PerkinElmer HATR Manual de usuario

HATR SAMPLING ACCESSORY

User’s Guide

MOLECULAR SPECTROSCOPY

Release History

Part Number Release Publication Date

L1050081 B February 2011

Any comments about the documentation for this product should be addressed to:

User Assistance

PerkinElmer Ltd

Chalfont Road

Seer Green

Beaconsfield

Bucks HP9 2FX

United Kingdom

Or emailed to: info@perkinelmer.com

Notices

The information contained in this document is subject to change without notice.

Except as specifically set forth in its terms and conditions of sale, PerkinElmer makes no

warranty of any kind with regard to this document, including, but not limited to, the

implied warranties of merchantability and fitness for a particular purpose.

PerkinElmer shall not be liable for errors contained herein for incidental consequential damages in

connection with furnishing, performance or use of this material.

This document contains proprietary information that is protected by copyright.

All rights are reserved. No part of this publication may be reproduced in any form whatsoever or

translated into any language without the prior, written permission of PerkinElmer, Inc.

Produced in the UK.

Trademarks

Registered names, trademarks, etc. used in this document, even when not specifically marked as such,

are protected by law.

PerkinElmer is a registered trademark of PerkinElmer, Inc.

Frontier and Spectrum are trademarks of PerkinElmer, Inc.

Contents

Conventions Used in this Manual........................................................................ 4

Notes, Cautions and Warnings..................................................................... 4

Warnings and Safety Information....................................................................... 5

ZnSe (zinc selenide) crystals........................................................................ 5

Ge (germanium) crystals............................................................................. 6

AMTIR-1 crystals ........................................................................................ 6

Introduction...................................................................................................... 7

Installing the Accessory..................................................................................... 9

Fitting the Accessory................................................................................... 9

Accessory Detection by Spectrum Software .................................................11

Contamination Check........................................................................................13

Applying Pressure.............................................................................................14

Using the Accessory with Spectrum Software .....................................................15

4 . HATR Sampling Accessory User’s Guide

Conventions Used in this Manual

Normal text is used to provide information and instructions.

Bold text refers to text that is displayed on the screen.

UPPERCASE text, for exampleENTER or ALT, refers to keys on the PC keyboard. '+' is

used to show that you have to press two keys at the same time, for example, ALT+F.

All eight digit numbers are PerkinElmer part numbers unless stated otherwise.

The term ‘instrument’ refers to a Frontier IR System, Spectrum 400 Series or Spectrum 100

Series spectrometer, and any sampling accessory fitted.

Notes, Cautions and Warnings

Three terms, in the following standard formats, are also used to highlight special

circumstances and warnings.

NOTE: A note indicates additional, significant information that is provided with some

procedures.

CAUTION

We use the term CAUTION to inform you about situations that could

result in

serious damage

to the instrument

or other equipment.

Details about these circumstances are in a box like this one.

WARNING

We use the term WARNING to inform you about situations that could

result in personal injury to yourself or other persons. Details about these

circumstances are in a box like this one.

HATR Sampling Accessory User’s Guide . 5

Warnings and Safety Information

Before handling ZnSe (zinc selenide), Ge (germanium) or AMTIR-1 crystals, please ensure

that you have read the appropriate Material Safety Data Sheets (MSDS).

You can search for up-to-date copies of safety data sheets on materials used in PerkinElmer

products that are known to have safety issues from the Technical Resources section of the

PerkinElmer website. The MSDS information is available in a range of languages, and includes

data items required in specific national, supra-national and state jurisdictions.

To obtain a safety data sheet for a particular compound, follow the steps described below.

NOTE:

To read MSDS .pdf files you will need Adobe Reader 5.0 or later. An installation of

this software is available on the

Software Utilities CD

1. Launch your web browser and navigate to the PerkinElmer web site:

www.perkinelmer.com

If you are not redirected automatically you may have to select the home page

appropriate to your location.

2. Search for the term MSDS using the search box located at the top of the home page.

The Search for Material Safety Data Sheets (MSDS) page is displayed.

3. Enter the key words for the compound, in the Product name box, and then click Go.

A full list of all MSDS documents that refer to the compound is displayed.

4. Select the MSDS document you want to view.

ZnSe (zinc selenide) crystals

WARNING

During routine use of your HATR Sampling Accessory the ZnSe crystal

presents no hazard, but:

wear protective gloves when handling the crystal.

DO NOT

use acids to wash the crystal because they react to emit H2Se,

which is very toxic and irritating.

DO NOT

allow the crystal to come into contact with oxidizers.

The crystal is highly toxic by ingestion.

6 . HATR Sampling Accessory User’s Guide

Cleaning ZnSe crystals

Avoid contact of the crystal with oxidizers and acids. ZnSe can be cleaned in pure dry acetone

or methanol using a soft, lint-free cloth. Dry in a current of warm air so that there is no

possibility of condensation forming on the crystal. Other suitable solvents are petroleum ether

and hexane. It may also be cleaned in some commercial laboratory detergents, but they

must be neutral. Alkaline solutions will slightly etch the surface, and acids will severely attack

the material. A final rinse in distilled water and then drying in a current of warm air is

recommended.

Ge (germanium) crystals

WARNING

During routine use of your HATR Sampling Accessory the Ge crystal

presents no hazard, but:

wear protective gloves when handling the crystal.

May be harmful if ingested in quantity, and may irritate or cause

physical damage to eyes.

DO NOT

use acids to wash the crystal.

Ge can react violently with oxidizers, and can ignite in contact with

chlorine and bromine.

Cleaning Ge crystals

Clean the crystal using an organic solvent; do not use acids or oxidizers.

AMTIR-1 crystals

WARNING

During routine use of your HATR Sampling Accessory the

AMTIR-1 crystal presents no hazard, but:

wear protective gloves when handling the crystal.

DO NOT

use strong acids, strong bases or strong oxidizers with

the AMTIR-1 crystal.

Cleaning AMTIR-1 Crystals

Use an organic solvent to clean the crystal.

HATR Sampling Accessory User’s Guide . 7

Introduction

Figure 1 The HATR Sampling Accessory

What is the HATR used for?

The HATR (Horizontal Attenuated Total Reflectance) Sampling Accessory is an internal

reflection accessory used with Frontier IR System, Spectrum 100 Series or Spectrum 400

Series spectrometers for simplifying the analysis of solids, powders, pastes, gels and liquids.

The technique is non-destructive.

As the beam does not penetrate too far into the sample, this technique is ideal for analyzing

strong infrared absorbing solutions, such as emulsions or aqueous solutions. The technique

can also prove useful in measuring homogenous solid samples, solid surfaces and coatings on

solid samples.

How it works

The technique involves placing a sample on top of a crystal with a high refractive index. An

infrared beam from the instrument is passed into the accessory and up into the crystal. It is

then reflected internally along the crystal, and back towards the detector that is housed

within the instrument. Each time the beam is reflected within the crystal, it penetrates into

the sample by a few microns. Figure 2 illustrates this process.

Figure 2 Principle of HATR operation

8 . HATR Sampling Accessory User’s Guide

Choosing the top plate

The HATR can be used to analyze powders, pastes, gels and liquids using a trough top plate,

where the sample is poured into the trough. Alternatively, a flat plate may be used for

homogenous solid samples, solid surfaces, or coatings on solid samples. Force may be

applied to ensure good contact between the sample and the crystal. The flat plate can also

be used to analyze gels and pastes, by spreading them on the surface of the plate.

The HATR can be supplied with top plates fitted with zinc selenide (ZnSe), germanium (Ge)

or AMTIR-1 crystals. Consult your PerkinElmer Sales Representative for further information

about available top plates.

Choosing the correct crystal

Zinc selenide (ZnSe) crystals are most commonly used as they have a wide range

(650–17000 cm−1) and a refractive index of 2.4. However, zinc selenide is incompatible with

many acids and bases. Therefore AMTIR-1 is often used as its properties are very similar, but

it is more resistant to acids.

Germanium (Ge) crystals have a high refractive index of 4.0 and are used for highly

absorbing samples such as carbon-filled polymers and rubbers, and samples with a high

water content. These crystals are also resistant to strong acids and bases.

NOTE: Derivative shaped bands can be observed in the spectrum if the refractive index of

the sample is too close to the refractive index of the crystal. For this reason,

alternative crystal types may be required for specific sample types. Consult your

PerkinElmer Sales Representative for advice.

Details of the top plate crystal are displayed in Spectrum software, and this information is

stored in the status information for each spectrum collected.

Figure 3 Top plate details displayed on the Setup Instrument Basic tab in

Spectrum software

Please ensure that you have read the safety information starting on page 4 of this User’s

Guide for your crystal type before continuing.

Choosing the angle of the crystal face

The number of internal reflections and depth of penetration of the beam can be decreased

and absorbance bands in the spectrum weakened by using, for instance, a 60° crystal rather

than a 45° crystal.

HATR Sampling Accessory User’s Guide . 9

Installing the Accessory

Fitting the Accessory

The HATR Sampling Accessory can be simply installed into the sample compartment of the

spectrometer, after first removing any other sampling accessory that is currently fitted.

To remove the current accessory and then install the HATR:

1. Raise the sample cover to the vertical position, press the release clip and lift the cover

upwards, clear of the instrument.

Store it in a safe place for future re-use.

2. Reach in under the base of the current accessory and pull the release handle towards

you to release the accessory.

3. Now simply slide the accessory out of the sample area (Figure 4).

Store it in a safe place for future re-use.

Figure 4 Removing the basic sample slide

10 . HATR Sampling Accessory User’s Guide

4. Slide in the HATR Sampling Accessory, rest the back of it on the ledge in the sample

area and slide it into position. Push it firmly home to ensure that the connector on the

rear of the HATR Sampling Accessory mates properly with the spectrometer connector.

Figure 5 Installing the HATR accessory

5. Place the required top plate (trough or flat plate type) on the HATR accessory, with the

arrows pointing towards the back (Figure 6).

Figure 6 HATR accessory top plate with arrows circled

The HATR Sampling Accessory is now ready for use.

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