Metrohm 750 Autosampler Manual de usuario

CH-9101 Herisau/Switzerland

Tel. ++41 71 353 85 85

Fax ++41 71 353 89 01

Internet www.metrohm.ch

E-Mail [email protected]

750 Autosampler

2.750.0020 Instrument version

8.750.1023 Instructions for Use

23.02.2000 / dö

Table of contents

750 Autosampler I

Table of contents

1Introduction............................................................................................1

1.1 Instrument description.............................................................................1

1.2 Theory of operation ..................................................................................2

1.3 Control elements.......................................................................................4

1.4 Information on the Instructions for Use................................................6

1.4.1 Organization....................................................................................6

1.4.2 Notation and pictograms ................................................................7

1.5 Safety notes ...............................................................................................8

1.5.1 Electrical safety ...............................................................................8

1.5.2 General precautionary rules............................................................8

2Installation..............................................................................................9

2.1 Setting up the instrument........................................................................9

2.1.1 Packaging .......................................................................................9

2.1.2 Check..............................................................................................9

2.1.3 Location...........................................................................................9

2.2 Connection to IC system........................................................................10

2.2.1 750 Autosampler as "Master"........................................................ 10

2.2.2 732 IC Detector as "Master" ..........................................................11

2.2.3 Connection to 762 with «IC Net»...................................................12

2.2.4 Tubing connection ........................................................................14

2.3 Mains connection....................................................................................15

2.3.1 Check fuses ..................................................................................15

2.3.2 Mains cable and mains connection..............................................16

2.3.3 Switching the instrument on/off ....................................................16

2.4 Initial checkout ........................................................................................17

3Operation...............................................................................................19

3.1 Fundamentals of operation ...................................................................19

3.1.1 Display and instrument dialog ......................................................19

3.1.2 Overview of key functions .............................................................20

3.2 System settings.......................................................................................23

3.3 Manual rinsing.........................................................................................26

3.4 Manual injection......................................................................................26

3.5 Methods ....................................................................................................28

3.6 Method procedure...................................................................................34

3.7 Priority sample.........................................................................................35

3.8 Remote control........................................................................................36

Inhaltsverzeichnis

750 Autosampler

4Notes – Maintenance – Faults...................................... 39

4.1 Operating information............................................................................ 39

4.1.1 Loading sample vials.................................................................... 39

4.1.2 Sample preparation ...................................................................... 39

4.1.3 Operating parameters................................................................... 40

4.2 Maintenance and servicing ................................................................... 41

4.2.1 General information ...................................................................... 41

4.2.2 Transfer needle replacement........................................................ 41

4.2.3 Sample preparation ...................................................................... 42

4.3 Remedying malfunctions....................................................................... 43

4.3.1 Non-reproducible injections ......................................................... 43

4.3.2 Missed injections.......................................................................... 44

4.4 Error messages....................................................................................... 45

4.4.1 Entry error messages.................................................................... 45

4.4.2 System error messages................................................................ 47

4.4.3 Remote control error codes.......................................................... 48

5Appendix ................................................................................................ 49

5.1 Technical data ......................................................................................... 49

5.2 Interfaces.................................................................................................. 51

5.2.1 Contact closure strips................................................................... 51

5.2.2 RS232 interface............................................................................. 53

5.3 Standard equipment............................................................................... 54

5.4 Optional accessories.............................................................................. 55

5.5 Warranty and conformity....................................................................... 56

5.5.1 Warranty........................................................................................ 56

5.5.2 EU Declaration of conformity........................................................ 57

5.5.3 Certificate of conformity and system validation............................ 58

5.6 Index.......................................................................................................... 59

List of figures

Fig. 1:Autosampler 750 ............................................................................................... 1

Fig. 2:Positive displacement sample injection ............................................................ 2

Fig. 3:Displacement volume versus needle position .................................................. 3

Fig. 4:Front of 750 Autosampler.................................................................................. 4

Fig. 5:Rear of 750 Autosampler................................................................................... 5

Fig. 6:Connection of 750 Autosampler to 732/733 ................................................... 11

Fig. 7:Connection of 750 Autosampler to 732/733 and 762 ..................................... 13

Fig. 8:Keypad ............................................................................................................ 20

Abb. 9:Manual sample filtering ................................................................................... 39

Fig. 10:Sample filtering with FilterCaps....................................................................... 40

Fig. 11:Transfer needle replacement........................................................................... 51

Fig. 12:Valve control .................................................................................................... 57

Fig. 13:Inputs/outputs.................................................................................................. 51

1.1 Instrument description

750 Autosampler 1

1 Introduction

1.1 Instrument description

The 750 Autosampler is a microcomputer-operated sampling/con-

troller system designed to be used with the ion chromatographic in-

struments 732 IC Detector and 733 IC Separation Center. It has a ca-

pacity of up to 128 samples, which are transferred automatically into

the sample loop of the 733 IC Separation Center.

The 750 Autosampler performs up to four, fixed loop injections per vial

at user-selectable time intervals. All operating parameters are entered

from the front panel. Additionally, the instrument can be controlled re-

motely either by an externally programmable contact closure or through

the RS232 connector located on the rear panel.

Fig. 1: 750 Autosampler

1 Introduction

750 Autosampler

1.2 Theory of operation

Displacement principle

The 750 Autosampler operates using the positive displacement princi-

ple of sample transfer. This sample transfer process into the sample

loop of the 733 IC Separation Center is illustrated in Fig. 2. When an in-

jection is initiated, the hollow transfer needle 55 descends into the vial.

The needle tip punctures the polyethylene cap of the sample vial. The

opening into the needle is located on the side to minimize plugging by

cap material as the cap is punctured. The needle continues downward

until the pushrod contacts the area around the puncture in the cap

which forces the cap down into the vial. The piston action of the cap

pressurizes the sample and forces it up through the needle and the

transfer tubing 88 that is connected to the needle. From the transfer

tubing, the sample flows through the injection valve and sample loop

with the excess passing on through the waste tube to a waste con-

tainer.

Rinsing by air bubbles

The air bubble (minimum 150 µL), which is always present at the top of

a properly filled and capped vial, precedes the sample stream through

the plumbing. The bubble disrupts the laminar flow of the fluid in the

tubing while pushing out the previous sample and solvent. This effect,

in addition to the large excess volume of sample, helps to minimize

sample carryover.

RUN FILL/LOAD INJECT RUN

A B C D

Fig. 2: Positive displacement sample injection

Column

Waste

Eluent

Sample

Needle

Cap

Sample vial

Valve

1.2 Theory of operation

750 Autosampler 3

Number of injections

The number of injections per sample with the 750 Autosampler de-

pends on the sample loop size. With sample loops >10 µL max. 3,

with sample loops ≤10 µL max. 4 injections are possible. Fig. 3 details

the needle position and displacement volume at the sample delivery

action. Care should always be taken that the injection volume is at least

three times greater than the volume of the sample loop. This is why only

a maximum of 2 injections per sample should be made with 100 µL

loops; the minimum sample volume is 300 µL for 1 and 600 µL for 2 in-

jections. For sample loops with a volume ≤10 µL up to 4 injections per

sample are possible. The minimum sample volume required is 150 µL

for 1, 300 µL for 2, 450 µL for 3 and 600 µL for 4 injections.

Rinsing

Rinsing will be necessary for highly concentrated samples or for sam-

ples that may absorb in the tubing or in the injection valve. Rinse vials

are filled with eluent or other suitable solvent. The Rinse process is

shown in Fig. 3. Rinse vials can be used either after each vial (every

even numbered or odd numbered vial) or at programmed vial intervals.

There are two types of Rinses, the Normal Rinse and the Quick Rinse.

The Normal Rinse occurs after all the injections have been made from

the sample vial and the run time has elapsed. A Quick Rinse occurs

immediately after an injection and is used in applications where the

sample solution must not be left in the needle, transfer tubing or valve

for whatever reason. Only one injection per vial can be programmed

when using a Quick Rinse.

Injection 1 Injection

per vial 2 Injections

per vial 3 Injections

per vial 4 Injections

per vial Rinse

2.65 cm

730 µL

1.63 cm

450 µL

1.02 cm

280 µL

1.63 cm

450 µL

0.51 cm

140 µL

0.51 cm

140 µL

1.12 cm

310 µL

0.51 cm

140 µL

0.51 cm

140 µL

0.51 cm

140 µL

2.65 cm

730 µL

Fig. 3: Displacement volume versus needle position

1 Introduction

750 Autosampler

1.3 Control elements

750 Autosampler

RINSEINJECTION

MANUAL

METHOD

REM/LOCTEMPSYSTEM

F3F2F1

.CLEAR

8 9

5 6

2 3

FUNCTION

RUN/STOP

PRIORITY

ENTER

556677

Fig. 4: Front of the 750 Autosampler

11 Display (LCD)

comprising 4 lines each of

20 characters

55 Transfer needle

22 Keypad

with function, numeric and cursor

keys (details see chap. 3.1.2)

66 Holder for transfer tubing

33 Sample rack (6.2041.600)

for 128 sample vials

77 Holder stopper

44 Sample vial

6.2743.000 sample vial (PP) or

6.2413.000 sample vial (glass)

88 Transfer tubing

6.1803.000 PTFE capillary for the

connection of the 750 Autosampler

with the injector of the 733 IC

Separation Center

1.3 Control elements

750 Autosampler 5

Type:

Nr.:

Switzerland

1010

1212

1313

1414

1515

RS-232

PRINTER

EXT PWR

CONTROL

BCD

IEEE

INJECT

LOAD

1111

Fig. 5: Rear of the 750 Autosampler

99 Contact closure strip for valve

control

details see chap. 5.2.1

1313 Mains switch

switch to switch the instrument on

and off: I = ON 0 =

OFF

1010 Contact closure strip for external

control

details see chap. 5.2.1

1414 Mains connection plug

mains connection see chap. 2.3

1111 RS232 interface

details see chap. 5.2.2 1515 Fuse cassette

changing the fuses, see chap. 2.3.1

1212 Model plate

with instrument and serial number,

mains voltage, mains frequency,

power consumption

1 Introduction

750 Autosampler

1.4 Information on the Instructions for Use

Please read through these Instructions for Use carefully before you put

the 750 Autosampler into operation. The Instructions for Use contain

information and warnings which must be heeded by the user to assure

safe operation of the instrument.

1.4.1 Organization

These 8.750.1023 Instructions for Use for the 750 Autosampler pro-

vide a comprehensive overview of the installation, startup procedure,

operation, fault rectification and technical specifications of the instru-

ment. The Instructions for Use are organized as follows:

Section 1 Introduction

General description of instruments, control parts

and safety notes

Section 2 Installation

Installation of the 750 Autosampler, connection to

IC Separation Center 733, initial checkout

Section 3 Operation

Detailed description of the operation and

explanation of functions of all keys

Section 4 Notes – Maintenance – Faults

Notes on operation, maintenance,

fault rectification, diagnostic tests

Section 5 Appendix

Technical data, interfaces, standard equipment,

options, warranty, declarations of conformity, index

To find the required information on the instruments, you will find it an

advantage to use either the Table of contents or the Index at the

back.

1.4 Information on the Instructions for Use

750 Autosampler 7

1.4.2 Notation and pictograms

The following notations and pictograms (symbols) are used in these In-

structions for Use:

<PARAM> Key

"Run Time"Parameter or entry value

55 Control element of 750

(see chap. 1.3)

8484 Control element of 732/733

(see Instructions for Use 732)

1414 Control element of 762

(see Instructions for Use 762)

READY

SELECT A FUNCTION

Display

Text in display 11 of the 750 Auto-

sampler

Hazard

This symbol draws attention to a

possible danger to life or of injury if

the associated directions are not

followed correctly.

Warning

This symbol draws attention to

possible damage to instruments or

instrument parts if the associated

directions are not followed cor-

rectly.

Caution

This symbol marks important in-

formation. First read the associ-

ated directions before you con-

tinue.

Comment

This symbol marks additional in-

formation and tips.

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