

Unit dimensions, 155 x 495 x 400 mm (width x height x depth)

Packaging dimensions, 630 x 460 x 680 mm (width x height x depth)

Weight (net) 10.9 kg

Vial capacity 48

Line voltage 230 V/50/60 Hz

Power input 55 VA

Ambient temperature 10 – 40°C

Table 11: Technical data B-821

* When using a transformer (120 V -> 230 V), the latter must have a

power consumption of at least 3 kW.

9 Appendix

BÜCHI Fat Determination B-820/B-821

9.2 Error messages

The unit is equipped with a comprehensive error message system, which will inform the user of the steps that can be taken when a system error occurs or following an incorrect application.

9 Appendix

Error Description Correction of the error Error 01 Gas flow is not correct. The air or the hydrogen pressure

is outside the tolerance range of ± 3kPa for more than 2 minutes.

Check:

1. Gas supply / re duction valve

2. Seal of the gas saturation vessel

3. Septum in the injection head

4. Assembly of the column

5. The column and the Vespel seal for cracks

Error 02 Temperature control of the oven is not OK. 1. Check that the oven door is completely closed

2. Check the Preheating rate: start a pre-heating cycle, and measure the time

necessary for the oven to heat up T(Start) > T(Stop) 90 °C > 250 °C: max. 2’30” 130 °C > 250 °C: max. 1’50” 150 °C > 250 °C: max. 3’30” If these target times are exceeded, please contact your local Büchi Service office or Büchi Labortechnik AG (see Chapter 6.10).

Error 03 The temperature control of the injection head and/or the

FID is not OK. The temperature of the injection head and/or the FID is outside the tolerance range of ± 3 °C for mo re than 2 minutes.

Defective heating cartridge or temperature sensor; please contact your local Büchi Service office or Büchi Labortechnik AG (see Chapter 6.10).

Error 04 The FID signal is outside the measurement range. Check:

1. The quality of the gas

2. The quality of the formic acid (85% purity)

3. FID for possible deposits (clean jet if necessary See Chapter 6.3)

Error 05 The communication between the unit keypad and the

display does not work. This error message is also output from the internal printer.

Defect in the electronics. Please contact your local Büchi Service office or Büchi Labortechnik AG (see Chapter 6.10).

Error 06 The pressures and the temperatures do not correspond to

the set values. This error message is given if a “Heating off” or a determination is started too soon. The unit is n ot in a condition in which it can make measurements.

Wait until the “READY” LED lights up.

Error 07 The external printer is not ready or is not connected. Check:

1. The functionality of the printer

2. That the printer is connected using the corresponding printer cable

3. The selection of the correct printer type in the C onfiguration menu

Error 08 The internal printer does not function. Defective communication between the printer and the electronics.

Please contact your local Büchi Service office or Büchi Labortechnik AG (see Chapter 6.10).

Error 09 The connection to the external PC does not function. Check:

1. The connection of t he PC via the corresponding communication cable (029502)

2. PC settings in the Configuration menu

Error 10 Either no balance is connected, or is not correspondingly

configured.

Check:

1. The connection of the balance using the correct communication cable

2. The selection of the corresponding balance type in the Configuration menu

3. The parameter settings of the balance (parameters for the weight transfer)

Error 11 Unexpected injection.

A signal has been detecte d on the FID without opening the Determination menu and/or without having started a determination in the Determination menu.

Proceed a “Preheating” for at least 360 seconds.

Error 12 “Preheating” is running. This error message occurs if an

attempt is made to start a determination or to check the flow during the “Preheating off” time.

Wait until the “Preheating” is finished or stop the “Preheating” and continue.

Error 13 No FID signal. This error message is only output during a

sample change operation, if no measurement signal is detected on the FID after injecting twice.

Check:

1. The filling of the sample vial (air injected?)

2. The passage through the injection needle

3. The ignition spiral in the FID (does the ignition spiral glow when “SHIFT” is

pressed in the Determinatio n menu?)

Error 14 The connection to the Autosampler does not function. Check:

1. That the connection cable is connected

2. That the Autosampler is ready for operation (close the carousel holder, wait until

the injection carriage is positioned)

Error 15 The Autosampler is not ready for operation. The Auto-

sampler controller has detected a faulty operational mode, and will not operate further.

Please contact your local Büchi Service office or Büchi Labortechnik AG (see Chapter 6.10).

Error 16 A determination is running. This error message appears if

an attempt is made to start a “Preheating” or to check the flow during the “determination” is running.

Wait until the “determination” is finished.

Error 17 Loss of the specific calibration data for the unit. Please contact your local Büchi Service office or Büchi Labortechnik AG

(see Chapter 6.10.

If the error re-appears continually (even after switching the unit off and on again), and the error cannot be corrected, please contact your local Büchi Service office or Büchi Labortechnik AG (see Chapter 6.10).

BÜCHI Fat Determination B-820/B-821

9 Appendix

If the measuring results continue to deteriorate, check the following possible sources of error:

1. Extraction procedure insufficient (e.g. time)

2. Poor gas quality

3. Sufficient formic acid in the bottle

4. Separation column possibly defective or worn

5. Preheating time too short

6. Incorrect mode selected

7. Incorrect sample weights entered

8. Incorrect factor entered

9. Faulty injection technique

10. Incorrect injection volume

11. Air injected

12. Injection needle not fitted securely (solution is leaking from needle)

13. Needle clogged

14. Insufficient flow rate

15. FID dirty

Before you assume that the Autosampler B-821 is faulty, make one or more injections by hand. If the problem remains, check the Autosampler. While it is frequently assumed that the sampler is defective, the problem may rather be caused by the B-820 unit.

9.3 Materials used

Description Materials:

Oven Insulations:

Doors: Insultherm 550

Exhaust: Insultherm 550

Air inlet: Insultherm 550

Exhaust duct: Insultherm 550

Exhaust flap: Insulglatex 620

Top: Insultherm 550

Bottom: Insultherm 550

Back: Insultherm 550

Sides: Microtherm

Foil keypad:

Carousel (B-821) Polymerplastic

Various lines (B-821) PTFE

Other materials used:

Metals: Steel, aluminium, brass

Glass parts: Soap bubble meter of

borosilicate glass Separation column of borosilicate glass Gas saturation vessel of Pyrex

Electrical components: Various printed circuitboards,

hot-air fan, axial ventilator, lifting magnet

Table 12: Materials

BÜCHI Fat Determination B-820/B-821

9 Appendix

9.4 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 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 règlementation FCC à la règlementation des radio-interférences du Canadian Department of communications. Ces limites sont destinées à fournir une protection odéquate contre les interférences nétastes lorsque l'appareil est utilisé dans un environnement commercial.

Cet appareil génère, utilise et peut radier une énergie à fréquence radioélectrique, il est en outre susceprible d'engendrer des interferences 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 nèfastes, auquel cas l'exploitant sera amené à prendre les dispositions utiles pour polier aux interférences à ses propres frais.

BÜCHI Fat Determination B-820/B-821

9.5 Declaration of conformity

BÜCHI Labortechnik AG Postfach, CH-9230 Flawil Switzerland

declare under our sole responsibility that the product:

BÜCHI Fat Determination B-820/B-821

to which this declaration relates is in conformity with the following standards:

EN 61010-1:1993 (~ IEC 1010-1, VDE 0411-1) Safety requirements for electrical equipment for mesurement, control and laboratory use: General requirements

EN 55011:1991/B (~ VDE 0875/B, VDE 0871/B) Limits and methods of measurement of radio disturbance characteristics of industrial, scientific and medical radiofrequency equipment

EN 50082-1:1992 Electromagnetic compatibility - Generic immunity standard: Residential, commercial, light industry.

EN 60555-2:1987 (~ IEC 555-2) Disturbances in supply systems caused by hosehold Rotavapors and similar electrical equipment: Harmonics

EN 60555-3:1987 (~ IEC 555-3) Disturbances in supply systems caused by hosehold Rotavapors and similar electrical equipment: Voltage fluctuations

EN 61000-3-2: 1995/1996 Limits for harmonic current emissions

EN 61000-3-3: 1995 Limitation of voltage fluctuations and flicker

following the provisions of EU-Directive:

Directive 73/23/EWG (Electrical apparatus/low tension recommendations) Directive 89/336/EWG (Electromagnetic compatibility)

Flawil, 16.02.2001

Quality Management BÜCHI Labortechnik AG Meierseggstrasse 40 9230 Flawil Schweiz

Tel +41 (0)71 394 63 63 Guido Worch Fax +41 (0)71 394 65 65 Qualitymanager buchi@buchi.com www.buchi.com

9 Appendix

Buchi B-820, B-821 User Manual

Specifications and Main Features

Frequently Asked Questions

User Manual