Ocean Optics LIBS2000+ User Manual

Laser-Induced Spectroscopy
LIBS2000+

Installation and Operation Manual

Document Number 161-00000-000-02-0406

Offices:

E-mail: [e-mail] (General sales inquiries)

Ocean Optics, Inc.

830 Douglas Ave., Dunedin, FL, USA 34698

Phone [phone]

Fax [phone]

8 a.m.– 8 p.m. (Mon-Thu), 8 a.m.– 6 p.m. (Fri) EST

Ocean Optics B.V. (Europe)

Geograaf 24, 6921 EW DUIVEN, The Netherlands

Phone [phone]

F ax 31-(0)26-3190505

[e-mail] (European sales inquiries)
[e-mail] (Questions about orders)
[e-mail] (Technical support)

Copyright © 2001-2006 Ocean Optics, Inc.

All rights reserved. No part of this publication may be reproduced, stored in a retrieval system, or transmitted, by any means, electronic,
mechanical, photocopying, recording, or otherwise, without written permission from Ocean Optics, Inc.
This manual is sold as part of an order and subject to the condition that it shall not, by way of trade or otherwise, be lent, re-sold, hire d out or
otherwise circulated without the prior consent of Ocean Optics, Inc. in any form of binding or cover other than that in which it is published.

Trademarks

All products and services herein are the trademarks, service marks, registered trademarks or register ed service marks of their respective owners.

Limit of Liability

Every effort has been made to make this manual as complete and as accurate as possible, but no warranty or fitness is implied. The information
provided is on an “as is” basis. Ocean Optics, Inc. shall have neither liability nor responsibility to any person or entity with respect to any loss or
damages arising from the information contained in this manual.

Important Safety Notices

WARNING

The LIBS System uses a Class IV laser. Exposure to the laser can cause eye and skin
damage. Although the LIBS System incorporates numerous safety features, due care
is required when using a laser to prevent injury.

1. Use safety goggles at all times when operating the laser as a standalone unit.

2. Only permit trained personnel to operate the laser.

3. Read all the instructions that accompanied your laser.

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Important Safety Notices

ii 161-00000-000-02-0406

Table of Contents

About This Manual .......................................................................................................... v

Document Purpose and Intended Audience.............................................................................. v

What’s New In This Document .................................................................................................. v

Document Summary.................................................................................................................. v

Product-Related Documentation ............................................................................................... v

Upgrades......................................................................................................................... vi

Chapter 1: Introduction ......................................................................1

Product Overview ............................................................................................................ 1

How the LIBS2000+ Works ....................................................................................................... 1

Advantages of Broadband LIBS Techniques ............................................................................1

LIBS Emission ID....................................................................................................................... 2

Applications ..................................................................................................................... 3

Laser Requirements for LIBS2000+ ................................................................................ 3

Shipment Components.................................................................................................... 4

Standard LIBS System .............................................................................................................. 4

Other Required Equipment........................................................................................................4

Additional Recommended Equipment ....................................................................................... 5

Chapter 2: Installing the LIBS System..............................................7

Overview ......................................................................................................................... 7

Hardware Set-up ............................................................................................................. 7

Software Installation ........................................................................................................ 9

OOIBase32 Software Installation .............................................................................................. 9

OOILIBS Software ..................................................................................................................... 10

Hardware Cabling............................................................................................................ 10

System Start-up............................................................................................................... 13

Assigning Spectrometers........................................................................................................... 13

Loading the Element Library .....................................................................................................15

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Table of Contents

Chapter 3: Operation ..........................................................................17

Overview ......................................................................................................................... 17

Configuration ...................................................................................................................17

Set Q-Switch Delay ................................................................................................................... 17

Setup Options............................................................................................................................18

Set up Radiometric Information................................................................................................. 19

Initial Testing ................................................................................................................... 20

Using OOILIBS Software Modes ..................................................................................... 21

Pixel Correlation Mode .............................................................................................................. 21

Pixel Correlation Procedure .................................................................................................. 22

Element ID Mode.......................................................................................................................24

Elemental ID Procedure........................................................................................................ 24

Peak Analysis Mode .................................................................................................................. 25

Lines to Analyze Options ...................................................................................................... 25

Lines Information................................................................................................................... 26

Peak Analysis Procedure ...................................................................................................... 26

Performing Correlation in OOILIBS ................................................................................. 27

Accessing the Correlation Window............................................................................................ 27

Adding Samples to the Correlation Library................................................................................ 28

Saving the Correlation Library...................................................................................................30

Correlation Tips ......................................................................................................................... 30

Chapter 4: Troubleshooting...............................................................31

Overview ......................................................................................................................... 31

HR2000 Connected to PC Prior to OOILIBS Installation................................................. 31

Remove the Unknown Device from Windows Device Manager................................................31

Remove Improperly Installed Files ............................................................................................ 32

Laser Troubleshooting..................................................................................................... 33

Problem ..................................................................................................................................... 33

Probable Cause.........................................................................................................................33

Solution...................................................................................................................................... 33

Spectrometer Troubleshooting ........................................................................................ 33

Continuous Beeping from System............................................................................................. 33

Problem.................................................................................................................................33

Probable Cause .................................................................................................................... 33

Solution ................................................................................................................................. 33

System Prompts for ezusb.sys or an .inf File ............................................................................ 34

Problem.................................................................................................................................34

Probable Cause .................................................................................................................... 34

Solution...................................................................................................................................... 34

Verifying Device Setup .............................................................................................................. 34

Problem.................................................................................................................................34

Solution ................................................................................................................................. 34

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Table of Contents

OOILIBS Software Troubleshooting ................................................................................ 35

Program Keeps Freezing or Locking Up ................................................................................... 35

Problem.................................................................................................................................35

Probable Cause .................................................................................................................... 35

Solution ................................................................................................................................. 35

Appendix A: Specifications................................................................37

Appendix B: User Interface................................................................39

Menu Bar......................................................................................................................... 39

File Menu...................................................................................................................................39

View Menu................................................................................................................................. 40

Overlay Sub-Menu ................................................................................................................40

ScanType Menu ........................................................................................................................ 41

Mode Menu................................................................................................................................ 41

Background Menu .....................................................................................................................42

Background | Mode Menu..................................................................................................... 42

Library Options Menu ................................................................................................................ 42

Library Options | Element ID Menu....................................................................................... 43

Library Options | Correlation Menu ....................................................................................... 43

Tools Menu................................................................................................................................ 44

Stage Menu ............................................................................................................................... 44

Tool Bar........................................................................................................................... 44

Dialog Bar........................................................................................................................ 45

Status Bar.................................................................................................................................. 46

Graph Window................................................................................................................. 47

Index .....................................................................................................49

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Table of Contents

iv 161-00000-000-02-0406

About This Manual

Document Purpose and Intended Audience

This document provides the user of the LIBS 2000+ for setting up, calibrating and performing
experiments with their system.

What’s New In This Document

This version of the Laser-Induced Spectroscopy LIBS2000+ Installation and Operation Manual updates
the safety instructions.

Document Summary

Chapter Description

Chapter 1: Introduction

Chapter 2: Installing the LIBS

System

Chapter 3: Operation

Chapter 4: Troubleshooting

Appendix A: Specifications

Appendix B: User Interface

Contains descriptive information about the LIBS2000+ system.
It also provides laser requirements and shipment components.

Provides installation and configuration instructions.

Contains instructions for operating the LIBS2000+ System.

Contains recommended steps to isolate and correct common
problems.

Provides product specification data.

Contains a quick reference guide to the OOILIBS user
interface features.

Product-Related Documentation

You can access documentation for Ocean Optics products by visiting our website at

http://www.oceanoptics.com. Select Technical → Operating Instructions, then choose the appropriate

document from the available drop-down lists. Or, use the Search by Model Number field at the bottom
of the web page. You can also access operating instructions for Ocean Optics products from the Software
and Technical Resources CD that ships with the product. Engineering-level documentation is located on
our website at Technical → Engineering Docs.

Other Ocean Optics documentation related to your LIBS system includes the following:

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About This Manual

• HR2000 and HR2000CG-UV-NIR High-Resolution Fiber Optic Spectrometers Installation and

Operation Manual located at http://www.oceanoptics.com/technical/hr2000.pdf

.

• LIBS Imaging Module Installation and Operation Instructions located at

http://www.oceanoptics.com/technical/LIBS Install.pdf

• OOIBase32Spectrometer Operating Software located at

http://www.oceanoptics.com/technical/ooibase32.pdf

• Correcting Device Driver Issues located at

http://www.oceanoptics.com/technical/engineering/correctingdevicedriverissues.pdf

Upgrades

Occasionally, you may find that you need Ocean Optics to make a change or an upgrade to your system.
To facilitate these changes, you must first contact Customer Support and obtain a Return Merchandise
Authorization (RMA) number. Please contact Ocean Optics for specific instructions when returning a
product.

vi 161-00000-000-02-0406

Chapter 1

Introduction

Product Overview

The Ocean Optics LIBS2000+ Laser-induced Breakdown Spectrometer is a detection system that permits
real-time, qualitative measurements of trace elements. This broadband, high-resolution instrument allows
for spectral analysis from 200-980 nm, with resolution of ~0.1 nm (FWHM). Sensitivity has been
reported to parts-per-billion and picogram levels.

The LIBS2000+ comes in a standard 3U rack case with handles for extra convenience. The LIBS2000+
operates with any 32-bit, USB-compatible Windows PC. We provide OOILIBS Application Software
with spectral-saving and data-logging capabilities for operating the LIBS2000+ and for firing the laser.
Correlation Software, developed with the University of Florida, provides instant material identification
when using the LIBS2000+ and a spectral library consisting of 2500 atomic emission lines from the NIST
(National Institute of Standards and Technology) tables for elemental identification.

The LIBS Imaging Module is available for use with the LIBS system to enable you to precisely adjust the
laser to focus on the exact spot on the sample that you wish to analyze. The LIBS Imaging Module also
comes with PixeLINK™ software for the camera to capture high quality images on your PC.

How the LIBS2000+ Works

A high-intensity, 10 nanosecond-wide laser pulse beam is focused on the
sample area. When the laser is fired, the high temperature of the laser ablates
the surface of the sample and creates plasma. As the plasma decays or cools,
excited atoms in the plasma emit light of characteristic wavelengths distinct to
the elements present. All elements have emission spectra in the 200-980 nm
region. The detection system uses seven of our HR2000 High-resolution
Miniature Fiber Optic Spectrometers, each with a 2048-element linear CCD
array. All spectrometers are triggered to acquire and read out data
simultaneously. The detectors in the broadband (200-980 nm) LIBS2000+
collect the signal; software included with the system displays and identifies the
emission spectrum.

Advantages of Broadband LIBS Techniques

Many LIBS systems have a small spectral range. The LIBS2000+ is the first to provide broadband
spectral analysis. Because the system is noninvasive, you can perform real-time measurements in situ, in
hostile industrial, chemical and biochemical environments with little or no sample preparation.

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1: Introduction

LIBS Emission ID

The reason we at Ocean Optics have designed a broadband high-resolution spectrometer is to be able to
both see and resolve all the lines from all the elements. Our resolution is ~0.1 nm, less than this in the
UV-blue and a bit higher in the red-IR. Because the LIBS-generated lines are stark broadened to about 0.2
nm or so in the UV and about 0.3 nm in the IR, the system can resolve everything that is possible to
observe.

The laser-induced plasma begins life as very hot 15,000 K plasma emitting a large bremsstrahlung
continuum. Depending on the sample matrix, most emission analysis is performed for a few microseconds
for this to decay so as to not mask the line structure. During this time, the higher order transitions decay
away, leaving mostly I and II atomic emissions. These are the ones that are idenified.

Also entering into the emissions from the elements in the interrogated plasma are the collision dynamics
of the plasma. Rate equations can be used to analyze the target, but emission signatures, sample-standards
and correlation techniques are preferred to identify materials with the OOILIBS Software.

Elemental analysis and identification are very important in understanding content, and in some cases are
used for quantitative analysis. To perform analysis and identification, you must use an element catalog to
help determine when a particular element is present.

Currently we use a catalog that was derived from the MIT wavelength tables. It consists of the persistent
lines of the elements from spark spectra and is the closest to a complete catalog of the brightest lines
around the temperature of the decayed plasma. As part of an international standards committee project,
Ocean Optics is in the process of compiling a persistent line emission set for LIBS, using the LIBS
plasma. This will take some time and will be integrated into our base table as time goes on. These studies
are to be done in an Argon gas environment.

How can we be sure that the identified elements are actually present? OOILIBS software contains two
rating mechanisms:

• The first rating mechanism indicates how many lines of those in our persistent line set are
present. Thus, if 5 of 7 possible have been identified, you can be fairly certain that that element is
present. If one of 7 is present, could it be something else? Perhaps a line that is not in our catalog
from another species?

• For the second analysis technique, the emission lines have an appearance value based on
experimental observation. It could be that this single line is the brightest of those from this
element and the others are weak. So, we rate the element using a formula based on these
appearance levels. If only the weakest line of the 7 appears, it is ranked very low and indicates
that this is from one of the unknowns. If it is the strongest line, it will be rated high, allowing you
to be certain that it was present. If you have the highest 5 of the 7 in the table, the rating will be
extremely high.

OOILIBS software allows you to call any number of spectral libraries you wish to use. Our present library
has greater than 2000 lines available. There are no overlaps, but as we advance to more sophisticated
libraries, there certainly will be. The full NIST catalog has so many lines (>100,000) that everything
would be identified many times over, even though the probability of appearance may be small to zero.
That is why we have not included it.

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1: Introduction

Refer to http://physics.nist.gov/PhysRefData/contents-atomic.html to print lists and observe the latest
work. For a list of the persistent lines of spark spectra, consult one of the CRC manuals (Handbook of
Chemistry and Physics). Even the old publications are quite accurate.

LIBS2000+ Spectra of Anthrax SurrogatesBC (Bacillus Cereus), BG (Bacillus Globigii), BT

(Bacillus Thuringiensis)

Applications

The LIBS technique is useful in areas such as:

• Environmental monitoring (soil contamination, particulates)

• Materials analysis (metals, plastics)

• Forensics and biomedical studies (teeth, bones, glass)

• Military and safety applications (explosive particles, chemical and biological warfare agents)

• Art restoration/conservation (pigments, precious/ancient metals)

Laser Requirements for LIBS2000+

You can supply your own Q-switched laser (from our certified list), or you can purchase one through
Ocean Optics. We recommend the ULTRA CFR Nd:YAG laser from Big Sky Laser Technologies
(www.bigskylaser.com/compactseries.html). The ULTRA CFR was used when testing prototypes of the
LIBS2000+. The rugged and field-portable ULTRA CFR delivers Q-switched pulses at 1.06 µm, with
variable repetition rates from 1 to 20 Hz. At 1.06 µm, the laser has a pulse stability of ±3%.

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1: Introduction

Shipment Components

Ocean Optics’ LIBS functionality can be purchased as a complete system, including the spectrometers
and related fibers, laser, LIBS Imaging Module, and OOILIBS software. The system is also completely
customizable. The modular nature of the LIBS2000+ system allows you to purchase just the spectrometer.
Users can then provide their own fixtures and/or Q-switched laser. You can specify the number of
spectrometers (1–7), as well as their gratings, lenses, slits and filters. Contact an Ocean Optics
Application Scientist for more information on customizing your LIBS System.

Standard LIBS System

A standard-channel LIBS System ships with the following components:

 Seven (7) HR2000 Spectrometers in a rack enclosure
 One (1) + 5 VDC Power Supply – For the spectrometer rack assembly
 Four (4) BNC cables
 One (1) heptafurcated fiber (seven-to-one furcation)
 One (1) fiber bundle
 One USB interface cable
 Packing List – The packing list is inside a plastic bag attached to the outside of the shipment box

(the invoice arrives separately). It lists all items in the order, including customized components in
the spectrometer (such as the grating, detector collection lens, and slit). The packing list also
includes the shipping and billing addresses, as well as any items on back order.

 OOILIBS CD – This disc contains the OOILIBS software that not only controls the

spectrometer and the laser, but also provides for extensive data analysis. It also contend
OOIBase32 software, which is required to use OOILIBS software.

 Software and Technical Resources CD -- This disc contains software, operating instructions,

and product information for all Ocean Optics products. You need Adobe Acrobat Reader version

6.0 or higher to view these files (version 7.0 is included on the CD).
With the exception of OOIBase32 Spectrometer Operating Software, all Ocean Optics software

requires a password during the installation process. You can locate passwords for the other
software applications on the back of your CD package.

 Laser Safety Manual

Other Required Equipment

 LIBS Sample Chamber (LIBS-SC) and 12-VDC power supply – Permits a clear view of the

sample ablation. Includes a manual x-y-z stage. The inside lens and spectrometer probe mounting
hardware are reconfigurable with additional components readily available. The sample chamber
also includes a blower and evacuation system to feed in alternate gasses (such as argon) and a
laser safety cutoff switch.

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1: Introduction

 Laser (LIBS-LASER) – You can supply your own laser or purchase one through Ocean Optics.

We recommend the ULTRA CFR Nd:YAG laser from Big Sky Laser Technologies
(www.bigskylaser.com/compactseries.html

). Laser requirements include a low-divergence laser
beam (a tight focus is required to achieve a spark), an active electro-optic Q-switch, and external
triggering and synchronization for the laser flashlamp and Q-switch through the OOILIBS
Software.

 Personal computer – With Windows 98/Me/2000/XP operating system

Additional Recommended Equipment

 LIBS Imaging Module – Consists of a PixeLINK™ Megapixel FireWire Camera, either black

and white (LIBS-IM) or color (LIBS-IM-SC), in a box mounted in between the LIBS laser and
the LIBS Sample Chamber. This product is designed to enable you to precisely adjust the laser to
focus on the exact spot on the sample that you wish to analyze. The imaging module also comes
with PixeLINK software for the camera to capture high quality images on your PC and a 12 VDC
power supply.

 Argon Gas Tank and Cable – Supplies argon gas to the LIBS Sample Chamber to prevent

Pennington-type reactions from occurring

 Safety goggles – Although the LIBS Sample Chamber is constructed of special safety glass to

protect you from the laser, it is recommended that you purchase safety goggles to use whenever
you are working with a Class III or above laser.

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1: Introduction

6 161-00000-000-02-0406

Chapter 2

Installing the LIBS System

Overview

In general, installing the LIBS2000+ involves the following steps:

Procedure

►

1. Unpack and set up the LIBS2000+ components. See Hardware Set-up.

2. Install the OOILIBS software on the PC you intend to use with your LIBS 2000+ System, and
then restart the PC. See Software Installation

.

3. Connect the cables to the appropriate connectors on the LIBS2000+ equipment (see Hardware

Cabling

4. Test that the LIBS 2000+ System is operational (see System Start-up

Consult the instructions provided with the LIBS Imaging Module and the laser being
used for complete installation and operation instructions for those products. General
guidelines are provided in this manual, but may not cover all the information that you
need to install and operate these components of your LIBS System.

).

).

Note

Hardware Set-up

Set up your LIBS2000+ System in the configuration shown in the following figure. Do NOT connect any
of the cables until you have installed the OOILIBS Software.

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2: Installing the LIBS System

LIBS2000+ Hardware Set-up

► Procedure

1. Remove the LIBS2000+ components and laser from their packaging.

2. Place the sample chamber and the rack of spectrometers on a clean, flat surface.

3. If you have purchased the LIBS Imaging Module, place it on top of the sample chamber.

4. Mount the laser head on top of the LIBS Imaging Module (if purchased), or directly on top of

the sample chamber if you do not have an imaging module. A mounting bracket is attached to
the laser head with steel rods to facilitate mounting and laser alignment into the sample
chamber.

5. Insert rods from the laser through the imaging module and into the sample chamber for firm

support. The laser rests flush on top of the imaging module (or sample chamber, if you do not
have an imaging module).

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2: Installing the LIBS System

Mounting the Laser (Rear View)

6. Fill the laser power supply with distilled water (only).

7. Go on to Software Installation

.

Software Installation

OOIBase32 Software Installation

OOIBase32 Spectrometer Operating Software must be installed for you to use OOILIBS software.
OOIBase32 is located both on your OOILIBS CD and on the Software and Technical Resources CD. You
can install it from either CD. This software is also available from our Ocean Optics website at

http://www.oceanoptics.com/technical/softwaredownloads.asp. You can also install it from the web.

For further OOIBase32 installation instructions, see the OOIBase32 Spectrometer Operating Software
Installation and Operation Manual on either the OOILIBS CD or the Software and Technical Resources
CD.

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