SofTA 1300 ELSD Betriebsanleitung

SofTA 1300 ELSD

Installation and Operation Guide

#8-243104

Rev. A, November 2018

SofTA 1300 ELSD

Safety

SofTA 1300 ELSD

Safet y

Before installing, operating, or maintaining this equipment, it is

imperative that all hazards and preventive measures are fully

understood. While specific hazards may vary according to

location and application, take heed in the following general

warnings:

WARNING

LASER SAFETY: This ELSD is a Class I laser product with

a Class IIIa (3R) embedded laser. The embedded laser beam

is less than 5 mW, 650 nm, and is collimated. There are no

user adjustments for power, alignment, or collimation.

Under use conditions, the laser is never visible, and

presents no special safety considerations.

As required by regulation, the back panel has the following

laser related labels, in addition to a serial number label.

Internal components may have the following label:

Never remove a component with this label. Doing so could

expose a user to a potentially hazardous laser beam. Always

refer service to qualified personnel.

WARNING

Do not use gases that support combustion with

combustible solvents. Always use inert gases.To avoid

inhaling harmful organic solvents and other materials, the

detector exhaust should not be allowed to enter the

laboratory atmosphere.

DANGER

To avoid burns, turn off the power at least 30

minutes before performing maintenance

procedures.

SofTA 1300 ELSD

Safety

WARNING

Liquids associated with this instrument may be classified

as carcinogenic, biohazard, flammable, or radioactive.

Should these liquids be used, it is highly recommended that

this application be accomplished in an isolated

environment designed for these types of materials in

accordance with federal, state, and local regulatory laws,

and in compliance with your company’s chemical/hygiene

plan in the event of a spill.

WARNING

Avoid hazardous practices! If you use this instrument in

any way not specified in this manual, the protection

provided by the instrument may be impaired.

WARNING

If you are using flammable solvents or chemicals with this

system, vapor concentration levels may exceed the

maximum exposure levels as recommended by OSHA

Guide 1910.1000. To reduce those levels to a safe exposure,

Teledyne Isco recommends that you place the system in a

laboratory hood designed for the purpose of ventilation.

This hood should be constructed and operated in

accordance with federal state and local regulations. In the

event of a solvent or chemical spill, your organization

should have a plan to deal with these mishaps. In all cases,

use good laboratory practices and standard safety

procedures.

Hazard Severity Levels This manual applies Hazard Severity Levels to the safety alerts.

These three levels are described in the sample alerts below.

CAUTION

Cautions identify a potential hazard, which if not avoided, may

result in minor or moderate injury. This category can also warn

you of unsafe practices, or conditions that may cause property

damage.

WARNING

Warnings identify a potentially hazardous condition, which

if not avoided, could result in death or serious injury.

DANGER

DANGER – limited to the most extreme situations

to identify an imminent hazard, which if not

avoided, will result in death or serious injury.

SofTA 1300 ELSD

Safety

Hazard Symbols The equipment and this manual use symbols used to warn of

hazards. The symbols are explained in the table below.

Hazard Symbols

Warnings and Cautions

The exclamation point within the triangle is a

warning sign alerting you of important instructions

in the instrument’s technical reference manual.

The lightning flash and arrowhead within the trian-

gle is a warning sign alerting you of “dangerous

voltage” inside the product.

Symboles de sécurité

Ce symbole signale l’existence d’instructions

importantes relatives au produit dans ce manuel.

Ce symbole signale la présence d’un danger

d’électocution.

Warnungen und Vorsichtshinweise

Das Ausrufezeichen in Dreieck ist ein Warn-

zeichen, das Sie darauf aufmerksam macht, daß

wichtige Anleitungen zu diesem Handbuch

gehören.

Der gepfeilte Blitz im Dreieck ist ein Warnzeichen,

das Sei vor “gefährlichen Spannungen” im

Inneren des Produkts warnt.

Advertencias y Precauciones

Esta señal le advierte sobre la importancia de las

instrucciones del manual que acompañan a este

producto.

Esta señal alerta sobre la presencia de alto

voltaje en el interior del producto.

SofTA 1300 ELSD

Safety

For Additional

Information

Technical assistance for the 1300 ELSD can be obtained from:

Teledyne Isco

4700 Superior St.

Lincoln NE 68504

Phone: (800) 775-2965 or (402) 464-0231

Fax: (402) 465-3001

E-mail: IscoService@teledyne.com

SofTA 1300 ELSD

Table of Contents

SofTA 1300 ELSD

Table of Contents

Section 1 Introduction

1.1 ELSD Principle of Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1

1.1.1 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1

Section 2 Unpacking and Installation

2.1 Requirements and Steps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1

2.1.1 Unpacking . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1

2.2 Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1

2.3 Installation Qualification Checklists . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3

2.3.1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3

2.3.2 Installation Qualification (IQ) for SofTA ELSDs . . . . . . . . . . . . . . . . . . . . . 2-4

2.3.3 Operational Qualification (OQ) for SofTA ELSDs . . . . . . . . . . . . . . . . . . . . 2-5

2.3.4 Performance Qualification (PQ) for SofTA ELSDs . . . . . . . . . . . . . . . . . . . 2-7

2.3.5 Overall Detector Performance for SofTA ELSDs . . . . . . . . . . . . . . . . . . . . . 2-9

Section 3 Operation

3.1 Instrument Controls . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1

3.1.1 Power Key . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1

3.1.2 A/Z Key . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1

3.2 Display Screens . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1

3.3 Operating Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-7

3.3.1 Start Up Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-7

3.3.2 Shut Down Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-8

3.4 Choosing Operating Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-8

3.4.1 Thermo-Split Spray Chamber Temperature . . . . . . . . . . . . . . . . . . . . . . . . 3-9

3.4.2 Drift Tube Temperature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-10

3.4.3 Mobile Phase Flowrate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-11

3.4.4 Gradient Separations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-11

3.5 Mobile Phase Considerations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-12

3.5.1 Selecting a Solvent . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-12

3.5.2 Mobile Phase Flowrate and Composition . . . . . . . . . . . . . . . . . . . . . . . . . . 3-12

3.5.3 Buffer Compatibility . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-12

3.5.4 Column Pre-Treatment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-12

3.5.5 QC Test Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-13

Appendix A Speciations

A.1 Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-1

SofTA 1300 ELSD

Table of Contents

1-1

SofTA 1300 ELSD

Section 1 Introduction

1.1 ELSD Principle of

Operation

ELSDs are near universal detectors primarily used in High Per-

formance Liquid Chromatography (HPLC), though they have

been used successfully in other types of chromatography as well.

Their principal requirement is that the analyte be less volatile

than the mobile phase. An ELSD cannot detect highly-volatile

analytes. However, most analytes of interest are less volatile

than the eluting solvents.

Evaporative light scattering detectors are complementing ultra-

violet (UV) detection because they can detect most analytes, are

stable during gradient elutions, and respond to the relative mass

of the analyte (even those that do not absorb UV radiation). This

is an important feature that is useful when detecting unknown

materials. The ELSD is superior to the refractive index detector

(RID) as it can be used with gradient chromatography, it is not

susceptible to ambient temperature changes, and it does not

produce negative peaks (which can be difficult to quantify). The

ELSD does not respond to the mobile phase disruption seen as

solvent front peaks in the void volume with UV and RI detectors,

so early eluting analytes can be easily quantified. Mass spec-

trometry (MS) detection is also a nearly universal detector, but

its high cost and complexity may be unnecessary in many appli-

cations. In fact, the operation requirements of MS closely match

that of the ELSD. This allows the less expensive and less compli-

cated ELSD to be used as a method development detector for

methods to be used on the MS systems.

1.1.1 Operation The 1300 ELSD employs a unique method of detection. The

process involves the nebulization of the column eluent which

transforms it into an aerosol cloud. As this cloud travels through

a heated zone within the instrument, the more volatile mobile

phase evaporates and leaves a smaller cloud of analyte particles.

These particles pass through a beam of light and scatters some of

the light which is converted into an electronic signal.

Nebulization Nebulization transforms the liquid phase leaving the column into

an aerosol cloud of fine droplets. The size and uniformity of the

droplets are extremely important in achieving sensitivity and

reproducibility. The 1300 ELSD uses a special concentric flow

nebulizer and a constant flow of an inert gas to ensure a narrow

droplet size distribution. This nebulizer is constructed entirely

from PTFE which accumulates fewer deposits than either glass

or stainless steel.

To handle flow rates and mobile phases common in HPLC, all

ELSDs need a way to divert part of the aerosol cloud to waste.

The 1300 ELSD uses patented Thermo-Split technology.

SofTA 1300 ELSD

Section 1 Introduction

1-2

The Thermo-Split chamber combines a gentle bend with temper-

ature-controlled walls. When the aerosol exiting the nebulizer

encounters a cool environment, it partially condenses into larger

particles whose momentum carries them into the wall and down

the drain (Figure 1-1).

Figure 1-1 Thermo-Split chamber without heating

To increase sensitivity with easy-to-evaporate solvents, the tem-

perature of the spray chamber may be elevated. As the aerosol

traverses the chamber, it partially evaporates and shifts the par-

ticle size distribution low enough for essentially all the particles

to negotiate the bend. Under these conditions, a majority of the

aerosol particles pass through the chamber and are carried into

the evaporative zone (Figure 1-2).

Figure 1-2 Thermo-Split chamber with heating

Evaporation After passing through the nebulization chamber, the aerosol

cloud is propelled through the heated evaporation tube assisted

by the carrier gas. In the evaporation tube, the solvent is vola-

tilized to produce particles or droplets of pure analyte.

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