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10 . Spectrum Two HATR User's Guide

Table 2 Properties of crystal materials

ZnSe

KRS5

AMTIR-1

ATR range (cm

−1

)

17 000–650

5500–600

14 000–400

11 000–700

Refractive index at

1000 cm

−1

2.4

4.0

2.37

2.50

Density (g/cm

)

5.27

5.32

7.37

4.4

Max. useful temp.

in air (°C)

300

270

200

300

Hardness

(Knoop #)

150

1150

40.2

170

Cleaning agents

acetone, water

toluene, water

MEK

organic solvents

Solvents that

attack material

acids,

strong alkalis

hot H

aqua regia

complexing

agents

strong acids,

strong bases,

strong oxidizers

Remarks

hard,

easily cracked

hard and brittle,

high reflection

loss

deforms under

pressure, toxic,

does not cleave

hard and brittle

NOTE: The ATR crystal is bonded to the sample plate with an adhesive, we therefore

recommend that you do not leave the crystal in contact with solvents, particularly

chlorinated solvents, for long periods.

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

Guide for your crystal type before continuing.

Содержание Spectrum Two HATR

Страница 1: ...SPECTRUM TWO HATR User s Guide MOLECULAR SPECTROSCOPY ...

Страница 2: ...lity 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 Copyright Information 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...

Страница 3: ...e crystals 5 Ge germanium crystals 6 AMTIR 1 crystals 6 KRS5 Thallium bromide iodide Crystals 7 Introduction 8 Installing the Accessory 11 Accessory Detection by Spectrum Software 12 Aligning the HATR 14 Purging the HATR 17 Installing the Pressure Clamp 18 Using the Accessory with Spectrum Software 20 Contamination Check 25 ...

Страница 4: ...IR 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...

Страница 5: ...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 Ente...

Страница 6: ...mmended Ge germanium crystals WARNING During routine use of your HATR Sampling Accessory the Ge crystal presents no hazard but DO 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 Clean...

Страница 7: ...otective gloves when handling the crystal DO NOT allow the crystal to come into contact with oxidizers We recommend that you DO NOT wash the crystal with water The crystal is extremely toxic by ingestion and is harmful in contact with skin May evolve toxic fumes in a fire Cleaning KRS5 Crystals Clean the crystal using an organic solvent do not use an oxidizer ...

Страница 8: ...lutions 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 ...

Страница 9: ... with many acids and bases AMTIR 1 has a similar hardness and refractive index to ZnSe so absorption bands will be of similar intensity to within approximately 10 The transmission range is slightly narrower than ZnSe 11 000 700 cm 1 AMTIR 1 is more resistant than ZnSe to acids to approximately 6 N and is therefore more appropriate for use with some acidic solutions We recommend that you DO NOT use...

Страница 10: ...t attack material acids strong alkalis hot H2SO4 aqua regia complexing agents strong acids strong bases strong oxidizers Remarks hard easily cracked hard and brittle high reflection loss deforms under pressure toxic does not cleave hard and brittle NOTE The ATR crystal is bonded to the sample plate with an adhesive we therefore recommend that you do not leave the crystal in contact with solvents p...

Страница 11: ... Spectrum Two if fitted 2 Pull the baseplate of the current sample accessory towards you and slide the accessory out of the sample area Figure 3 Store it in a safe place for future re use Figure 3 Removing the sampling accessory 3 Start Spectrum software and connect to the instrument 4 Select Monitor from the Measurement menu in Spectrum software and record the energy throughput of the open beam W...

Страница 12: ...mmended that you maximize the energy throughput of the system as described in Aligning the HATR on page 14 after installing the accessory or after changing between top plates with crystals of very different refractive index Accessory detection by Spectrum software When the accessory is installed in the sample compartment Spectrum software detects it and the Setup Instrument Basic Figure 5 and Setu...

Страница 13: ...Spectrum Two HATR User s Guide 13 Figure 6 Setup Instrument BeamPath tab with HATR icon circled ...

Страница 14: ...HATR from the spectrometer and then measure the value If you do not observe an energy throughput or if you are aligning your accessory for the first time continue at Step 4 If you do observe an energy throughput and your accessory has been aligned previously continue at Step 15 4 Click Halt to exit the Live tab 5 Insert the alignment tool in position on the baseplate Figure 7 Press the alignment t...

Страница 15: ...ear of the HATR are shown Mirror 1 should be rotated fully clockwise and mirror 4 should be rotated fully counterclockwise looking from the front of the sample compartment Figure 9 HATR with top plate removed viewed from rear to show the adjustment nuts Figure 10 shows the optical path of the accessory viewed from the rear as in Figure 9 Figure 10 Optical path of the accessory Mirror 2 Mirror 4 Mi...

Страница 16: ...e light alignment tool from the baseplate 14 Select Monitor from the Measurement menu The Live tab is displayed 15 Gently adjust mirror 2 using a wrench until you obtain an energy maximum 16 Repeat for mirror 3 NOTE You may need to adjust mirror 2 and mirror 3 several times to find the optimum position 17 Record the maximum throughput energy and then click Halt 18 Compare the maximum energy with t...

Страница 17: ...iameter to carry the gas to the purge inlet on the HATR 1 Loosen the knurled nut on the HATR Figure 11 Figure 11 The purge connection on the HATR 2 Push the tube through the nut until it rests against the interior connector 3 Tighten the nut to clamp the tube in place 4 Purge the HATR using a flow rate of approximately 1 or 2 l min 5 Monitor the baseline until H2O CO2 vapor is reduced or negligibl...

Страница 18: ...d the sample plate When analyzing powder samples it can also be used to apply pressure to powder in the sample trough The pressure clamp is used in conjunction with either a volatiles cover L1205436 or a powder spacer L1362431 as described in Table 3 Table 3 Use of volatiles cover and powder spacer Item Flat top plate Trough top plate Volatiles cover Used to apply pressure to polymer films or lami...

Страница 19: ...y 50 newtons of pressure to a flat crystal assembly 45 ZnSe This is a satisfactory setting for most applications 1 Read the scale on the pressure pad and use Figure 13 to calculate the approximate pressure being applied Figure 13 Pressure as a function of the spring height of the clamp 2 To adjust the pressure turn the screw on the top of the clamp CAUTION Excessive pressures can crack and permane...

Страница 20: ...ault scan parameters to values that are appropriate to the HATR If you want to set any of the instrument parameters that are not included on the toolbars select Instrument from the Setup menu to display the Setup Instrument tabs 2 If you want enter a unique Sample ID and Description for the sample on the Measurement bar 3 Ensure that the top plate is clean and then click to collect a background sp...

Страница 21: ...in as there is poor contact 7 Click again to collect the spectrum By default during scanning the sample data is displayed on the Live tab in the Viewing Area The completed spectrum is displayed on the Graph tab and added to the current Samples View in the Data Explorer If for any reason you want to stop scanning your sample click NOTE When your accessory is next installed in the instrument Spectru...

Страница 22: ...he sample trough This prevents vapor entering the beam path and contributing to the collected spectrum 3 Collect the sample spectrum ratioing against the background spectrum 4 Clean the sample off the crystal using a cotton swab moistened with an appropriate solvent see Table 2 on page 10 Analyzing Powders When analyzing powders we recommend that you use the sample trough and apply pressure to the...

Страница 23: ... spectrum 8 Clean the sample off the crystal using a cotton swab moistened with an appropriate solvent see Table 2 on page 10 Analyzing Films When analyzing films we recommend that you use the flat sampling plate 1 Make sure that the pressure clamp is properly installed If required refer to Installing the Pressure Clamp on page 18 2 Collect a background spectrum with the empty clean sample plate 3...

Страница 24: ... Spectrum Two HATR User s Guide 5 Collect the sample spectrum ratioing against the background spectrum 6 Clean the crystal using a cotton swab moistened with an appropriate solvent see Table 2 on page 10 ...

Страница 25: ...he crystal is completely dry before re use Contamination Ready Check NOTE For information about setting up Ready Checks see the Spectrum on screen Help The following description assumes that Ready Checks are already set up and enabled To perform a Ready Check 1 From the Measurement menu select the Instrument Checks sub menu and then Contamination from the Ready Checks available The Ready Checks di...

Страница 26: ...26 Spectrum Two HATR User s Guide ...

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