206-97503B

Feb. 2014

LabSolutions DB/CS IR

Instruction Manual
System Users Guide [IR Volume]
Read the instruction manual thoroughly before you use the product.
Keep this instruction manual for future reference.
 Introduction
Read this Instruction Manual thoroughly before using
the product.
Thank you for purchasing this product.
This operation manual describes the product's operation procedures and related options. Read the manual
thoroughly and use the product in accordance with the described instructions.

Also, keep this manual for future reference.

 IMPORTANT
 If the user or usage location changes, ensure that this Instruction Manual is always kept together
with the product.
 If this manual or a product warning label is lost or damaged, immediately contact your Shimadzu
representative to request a replacement.
 To ensure safe operation, read all Safety Instructions before using the product.

 To ensure safe operation, contact your Shimadzu representative if product installation, adjustment,
or re-installation (after the product is moved) is required.

 Notice
 Information in this manual is subject to change without notice and does not represent a commitment
on the part of the vendor.
 Any errors or omissions which may have occurred in this manual despite the utmost care taken in its
production will be corrected as soon as possible, although not necessarily immediately after
detection.
 All rights are reserved, including those to reproduce this manual or parts thereof in any form
without permission in writing from Shimadzu Corporation.
 Microsoft and Windows are registered trademarks of Microsoft Corporation in the United States
and/or other countries. Other company names and product names mentioned in this manual are
trademarks or registered trademarks of their respective companies. The TM and ® symbols are
omitted in this manual.
 LabSolutions IR is a registered trademark of Shimadzu Corporation in the United States and Europe
(Office for Harmonization in the Internal Market).
 This product uses WinWrap® Basic, Copyright 1993-2009 Polar Engineering and Consulting
(http://www.winwrap.com/ ).
© 2012-2014 Shimadzu Corporation. All rights reserved.
Original version is approved in English.

LabSolutions IR System Users Guide IR Volume i

Introduction

About the Instruction Manual

 Indications Used in This Manual
The following symbols are used in this manual:
Notation Meaning
Emphasizes additional information that is provided to ensure the proper use
of this product.

Indicates the location of related reference information.

 Mouse and Window Operations

Description Meaning
Click Means pointing to an object and pressing the left mouse button once.
Right click Means pointing to an object and pressing the right mouse button once.
Double click Means pointing to an object and pressing the left mouse button twice.
Means pointing to an object and then moving the mouse pointer while
Drag
holding the left mouse button down.
Means dragging an object to the target location and then releasing the left
Drag and drop
mouse button.
The names of buttons in a window, and window names, are enclosed in
Text in square brackets [ ] square brackets.
Example: Click [OK].
Entered numerical values, text, and keyboard key names are indicated
Text in quotation marks " " enclosed in quotation marks.
Example: Press the "N" key while holding down the "Ctrl" key.

ii LabSolutions IR System Users Guide IR Volume

 Use of Instruction Manuals

Use of Instruction Manuals

The LabSolutions IR software comprises the LabSolutions Manager program and the LabSolutions IR
program. The instruction manuals, including this manual, are organized as follows.
Refer to the corresponding instruction manual for details on the operation of LabSolutions IR.

Instruction Manual Description

LabSolutions Manager DB
Installation & Maintenance Guide
This manual explains software installation, troubleshooting, and
or
environment settings.
LabSolutions Manager CS
Installation & Maintenance Guide
LabSolutions DB/CS IR
This manual explains FTIR model-specific installation,
Installation & Maintenance Guide
troubleshooting, and environment settings.
IR Volume (this manual)
LabSolutions Manager DB
System Users Guide IR Volume This manual explains how to use the management function, data
or management function, and validation software with respect to
LabSolutions Manager CS LabSolutions system.
System Users Guide
LabSolutions DB/CS IR
This manual explains how to use the FTIR model-specific
System Users Guide IR Volume
management function and validation software.
(this manual)
LabSolutions IR This manual explains specifically how to perform basic operations
Basic Operation Guide using the software.
This quick guide briefly introduces software startup through to initial
LabSolutions IR Quick Guide
operation.

For details on each command in the LabSolutions IR software and execution method, refer to help file
provided with the LabSolutions IR software.

The LabSolutions IR software comprises LabSolutions IR (file management version), LabSolutions DB IR

(database version), and LabSolutions CS IR (client server version).
The procedures for data management, startup, and network connection differ between each version.

Name LabSolutions IR LabSolutions DB IR LabSolutions CS IR

Edition File Management Edition Database Edition Client Server Edition
Data management Measured data files are Measured data files are saved and managed in the
method saved and managed in LabSolutions database.
folders on the PC. The existence of data files cannot be checked using
The existence of data Windows Explorer.
files can be checked
using Windows Explorer.
Data references The software references The software references files in the database.
files on drives or in
folders on the PC.
Transferring Transfer of files Loading via import
LabSolutions IR data (Data can be either copied to a local destination
between PCs using the data file export function or downloaded
from the database manager.)
LabSolutions database Unavailable Available Available
(The database resides on (The database resides on
a local PC) a server or local PC)

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Introduction

Name LabSolutions IR LabSolutions DB IR LabSolutions CS IR

CLASS-Agent database Available (Option) Unavailable
(The contents of the CLASS-Agent database can be
transferred to the LabSolutions database.)
User administration Available
Rights group Available
administration
Project administration Unavailable Available
Standalone/network Either can be used. Only the standalone Only databases on the
configuration can be network can be used.
used. (LabSolutions IR data
can be viewed using the
database manager on a
PC set up for viewing
purposes. Note that
LabSolutions IR must be
installed on the PC used
for viewing.)
Data backup Performed on a Performed for each database.
file-by-file basis using
Windows Explorer.
Startup method LabSolutions IR icon LabSolutions icon
LabSolutions icon
Easy macro programs Available Cannot use the file loading function.
Validation program Available Only validation through measurement can be used.
Validation of previously measured spectra can be
used after copying the necessary files from the
database to a local folder.
Identification test Available Only identification tests through measurement can be
program used.
Identification tests of previously measured spectra
can be used after copying the necessary files from
the database to a local folder.
Contaminant analysis Available Can be used after copying files from the database to
program a local folder.
[Easy Scan] program Available Available
Report viewer Available Unavailable

iv LabSolutions IR System Users Guide IR Volume

 Warranty

Warranty
Shimadzu provides the following warranty for this product.

1. Period: Please contact your Shimadzu representative for information about the period of
this warranty.

2. Description: If a product/part failure occurs for reasons attributable to Shimadzu during the
warranty period, Shimadzu will repair or replace the product/part free of charge.
However, in the case of products which are usually available on the market only
for a short time, such as personal computers and their peripherals/parts, Shimadzu
may not be able to provide identical replacement products.

3. Limitation of 1. In no event will Shimadzu be liable for any lost revenue, profit or data, or for
special, indirect, consequential, incidental or punitive damages, however caused
Liability:
regardless of the theory of liability, arising out of or related to the use of or
inability to use the product, even if Shimadzu has been advised of the possibility
of such damage.
2. In no event will Shimadzu's liability to you, whether in contract, tort (including
negligence), or otherwise, exceed the amount you paid for the product.

4. Exceptions: Failures caused by the following are excluded from the warranty, even if they
occur during the warranty period.
1. Improper product handling
2. Repairs or modifications performed by parties other than Shimadzu or Shimadzu
designated companies
3. Product use in combination with hardware or software other than that designated
by Shimadzu
4. Computer viruses leading to device failures and damage to data and software,
including the product's basic software
5. Power failures, including power outages and sudden voltage drops, leading to
device failures and damage to data and software, including the product's basic
software
6. Turning OFF the product without following the proper shutdown procedure
leading to device failures and damage to data and software, including the
product's basic software
7. Reasons unrelated to the product itself
8. Product use in harsh environments, such as those subject to high temperatures or
humidity levels, corrosive gases, or strong vibrations
9. Fires, earthquakes, or any other act of nature, contamination by radioactive or
hazardous substances, or any other force majeure event, including wars, riots,
and crimes
10. Product movement or transportation after installation
11. Consumable items
Note: Recording media such as floppy disks and CD-ROMs are considered
consumable items.

* If there is a document such as a warranty provided with the product, or there is a separate
contract agreed upon that includes warranty conditions, the provisions of those documents
shall apply.

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Introduction

After-Sales Service and Availability of

Replacement Parts
After-Sales If any problem occurs with this product, perform an inspection and take
appropriate corrective action as described in the "LabSolutions IR Installation
Service
and Maintenance Guide" and "LabSolutions IR Basic Operation Guide".
If the problem persists, or the symptoms are not covered in the troubleshooting
section, contact your Shimadzu representative.

Replacement Replacement parts for this product will be available for a period of seven (7)
years after the product is discontinued. Thereafter, such parts may cease to be
Parts Availability
available.
Note, however, that the availability of parts not manufactured by Shimadzu
shall be determined by the relevant manufacturers.

vi LabSolutions IR System Users Guide IR Volume

 Software License Agreement

Software License Agreement

PLEASE READ THIS AGREEMENT CAREFULLY BEFORE USING THE SOFTWARE.
SHIMADZU Corporation ("SMZ") is willing to license the SMZ software provided herein, together with
accompanying documentation (collectively "SOFTWARE") to you only upon the condition that you accept
all of the terms and condition contained in this License Agreement. By using the SOFTWARE, you agree to
be bound by the terms of this Agreement. If you do not agree to all these terms of this Agreement,
promptly return the unused SOFTWARE to the party (either SMZ or its reseller) from whom you acquired it
to receive a refund of the amount you paid.

SMZ grants you a non-exclusive and nontransferable license to use the

1. LICENSE. SOFTWARE subject to the following terms and conditions.
Except as specifically authorized by SMZ, you may NOT:
2. LIMITATION OF a. Use the SOFTWARE, or permit the SOFTWARE to be used, on more than one
USE. computer at any one time.
b. Copy the SOFTWARE except one (1) archival copy of the SOFTWARE.
c. Modify, reverse engineer, decompile, disassemble, or create derivative works
based upon the SOFTWARE.
d. Transfer, rent, lease or grant any rights in the SOFTWARE in any form to
anyone else.
This license is not for sale and it may not be assigned or sublicensed to anyone
3. TITLE AND else. Title and all associated intellectual property rights to the SOFTWARE shall
OWNERSHIP. remain in SMZ and/or its licensor.
You are entitled to receive all official software upgrades for the SOFTWARE that
4. UPGRADES. SMZ will release as deemed necessary by SMZ. An upgrade means certain
supplemental program modules and/or information for bug fixing and/or updates to
the defects and/or failures of the SOFTWARE that are acknowledged or confirmed
by SMZ. An upgrade excludes hardware, network, consulting services, third party
products, operation and general computer system maintenance.
All supplemental program module for upgrades and enhancements furnished to
you shall be deemed to be part of the SOFTWARE and subject to the terms and
conditions set forth in this Agreement.
SMZ warrants that for a period of one (1) year from the date of purchase, as
5. LIMITED evidenced by a copy of the receipt, the media on which SOFTWARE is furnished
WARRANTY. will be free of defects in materials and workmanship under normal use.
Except for the foregoing, SOFTWARE is provided AS IS. Your exclusive remedy
and the entire liability of SMZ and its suppliers under this limited warranty will be,
at SMZ's option, repair, replacement, or refund of the Software if reported (or,
upon request, returned) to the party supplying the SOFTWARE to you. In no event
does SMZ warrant that the Software is error free or that you will be able to operate
the SOFTWARE without problems or interruptions.
EXCEPT AS SPECIFIED IN THIS WARRANTY, ALL EXPRESS OR IMPLIED
CONDITIONS, REPRESENTATIONS, AND WARRANTIES INCLUDING,
WITHOUT LIMITATION, ANY IMPLIED WARRANTY OF MERCHANTABILITY,
FITNESS FOR A PARTICULAR PURPOSE, NONINFRINGEMENT, ARISING
FROM A COURSE OF DEALING, USAGE, OR TRADE PRACTICE, ARE
HEREBY EXCLUDED TO THE EXTENT ALLOWED BY APPLICABLE LAW.
IN NO EVENT WILL SMZ BE LIABLE FOR ANY LOST REVENUE, PROFIT OR
6. LIMITATION OF DATA, OR FOR SPECIAL, INDIRECT, CONSEQUENTIAL, INCIDENTIAL OR
LIABILITY. PUNITIVE DAMAGES, HOWEVER CAUSED REGARDLESS OF THE THEORY
OF LIABILITY, ARISING OUT OF OR RELATED TO THE USE OF OR INABILITY
TO USE SOFTWARE, EVEN IF SMZ HAS BEEN ADVISED OF THE
POSSIBILITY OF SUCH DAMAGE. IN NO EVENT WILL SMZ’S LIABILITY TO
YOU, WHETHER IN CONTRACT, TORT (INCLUDING NEGRIGENCE), OR
OTHERWISE, EXCEED THE AMOUNT YOU PAID FOR SOFTWARE.
This License is effective until terminated. You may terminate this License at any
7. TERMINATION. time by destroying all copies of SOFTWARE including any documentation.
This License will terminate immediately without notice from SMZ if you fail to
comply with any provision of this License. Upon termination, you must destroy all
copies of SOFTWARE.

LabSolutions IR System Users Guide IR Volume vii

Introduction

a. This Agreement is the entire agreement. If any provision of this agreement is

8. GENERAL held invalid, the remainder of this agreement shall continue in full force and
effect.
b. This Agreement shall be construed and governed in accordance with the laws
of Japan, excluding its conflict of law rules.
c. The exclusive jurisdiction for any disputes arising out of or in connection with
this Agreement shall be Kyoto District Court of Japan.
d. The invalidity or unenforceability of any provision of this Agreement shall not
affect the validity or enforceability of any other provision.

viii LabSolutions IR System Users Guide IR Volume

 Contents
Introduction ...................................................................................................... i
About the Instruction Manual......................................................................................................................ii
Use of Instruction Manuals........................................................................................................................ iii
Warranty .....................................................................................................................................................v
After-Sales Service and Availability of Replacement Parts .......................................................................vi
Software License Agreement ................................................................................................................... vii

Chapter 1 System Administration .................................................................1

1.1 System Administration Policy (Security Policy) for LabSolutions IR ............................................. 1
1.2 Numerical Rounding and Number of Displayed Digits.................................................................. 3
1.3 System Operation ......................................................................................................................... 5
1.3.1 Screen Lock to Protect System..................................................................................................... 5

Chapter 2 Data Management .......................................................................7

2.1 LabSolutions IR File Formats........................................................................................................ 7
2.1.1 Tree View...................................................................................................................................... 7
2.1.2 Data Formats of the LabSolutions IR Software ............................................................................. 8
2.1.3 File Formats of the LabSolutions IR Software............................................................................. 10
2.2 Other Functions in DataManager ................................................................................................ 13
2.2.1 Data Set and Result File Operations........................................................................................... 13
2.2.2 Relating the File Type of Registered Data to Programs .............................................................. 13

Chapter 3 Audit Trail Function ....................................................................15

3.1 Audit Trail Functions.................................................................................................................... 15
3.2 Checking the LabSolutions IR Operation Log............................................................................. 15
3.3 Checking the Data History Using the [History] Tab ..................................................................... 16
3.4 Checking the Data History Using [Tree view].............................................................................. 17

Chapter 4 Validation Program ....................................................................19

4.1 Introduction ................................................................................................................................. 19
4.2 Notes ........................................................................................................................................... 20
4.2.1 Preparation for Execution............................................................................................................ 20
4.2.2 During Operation......................................................................................................................... 20
4.2.3 Important Notes Regarding LabSolutions DB IR (Database Edition) and LabSolutions CS IR
(Client Server Edition)................................................................................................................. 21
4.3 Software Usage - JP/EP/ChP Compliant Validation ................................................................... 22
4.3.1 Starting the Validation Program................................................................................................... 23
4.3.2 Settings ....................................................................................................................................... 26
4.3.3 Scan............................................................................................................................................ 27
4.3.4 Validation Using Stored Data (JP/EP/ChP ) ................................................................................ 30
4.3.5 Judgement and End of Program ................................................................................................. 33
4.4 Operation for the ASTM Validation Program............................................................................... 35
4.4.1 Starting the Software................................................................................................................... 36

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Contents

4.4.2 Settings....................................................................................................................................... 40
4.4.3 Scan ........................................................................................................................................... 41
4.4.4 Validation Using Stored Data (ASTM)......................................................................................... 43
4.4.5 Judgement and End of Program ................................................................................................. 44
4.4.6 Troubleshooting .......................................................................................................................... 46
4.5 Operation of the Report Viewer................................................................................................... 47
4.5.1 Starting up the Report Viewer ..................................................................................................... 47
4.5.2 Operation Method ....................................................................................................................... 49
4.5.3 End of Program........................................................................................................................... 50
4.6 The Japanese Pharmacopoeia ................................................................................................... 51
4.6.1 Power Spectrum ......................................................................................................................... 51
4.6.2 Resolution................................................................................................................................... 51
4.6.3 Wavenumber Accuracy ............................................................................................................... 52
4.6.4 Wavenumber Reproducibility ...................................................................................................... 52
4.6.5 Transmittance Reproducibility..................................................................................................... 52
4.7 The European Pharmacopoeia ................................................................................................... 53
4.7.1 Power Spectrum ......................................................................................................................... 53
4.7.2 Resolution................................................................................................................................... 54
4.7.3 Wavenumber Accuracy ............................................................................................................... 54
4.7.4 Wavenumber Reproducibility ...................................................................................................... 54
4.7.5 Transmittance Reproducibility..................................................................................................... 54
4.8 The Chinese Pharmacopoeia ..................................................................................................... 55
4.8.1 Power Spectrum ......................................................................................................................... 55
4.8.2 Resolution................................................................................................................................... 55
4.8.3 Wavenumber Accuracy ............................................................................................................... 56
4.8.4 Wavenumber Reproducibility ...................................................................................................... 56
4.8.5 Transmittance Reproducibility..................................................................................................... 56
4.8.6 Peak Resolution Function........................................................................................................... 57
4.9 ASTM E1421-94 Level Zero ....................................................................................................... 58
4.9.1 Energy Spectrum Test................................................................................................................. 58
4.9.2 One Hundred Percent Line Test.................................................................................................. 59
4.9.3 Polystyrene Test ......................................................................................................................... 59

x LabSolutions IR System Users Guide IR Volume

 Chapter 1 System Administration
This chapter explains the system administrator functions that are specific to LabSolutions IR.
For details on other functions, refer to the LabSolutions Manager CS or LabSolutions Manager DB
System Users Guide.

1.1 System Administration Policy (Security Policy) for

LabSolutions IR

For details, refer to " Instrument Policies" in "1.2.1 Set System Administration Policy (Security
Policy)" in the LabSolutions Manager CS or LabSolutions Manager DB System Users Guide.

 Instrument Policies

1. Double-click the (Security Policy) icon in the [Administration Tools] sub-window of the
[LabSolutions Main] window.

2. Click the [Instrument] tab.

3. Select [IR] from the [Instrument Type] list.

4. Set each item and click [OK].

Saving by overwriting a file of the same name for each file type is prohibited when saving files in this
software.
However, files are saved by overwriting after performing manipulation, searching, and quantitative
calculations and when the results are added to a data set.

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Chapter 1 System Administration

1
2
3

No. Name Function

1 Output data status in Output the data file's information to a report when printing without
header of report saving the data file.
2 Prohibit overwriting of Prohibit saving by overwriting existing data files when saving a
other data files data file using a different name.
3 Overwrite the data file at Immediately save the data file by overwriting when a data set that
the same time adding the contains the results of searching and manipulation is added to the
IR data set data file.

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 1.2 Numerical Rounding and Number of Displayed Digits

1.2 Numerical Rounding and Number of Displayed

Digits

For details, refer to "1.2.8 Numerical Rounding and Number of Displayed Digits" in the LabSolutions
Manager CS or LabSolutions Manager DB System Users Guide..

The rounding method and number of displayed digits can be batch-set in the [Data Processing
Settings] sub-window.

Since system settings are changed in this sub-window, log in with a user ID having [Change System
Settings] rights.

1. Double-click the (System Settings) icon in the [Administration Tools] sub-window of the
[LabSolutions Main] window.

2. Click [Data Proc. Settings].

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Chapter 1 System Administration

3. Select the rounding method and number of displayed digits for specific calculation results, and
click [OK].
In this example, the [Area/Corr. Area] display format is set to 3 digits past the decimal point (i.e. the
4th digit past the decimal point is rounded down).
1 2 3 4

1. The type of the instrument is displayed.

2. Open the [Display Type] list for the [Area/Corr. Area] row, and select [Default] from among
[Default]/[Exponential]/[Significant Digits].
3. Enter 2 in the [Decimal Digits] column of the [Area/Corr. Area] row.
4. Open the [Rounding] list for the [Area/Corr. Area] row, and select [Round Down] from among
[Half Adjust]/[Round Up]/[Round Down].

If [Default] or [Exponential] is selected as the [Display Type], enter the number of decimal
places in the [Decimal Digits] column, and if [Significant Digits] is selected, enter the number of
digits in the [Significant Digits] column.

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 1.3 System Operation

1.3 System Operation

For details, refer to "1.3.2 Screen Lock to Protect System" in the LabSolutions Manager CS or
LabSolutions Manager DB System Users Guide.

1.3.1 Screen Lock to Protect System

The [LabSolutions Main] window and sub-windows can be individually locked to protect the system
from accidents or manipulation by other operators if the logged in operator temporarily leaves the
PC.
When the lock function is enabled, the window is minimized and displayed as an icon on the taskbar.
If the icon is clicked, the [User Authentication] sub-window opens to prompt the user to enter the
user ID and password.
This section describes an example of how to lock screens in the [Postrun] window.

1. Click [Lock] on the [Window] menu.

The [Postrun] window is minimized and an icon is displayed on the taskbar.

2. Click the [Postrun] icon on the taskbar to open the application.

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3. Enter a [User ID] and [Password], and click [OK].

Only the user who locks the window can release the lock.

6 LabSolutions IR System Users Guide IR Volume

 Chapter 2 Data Management
This chapter explains the data formats used in LabSolutions IR and the tree view used for managing
displayed data.
For details on other functions, refer to the LabSolutions Manager CS or LabSolutions DB System
Users Guide.

2.1 LabSolutions IR File Formats

2.1.1 Tree View
The tree view displays scan parameters, peak pick tables, and data history saved together with the
data opened in a hierarchical view in LabSolutions IR.
Click [+] on each node to expand the hierarchy contained within.
The tree view structure is shown below.
Display or hide the tree view by clicking [Tree View] on the [View] menu.
[Data file.ispd]
[Original data] (absorbance or transmittance)
[Properties] (Scan parameters)
(History)
(Annotation)
(Peak pick table)
(Spectrum search results)
(Quantitative results)
[Sample interferogram]
[Background interferogram]
[Manipulation [Properties] (History)
result 1]
(Annotation)
(Peak pick table)
[Manipulation [Properties]
result 1 of 1]
(Annotation)
(Peak pick (History)
table)
[Manipulation [Properties] (History)
result 1]
(Annotation)
(Peak pick table)

Example of Spectrum Data

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Measure a sample or open data to display data in the tree view and data area.
At first, data is displayed at the top of the hierarchical structure. When data is processed, new data
is added at the lower levels.
If other data is added, it is displayed at the top of the hierarchical structure. Close the data to remove
the data from the tree view and data area.
For details on the data format of displayed data, see "2.1.3 File Formats of the LabSolutions IR
Software".
The following operations can be performed on data in the tree view.
Operation Description
Click [+] or ] to the left of Display or hide the contents of the data in the tree view.
data Click [+] to display data lower in the hierarchy.
Click [] to hide data lower in the hierarchy.
Double-click Double-click on data to perform processing on it.
The type of processing differs depending on the program or displayed
window.
Double-click when the postrun program is running or the view window is
shown to display the corresponding data.
Double-click when the Quantitation program, Photometric program, or
chemometrics window is shown to add the corresponding spectrum to the
sample table.
Right-click Right-click on data to execute any of the following operations on the
command menu, which are displayed according to the context of the task.
 Clear the data tab display
 Select to display or hide parameters
 Specify a file for manipulation
 Add data to a library
Drag Drag data to the data area to perform processing on it.
The type of processing differs depending on the program or displayed
window.
Double-click when the postrun program is running or the view window is
shown to display the corresponding data.
Drag when the Quantitation program, Photometric program, or chemometrics
window is shown to add the corresponding spectrum to the sample table.

2.1.2 Data Formats of the LabSolutions IR Software

Because LabSolutions IR data files are compatible with GLP/GMP, original data obtained during
measurement and all calculation results obtained using various manipulation functions are saved in
a single file.
Accordingly, a single data file stores multiple data.
For this reason, files that contain all of the data are referred to as "containers" and each set of data
within a container is referred to as a "data set". In addition, each data set is appended with auxiliary
information.
 Data sets included in the container for spectrum data
Item Description
Sample transmittance or This is the data of the sample that is normally used.
absorbance data This data set is used in the analysis of the sample.
Sample interferogram Raw measurement data of the sample obtained from the instrument.
Background interferogram Raw measurement data of the background obtained from the instrument.
All manipulation results Result data obtained from applying various manipulation functions to the
data set. This data is regarded as independent data and added to the
container.
Quantitative results The results of quantitative calculation.
Spectrum search results Spectrum search results (hit list) and spectral subtraction calculation
results.

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 2.1 LabSolutions IR File Formats

 Data sets included in the container for mapping measurement data and Time course
measurement data
Item Description
3D/4D data A 3D display of mapping measurement data and Time course
measurement data.
Constructed spectrum Spectrum data of each position vs. time.
Each position contains its own data chart (data set of spectrum data).
TAC/SAC TAC/SAC data calculated from mapping measurement data or Time
course measurement data.

 Data sets included in the container for quantitation measurement data and photometric
measurement data
Item Description
Standard sample table Table data with information including the sample name and concentration.
Unknown sample table
Sample table
Constructed spectrum Standard sample, unknown sample, and sample spectrum data.
Each position contains its own data chart (data set of spectrum data).

 Auxiliary data appended to each data set

Item Description
History History of data set generation and modification
Scan parameters Parameters used during measurement
Annotation A list of comments entered in the spectrum window using the commenting
function
Peak pick table Peak pick table generated using the peak pick function
Point pick table Point pick table generated using the Point pick function.

When these data sets are created through measurement or a saved container is loaded into the
software, they are displayed on screen in the tree view so that dependencies between data sets are
apparent.
In the case of spectrum data, although transmittance or absorbance data of a sample is created
during measurement, this data is displayed at the top of the hierarchy in the tree view. Other data
sets and auxiliary data appended directly to the top data set are displayed at lower levels in the
hierarchy.
Auxiliary data is also appended to each data set other than the top data set. When manipulation is
executed, the resulting spectrum is inserted as a new data set directly under the original data set for
which processing was executed.
One of the data sets among these is regarded to represent the entire container file and is used for
display and data analysis by the software. This data set is referred to as the "active data set" and
usually specifies the original transmittance or absorbance data of sample. If any manipulation is
performed on the active data set, the result of such processing then becomes the new active data
set. The software also allows the active data set to be selected manually.

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2.1.3 File Formats of the LabSolutions IR Software

The following file formats can be used with the LabSolutions IR software.
It is possible to set the data formats (filters) for use in [File Preferences] - [File Filters] on the [Tool]
menu.
 Data files
Name Extension Description
Spectrum file ispd This file contains spectrum data.
In addition to sample spectra, this file contains spectra of manipulation
in progress, background and sample interferograms, scan parameters
and peak pick tables, Point pick tables, and search results.
Area mapping file i4dd This file contains area mapping measurement data.
In addition to data for 3D display, this file contains visible images, a
sample spectrum for each position, background and sample
interferograms, and scan parameters.
Execute [3D Manipulation] to replace the metadata in the sample
spectrum with that of the calculation results. Any subsequent
manipulation can only be executed with respect to the latest
calculation results.
Manipulation with respect to each sample spectrum is performed after
the corresponding spectra have been exported.
Line mapping file i3dd This file contains line mapping measurement data.
In addition to data for 3D display, this file contains visible images, a
sample spectrum for each position, background and sample
interferograms, and scan parameters.
Execute [3D Manipulation] to replace the metadata in the sample
spectrum with that of the calculation results. Any subsequent
manipulation can only be executed with respect to the latest
calculation results.
Manipulation with respect to each sample spectrum is performed after
the corresponding spectra have been exported.
Time course file itcd This file contains Time course measurement data.
In addition to data for 3D display, this file contains a sample spectrum
for each point in time, background and sample interferograms, and
scan parameters.
Execute [3D Manipulation] to replace the metadata in the sample
spectrum with that of the calculation results. Any subsequent
manipulation can only be executed with respect to the latest
calculation results.
Manipulation with respect to each sample spectrum is performed after
the corresponding spectra have been exported.
Rapid scan file rspc This file contains rapid scan measurement data.
In addition to data for 3D display, this file contains a sample spectrum
for each point in time, background and sample interferograms, and
scan parameters.
Execute [3D Manipulation] to replace the metadata in the sample
spectrum with that of the calculation results. Any subsequent
manipulation can only be executed with respect to the latest
calculation results.
Manipulation with respect to each sample spectrum is performed after
the corresponding spectra have been exported.
While this file can be loaded, it cannot be output.
2D file i2dd This file contains a change of position graph cut from line mapping
measurement data using [Extract] or a change over time graph cut
from Time course measurement data using [Extract].
Calibration curve file istd This file contains the calibration curve data used in quantitation
measurement.
It comprises a standard sample table, calibration curve parameters,
and standard sample spectra.

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 2.1 LabSolutions IR File Formats

Name Extension Description

Quantitation irqt This file contains the quantitative result data from quantitation
measurement.
It comprises a standard sample table, calibration curve parameters,
standard sample spectra, unknown sample table, and unknown
sample spectra.
CLS calibration curve irqc These files contain the calibration curve data used in CLS and PLS
file quantitation measurement.
PLS calibration curve It comprises a standard sample table, calibration curve parameters,
file and standard sample spectra.
Photometric file ipht This file contains the photometric result data from photometric
measurement.
It comprises a sample table, photometric parameters, and sample
spectra.
JCAMP-DX file dx/cs/jpx This is a JCAMP-DX format file.
/jcm This file can be loaded and saved (exported).
This file format is used when sharing data with software products
developed by other companies.
Only one set of data (one spectrum) can be saved per file.
JCAMP-DX format settings can be configured in [File Preferences] -
[File Filters] - [JCAMP-DX Files] on the [Tool] menu.
ASCII file asc This is an ASCII format file.
This file can be loaded and saved (exported).
It consists of a predetermined header file and a list of vertical axis
value data (such as transmittance or absorbance).
Only one set of data (one spectrum) can be saved per file.
ASCII Simple Text txt This text format file format contains horizontal axis values (such as
(text) file wavenumbers) and the corresponding vertical axis values (such as
transmittance or absorbance) delimited with commas.
This file can be loaded and saved (exported).
It is used when handling data in spreadsheet software.
Only one set of data (one spectrum) can be saved per file.
ASCII UVProbe txt A spectrum file which is saved as Data pritn format on UVProbe can
Spectrum (text) file be imported to LabSolutions IR.
A spectrum file is exported to a text format which can be loaded on
UVProbe.
Only one set of data (one spectrum) can be saved per file.
HYPER-IR file irs This file format was used in the HYPER-IR software.
This file can be loaded and saved (exported).
Only one set of data (one spectrum) can be saved per file.
IRsolution file smf This file contains the data measured using the IRsolution software.
While this type of file can be loaded, smf format files cannot be output.
This file can contain spectra, 3D, 4D, calibration curve, or 2D files.
In addition to sample spectra, this file contains spectra of manipulation
in progress, background and sample interferograms, scan parameters
and peak pick tables, Point pick tables, search results, and calibration
curves.
3D file 3d This is a 3D data file obtained using mapping measurement with the
HYPER-IR software.
While this file can be loaded, it cannot be output.
4D file 4d This is a 4D data file obtained using mapping measurement with the
HYPER-IR software.
While this file can be loaded, it cannot be output.

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Chapter 2 Data Management

 Parameter files
Name Extension Description
Scan parameters iscp This file stores scan parameters.
It is not compatible with the IRsolution software.
Time course scan itcp This file stores Time course scan parameters.
parameter file It contains Time course measurement settings, scan parameters, and
equation settings.
Photometric condition iphp This condition file is used for photometric measurement.
file It contains photometric parameters, scan parameters, and equation
settings.
Point pick template file iptm This template file is used for Point pick.
Equation file iequ This file stores equations used in mapping measurement, Time course
measurement, quantitation measurement, and photometric
measurement.
Report template file irtm This is a report template file.
It is not compatible with the IRsolution software.
Search parameter file isrp This file contains the search parameters used in spectrum search.
It is not compatible with the IRsolution software.

 User libraries
Name Extension Description
User library file Idx This library file comprises five types of identically named files that
idx2 have different file extensions.
sig Regard the five types as a single group.
nam
l+
two-digit
number

 Easy macro program and VB macro program files

Name Extension Description
Easy macro sequence iscq This is an easy macro program.
file
Macro container file ilcm/lcm This is a Visual BASIC macro program in container format.
BASIC file bas This is the file format of Visual BASIC macro programs.

 Other
Name Extension Description
Log log This file contains the history of operations performed using the
software.
The contents of this file can be checked in [Operation Log] - [View] on
the [Tool] menu.

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 2.2 Other Functions in DataManager

2.2 Other Functions in DataManager

2.2.1 Data Set and Result File Operations
 Import Files Related to Data Acquisition Results as Result Files

For details, refer to "2.2 Other Functions in DataManager" and " Import Files Related to Data
Acquisition Results as Result Files" in "2.2.3 Data Set and Result File Operations" in the LabSolutions
Manager CS or LabSolutions Manager DB System Users Guide.

Any file can be registered to the database related to a row (i.e. sample information) displayed in
[Sample Information View]. This section describes an example of the procedure for importing a file to
[Result File View].

 To import a file, log in by a user ID having the [Import Files] rights.

 [DataManager] has a function for directly referencing the content of backup databases. Files,
however, cannot be imported to backup database since backups are read-only.
 The following table summarizes files that can be imported related to sample information:
File Type Displayed in
Imported Location Importable File
[Sample Information View]
Data file [Sample Information View] Data file
[Result File View] Files of all types

2.2.2 Relating the File Type of Registered Data to Programs

For details, refer to Section "2.2 Other Functions in DataManager" and "2.2.5 Relate the File Type of
Registered Data to Programs" in the LabSolutions Manger CS or LabSolutions Manager DB System
Users Guide.

With [DataManager], result files or files contained in rows of sample information can be related to
programs used for viewing and printing.
As the default, the following relations are set:
File Type Extension Program
Spectrum files ispd IRsolution.exe (Postrun)
smf IRView.exe
Time course file itcd IRsolution.exe (Postrun)
Mapping file i4dd IRsolution.exe (Postrun)
i3dd
2D file i2dd IRsolution.exe (Postrun)
Calibration curve file istd IRsolution.exe (Quantitation)
Quantitation file irqt IRsolution.exe (Quantitation)
CLS Calibration curve file irqc IRsolution.exe (Postrun)
PLS Calibration curve file
Photometric file ipht IRsolution.exe (Photometric)

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14 LabSolutions IR System Users Guide IR Volume

 Chapter 3 Audit Trail Function
This chapter explains the operations for checking audit trail logs.

3.1 Audit Trail Functions

LabSolutions IR keeps the following audit trail logs.
 An operation log that records LabSolutions IR software operations, warnings, and errors
 A history (data log) that records manipulation performed from data creation to the current point in
time

Information including scan parameters, peak pick tables, and data history are saved in the data file
together with raw data from measurement. When manipulation is performed with respect to this data,
the result of manipulation is added as child data below the original data in the hierarchy.

These audit trail functions are always operating.

3.2 Checking the LabSolutions IR Operation Log

Display the operation log that records LabSolutions IR software operations, warnings, and errors.

1. Start the LabSolutions IR measurement program or postrun program.

2. Click [Operation Log] - [View] on the [Tool] menu.

The [Operation Log] window is displayed.

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Chapter 3 Audit Trail Function

3.3 Checking the Data History Using the [History] Tab

Display the history (data log) that records manipulation performed from data creation to the current
point in time.

1. Start the LabSolutions IR measurement program or postrun program.

2. Click [Open] on the [File] menu and open the data whose history is to be checked.

3. Click [Parameters] on the [View] menu to add a check mark.

The [Parameters] window is displayed.
 The [Data] tab displays information on data including data type and data points.

 The [Measurement] tab displays data scan parameters.

However, scan parameters are not displayed for imported data, data that has undergone
manipulation, and data other than raw data.

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 3.4 Checking the Data History Using [Tree view]

 The [History] tab displays a history (data log) of recorded manipulation performed from data
creation to the current point in time.

3.4 Checking the Data History Using [Tree view]

When manipulation is performed with respect to data in LabSolutions, the result of manipulation is
added as child data below the original data in the hierarchy in a tree structure.
Viewing data in this tree structure allows users to check the type of processing that data has
undergone from data creation to the current point in time.

The tree view structure is shown below.

[Data file.ispd]
[Original data] (absorbance or transmittance)
[Properties] (Scan parameters)
(History)
(Annotation)
(Peak pick table)
(Spectrum search results)
(Quantitative results)
[Sample interferogram]
[Background interferogram]
[Manipulation [Properties] (History)
result 1]
(Annotation)
(Peak pick table)
[Manipulation [Properties]
result 1 of 1]
(Annotation)
(Peak pick (History)
table)
[Manipulation [Properties] (History)
result 1]
(Annotation)
(Peak pick table)

Example of Spectrum Data

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Chapter 3 Audit Trail Function

The following operations can be performed on data in the tree view.

Operation Description
Click [+] or ] to the left of Display or hide the contents of the data in the tree view.
data Click [+] to display data lower in the hierarchy.
Click [] to hide data lower in the hierarchy.
Double-click Double-click on data to perform processing on it.
The type of processing differs depending on the program or displayed
window.
Double-click when the postrun program is running or the view window is
shown to display the corresponding data.
Double-click when the Quantitation program, Photometric program, or
chemometrics window is shown to add the corresponding spectrum to the
sample table.
Right-click Right-click on data to execute any of the following operations on the
command menu, which are displayed according to the context of the task.
 Clear the data tab display
 Select to display or hide parameters
 Specify a file for manipulation
 Add data to a library
Drag Drag data to the data area to perform processing on it.
The type of processing differs depending on the program or displayed
window.
Double-click when the postrun program is running or the view window is
shown to display the corresponding data.
Drag when the Quantitation program, Photometric program, or chemometrics
window is shown to add the corresponding spectrum to the sample table.

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 Chapter 4 Validation Program
This chapter explains the validation program for the FTIR system.

This software includes a validation program that is used to check the performance of the FTIR
system. The program measures data and performs FTIR system validation according to Japanese
Pharmacopoeia, European Pharmacopoeia, Chinese Pharmacopoeia, and American Society for
Testing and Materials standards.

4.1 Introduction
The validation program performs validation of the Shimadzu Fourier transform infrared
spectrophotometer IRPrestige-21/IRTracer-100/IRAffinity-1 series/FTIR-8000 series on the
LabSolutions IR software, which is used to perform FTIR control and data processing.
This software complies with the description in 'General Test 23, Infrared Spectrophotometry' of the
Sixteenth Edition of Japanese Pharmacopoeia, "Absorption Spectrophotometry, Infrared" of the
European Pharmacopoeia 7.0, 'Equipment and Calibration' in 'Appendix IV C Infrared
Spectrophotometry' of the Chinese Pharmacopoeia 2010 and ASTM (American Society for Testing
and Materials) E1421-94 Level Zero. Either of polystyrene film of the standard accessory of FTIR,
supplied by NIST, or installed on the Beam Switching Kit is used for the validation. The result is
output to the screen and the printer. The report viewer program is included to display and print the
validation result later.
Because this software works on LabSolutions IR, the measurement and the calculation can be
executed as a series of operations. It is also possible to validate using the data, which is already
measured and saved from the disk.

 Please purchase and use polystyrene film designated as Standard Reference Material and
supplied by NIST or its secondary standard when traceable polystyrene film is needed.
 Please use polystyrene film designated as Standard Reference Material and supplied by NIST or
its secondary standard to run the ChP Validation program.
 Only the FTIR-8300/8400/8400S, IRPrestige-21, IRTracer-100, and IRAffinity-1 series are
compliant with European Pharmacopoeia 7.0.
In other FTIR-8000 series (FTIR-8700/8900), please use the validation program that complies with
the Chinese Pharmacopoeia 2010 / the sixteenth edition of Japanese Pharmacopoeia.
 Always input half-width numbers when requested for numeric input by this program.

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4.2 Notes
4.2.1 Preparation for Execution
 Beam Switching Kit
It is necessary to install the optional Beam Switching Kit (P/N 206-70125-91/92) for the Automatic
validation.

 Configuration of LabSolutions IR
Configure the following on the spectrum measurement toolbar in the spectrum measurement
program in LabSolutions IR.
 Select the [View background] checkbox.
 Deselect the [Continuous] checkbox.

 When "View Background" is not checked, you can't measure a polystyrene film.
 FTIR-8400S hasn't function of "continuous" measurement.

 Scan Parameters
When the program runs, scan parameters are changed for it. When the LabSolutions IR is activated
as a user without a right of "Edit scan parameters", scan parameters are changed for the program.
Memorizing or saving scan parameters before running the program is recommended.
When a user without a right of "Edit scan parameters" uses a Measurement program after executing
this program, he loads a scan parameter file which was saved by Administrator.

 Initilization
To stabilize Ceramics light source, Validation program must be run 30 minites for
Japanese/European/Chinese Pharmacopoeia validattion or 2 hours for ASTM validation after turning
ON the ceramics light source for middle IR after initiliation with middle IR scan parameters on
Spectrum program. Set scan parameters as below.
Light source; Infrared
Range; MID
Beam; Internal
Detector; Stanadard
If FTIR was initilized with scan parameters for NIR (Light source; Tungsten), Validation does not give
you correct resultm because Ceramics light source is not used.

 Re-execution of Validation program

Validation program must be closed and re-executed when validation program must be executed
agaian.

4.2.2 During Operation

The following operations will cause [Automation Error] to be displayed.
 [Cancel] is clicked in the [LabSolutions Main] window.
 Spectrum data is not obtained because scanning of the sample spectrum is aborted.
 Spectrum data is not opened because [Cancel] is clicked in the [File open] window.

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 4.2 Notes

4.2.3 Important Notes Regarding LabSolutions DB IR (Database Edition)

and LabSolutions CS IR (Client Server Edition)
LabSolutions DB IR (database edition) and LabSolutions CS IR (client server edition) store scanned
spectra in a database, which results in the following restrictions.
 Spectra scanned using the validation program in LabSolutions DB IR (database edition) and
LabSolutions CS IR (client server edition) are stored in a database instead of a local PC.
 Because the validation program cannot open spectra in the database, export the required
spectrum from the database to a local folder on the PC in advance and then select the exported
spectrum.

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Chapter 4 Validation Program

4.3 Software Usage - JP/EP/ChP Compliant Validation

The JP/EP/ChP compliant validation software described here performs validation using a method
compliant with the sixteenth edition of Japanese Pharmacopoeia , European Pharmacopoeia 7.0
and Chinese Pharmacopoeia, and allows manual validation using polystyrene film, which is supplied
as an accessory with Shimadzu's FTIR series, standard sample supplied by NIST, or some other
compliant product. The optional beam switching kit (P/N 206-70125-91/92) must be installed to
perform automatic validation.
Automatic validation can also be performed by using the polystyrene film installed in the optional
beam switching kit (P/N 206-70125-91/92).
The spectrum required for validation can be acquired using either of the following two methods.
 By performing measurement at execution
 By loading data measured using Shimadzu's FTIR series that was saved in advance
The following 3 spectra should be prepared to validate the FTIR with stored spectra.
 Power spectrum
 Polystyrene spectrum 1
 Polystyrene spectrum 2

 Please purchase and use polystyrene film designated as Standard Reference Material and
supplied by NIST or its secondary standard when traceable polystyrene film is needed.
 Please use polystyrene film designated as Standard Reference Material and supplied by NIST or
its secondary standard to run the ChP Validation program.
 Only the FTIR-8300/8400/8400S, IRPrestige-21, IRTracer-100, and IRAffinity-1 series are
compliant with European Pharmacopoeia 7.0.
In other FTIR-8000 series (FTIR-8700/8900), please use the validation program that complies with
the Chinese Pharmacopoeia 2010 / the sixteenth edition of Japanese Pharmacopoeia.
 Always input half-width numbers when requested for numeric input by this program.

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 4.3 Software Usage - JP/EP/ChP Compliant Validation

4.3.1 Starting the Validation Program

1. Close all LabSolutions IR measurement programs and the Postrun program, and then run
Spectrum program.

2. Initilize your FTIR with scan parameters for Mid-IR.

Set scan parameters as below.
Light source; Infrared
Range; MID
Beam; Internal
Detector; Stanadard

3. Click the [Macro] tab in the LabSolutions IR launcher, and then double-click [JP Validation],
[EP Validation] or [ChP Validation].

The [Macro Execute] window is displayed.

4. Click [Run].

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Chapter 4 Validation Program

5. Enter a user ID and password into the [Login] window and click [OK].

When [Cancel] is clicked, [Automation Error] is displayed. Click [OK].

Program starts.
LabSolutions IR Spectrum program starts and the [Select Instrument Type], [Select Language], and
[Select change-beam] window is displayed.
This dialog box is displayed when the Validation program is run for the first time. After that, it is not
displayed, but the setting can be changed later.

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 4.3 Software Usage - JP/EP/ChP Compliant Validation

6. Click [ ] next to [Instrument] to select the instrument for use, then click [OK].
Instrument Instrument Type
IRPrestige / IRAffinity / IRTracer / 8400S FTIR-8300, FTIR-8400 series, IRPrestige-21,
IRTracer-100, IRAffinity-1 series
FTIR-8000 series FTIR-8700, FTIR-8900

While the items for inspection are basically the same when "FTIR-8000 Series" is selected, power
spectrum inspection is not performed at 351 cm-1. In addition, the reference used in power spectrum
inspection is different for each instrument type.
After clicking [OK], the [Select Language] dialog box is displayed.

Only the FTIR-8300/8400/8400S, IRPrestige-21, IRTracer-100 and IRAffinity-1 series are

compliant with European Pharmacopoeia 7.0.
In other FTIR-8000 series (FTIR-8700/8900), please use the validation program that complies
with the Chinese Pharmacopoeia 2010 / the sixteenth edition of Japanese Pharmacopoeia.

7. Click [ ] next to [Language] to select the language (English or Japanese), then click [OK].

8. Click [ ] next to [Change-Beam] to select the Validation mode (manual or automatic), then
click [OK].

 Select "Use" and click [OK] when the optional Beam Switching Kit (P/N 206-70125-91/92) is
installed on Shimadzu FTIR series instruments. When the kit is not installed, select "Un-using" and
click [OK].
 The Manual Validation program displays a message on screen prompting the operator to set the
polystyrene film in the sample compartment. Set the polystyrene film into the sample holder. The
Automatic Validation program automatically inserts the polystyrene film installed on the Beam
Switching Kit and scans the necessary spectra.

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Chapter 4 Validation Program

The following dialog box is displayed.

Item Function
Load Run the Validation program with loading saved spectra.

"4.3.4 Validation Using Stored Data (JP/EP/ChP )"

Measurement Run the Validation program with scanning a polystyrene film.

"4.3.3 Scan"
Settings Configures language and the Validation mode (manual/auto).

"4.3.2 Settings"
Cancel Cancels the program.

4.3.2 Settings
The following settings should be configured before running the Validation program.
 Instrument type is selected from IRPrestige/IRAffinity/IRTracer/8400S or the FTIR-8000 series.
 Validation mode is selected between Manual validation and Automatic validation.
 Language is selected between Japanese and English.

1. Click the [Settings] button.

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 4.3 Software Usage - JP/EP/ChP Compliant Validation

2. Click the button of the item to be changed.

Item Function
Instrument Select the instrument type.
“IRPrestige/IRAffinity/IRTracer/ 8400S”
FTIR-8300, FTIR-8400 series、IRPrestige-21, IRAffinity-1 series,
IRTracer-100
“FTIR-8000 series”
FTIR-8700/8900
Language Select Language between Japanese and English.
Change-Beam Select Validation mode between Manual validation and Automatic
validation.
Cancel Aborts the program.

4.3.3 Scan
Measure spectra and perform validation.

1. Click [Measurement].

2. Input can be added to "Instrument", "Serial No.", "Temperature", "Sample name", "Relative
Humidity", "Inspected by" and "No. of Scans." When IRTracer-100 is tested, Type of window
at Sample compartment now used must be selected.
Sutable inspection stabndards for shape of the power spectrum is used.
Printer output will display information provided by the user, columns left empty will appear blank.

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Chapter 4 Validation Program

The number of scans guaranteed by Shimadzu is 45. When setting a number of scans less than
this value, make sure that a spectrum of sufficient quality has been acquired in advance and
that adequate verification has been performed with respect to the desired setting for the number
of scans.

The following message is displayed and processing to determine the shape of the power spectrum is
started.

The message "Remove Sample from Sample compartment" is displayed.

3. Confirm that no sample is set on the sample compartment and then click the [OK] button.
The scan parameter is sent to the interferometer and the measurement of the power spectrum starts.
This power spectrum will also be the background of the following measurement.

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 4.3 Software Usage - JP/EP/ChP Compliant Validation

After power spectrum measurement is complete, processing proceeds to polystyrene measurement.

The following message is displayed.

After a short wait, the message "Set Polystyrene Film into Sample Compartment" is displayed.

4. If performing manual validation, set the polystyrene film in the sample compartment and click
[OK].
If performing automatic validation, user intervention is not required because the beam switching kit
automatically switches to polystyrene film, which is supplied as an accessory.
This sample measurement is performed twice.
The following conditions are used in sample measurement.
Parameters Settings
Resolution 2 cm-1
No. of scans 45
Mirror speed 2.8 (low) mm/sec
Apodization HAPP-GENZEL
Gain Auto

The resulting spectrum from this measurement is saved to the database and a folder named with the
year of measurement (the folder is automatically created if it does not exist), which is located under.
"\Program Files\LabSolutions\IR\Data\JP\" in the case of Japanese Pharmacopoeia
"\Program Files \LabSolutions\IR\Data\EP\" in the case of European Pharmacopoeia
"\Program Files \LabSolutions\IR\Data\ChP\" in the case of Chinese Pharmacopoeia
The filename consists of the month, day, and time of measurement (e.g. 0207180743_1).
For this reason, subsequent validations performed in the same manner will not generally overwrite
previous validations.
After scanning, calculation and judgement are performed.

C:\Program Files\ is the default location of the LabSolutions installation folder in a 32-bit OS.
When using a 64-bit OS or when the installation folder has been changed, enter the location of
the LabSolutions installation folder.

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4.3.4 Validation Using Stored Data (JP/EP/ChP )

The Validation program can validate FTIR using stored spectra.

1. Prepare the spectra to the data folder.

Spectra in the database cannot be selected in the validation program.
To access spectra in the database, export the required spectrum from the database to a local folder on
the PC in advance using the following procedure and then select the exported spectrum when the
validation program is running.
1. Use Windows Explorer to display the contents of the data folder that serves as the export
destination.
The data folder is under.
" \Program Files\LabSolutions\IR\Data\JP\(year of measurement)" in the case of Japanese
Pharmacopoeia
" \Program Files \LabSolutions\IR\Data\EP\(year of measurement)" in the case of European
Pharmacopoeia
" \Program Files \LabSolutions\IR\Data\ChP\(year of measurement)" in the case of Chinese
Pharmacopoeia.
For example, if measurement occurred in 2012, the data folder is "...\LabSolutions\IR\Data\JP\2012".

C:\Program Files\ is the default location of the LabSolutions installation folder in a 32-bit
OS. When using a 64-bit OS or when the installation folder has been changed, enter the
location of the LabSolutions installation folder.

2. Check for the single spectrum data file that corresponds to the validation result in the folder.
The filename is determined in the following manner according to the date and time that validation
measurement started.
(month - 2 digits)(day - 2 digits)(hour - 2 digits)(minutes - 2 digits)(seconds - 2 digits)_1.ispd
For example, if measurement commenced at 08:37:48 on September 19, the filename is
"0919083748_1.ispd".
Make a guess at the period of time in which the validation measurement was performed.

3. Start the data manager and search for filenames in the database that include "_2" and "_3"
(where the spectrum data file from above includes "_1").
In accordance with the above example, these filenames are "0919083748_2.ispd" and
"0919083748_3.ispd".
4. Export these files to a local folder on the PC.
Only export the above files with a file extension of ".ispd".
When performing an export operation, these files are copied to folders created with the same name as
the files.
5. Copy these files to the data folder.
In accordance with the above example, you should end up with the following files in the data folder.
0919083748_1.ispd
0919083748_2.ispd
0919083748_3.ispd

These files can be used in subsequent validations.

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 4.3 Software Usage - JP/EP/ChP Compliant Validation

2. Click [File].

3. Input can be added to "Instrument", "Serial No.", "Temperature", "Sample name", "Relative
Humidity", and "Inspected by." When IRTracer-100 is tested, Type of window at Sample
compartment now used must be selected.
Sutable inspection stabndards for shape of the power spectrum is used.
Printer output will display information provided by the user, columns left empty will appear blank.
Click the [OK] button after inputting the necessary information.

The following message is displayed and processing to determine the shape of the power spectrum is
started.

4. Click [OK].

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5. Select the necessary spectrum then click the [Open] button.

The power spectrum is named with a file name based on created date and "_1."

6. After the power spectrum is loaded, the loading polystyrene spectra starts.
The following message is displayed.

7. Select the two polystyrene spectra from the screen similar to the one in Step 5 in the same
manner as the case of the power spectrum.
The polystyrene spectra are named with a file name based on created date and "_2" or "_3."
After selection, calculation and judgement are performed.

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 4.3 Software Usage - JP/EP/ChP Compliant Validation

4.3.5 Judgement and End of Program

When measurement or selection of spectra is finished, calculation for the inspection is done
automatically.
The Validation program inspects 5 tests. When all the tests are completed, the validation is passed.
The following judgment dialog box shows "PASS" and a validation report is printed out.

If one of the tests is not passed, the validation fails. The following judgment dialog box displays
"FAIL" and a validation report is printed out.

1. Click [OK] to clear this message.

A report is printed out.

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A third page of results is only printed for ChP validation.

The LabSolutions IR Spectrum program closes.

2. Click [Close] in the [Macro Execute] window.

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 4.4 Operation for the ASTM Validation Program

4.4 Operation for the ASTM Validation Program

"ASTM E1421-94 Level Zero" compares obtained data with stored reference data to detect changes.
A polystyrene film which is a standard accessory of the FTIR or is supplied from NIST is used as the
sample. The same sample must be used in every inspection. If another sample is used, new
reference data must be obtained. When an optical alignment is done or a window at the sample
compartment is replaced for your FTIR, the reference data must be scanned again.
When the ASTM Validation program runs for the first time, it runs as a reference file measurement
mode because there is no reference data. After that, the ASTM Validation program calculates data
using the saved reference data.
However, one of the reference file is stored in the database. Spectra in the database cannot be
selected in the validation program. To access spectra in the database, export the required spectrum
from the database to a local folder on the PC in advance.
The ASTM Validation program uses the reference file in the following folder.
" \Program Files\LabSolutioins\IR\Data\ASTM2\Ref"
 R1.ispd Reference power spectrum1
 R2.ispd: Reference power spectrum2
 R3.ispd Reference polystyrene spectrum

 C:\Program Files\ is the default location of the LabSolutions installation folder in a 32-bit OS. When
using a 64-bit OS or when the installation folder has been changed, enter the location of the
LabSolutions installation folder.
 Please purchase and use the Standard Reference Material of polystyrene film supplied by NIST or
its secondary standard when traceable polystyrene film is needed.
 ASTM validation must be performed after 2 hours and warming up of your FTIR.
 If ASTM validation fails, Auto-adjustment must be performed for optical alignment. After
autoadjustment, perform the JP and EP validation to check up the FTIR alignment. If the JP and
EP validation fails, please contact your Shimadzu representatives. When the JP and EP validation
passes, reference data for ASTM validation should be scanned again, and then ASTM validation
should be run again.
 Always input half-width numbers when requested for numeric input by this program.

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4.4.1 Starting the Software

1. Close all LabSolutions IR measurement programs and the Postrun program, and then run
Spectrum program.

2. Initilize your FTIR with scan parameters for Mid-IR.

Set scan parameters as below.
Light source; Infrared
Range; MID
Beam; Internal
Detector; Stanadard

3. Click the [Macro] tab in the LabSolutions IR launcher, and then click [ASTM Level 0
Validation].

The [Macro Execute] window is displayed.

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 4.4 Operation for the ASTM Validation Program

4. Click [Run].

5. Enter a user ID and password into the [Login] window and click [OK].

When [Cancel] is clicked, [Automation Error] is displayed. Click [OK].

The Program starts.

The LabSolutions IR Spectrum program starts and the [Select Language], and [Select Change-beam]
window is displayed.
These dialog boxes are displayed when the Validation program is run for the first time. Note that each
setting can be changed later if necessary.

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6. Click [ ] next to [Language] to select the language (English or Japanese) , then click [OK].
This dialog box is displayed when the Validation program is run for the first time. Note that the
language setting can be changed later if necessary.
After clicking [OK], the [Select Change-Beam] dialog box is displayed.

7. Click [ ] next to [Change-Beam] to select the Validation mode (manual or automatic), then
click [OK].

 Select "Use" and click [OK] when the optional Beam Switching Kit (P/N 206-70125-91/92) is
installed on Shimadzu FTIR series instruments. When the kit is not installed, select "Un-using" and
click [OK].
 The Manual Validation program displays a message on screen prompting the operator to set the
polystyrene film in the sample compartment. Set the polystyrene film into the sample holder. The
Automatic Validation program automatically inserts the polystyrene film installed on the Beam
Switching Kit and scans the necessary spectra.

8. Reference spectra must be scanned when ASTM Level 0 Validation is performed first.
After the measurement of the reference spectra, ASTM Level 0 Validation ends.Export the Reference
spectra from the database to a local folder on the PC, and then run the program again.

1. Click [OK].

2. Click [Referrence].
The message "Remove Sample from Sample compartment" is displayed.
3. Confirm that no sample is set on the sample compartment and then click the [OK] button.
The power spectrum is scanned twice.
4. In the case of Manual Validation, set the polystyrene film after the corresponding message is
displayed.
In case of Automatic Validation, wait a short while.
5. The polystyrene spectrum is scanned.
After scanning polystyrene film, the message indicating that could not save in the reference data folder
is displayed.

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 4.4 Operation for the ASTM Validation Program

6. Click [OK].
ASTM Level 0 Validation exits.

The data of polystyrene spectrum is stored in the database.

7. Use Windows Explorer to display the contents of the data folder.

The data folder is " \Program Files\LabSolutions\IR\Data\ASTM2\(year of measurement)".
For example, if measurement occurred in 2012, the data folder is
"...\LabSolutions\IR\Data\ASTM2\2012".

C:\Program Files\ is the default location of the LabSolutions installation folder in a 32-bit
OS. When using a 64-bit OS or when the installation folder has been changed, enter the
location of the LabSolutions installation folder.

8. Check for the two spectrum data files that correspond to the validation result in the folder.
The filename for this type of file is determined in the following manner.
(month - 2 digits)(day - 2 digits)(hour - 2 digits)(minutes - 2 digits)(seconds - 2 digits)_1.ispd
(month - 2 digits)(day - 2 digits)(hour - 2 digits)(minutes - 2 digits)(seconds - 2 digits)_2.ispd
In accordance with the above example, these filenames are "0601130530_1.ispd" and
"0601130530_2.ispd".
9. Start the data manager and search for filenames in the database that include "_3" (where the
spectrum data file from above includes "_1" and "_2").
In accordance with the above example, this filename is "0601130530_3.ispd".
10.Export these files to a local folder on the PC.
Only export the above files with a file extension of ".ispd".
When performing an export operation, these files are copied to folders created with the same name as
the files.
11.Change the name of the spectrum file copied to the reference data folder to "R3.ispd".
In accordance with the above, you should end up with the following files in the refernce data folder.
R1.ispd
R2.ispd
R3.ispd

C:\Program Files\ is the default location of the LabSolutions installation folder in a 32-bit
OS. When using a 64-bit OS or when the installation folder has been changed, enter the
location of the LabSolutions installation folder.

12.Run the program from Launcher again.

13.Enter a user ID and password into the [Login] window and click [OK].
The following dialog box is displayed.

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Chapter 4 Validation Program

Item Function
Load Run the Validation program with loading saved spectra.

" 4.4.4 Validation Using Stored Data (ASTM)"

Measurement Run the Validation program with scanning a polystyrene film.

"4.4.3 Scan"
Settings Configures language and the Validation mode (manual/auto).

"4.4.2 Settings"
Cancel Cancels the program.

4.4.2 Settings
The following settings should be configured before running the Validation program.
 Validation mode selected between Manual validation and Automatic validation.
 Report language selected between Japanese and English.
 Scanning reference spectra.

1. Click the [Settings] button.

2. Click the button of the item to be changed.

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 4.4 Operation for the ASTM Validation Program

Item Function
Language Select Language between Japanese and English
Change-Beam Select Validation mode between Manual validation and Automatic
validation.
Reference Scans reference spectra.
Cancel Aborts the program.

4.4.3 Scan
Measure spectra and perform validation.

Click [OK] if a message appears that states that the scan wavenumber range has changed.

1. Click [Measurement].

2. Input can be added to "Instrument", "Serial No.", "Temperature", "Sample name", "Relative
Humidity", and "Inspected by." When IRTracer-100 is tested, Type of window at Sample
compartment now used must be selected.
Printer output will display information provided by the user, columns left empty will appear blank.

When the [OK] button is clicked, the following message "Remove Sample from Sample compartment"
is displayed.

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Chapter 4 Validation Program

3. Confirm that no sample is set on the sample compartment and then click the [OK] button.
The scan parameter is sent to the interferometer and the measurement of the power spectrum starts.
This power spectrum will also be the background of the following measurement.

After power spectrum measurement completes twice, processing proceeds to polystyrene measurement.
The message "Set Polystyrene Film into Sample Compartment" is displayed.

4. If performing manual validation, set the polystyrene film in the sample compartment and click
[OK].
If performing automatic validation, user intervention is not required because the beam switching kit
automatically switches to polystyrene film, which is supplied as an accessory.
This sample measurement is performed twice.
The following conditions are used in sample measurement.

Parameters Settings
-1
Resolution 4 cm
No. of scans 20
Mirror speed 2.8 (low) mm/sec
Apodization HAPP-GENZEL
Gain Auto

The resulting spectrum from this measurement is saved to the database and a folder named with the
year of measurement (the folder is automatically created if it does not exist), which is located under
" \Program Files\LabSolutions\IR\Data\ASTM2\" in the case of ASTM level 0 validation.
The filename consists of the month, day, and time of measurement (e.g. 0207180743_1).
For this reason, subsequent validations performed in the same manner will not generally overwrite
previous validations.
After scanning, calculation and judgement are performed.

C:\Program Files\ is the default location of the LabSolutions installation folder in a 32-bit OS.
When using a 64-bit OS or when the installation folder has been changed, enter the location of
the LabSolutions installation folder.

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 4.4 Operation for the ASTM Validation Program

4.4.4 Validation Using Stored Data (ASTM)

The Validation program can validate FTIR using stored spectra.

When re-executing ASTM validation using the spectrum file from the previous ASTM
validation, the reference data used when measuring the stored spectrum may differ from the
current reference data. In this case, ASTM validation does not perform judgment correctly.

1. Click [Load].

2. Input can be added to "Instrument", "Serial No.", "Temperature", "Sample name", "Relative
Humidity", and "Inspected by." When IRTracer-100 is tested, Type of window at Sample
compartment now used must be selected.
Printer output will display information provided by the user, columns left empty will appear blank.
Click the [OK] button after inputting the necessary information.

3. Click [OK].

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4. Select the necessary spectrum then click the [Open] button.

If the file was measured using this software, the files with "_1" and "_2" after the 10 digits that
represent the date and time are the files for power spectra 1 and 2 and the file with "_3" is the
polystyrene spectrum file.

After selection, calculation and judgement are performed.

4.4.5 Judgement and End of Program

When no reference data exists, only collection and saving reference spectra are done and
calculation processing is not executed.
Execute this program again to make a validation report. When the measurement is finished,
calculation for the inspection is automatically done.

When measurement or selection of spectra is finished, calculation for the inspection is done
automatically.
The Validation program inspects 5 tests. When all the tests are completed, the validation is passed.
The following judgment dialog box shows "PASS" and a Validation report is printed out.

The validation fails if any tests are not passed. In this case, the following judgement dialog box
shows "FAIL" and a validation report is printed out.

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1. Click [OK] to clear this message.

A report is printed out.

The LabSolutions IR Spectrum program closes.

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Chapter 4 Validation Program

2. Click [Close] in the [Macro Execute] window.

4.4.6 Troubleshooting
 ASTM Validation Has Failed
If ASTM validation has failed, Auto-adjustment must be performed for optical alignment. After
autoadjustment, perform the JP and EP validation to check up the FTIR alignment. If the JP and EP
validation has failed, please contact your Shimadzu representatives. When the JP and EP validation
has passed, reference data for ASTM validation should be scanned again, then the ASTM validation
should be run again.

 Abnormal Spectra are on the Report

If abnormal results report are obtained, the reference spectra may be damaged for some reason.
See "4.3.2 Settings" and click [Reference] to measure the reference file again.
Example of abnormal report.
 Page 2
A Transmittance spectrum on upper side and a Power spectrum on the bottom side are printed,
instead of Power spectra on the top and a 100%T spectrum on the bottom.
 Page 3
A Transmittance spectrum on upper side and a Power spectrum on the bottom side are printed,
instead of Power spectra on the top and a 100%T spectrum on the bottom.
 Page 4
Two Transmittance spectra are printed, instead of Polystyrene spectra on the top and a 100%T
spectrum on the bottom.

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 4.5 Operation of the Report Viewer

4.5 Operation of the Report Viewer

The inspection result is printed out and saved as a file on the hard disk. The report Viewer displays
and prints out the stored Validation report.
This section describes the operation of the Report Viewer.

4.5.1 Starting up the Report Viewer

1. Close all LabSolutions IR measurement programs and the Postrun program.

2. Click the [Macro] tab in the LabSolutions IR launcher, and then click [Report Viewer].

The [Macro Execute] window is displayed.

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Chapter 4 Validation Program

3. Click [Run].

4. Enter a user ID and password into the [Login] window and click [OK].

When [Cancel] is clicked, [Automation Error] is displayed. Click [OK].

The program starts.

The LabSolutions IR Postrun program starts.
If validation has not been performed, the following message is displayed.

If a report exists, the [Review of an Evaluation Report] window is displayed.

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 4.5 Operation of the Report Viewer

4.5.2 Operation Method

An explanation of each item is listed in the following table.

No. Description
1 The content of the report is displayed here.
When the whole of the screen is not displayed, the scrollbar displays the whole screen.
2 Switches displayed report.
 ASTM-Lv.0; Displays "ASTM E1421-94 Level Zero" validation report older than Ver.
1.10 program.
 ASTM-Lv.0 [V1.10]; Displays "ASTM E1421-94 Level Zero" validation report in Ver. 1.10 or
later.
 Validation; Displays Reports created by JP and EP Validation with IRsolution Ver. 1.30
or older.
 JP Validation; Displays Reports created by JP Validation, a standard accessory of
IRsolution Ver. 1.40 or later.
 EP Validation; Displays Reports created by EP Validation, a standard accessory of
IRsolution Ver. 1.40 or later.
 ChP Validation; Displays Reports created by ChP Validation.
3 The Validation report is stored in a different folder according to the year when the validation was
done.
Select the year of the data to be displayed.
4 Displays the date and time when the report is created.
Double-click one on the part to display it on the main screen (1).
5 Prints the report displayed on the screen.
Click this button to print the report.
The report assumes the A4 size form. Use papers of the A4 size.
6 Exits the Report Viewer.

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4.5.3 End of Program

1. Click [OK] in the [Review of an Evaluation Report] window.

The LabSolutions IR Postrun program closes.

2. Click [Close] in the [Macro Execute] window.

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 4.6 The Japanese Pharmacopoeia

4.6 The Japanese Pharmacopoeia

The validation procedure complies with the description in 'General Test 23, Infrared
Spectrophotometry' of the Sixteenth Edition of Japanese Pharmacopoeia. The software validates the
equipment's performance by comparing the measured results to the standard values.
There are five parameters checked by this program: power spectrum, resolution, wavenumber
accuracy, wavenumber reproducibility, and transmittance reproducibility.
The performance of FTIR is validated through comparison between the measurement result and
standard values.
These characteristics are described in this chapter.

4.6.1 Power Spectrum

The intensity of the power spectrum is used to evaluate the basic performance of the FTIR. The
power spectrum intensity is compared to a standard with specified wavenumbers. If the measured
values are higher than the standard values at all the wavenumbers, the results are labeled "PASS."
The standard values are shown in the following table. They comprise the maximum value of power
(shown in the center) and relational values of power, expressed as a percentage of the maximum
value at a specified wavenumber. The standard values printed on the Validation report are
calculated by the following specifications based on the actual maximum value of the power
spectrum.
・ IRTracer-100
Wavenumber (cm-1) Window: KBr Window: KRS-5
4600 10% or more of Max. 10% or more of Max.
4000 25% or more of Max. 25% or more of Max.
3000 50% or more of Max. 50% or more of Max.
Maximum value 50.0 or more 37.5 or more
700 10% or more of Max. 10% or more of Max.
500 2% or more of Max. 2% or more of Max.
1
403 ＊ 0.5% or more of Max. 0.5% or more of Max.
351 ＊2 0.01% or more of Max. 0.01% or more of Max.

・ IRPrestige/IRAffinity/ FTIR-8000 series

Wavenumber (cm-1) IRPrestige/IRAffinity/FTIR-8400S FTIR-8000 series
4600 10% or more of Max. 10% or more of Max.
4000 25% or more of Max. 30% or more of Max.
3000 50% or more of Max. 60% or more of Max.
Maximum value 50.0 or more 60.0 or more
700 10% or more of Max. 10% or more of Max.
500 2% or more of Max. 2% or more of Max.
403 ＊1 0.5% or more of Max. 0.5% or more of Max.
351 ＊2 0.01% or more of Max.
＊1
Water has a peak at 400 cm-1 and thus this program cannot calculate the correct value of the power
-1
spectrum at this value. The program uses the value 403 cm as a baseline of the power spectrum
-1
instead of 400 cm .
＊2
Inspection at 351 cm-1 is not performed when "FTIR-8000 series" is selected for the "Instrument" setting.

4.6.2 Resolution
The resolution is validated by measuring the absorption spectrum of polystyrene film with a
thickness of approximately 0.04 mm. The measured absorption spectrum should have a
transmittance (%T) difference of 18% or more between a minimum of approximately 2870 cm-1 and
a maximum of approximately 2850 cm-1. It should also have a transmittance (%T) difference of 12%
or more between a minimum of approximately 1589 cm-1 and a maximum of approximately
1583 cm-1. If the measured absorption spectrum has both transmittance differences higher than the
standard value, the results are labeled "PASS."

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4.6.3 Wavenumber Accuracy

Evaluating wavenumber accuracy is described in the Japanese Pharmacopoeia as follows:
The wavenumber scale is usually calibrated by using some of the following absorption bands of polystyrene
film shown below. The numbers in parentheses indicate the allowable range.
Standards
3060.0 (±1.5)cm-1
-1
2849.5 (±1.5)cm
1942.9 (±1.5)cm-1
1601.2 (±1.0)cm-1
-1
1583.0 (±1.0)cm
1154.5 (±1.0)cm-1
-1
1028.3 (±1.0)cm

This program uses seven wavenumber points for judging and obtains the peak wavenumbers from
the measured spectrum of polystyrene film. The software then judges whether the values are within
the allowable range. The program labels the results "PASS" if all the specified peak wavenumbers
are within the allowable range.

4.6.4 Wavenumber Reproducibility

The Japanese Pharmacopoeia describes the wavenumber reproducibility as follows:
The wavenumber reproducibility should satisfy 5 cm-1 around 3000 cm-1 of the polystyrene absorption
-1 -1 -1
wavenumber, 1 cm around 1000 cm when several points of polystyrene absorption, from 3000 cm to
-1
1000 cm , are measured twice.

This program specifies three points for peak wavenumber measurement. It then obtains the actual
peak wavenumbers at each point by measuring the polystyrene film twice. The software determines
whether the differences between each of the two measurements are within the allowable range. The
software labels the result "PASS" if all the specified peak wavenumbers are within the allowable
range.

4.6.5 Transmittance Reproducibility

The Japanese Pharmacopoeia describes the transmittance reproducibility as follows:
The transmittance reproducibility should satisfy 0.5%T when the several points of polystyrene absorption
from 3000 cm-1 to 1000 cm-1 are measured twice.

This program specifies the peak wavenumber at three points and the transmittance at each point is
measured twice. Then it is determined whether the differences between the two data are within the
allowable range or not. If all the transmittance differences satisfy the allowable range, the results are
labeled "PASS."

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 4.7 The European Pharmacopoeia

4.7 The European Pharmacopoeia

The validation procedure complies with the description in "Absorption Spectrophotometry, Infrared"
of the European Pharmacopoeia 7.0. The software validates the equipment's performance by
comparing the measured results to the standard values.
There are five parameters checked by this program: power spectrum, resolving power (resolution),
wavenumber accuracy, wavenumber reproducibility, and absorbance reproducibility.
The performance of FTIR is validated through comparison between the measurement result and
standard values. The items different from EP4.0 are "Resolving Power (Resolution)", "Wavenumber
Accuracy" and "Absorbance reproducibility". There are no items different from EP5.0, 6.0.
These characteristics are described in this chapter.

Only the FTIR-8300/8400/8400S, IRPrestige-21, IRTracer-100, and IRAffinity-1 series are compliant
with European Pharmacopoeia 7.0.

4.7.1 Power Spectrum

The intensity of the power spectrum is used to evaluate the basic performance of the FTIR. The
power spectrum intensity is compared to a standard with specified wavenumbers. If the measured
values are higher than the standard values at all the wavenumbers, the results are labeled "PASS."
The standard values are shown in the following table. They comprise the maximum value of power
(shown in the center) and relational values of power, expressed as a percentage of the maximum
value at a specified wavenumber. The standard values printed on the Validation report are
calculated by the following specifications based on the actual maximum value of the power
spectrum.
・ IRTracer-100
Wavenumber (cm-1) Window: KBr Window: KRS-5
4600 10% or more of Max. 10% or more of Max.
4000 25% or more of Max. 25% or more of Max.
3000 50% or more of Max. 50% or more of Max.
Maximum value 50.0 or more 37.5 or more
700 10% or more of Max. 10% or more of Max.
500 2% or more of Max. 2% or more of Max.
403 ＊1 0.5% or more of Max. 0.5% or more of Max.
351 ＊2 0.01% or more of Max. 0.01% or more of Max.
・ IRPrestige/IRAffinity/ FTIR-8000 series
Wavenumber (cm-1) IRPrestige/IRAffinity/FTIR-8400S FTIR-8000 series
4600 10% or more of Max. 10% or more of Max.
4000 25% or more of Max. 30% or more of Max.
3000 50% or more of Max. 60% or more of Max.
Maximum value 50.0 or more 60.0 or more
700 10% or more of Max. 10% or more of Max.
500 2% or more of Max. 2% or more of Max.
1
403 ＊ 0.5% or more of Max. 0.5% or more of Max.
351 ＊2 0.01% or more of Max.
＊1
Water has a peak at 400 cm-1 and thus this program cannot calculate the correct value of the power
-1
spectrum at this value. The program uses the value 403 cm as a baseline of the power spectrum
-1
instead of 400 cm .
＊2
Inspection at 351 cm-1 is not performed when "FTIR-8000 series" is selected for the "Instrument" setting.

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4.7.2 Resolution
When the spectrum of polystyrene film about 35 μm thick is recorded, the difference between the
absorbances at the absorption minimum at 2870 cm-1 and the absorption maximum at 2849.5 cm-1 is
greater than 0.33. The difference between the absorbances at the absorption minimum at 1589 cm-1
and the absorption maximum at 1583 cm-1 is greater than 0.08. If the measured absorption spectrum
has both absorbance differences higher than the standard value, the results are labeled "PASS."

4.7.3 Wavenumber Accuracy

Evaluating wavenumber accuracy is described in the European Pharmacopoeia as follows:
"The wavenumber (cm-1) scale may be verified using a polystyrene film, which has transmission minima
(absorbance maxima) at the wavenumbers (in cm-1)."
Standards
3060.0 (±1.0)cm-1
-1
2849.5 (±1.0)cm
1942.9 (±1.0)cm-1
1601.2 (±1.0)cm-1
1583.0 (±1.0)cm-1
1154.5 (±1.0)cm-1
1028.3 (±1.0)cm-1

This program uses seven wavenumber points for judging and obtains the peak wavenumbers from
the measured spectrum of polystyrene film. The software then judges whether the values are within
the allowable range. The program labels the results "PASS" if all the specified peak wavenumbers
are within the allowable range.

4.7.4 Wavenumber Reproducibility

The European Pharmacopoeia does not have this test but the validation program performs
inspection based on the Japanese Pharmacopoeia.
The Japanese Pharmacopoeia describes the wavenumber reproducibility as follows:
The wavenumber reproducibility should satisfy 5 cm-1 around 3000 cm-1 of the polystyrene absorption
wavenumber, 1 cm-1 around 1000 cm-1 when several points of polystyrene absorption, from 3000 cm-1 to
-1
1000 cm , are measured twice.

This program specifies three points for peak wavenumber measurement. It then obtains the actual
peak wavenumbers at each point by measuring the polystyrene film twice. The software determines
whether the differences between each of the two measurements are within the allowable range. The
software labels the result "PASS" if all the specified peak wavenumbers are within the allowable
range.

4.7.5 Transmittance Reproducibility

The European Pharmacopoeia does not have this test but the validation program performs
inspection based on the Japanese Pharmacopoeia. Tolerance is specified of absorbance which is
nearly equivalent to 0.5% transmittance at the wavenumber.
The Japanese Pharmacopoeia describes the transmittance reproducibility as follows:
The transmittance reproducibility should satisfy 0.5%T when the several points of polystyrene absorption
-1 -1
from 3000 cm to 1000 cm are measured twice.

This program specifies the peak wavenumber at three points and the transmittance at each point is
measured twice. Then it is determined whether the differences between the two data are within the
allowable range or not. If all the transmittance differences satisfy the allowable range, the results are
labeled "PASS."

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 4.8 The Chinese Pharmacopoeia

4.8 The Chinese Pharmacopoeia

The validation procedure complies with the description in 'Equipment and Calibration' in 'Appendix IV
C Infrared Spectrophotometry' of the Chinese Pharmacopoeia 2010. The software validates the
equipment's performance by comparing the measured results to the standard values.
There are five parameters checked by this program: power spectrum, resolution, wavenumber
accuracy, wavenumber reproducibility, and transmittance reproducibility.
The performance of FTIR is validated through comparison between the measurement result and
standard values.
These characteristics are described in this chapter.

4.8.1 Power Spectrum

The intensity of the power spectrum is used to evaluate the basic performance of the FTIR. The
power spectrum intensity is compared to a standard with specified wavenumbers. If the measured
values are higher than the standard values at all the wavenumbers, the results are labeled "PASS."
The standard values are shown in the following table. They comprise the maximum value of power
(shown in the center) and relational values of power, expressed as a percentage of the maximum
value at a specified wavenumber. The standard values printed on the Validation report are
calculated by the following specifications based on the actual maximum value of the power
spectrum.
・ IRTracer-100
Wavenumber (cm-1) Window: KBr Window: KRS-5
4600 10% or more of Max. 10% or more of Max.
4000 25% or more of Max. 25% or more of Max.
3000 50% or more of Max. 50% or more of Max.
Maximum value 50.0 or more 37.5 or more
700 10% or more of Max. 10% or more of Max.
500 2% or more of Max. 2% or more of Max.
1
403 ＊ 0.5% or more of Max. 0.5% or more of Max.
351 ＊2 0.01% or more of Max. 0.01% or more of Max.
・ IRPrestige/IRAffinity/ FTIR-8000 series
Wavenumber (cm-1) IRPrestige/IRAffinity/FTIR-8400S FTIR-8000 series
4600 10% or more of Max. 10% or more of Max.
4000 25% or more of Max. 30% or more of Max.
3000 50% or more of Max. 60% or more of Max.
Maximum value 50.0 or more 60.0 or more
700 10% or more of Max. 10% or more of Max.
500 2% or more of Max. 2% or more of Max.
403 ＊1 0.5% or more of Max. 0.5% or more of Max.
351 ＊2 0.01% or more of Max.
＊1
Water has a peak at 400 cm-1 and thus this program cannot calculate the correct value of the power
-1
spectrum at this value. The program uses the value 403 cm as a baseline of the power spectrum
-1
instead of 400 cm .
＊2
Inspection at 351 cm-1 is not performed when "FTIR-8000 series" is selected for the "Instrument" setting.

4.8.2 Resolution
The resolution is validated by measuring the absorption spectrum of polystyrene film with a
thickness of approximately 0.04 mm. The measured absorption spectrum should have a
transmittance (%T) difference of 18% or more between a minimum of approximately 2870 cm-1 and
a maximum of approximately 2851 cm-1. It should also have a transmittance (%T) difference of 12%
or more between a minimum of approximately 1589 cm-1 and a maximum of approximately
1583 cm-1. If the measured absorption spectrum has both transmittance differences higher than the
standard value, the results are labeled "PASS."

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4.8.3 Wavenumber Accuracy

Evaluating wavenumber accuracy is described in the Chinese Pharmacopoeia as follows:
The wavenumber scale is usually calibrated by using some of the following absorption bands of polystyrene
film shown below. The numbers in parentheses indicate the allowable range.
Standards
3027 (±1.5)cm-1
-1
2851 (±1.5)cm
1601 (±1.0)cm-1
1028 (±1.0)cm-1
-1
907 (±1.0)cm

This program uses seven wavenumber points for judging and obtains the peak wavenumbers from
the measured spectrum of polystyrene film. The software then judges whether the values are within
the allowable range. The program labels the results "PASS" if all the specified peak wavenumbers
are within the allowable range.

4.8.4 Wavenumber Reproducibility

The Chinese Pharmacopoeia does not have this test but the validation program performs inspection
based on the Japanese Pharmacopoeia.
The Japanese Pharmacopoeia describes the wavenumber reproducibility as follows:
The wavenumber reproducibility should satisfy 5 cm-1 around 3000 cm-1 of the polystyrene absorption
wavenumber, 1 cm-1 around 1000 cm-1 when several points of polystyrene absorption, from 3000 cm-1 to
-1
1000 cm , are measured twice.

This program specifies three points for peak wavenumber measurement. It then obtains the actual
peak wavenumbers at each point by measuring the polystyrene film twice. The software determines
whether the differences between each of the two measurements are within the allowable range. The
software labels the result "PASS" if all the specified peak wavenumbers are within the allowable
range.

4.8.5 Transmittance Reproducibility

The Chinese Pharmacopoeia does not have this test but the validation program performs inspection
based on the Japanese Pharmacopoeia.
The Japanese Pharmacopoeia describes the transmittance reproducibility as follows:
The transmittance reproducibility should satisfy 0.5%T when the several points of polystyrene absorption
-1 -1
from 3000 cm to 1000 cm are measured twice.

This program specifies the peak wavenumber at three points and the transmittance at each point is
measured twice. Then it is determined whether the differences between the two data are within the
allowable range or not. If all the transmittance differences satisfy the allowable range, the results are
labeled "PASS."

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 4.8 The Chinese Pharmacopoeia

4.8.6 Peak Resolution Function

The Chinese Pharmacopoeia states that "resolution capable of isolating seven peaks in the
wavenumber range of 3110 cm-1 to 2850 cm-1 is required". While the Chinese Pharmacopoeia does
not provide specific wavenumbers for these peaks, this validation program performs inspections that
check whether peaks are present in the following range with respect to the actual peak
wavenumbers.

Standards
3102.63 (±5.0)cm-1
3082.38 (±5.0)cm-1
3060.20 (±5.0)cm-1
-1
3025.48 (±5.0)cm
3001.37 (±5.0)cm-1
2921.32 (±5.0)cm-1
2849.95 (±5.0)cm-1

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4.9 ASTM E1421-94 Level Zero

This software complies with the description in the "ASTM (American Society for Testing and
Materials) E1421-94 Level Zero". There are three parameters checked by this program: Energy
Spectrum Test, One Hundred Percent Line Test, and Polystyrene Test.
These characteristics are described in this chapter.

 Brief explanation of the ASTM E1421-94 Level Zero

This is a simple test done within a couple of minutes. ASTM E1421-94 Level Zero compares
obtained data with stored reference data obtained after optical alignment to detect changes. It is not
the one to do a quantitative strict evaluation.

 Data
Name Description
Reference1 Reference power spectrum
Reference2 Reference polystyrene spectrum
Spectrum1 Blank power spectrum1
Spectrum2 Blank power spectrum2 measured after Spectrum1
Spectrum3 Polystyrene spectrum with Spectrum1 as BKG
The following evaluation is performed with respect to the above data.

4.9.1 Energy Spectrum Test

The Energy Spectrum Test compares the power spectrum to evaluate any changes in the long term.

 Report Format
 Spectrum1 and Reference1 overlaid.
 100%T line spectrum calculated by (Spectrum1)/(Reference1) in 100  10% scale.
 Energy Ratios listed up on following table. When the energy ratios are within the standard, result
is "PASS."

 Energy Ratio
Calculation Standard
R4000/2000=E4000/E2000 ±0.3
R2000/1000=E2000/E1000 ±0.3
R nonphysical=E150/Emax ±0.3

 Error Standard for 100%T Line

Position Standard
4000 cm-1 ±30
-1
2000 cm ±30
-1
1000 cm ±30
500 cm-1 ±30

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 4.9 ASTM E1421-94 Level Zero

4.9.2 One Hundred Percent Line Test

One Hundred Percent Line Test calculates 100%T line (Spectrum2/Spectrum1) to evaluate any
short-term changes.

 Report Format
 Spectrum1 and Spectrum2 overlaid.
 100%T line spectrum calculated of (Spectrum2)/(Spectrum1) in 100  10% scale.
 RMS or Peak-to-Peak noise levels of the 100%T line spectrum at 100 cm-1 range centered at
4000, 2000, 1000, 500 cm-1. When the noise levels are within the standard, "PASS" results.

 Peak-to-Peak Noise Level Standard

Position Standard
-1
4000 cm 1.00
2000 cm-1 0.10
1000 cm-1 1.00
500 cm-1 8.00

 RMS Noise Level Standard

Position Standard
-1
4000 cm 0.50
2000 cm-1 0.05
-1
1000 cm 0.50
500 cm-1 4.00

4.9.3 Polystyrene Test

Polystyrene Test compares the polystyrene spectrum (Reference2 and Spectrum3) to evaluate any
long term changes.

 Report Format
 Spectrum3 and Reference2 overlaid.
 Subtracted spectrum between Spectrum3 and Reference2 in 100  10%T scale*.
 When the differences are within the standard, "PASS" results.

 Standard Differences of the Subtracted Data

Position Standard
-1
4000 cm 10
2000 cm-1 10
1000 cm-1 10
500 cm-1 10
＊1
The subtracted spectrum should be printed in  1%T scale in section 7.3.1. on the ASTM
E1421-94. But this program prints out the subtracted spectrum in  10%, because the
maximum of standard in the program is  10%.

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