Polymer Laboratories PL-ELS 2100 Manuel utilisateur

OPERATOR’S MANUAL

FOR

PL-ELS 2100/2100

EVAPORATIVE

LIGHT SCATTERING

DETECTOR

Version 1.5

Polymer Laboratories Ltd, Essex Road, Church Stretton, Shropshire SY6 6AX, UK

Tel +44 01694 723581, Fax +44 01694 722171, Service Tel +44 01694 724333

Polymer Laboratories Varian Inc, 160 Old Farm Road, Amherst, MA 01002, USA

Tel: +1 413 253 9554, Fax +1 413 253 2476

Polymer Laboratories BV, Herclesweg 8, 4338 PL Middleburg, The Netherlands

Tel +31 118 671 500, Fax +31 118 623 193

Polymer Laboratories GmbH, PEKA Park T5 001 Otto-Hesse Straße 19 D 64293 Darmstadt,

Germany Tel +49 06151 860690, Fax +49 06151 860670

Polymer Laboratories SARL, GVIO Parc de Marseille Sud, Impasse du Paradou, Bâtiment D5, 13276

Marseille, France. Tel + 33 0491 176400, Fax + 33 0491 176401

Documentation Revision History

6/26069

Revision # Date Section

Changed Changes Approval

Draft April 2003 All Originated

Version A

(Version 1.0)

16th May 2003 All Release Reviewed by

SJOD, NJW,

PEC and EM

Version B

(version 1.01)

26th August 2003 I/O Controls –remote A/Z

Control software reference

Storage/drying details QC

Specifications

SJOD

Reviewed SB

Version C

(version 1.02)

25th March 2004

19/4/04

1.2, 1.6, 2.4,

4.2

2.3

Specifications AZ input & Gas

/Gain

Gas management

Software include Gain /Smooth

Cleaning Evap tube change

from S/BY to RUN

Addition of parameter menu

info

SJOD/AW

Version D

(version 1.1)

7th May 2004 Table 2.1 &

page 17 Min gas flow 0.9SLM and S/By

flow1.2SLM

Replaced new screen pics

Version E

(version 1.1E)

3/9/04 Table 1.1

section 1.9

Contact closure pins 4 & 10

Pump stop 3 & 10

Version F (1.2) 25/07/05 French address

Version G (1.3) 31/10/05 Safety

Practices,

1.10,

Appendix 6

Cleaning & Decontamination

Procedures, N2mandatory for

flammable solvents & pump

stop should be used

PEC

Version H (1.4) March 2006 Safety

Practices,

Health &

Safety, 1.2,

1.4 & 1.5

Digital output included.

Protective earth connection

requirement on mains supply.

Power switch & coupler

accessible at all times. IEC

60825-1 classification of LED

source.

SB/PEC

Version I

(1.5)

May 2006 All PL-ELS 2100/2100 Ice included SB

Reviewed

SJOD

DECLARATION OF CONFORMITY

We, Polymer Laboratories Ltd

Essex Road

Church Stretton

Shropshire SY6 6AX

U.K.

declare that the product:

______________________________________________________________________

Evaporative Light Scattering Detector

PL-ELS 2100 Part number 0860-0110/0860-0240

PL-ELS 2100 Ice Part number 0860-01110/0860-01240

______________________________________________________________________

conforms with the requirements of EC Directives 89/392, 91/368 & 89/336 by complying with the

following Harmonised European Standards:

Safety: EN61010 –1 Class I

Installation category II

Pollution degree 2

EN61010 –2 –010 Class 2

REINFORCED INSULATION

EMC: EN 61326:1998

Date: 17th May 2006 Dr. S.O’Donohue, Head or R&D –Instrumentation

Document # 6/26069I ii

PL-ELS 2100/2100 Ice WARRANTY

(Extract from General Conditions of Sale)

Subject as hereinafter stated, if any goods supplied are proved to the reasonable satisfaction of the Seller to be defective in material

or workmanship within a period of 12 months from the date of despatch and the Buyer notifies such defect to the Seller in writing

within fourteen days of it becoming apparent the Seller shall repair or replace at its option the goods or any part thereof free of

charge and any repaired (or replacement) goods will be guaranteed on these terms for the unexpired portion of the 12 month period

PROVIDED THAT the Seller shall be under no liability in respect of any defect that has arisen because:-

•of fair wear and tear; or

•where the goods have not been used, maintained, stored or protected in the proper manner; or

•the goods have been altered in any way whatsoever or have been subject to unauthorised repair; or

•the goods have been improperly installed or connected (unless the Seller carried out such installation and connection); or

•in the case of Instrument Consumables (lamps and wetted parts which includes the nebuliser and evaporator assemblies,)

they prove defective as aforesaid more than 30 days after delivery notwithstanding the foregoing provisions of this

condition; or

•the Buyer is in breach of any other contract made with the Seller such as the Company’s General Conditions of Sale.

SAVE AS PROVIDED ABOVE, THE SELLER WILL BE UNDER NO LIABILITY UNDER THE CONTRACT FOR ANY

PERSONAL INJURY, DEATH, LOSS OR DAMAGE OF ANY KIND WHATSOEVER WHETHER CONSEQUENTIAL OR

OTHERWISE INCLUDING BUT NOT LIMITED TO LOSS OF PROFITS AND THE SELLER HEREBY EXCLUDES ALL

CONDITIONS, WARRANTIES AND STIPULATIONS EXPRESS OR IMPLIED, STATUTORY, CUSTOMARY OR

OTHERWISE WHICH BUT FOR SUCH EXCLUSION WOULD OR MIGHT SUBSIST IN FAVOUR OF THE BUYER

EXCEPT THAT SUCH EXCLUSION WILL NOT APPLY TO ANY IMPLIED CONDITION THAT THE SELLER HAS OR

WILL HAVE THE RIGHT TO SELL THE GOODS WHEN THE PROPERTY IS TO PASS OR WHEN THE BUYER DEALS

AS A CONSUMER (AS DEFINED IN SECTION 12 OF THE UNFAIR CONTRACT TERMS ACT 1977), ANY IMPLIED

TERM RELATING TO THE CONFORMITY OF THE GOODS WITH THEIR DESCRIPTION OR SAMPLE OR AS TO

THEIR QUALITY OR FITNESS FOR A PARTICULAR PURPOSE.

IN NO CIRCUMSTANCES WILL THE SELLER OR ITS EMPLOYEES, AGENTS, OR SUB-CONTRACTORS BE LIABLE

FOR ANY LOSS OR DAMAGE OF ANY KIND WHATSOEVER WHETHER CONSEQUENTIAL OR OTHERWISE

CAUSED DIRECTLY OR INDIRECTLY BY ANY NEGLIGENCE OR OTHER TORTIOUS ACT OR BREACH OF

STATUTORY DUTY ON THE PART OF THE SELLER OR ON THE PART OF ANY OF ITS EMPLOYEES, AGENTS OR

SUB-CONTRACTORS IN CONNECTION WITH OR ARISING OUT OF THE MANUFACTURE OR SUPPLY OF THE

GOODS OR IN CONNECTION WITH ANY STATEMENT GIVEN OR MADE (OR ADVICE NOT GIVEN OR MADE) BY

OR ON BEHALF OF THE SELLER.

Any statement made about the Seller’s goods by the Seller or its servants or agents whether orally or in writing is intended for

guidance only and the Buyer should not place any reliance thereon without specific enquiry and without ensuring that any matter of

concern to him is specifically mentioned in the contract.

The Buyer is solely responsible for the suitability of the site for the installation of the goods, for obtaining all and any necessary

consents and approvals under planning and building regulations and by-laws and for the preparation of the site, the constitution of

foundations and the provision of services so that the site is suitable to receive the goods.

Unless expressly provided therein, the contract does notinclude the installation, erection or commissioning of any goods or

equipment or the supervision thereof. Where installation is included in the contract it is the responsibility of the Buyer to advise

the Seller of prevailing site conditions, and in particular but without prejudice to the foregoing, physical characteristics, availability

of services, normal labour working hours and any local or national labour arrangement or practices which might affect the work, and

any other relevant factors. Any additional costs caused by any interruption or delay not attributable to the Seller or to its

employees or because the Seller cannot gain access to the site shall be charged to the Buyer together with an appropriate allowance

for profit. The Buyer shall also be responsible for providing a safe and healthy working environment for the Seller’s employees and

the Seller’s subcontractors and their employees and shall bear (or reimburse the Seller against) any loss, damage or compensation

due to any person in relation to any death or personal injury or destruction or damage to property except to the extent that the

same is due to the negligence of the Seller and the Buyer shall except as aforesaid keep the Seller fully indemnified in respect

thereof.

Document # 6/26069I iii

SAFETY

Signs and Pictograms Used in this Manual

WARNING:

THE “WARNING SIGN” DENOTES A HAZARD. IT CALLS ATTENTION

TO A PROCEDURE, PRACTICE WHICH, IF NOT CORRECTLY DONE OR

ADHERED TO, COULD RESULT IN SEVERE INJURY OR DAMAGE OR

DESTRUCTION OF THE INSTRUMENT.

PLEASE DO NOT PROCEED BEYOND AWARNING SIGN UNTIL THE

INDICATED CONDITIONS ARE FULLY UNDERSTOOD AND MET.

ATTENTION:

The “ATTENTION sign” denotes relevant information.

Read this information first before proceeding, it will be helpful or

necessary to complete the task.

NOTE:

The “NOTE sign” denotes additional information.

It provides the user with advice and suggestions to facilitate the

operation of the instrument.

WARNING

ATTENTION

NOTE

Document # 6/26069I iv

Safety Practices

The following safety practices are intended to ensure the safe operation of the equipment.

Opening of instrument panels may expose potentially dangerous voltages. Disconnect the instrument from all power

sources before opening protective panels. Access to the interior of the instrument should be restricted to properly

trained and qualified service personnel only.

Replace defective fusesonlywith size and rating stipulated on the rear panel next to the fuse holder, and in the

manual.

Replace faulty or frayed power cords.

Check the actual line voltage to confirm its value, before connecting this instrument to it.

Ensure the power switch and appliance coupler at the rear of the instrument remain easily accessible at all times.

Hot surfaces may be exposed when the instrument is opened. These are indicated by a warning label. Allow these

surfaces to cool before touching them.

The individual or group responsible for the use and maintenance of this equipment must ensure that appropriate

decontamination is carried out if hazardous material is spilt on or inside the instrument.

Before using any cleaning or decontamination method except those recommended by Polymer Laboratories (see

Appendix), please check with Polymer Laboratories that the proposed method will not damage the equipment.

Perform periodic leak checks on supply lines.

Do not allow flammable and/or toxic solvents to accumulate.

Follow recommended procedures and protocols for evacuation and disposal of flammable and/or toxic solvents.

Never dispose of such products through municipal waste systems

The unit should not be stacked more than two high without additional means of support and suitable precautions

should be taken to prevent the units being knocked over

Eluents containing concentrations of >1% Acetic acid should be avoided

WARNING

!ELECTRICAL HAZARDS

NOTE

!GENERAL PRECAUTIONS

WARNING

!CLEANING

WARNING

!HOT SURFACE HAZARDS

Document # 6/26069I

HEALTH AND SAFETY

PL-ELS 2100/2100 Ice

WARNING: This instrument should be used only in accordance with the instructions stated within this

manual. Users should observe the following general safety precautions:

•Ensure that the instructions within this manual are understood and carried out in the operation of

the detector. All persons utilising the instrument should have adequate training in its proper set-

up, operation, and particularly its safety features.

•Voltages above 110V AC are present within the instrument; access covers should not be

removed by anyone other than properly trained personnel. No attempt should be made to

service the instrument without authorisation from PL’s service department and contravention of

this may result in personal hazard or damage to the instrument and will invalidate the

manufacturer’s warranty.

•We stress the importance of standard laboratory safe practice (e.g. COSHH regulations) for

dealing with electronic laboratory equipment, solvents, etc., in preventing accidents, fires, or

potentially hazardous conditions.

•This instrument contains a light source, which has been classified according to the methods

specified in IEC 60825-1 Ed 1.2 as a CLASS 1 LED PRODUCT.

If in any doubt about the use of the instrument contact your local office or local distributor.

In the UK and Europe United States Australia

Polymer Laboratories Ltd Polymer Laboratories Varian, Inc. Varian, Inc.

Technical Assistance Technical Assistance & Service Sales & Service

Tel +44 (0) 1694 723581 Tel, toll free 800 767 3963 Tel +61 395661134

Fax +44 (0) 1694 722171 Tel (413) 253 9554

Fax (413) 253 2476

Service

Tel +44 (0) 1694 724333

Fax +44 (0) 1694 723994

In the Benelux countries In Germany In France

Polymer Laboratories BV Polymer Laboratories GmbH Polymer Laboratories SARL

Technical Assistance & Service Technical Assistance & Service Technical Assistance & Service

Tel +31 118 671500 Tel +49 061 51 860690 Tel +33 04 91 176400

Fax +31 118 623193 Fax +49 061 51 860670 Fax +33 04 91 176401

Document # 6/26069I

TABLE OF CONTENTS

1.1 INTRODUCTION.............................................................................................................................................................1

1.2 SPECIFICATIONS...........................................................................................................................................................2

1.3 UNPACKING AND INSTALLATION..............................................................................................................................3

1.4 PACKING LIST ................................................................................................................................................................3

1.5 SITE PREPARATION CHECK LIST...............................................................................................................................4

1.6 CONNECTIONS...............................................................................................................................................................5

1.7 POWER CONNECTIONS.................................................................................................................................................7

1.8 EXTRACTION.................................................................................................................................................................7

1.9 CONNECTIONS...............................................................................................................................................................8

Control I/O connector..........................................................................................................................................................8

Serial RS232 Connector......................................................................................................................................................8

Gas Connection.....................................................................................................................................................................9

Fluid Connection..................................................................................................................................................................9

1.10 PRECAUTIONS................................................................................................................................................................9

Extraction...............................................................................................................................................................................9

Flammable solvents...........................................................................................................................................................10

CHAPTER 2 SYSTEM DESCRIPTION AND GENERAL OPERATION..........................................................................11

2.1 BASIC PRINCIPLES OF OPERATION..........................................................................................................................11

Nebulisation.......................................................................................................................................................................11

Evaporation........................................................................................................................................................................11

Detection.............................................................................................................................................................................11

Theory..................................................................................................................................................................................12

2.2 OPERATIONAL PARAMETERS...................................................................................................................................13

2.3 INSTRUMENT CONTROLS..........................................................................................................................................14

Power On/Off.......................................................................................................................................................................14

Display.................................................................................................................................................................................14

Keypad.................................................................................................................................................................................15

Interactive menu bar.........................................................................................................................................................15

Parameter Setting Menu...................................................................................................................................................16

Real Time Monitoring.......................................................................................................................................................18

Modes of Operation...........................................................................................................................................................18

Using Methods....................................................................................................................................................................19

Error Conditions................................................................................................................................................................20

2.4 PL-ELS 2100/2100 ICE PC SOFTWARE.............................................................................................................................20

Control Software-Overview.............................................................................................................................................21

Configuring your PC and Detector................................................................................................................................21

Connecting the Detector to your PC..............................................................................................................................21

Configuring the ELS Control Software.........................................................................................................................22

Operating the ELS Control Software.............................................................................................................................22

Control Software Features...............................................................................................................................................23

Automation..........................................................................................................................................................................24

System Test..........................................................................................................................................................................25

Method Editor -Overview.................................................................................................................................................25

Method Editor –Creating & Storing Methods............................................................................................................26

Method Editor –Downloading Method Sets................................................................................................................26

CHAPTER 3 SET-UP.................................................................................................................................................................27

3.1 GENERAL CONSIDERATIONS.....................................................................................................................................27

3.2 CONNECTING THE DETECTOR.................................................................................................................................27

3.3 OPTIMISATION PROTOCOL.......................................................................................................................................29

Document # 6/26069I

Gas Flow..............................................................................................................................................................................29

Evaporator Temperature..................................................................................................................................................29

Nebuliser Temperature.....................................................................................................................................................29

Procedure............................................................................................................................................................................29

CHAPTER 4 ROUTINE MAINTENANCE..............................................................................................................................31

4.1 DRYING THE DIFFUSER..............................................................................................................................................31

4.2 CLEANING EVAPORATOR TUBE ...............................................................................................................................31

4.3 INFORMATION FOR SERVICE PERSONNEL..............................................................................................................32

Heater PCB Fuses..............................................................................................................................................................32

Light Source........................................................................................................................................................................32

4.4 PUTTING THE INSTRUMENT INTO STORAGE........................................................................................................32

4.5 UPGRADING THE FIRMWARE USING TERMINAL...................................................................................................33

CHAPTER 5 TROUBLESHOOTING......................................................................................................................................38

5.1 INSTRUMENT ERRORS................................................................................................................................................38

5.2 GENERAL PROBLEMS..................................................................................................................................................39

APPENDIX 1................................................................................................................................................................................41

PL-ELS 2100/2100 ICE QUICK USER GUIDE..........................................................................................................................41

APPENDIX 2................................................................................................................................................................................43

METHOD RECORD SHEET ......................................................................................................................................................43

APPENDIX 3................................................................................................................................................................................44

PL-ELS 2100 TEST PROCEDURE .............................................................................................................................................44

APPENDIX 4................................................................................................................................................................................45

PL-ELS 2100 ICE TEST PROCEDURE ......................................................................................................................................45

APPENDIX 5................................................................................................................................................................................46

SPARE PART LISTING..............................................................................................................................................................46

APPENDIX 6................................................................................................................................................................................47

NITROGEN GENERATOR SPECIFICATIONS...........................................................................................................................47

APPENDIX 7................................................................................................................................................................................48

CLEANING & DECONTAMINATION PROCEDURES..............................................................................................................48

Cleaning..............................................................................................................................................................................48

Decontamination...............................................................................................................................................................48

Chapter 1 –General Information

Document # 6/26069I 1

Version 1.5 May 2006 PL-ELS 2100/2100 Ice Operator’s Manual

Chapter 1

General Information

1.1 Introduction

The PL-ELS 2100/2100 Ice evaporative light scattering detector or mass detector is a unique and

highly sensitive detector for semi-volatile and non-volatile solutes in a liquid stream. It is mainly used as

a concentration detector for High Performance Liquid Chromatography (HPLC). The solvent stream

containing the solute material is nebulised and carried by a gas flow through an evaporation chamber.

The solvent is volatilised, leaving a mist of solute particles that scatter light to a photosensitive device.

The signal is amplified and a voltage output results the “mass” or concentration of the solute particles

passing through the light.

The PL-ELS 2100/2100 Ice may be used alone, or as one of several detectors in a GPC or HPLC

system. As the solvent or eluent is evaporated in the course of the analysis, the PL-ELS 2100/2100 Ice

must be the last in series if used in conjunction with other detectors. If the PL-ELS 2100/2100 Ice is

being used as the last detector in a series, care must be taken not to exceed the recommended back-

pressure in detector cells in other units.

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