UV OQP ZEMA-2004B Rev310 1600

ZEMA-2004B
Document No.
SHIMADZU UV-VIS SPECTROPHOTOMETER

UV-1700 / UV-1800 / 1600 / 2450 / 2550 / 3600series
Operational Qualification
Operational Qualification Protocol
We here by confirm that all contents (including changes) of the operational qualification procedures described in this
document have been approved in the presence of the performer, reviewer and the manager.
Performer Signature Date
Print / /
Title
Certificate No.
(Shimadzu-certified Performer only)
Company
Reviewer Signature Date
Print / /
Title
Company
Manager Signature Date
Print / /
Title
Company
Operational Qualification Table of Contents
Table of Contents
1. Definitions......................................................................................................................... 3
1-1 Documentation ..............................................................................................................................3
1-2 Scope .............................................................................................................................................4
1-3 Entries and Revisions ....................................................................................................................4
2. Preliminary Checks ......................................................................................................... 7
2-1 Reviewer Confirmation .................................................................................................................7
2-2 Performer Identification & Approval .............................................................................................7
2-3 Planning Items to be Evaluated in Operational Qualification........................................................7
2-4 Calibration Certificate and Instruments Used ................................................................................8
2-5 Other Tools Used ...........................................................................................................................9
3. Operational Qualification Outline ............................................................................... 10
3-1 Outline of Inspection Procedures................................................................................................. 10
4. Operational Qualification Protocol .............................................................................. 14
4-1 UVProbe/Personal Computer and Peripherals ............................................................................. 14
4-2 Spectrophotometer ....................................................................................................................... 25
4-2-1 UV-1700 UV-VIS Spectrophotometer .............................................................................. 25
4-2-3 UV-1601PC/UV-1650 UV-VIS Spectrophotometer ......................................................... 44
4-3 Syringe Sipper N/CN ................................................................................................................... 81
4-4 Automatic Sample Changer ASC-5 ............................................................................................. 87
4-5 Elution Test 6-Cell Holder DIS-1200 .......................................................................................... 89
4-6 Elution Test 8-Cell Holder DIS-8 ................................................................................................ 90
4-7 Cell Positioner CPS-240A/B ....................................................................................................... 91
4-8 Thermoelectrically Temperature Controlled Cell Holder TCC-240A ......................................... 95
4-9 Screen Copy Printer HCP-1C ...................................................................................................... 96
4-10 Screen Copy Printer DPU-414................................................................................................... 97
4-11 Screen Copy Printer MPU ......................................................................................................... 98
4-12 ESC/P Compatible Screen Copy Printer .................................................................................... 99
4-13 PCL Compatible Screen Copy Printer .....................................................................................100
4-14 Time Course (Multi λ) Program Pack ......................................................................................101
4-15 DNA/Protein Quantitation Program Pack................................................................................102
4-16 Protein Quantitation Program Pack .........................................................................................103
4-17 CLASS-Agent..........................................................................................................................104
4-18 Validation Software Package ................................................................................................... 112
4-19 Color Measurement Software COL-UVPC ............................................................................. 113
4-20 Film Thickness Measurement Software FLM-UVPC ............................................................. 115
4-21 Invalidating Inspection Data .................................................................................................... 117
5. Change List.................................................................................................................... 118
Page 2 of 120 Rev 3.10

Operational Qualification Definitions
1. Definitions
1-1 Documentation
1. This document stipulates the procedures and the documentation of the Operational Qualification (OQ) of
Shimadzu Corporation’s UV-VIS Spectrophotometers. When all procedures are executed and all items pass
the inspection, it is verified that the system operates to satisfy the intended purpose. The contents of this
document must be checked and approved by the Performer, Reviewer and Manager before implementing
the Operational Qualification.
2. The following are established as the responsible parties in the execution of inspections.
· Performer
The Performer is the individual who actually performs the procedures stipulated in the Installation
Qualification Protocol and the Operational Qualification Protocol.
The Performer shall be an individual who, having been trained by the Quality Assurance Department of the
Analytical & Measuring Instruments Division of Shimadzu Corporation, has been certified as an IQ/OQ
inspector by the General Manager of the Quality Assurance Department, or an individual recognized by the
Manager to be equipped with the ability to conduct this inspection.
· Reviewer
The Reviewer is an individual designated by the Manager charged with responsibility for the system.
The Reviewer verifies the contents of the Installation Qualification Protocol and Operational Qualification
Protocol. In addition, the Reviewer shall attend the inspection procedures together with the Performer, and
evaluate the procedures.
The Manager can serve concurrently as the Reviewer.
· Manager
The Manager is the individual responsible for administering the entire UV-VIS system being inspected.
As well as verifying the contents of the Installation Qualification Protocol and Operational Qualification
Protocol, the Manager shall also grant final approval to the inspection procedures.
3. The Performer shall first check the content of this document. After checking all items, the Performer
shall sign and date the cover sheet of this document and submit this document as the Operational
Qualification Protocol report. (OQ must be performed by a trained and knowledgeable individual in
accordance with 21 CFR Part 211 Section 211.25 (cGMP, USA promulgated 29 September 1978)).
4. The Reviewer shall first check the content of this entire document. After checking all items, the Reviewer
shall sign and date the cover sheet of this document as approval of the Operational Qualification Protocol.
5. The Manager shall first check the content of this entire document. After checking all items, the Manager
shall enter a unique document control number in the Document No. column at the top right of the cover sheet,
and then sign and date the cover sheet of this document as final approval of the Operational Qualification
Protocol.
6. This document is comprised of 1. Definitions, 2. Preliminary Checks, 3. Operational Qualification Outline, 4.

Operational Qualification Protocol, and 5. Change List. All of these sections must be included.
7. This document contains important information and any form of duplication, photography, or reproduction
without the permission of the General Manager of the Quality Assurance Department, Analytical &
Measuring Instruments Division, Shimadzu Corporation, is prohibited.
Rev 3.10 Page 3 of 120

1-2 Scope
The Operational Qualification Protocol shall include the following.
· Spectrophotometer Operation Check
The spectrophotometer operation and some functions will be verified and the results will be checked against
pass criteria specified in this document.
· Personal Computer and Special Accessories Operation Check
Operation check will be conducted for the personal computer that controls the spectrophotometer, its
peripherals and installed special accessories.
· Software and firmware check
The Operational Qualification also checks the software and firmware provided.
The firmware checking is conducted based on version display and the Software Certificate of Compliance.
The software and firmware must be properly managed and change procedures must be properly clarified.
Analysis methods and data acquisition systems such as networks are not verified in the OQ of this system. These
must be separately verified by the customer.
1-3 Entries and Revisions

1. Making Entries
Use a black, permanent ballpoint pen, or equivalent, when recording results.
Names should be clearly printed.
Confirm that all items, except “Remarks” columns, are completed, and that there are no omissions.
Draw a diagonal line (from bottom left to top right) across all blank columns. (When making no entries, it is
not necessary to enter the “Change List No.__”, “Date” or “Signature”, or to enter the reason for the change
in the Change List of this document.)
Columns in which nothing has to be written in have been filled in with “N/A” in advance.
If choices are available within an item, place a checkmark in the box to select the appropriate decision.
2. Rounding of numeric values

If there are more significant figures in the measurement results than the specified criteria, round off the
result value at the number of significant figures required for the criteria. For example, if the criterion is
defined down to the first decimal place, round off the figure at the second decimal place of the result value.
3. Deletion and correction of mistakenly filled items

To correct mistaken entries, delete the entire entry by drawing a diagonal line through it and enter the
correction in the margins. To correct numerical values or symbols (checkmark), draw 2 horizontal lines
across the mistake and re-write the entry. Moreover, write the date, and the signature, and the reason for the
change. (When deletion and correction of mistakenly filled items, it is not necessary to enter the “Change
List No.__”, “Date” or “Signature”, or to enter the reason for the change in the Change List of this
document.)
4. Changing or deleting steps, procedures or acceptance criteria

If there are sections of the steps or procedures which will not be applied, draw a diagonal line through the
entire item and write “Change List No. __” above the line and assign a number to it. Date and sign it. Enter
the necessary information in the Change List of this document.
When making a change, delete the existing description as explained above, enter the change point, and then
record the reason for the change in the Change List.
5. Revising entries
If the need to alter the contents of an entry arises, change the entry in accordance with “3. Deletion and
correction of mistakenly filled items”, and then write the reason for the change in the Change List of this
document.
When adding a new description, write it in the margins of the relevant page, and write “Change List No. _”,
the date and signature. Then, write the reason for the change in the Change List.
Page 4 of 120 Rev 3. 10

6. Handling Problems
Any problems that are identified in the Operational Qualification must be investigated and appropriate
actions must be taken. All such actions must be documented and be approved by the Manager.
7. In the event of a Fail

If troubles occur during an inspection and the item fails the inspection, place a checkmark in the “Fail” box
and describe the problem in the margins of the relevant page. Write “Change List No. _” and date and sign
the entry. Enter an outline of the problem in the Change List.
After the problem is solved, describe the solution and the result (“Pass”) in the margins of the relevant page.
Write “Change List No.__” and date and sign the entry. Enter the summary of the solution in the Change
List of this document.
8. Attaching data
Attached data are added by assigning page numbers as “A, B, C…” for each inspection item. If, for example,
there is a total of 3 sheets for attachment A, notate the pages as “73-A-1/3 - A-3/3”, ensuring that no
numbers are omitted. The Performer shall date and sign the attached data.
9. Other
Every item entered into the Change List shall be approved by the Reviewer and Manager.
<Additional Information> Significant Figures

The concept of significant figures is outlined below.
<What are Significant Figures?>

Significant figures are digits that are statistically significant in a measurement. The last digit of a significant
figure includes an error.
If we take, for example, a measured value 5.67, an error is included in the final digit, “7”. Despite the error in
the final digit “7”, the previous digit “6” is correct, such that the number of significant digits is three.
When making measurements, it is important to ascertain the significant digits of each measuring instrument.
For instruments with a digital display, the measurement sensitivity generally extends to the last displayed digit,
such that the last digit is considered to represent the number of significant digits. However, the sensitivity must
be checked in the Instruction Manual.
For instruments with an analog display, increments which are 1/10th of the minimum scale represent the
significant digits. For example, measuring the length of an object with a ruler marked in 1-mm increments
permits measurement to 0.1 mm.
<Calculating Significant Figures>

Calculations based on measured values (such as calculating a mean value) result in more digits than the number
of significant digits used in the calculation. Such values must be rounded off to the number of significant digits
when the data is presented in reports. However, when a mean value, for example, is used in further calculations,
these calculations yield intermediate values with a larger number of digits, which are not rounded during the
calculations. No rounding for the purposes of bringing the figure in line with the significant figures is
conducted until the final result is obtained. When quantities are being added or subtracted, the number of
decimal places (not significant digits) in the answer should be the same as the largest number of decimal places
in any of the numbers being added or subtracted. In a calculation involving multiplication or division, the
number of significant digits in an answer should equal the least number of significant digits in any one of the
numbers being multiplied, divided etc.
Rev 3. 10 Page 5 of 120

Uncertain value
(underlined) Uncertain value
(underlined)
Uncertain value
(underlined)
The value 1.25 was measured only to
the 1/100 digit position.
Consequently, the result becomes
As the digit “0” already contains
5.62 (to three significant digits).
uncertainty, the result becomes 13.0
(to three significant digits).
<Format for Clearly Stating the Number of Significant Digits>

For example, the value 10, 000 can be represented as different numbers of significant digits as follows.
Five significant digits 1.0000 x 104
Four significant digits 1.000 x 104
Three significant digits 1.00 x 104
Two significant digits 1.0 x 104
One significant digit 1 x 104
<References>
1. Writing a value as 0.00123000 represents six significant digits.
2. Subtracting 1.230 (four significant digits) from 1.231 (four significant digits) produces the result 0.001,
which is one significant digit (1 x 10-3).
3. Dividing 2.462 (four significant digits) by 1.231 (four significant digits) produces the result 2.000, which
is four significant digits (not 2).
If the number of significant digits of the measured result exceeds the number of significant digits of the pass
criteria, round the final result down to the number of significant digits of the pass criteria.
Page 6 of 120 Rev 3. 10

Operational Qualification Preliminary Checks
2. Preliminary Checks
2-1 Reviewer Confirmation

Before conducting this inspection, the Manager shall designate the Reviewer. Record the Reviewer information
in the report. The Manager may also double as the Reviewer.
2-2 Performer Identification & Approval

The performer must be an individual who is trained and has adequate knowledge of this operational qualification
procedure. The Quality Assurance Department of the Analytical & Measuring Instruments Division of Shimadzu
Corporation performs such education, and recognizes individuals who are qualified to perform the IQ/OQ
procedures. An individual who is recognized as having been trained and who possesses sufficient knowledge is
certified by the General Manager of the Quality Assurance Department as a qualified IQ/OQ Inspector, as proven
by the certificate. A person who is recognized as having the ability to perform this inspection may also perform
this operational qualification procedure.
Before performing this operational qualification, the Performer’s qualification shall be confirmed and recorded
in the report.
2-3 Planning Items to be Evaluated in Operational Qualification

Prior to implementing this operational qualification, check the system configuration, determine the items to be
evaluated, record them in Operational Qualification Record and have them approved.
Rev 3.10 Page 7 of 120

2-4 Calibration Certificate and Instruments Used

The instruments and reagents used in the inspections are listed below.
When instruments controlled by the Shimadzu Representative are to be used, copies of the Certificate of
Traceability and the Quality Assurance sheet will be submitted. However, if the assured performance satisfies the
required specifications, calibrated instruments controlled by the customer may be used in the inspections.
(1) Instruments supplied by Shimadzu Representative
(1) Instruments for which traceability certification will be submitted

Shimadzu will provide copies of traceability certificates for the following instruments managed by the
Shimadzu Representative.
* Standard filters
This is used when verifying the “photometric accuracy” and “photometric repeatability” of the
spectrophotometer.
When conducting evaluation according to the instrument specifications, either NIST (National Institute of
Standard and Technology) filters or semi-standard optical filters that have been calibrated to the NIST
filters must be used.
In addition, these standard filters shall have an accuracy of ±1% (value relative to transmittance) as a
guaranteed performance specification when conducting evaluation based on criteria specified by the
Japanese Pharmacopoeia, and the filters shall be calibrated using the slit widths that can be set in the
instrument being inspected.
* Temperature-controlled cell holder

The temperature-controlled cell holder used to verify the spectrophotometer photometric accuracy shall
have a precision rating of ±0.5°C at the temperature required for the unit inspection as a guaranteed
performance specification.
* Thermometers
The thermometer used to measure the CPS-240A/B and TCC-240A set temperature accuracy shall have
a precision rating of ±0.4°C in the 10°C to 60°C temperature range required for the unit inspection as a
guaranteed performance specification.
The thermometer used to measure the CN syringe sipper temperature accuracy shall have a precision
rating of ±1°C at the 37°C required for the unit inspection as a guaranteed performance specification.
* Resistance temperature sensor

The resistance temperature sensor used to measure the CPS-240A/B and TCC-240A set temperature
accuracy and temperature control accuracy shall have a precision rating of ±0.2°C as a guaranteed
performance specification.
* Thermocouples
The thermocouples used to measure the CN type syringe sipper temperature control accuracy shall
conform to JIS Class 1 and have a precision rating of ±0.6°C at the 37°C required for the unit inspection
as a guaranteed performance specification.
(2) Items to be supplied by customer
* Electronic balance
This is used only when conducting the operation qualification tests for the Syringe Sipper N/CN.
Requires a calibrated balance able to weigh down to 0.001g.
Page 8 of 120 Rev 3. 10

2-5 Other Tools Used

Other equipment and solvent required to conduct the tests are listed below.
These are classed as customer-supplied items or Shimadzu Representative-supplied items.
(1) Customer-supplied items
The equipment and solvent below are used only for the operational qualification of the N/CN syringe sipper.
They are not needed if no syringe sipper is installed.
* Equipment
Beakers (2): capacity approx. 50 mL
* Solvent
Distilled water: 2L
(2) Items supplied by the Shimadzu Representative
The equipment and reagents below are used only for the operational qualification of specific devices. They are
not needed if applicable devices are not installed.
* Reagents
Potassium dichromate K2Cr2O7, 50mg: for N/CN syringe sipper
Perchloric acid HClO4(60%), 200 mg: for N/CN syringe sipper
* Other
Semi-micro cell [P/N 200-66501]: for N/CN syringe sipper
Rev 3. 10 Page 9 of 120

Operational Qualification Operational Qualification Protocol
3. Operational Qualification Outline

The inspection procedures for each component or system are listed below.
3-1 Outline of Inspection Procedures

1. UVProbe/Personal Computer and Peripherals
No. Item Outline

Personal Computer
1-1 Computer boot-up check Checks that the computer boots up and runs normally.
1-2 Time and date check Checks that the PC date and time are correct.
1-3 Hard disk drive check Checks that the hard disk operates correctly.
1-4 Print driver check Prints the print driver test page and checks the version number.
1-5 Network connection check Checks that the network connection is normal.
UVProbe
When the UVProbe application mode is Normal, the UVProbe inspection items are those except for items
2-3 - 2-6, for Security mode, those except for item 2-6, and for GLP mode, and all the inspection items
apply.
2-1 Software version check Checks that the software is not changed to an inappropriate version.
2-2 Program alteration check Conducts the program alteration check.
2-3 Shimadzu User Authentication Tool Checks the Shimadzu User Authentication Tool connection using database
connection check access and log registration.
2-4 Security function test Checks that the security functions operate, including restrictions on the
number of password characters.
2-4-1 Password log management function Checks that a duplicated password cannot be used.
check
2-4-2 Number of password characters Checks that the restriction on the minimum number of password
check characters operates.
2-4-3 Failed login detection Confirms that a failed login is detected.
2-4-4 User lockout function check Confirms that a user is locked out when the designated number of login
failures is exceeded.
2-4-5 Failed login record Confirms that a failed login attempt is registered in the log.
2-5 User access rights check Confirms that software use is restricted according to differences in
registered user access rights.
2-6 Lock function check Checks that during UVProbe startup, the manual access lock function
operates normally.
2-7 Software function check Checks that the software functions operate normally by actually
processing some UVProbe data and verifying the results. In addition, this
checks that the UVProbe data log recording function operates normally.
2-7-1 Peak detection/point pick check Checks that peak detection and point pick functions of the Spectrum
module operate normally.
2-7-2 Quantitation function check Checks that the quantitation function in the Photometric module operates
normally.
2-8 Communication check Checks that the spectrophotometer initialization settings are performed
using UVProbe, and that communication operates normally.
Page 10 of 120 Rev 3. 10

2. UV-1700/ UV-1800/UV-1650/2401PC/2450/2501PC/2550/3600
No. Item Outline

1 Firmware version check Checks the program version.
2 Initial setup check Checks that the instrument initial setup was completed correctly.
3 Wavelength accuracy check Uses the emission-line wavelengths (486.0, 656.1 nm) of the internal D2
lamp to check the accuracy of the displayed wavelengths.
4 Wavelength setting repeatability Uses the emission-line wavelengths (486.0, 656.1 nm) of the internal D2
check lamp to check the accuracy of the displayed wavelengths.
5 Photometric accuracy check Uses filters for transmittance calibration to check the photometric
accuracy.
6 Photometric repeatability check Uses filters for transmittance calibration to check the photometric
repeatability.
7 Baseline flatness check
(UV-1700/1800/UV-1600) Checks the baseline flatness in the range from 190 nm to 1100 nm.
(UV-2401PC/2450/2501PC/2550) Checks the baseline flatness in the range from 190 nm to 900 nm.
(UV-3600) Checks the baseline flatness in the range from 185 nm to 3300 nm.
3. Syringe Sipper N/CN
No. Item Outline

1 Initial operation check Checks that the cell holder home position is correctly detected when the
initialization command is used.
2 Intake volume accuracy check Confirms the intake accuracy by conducting three intake operations on
distilled water in a beaker and weighing the beaker before and after.
3 Intake volume repeatability check Confirms the intake repeatability from the discrepancy with the average
intake volume after conducting three intake operations on distilled
water in a beaker.
4 Carry-over check Uses an aqueous solution of potassium dichromate to check the
carry-over value (contamination from previous sample).
5 Temperature control accuracy check Checks the difference between the circulating water and cell holder
temperatures. For CN-type syringe sipper only.
4. ASC-5
No. Item Outline

1 Firmware version check Checks the program version.
2 Initial operation check
Checks that the initial operation is correct.
3 Manual operation check Uses manual key operation to check that the intake nozzle moves
smoothly in the X and Y directions one pitch at a time.
5. DIS-1200
No. Item Outline

Initialize command is used.
2 Cell position check Conduct three transmittance measurements at each cell position to
verify that the optical beam is not obstructed.
6. DIS-8
No. Item Outline

Initialize command is used.
Rev 3. 10 Page 11 of 120

7. CPS-240A/B
No. Item Outline

power is turned on.
2 Cell position check Conducts three transmittance measurements at each cell position to
confirm that the optical beam is not interrupted by thermal insulation,
etc.
3 Temperature accuracy check Checks the cell holder base temperature accuracy with respect to the set
temperature.
8. TCC-240A
No. Item Outline

1 Temperature accuracy check Checks the cell holder base temperature accuracy with respect to the set
temperature.
9. HCP-1C
No. Item Outline

1 Printing test Performs test printout, and checks control circuit operation and print
quality.
10. DPU-414
No. Item Outline

quality.
11. MPU
No. Item Outline

quality.
12. ESC/P Compatible Printer
No. Item Outline

quality.
13. PCL Compatible Printer
No. Item Outline

quality.
14. Time Course (Multi λ) Program Pack
No. Item Outline

1 Program version check Checks the program version.
2 Checksum value check Checks the checksum value, and checks that there is no problem with
the program.
15. DNA/Protein Quantitation Program Pack
No. Item Outline

the program.
Page 12 of 120 Rev 3. 10

16. Protein Quantitation Program Pack
No. Item Outline

the program.
17. CLASS-Agent
No. Item Outline

1-1 Software version check Checks that the software is not changed to an inappropriate version.
1-2 Program alteration check Conducts the program alteration check.
1-3 Shimadzu User Authentication Checks the Shimadzu User Authentication Tool connection using database
Tool connection check access and log registration.
1-4 Security function test Checks that the security functions operate, including restrictions on the
number of password characters.
1-4-1 Password log management Checks that a duplicate password cannot be used.
function check
1-4-2 Number of password characters Checks that the restriction on the minimum number of password
check characters operates.
1-4-3 Failed login detection Checks that a failed login is detected.
1-4-4 User lockout function check Checks that a user is locked out when the designated number of login
failures is exceeded.
1-4-5 Failed login record Checks that a failed login attempt is registered in the log.
1-5 User access rights check Checks that software use is restricted according to differences in
registered user access rights.
1-6 Test of function to prevent Checks that a duplicate user name cannot be registered.
duplicate user registration
1-7 Data display, search, and sort Checks that the sample search and sort work correctly and that the data is
displayed normally.
1-8 Data recovery Checks that the data files registered in a database can be correctly
recovered.
2 UVProbe auto registration check Checks that data is correctly registered by UVProbe automatic registration
to the database.
3 UVProbe manual registration Checks that data is correctly registered by UVProbe manual registration
check to the database.
4 Electronic signature check Checks the electronic signature function.
5 System log recording check Checks that the changes to the CLASS-Agent Manager system setting
conditions are recorded to the system log.
18. Validation Software Package

1 Software version check Checks that the software is not changed to an inappropriate version.
2 Program alteration check Conducts the program alteration check.
19. Color Measurement Software

3 Function check Checks the color measurement software functions.
20. Film Thickness Measurement Software

3 Function check Checks the film thickness measurement software functions.
Rev 3. 10 Page 13 of 120

Operational Qualification UVProbe Protocol
4. Operational Qualification Protocol
4-1 UVProbe/Personal Computer and Peripherals
1. Introduction
This section presents the standard operating procedure (SOP) for Operational Qualification of the
UVProbe/Personal Computer and Peripherals. Refer to the Instruction Manual for details about the operation
procedure and to clarify uncertain points.
Follow section 1-3 Entries and Revisions to change or delete the contents of the procedures.
2. Inspection Procedures
User Registration of Performer
If the UVProbe GLP or security mode is used, the system administrator must complete user registration for the
Performer who conducts the work (OQ User) before this Operational Qualification is conducted.
Simultaneously, register the Windows user ID to allow the OQ User to log in to Windows as a normal operator.
If the Class-Agent operation software is not used, user registration and authority setting is required for
UVProbe only.
Disable the Performer's user registration when all inspections are complete.
● CLASS-Agent User Registration

A user with User Registration authority starts the CLASS-Agent Manager and logs in. Click [Tools] ->
[User Administration] to open the [User Administration] screen. If the OQ User is already created but
disabled (displayed gray), select the required user and click [Active/Invalid] to enable this user. Click [Edit]
and check that the authority shown below is set for the user. To register a new user, click [New] and register
the user as shown in the table below.
● UVProbe User Registration

A user with Administration authority starts the UVProbe and logs in. Click [Edit] -> [Security] to open
[Users]. Create a new user, as shown in the table below. If the OQ User is already created but disabled
(displayed gray), select the required user and click [Active/Invalid] to enable this user. Click [Edit] and
check that the authority shown below is set for the user. To edit the authority, select a user below, click
[Properties] and set the authority shown in the table below.
<OQ User Registration> * ( ) Indicates name used with UVProbe
Login ID UVProbe
User name Password CLASS-Agent Authority Group
(User ID) Authority Group
Operator,
OQ_USER_1 OQ_Operator ******* Operator
but with additional “Approval”
authority for Agent Manager
OQ_USER_2 OQ_Approver ******* Administrator Administrator
The administrator shall issue the initial user password and inform the user.
● UVProbe Login
Use the User ID “OQ_USER_2” to log in UVProbe if not specified otherwise.
Page 14 of 120 Rev 3. 10

Personal Computer
Test 1-1
(Item) Computer boot-up check
(Outline) Checks that the computer boots up and runs normally. This test uses the self-test during
computer start-up to ensure that no memory errors occur.
(Procedure) 1) Turn on the PC.
2) Check that Windows starts up normally.
* If more than one OS is installed in the personal computer, follow the test procedure above to
check that each OS boots up normally.
(Criteria) Windows starts up without any errors.
Test 1-2
(Item) Time and date check
(Outline) Checks that the pc date and time are correct.
(Procedure) 1) Open the Windows Control Panel.
2) Double-click [Date/Time] in the Control Panel to display the Date/Time Properties.
3) Check that the date and time are correct. Check the time against an accurate clock, such
as the telephone time service.
(Criteria) Date and time are correct.
Test 1-3
(Item) Hard disk drive check
(Outline) Checks that the hard disk operates correctly.
(Procedure) In order to perform this test, the user must log into Windows with Administrator authorization.
In addition, when performing step 5) of the procedure, do not open or close any files.
(Disk error-checking procedure)

1) Open Windows Explorer.
2) Right-click on the hard disk drive to be checked.
3) Click [Properties] and then click the [Tools] tab.
4) Click [Check Now…] in the “Error Checking” frame.
5) Click [Start] without placing a check mark at either of the “Check disk options”.
(Criteria) “Disk Check Complete” is displayed.
Rev 3. 10 Page 15 of 120

Test 1-4
(Item) Print driver check
(Outline) Prints the print driver test page and checks the version number.
(Procedure) 1) Select [Printers] from the Windows Control Panel to display the printers used.
2) Right-click the printer used and select [Properties].
3) Click the [Print Test Page] button on the Properties [General] tab to print the test page.
* If more than one OS is installed in the personal computer, follow the test procedure above
to print the test page under each OS.
4) Check that the test page printed correctly and record the print driver version number
printed in it.
Test page prints correctly.
(Criteria)
The driver version number matches the version number on record.
Test 1-5
(Item) Network connection test
This inspection is required only for network connected PCs.
(Outline) Checks the network connection between the inspected computer and the reference computer
(e.g., the server computer).
(Procedure) 1) Run the Command Prompt and enter “C: ¥>PING***.***.***.***” (substituting the IP
address of the server computer or other reference computer for “***.***.***.***”).
2) Data communication is conducted with the designated computer and the results are
displayed.
3) Check that no packets were lost.
4) Maximize the screen. Hold down the [Alt] key and press [PrtSc] to copy the screen.
Paste the content into the Windows Paint accessory and print it out.
(Criteria) No packets lost.
Page 16 of 120 Rev 3. 10

UVProbe
Test 2-1
(Item) Software version check
(Outline)
Checks the version number of the UVProbe software and Shimadzu User Authentication Tool.
(Procedure) 1) Check the version number printed in the test results from the alteration test in Test 2-2.
2) Check that the version number matches the version number on record.
(Criteria)
Version number matches the version number on record.
Test 2-2
(Item) Program alteration check
(Outline) Checks that no modifications have occurred to the contents, date, or checksum of the files
(*.dll, *.exe, *.ocx, etc.) in the UVProbe or Shimadzu User Authentication Tool folders.
(Procedure) UVProbe Alteration Check Procedure
1) Click on the Windows [Start] button and select [Programs] -> [Shimadzu] -> [UVProbe –
Check the Program Files] to run the alteration check program.
2) When the login screen appears, enter the user ID “OQ_USER_2”.
3) When the [Check the Program] screen appears, select (highlight) “UVProbe VER.XXX”
and click the [Check] button.
* If the supplemental disk is installed, 2 UVProbe lists are displayed on the screen. In this
situation, be sure to select the one in which the version numbers match.
Example) If Supplemental Disk Ver2.00SU1 is installed,
-> select “UVProbe Ver.2.00SU1”.
4) Click the [Run] button to run the program alteration check.
5) When the check is complete, click the [NotePad] button.
6) The results are displayed as a text file. Ensure that all items are OK and print the results.
Shimadzu User Authentication Tool Alteration Check Procedure

7) Return to the dialog box at step 3) above, select (highlight) “Shimadzu User
Authentication Tool” and click the [Check] button.
8) Click the [Run] button to run the program alteration check.
(Criteria) All items are displayed as “OK”.
Rev 3. 10 Page 17 of 120

Test 2-3
(Item) Shimadzu User Authentication Tool connection check
(Outline) Checks the Shimadzu User Authentication Tool connection using database access and log
registration.
(Procedure)
1) Open the Windows Control Panel and double-click on the Shimadzu User Authentication
Tool icon to open the main menu.
2) Record the server name displayed at the bottom of the main menu and confirm that the
connected database is correct.
* Conduct steps 3) and 4) below after conducting Test 2-4-4.
3) Log in to [Log Display] as “OQ_USER_2” from the main menu. Set the test date and test
computer name in [Search Conditions]. Search the log and print out the results.
4) Confirm that the user lockout generated in Test 2-4-4 is registered and that the software
name is UVProbe.exe.
Server name for the connected database is correct.

(Criteria)
Login possible from [Log Display].
Lockout by UVProbe.exe is registered.
Page 18 of 120 Rev 3. 10

Test 2-4
(Item) 2-4-1 Password log management function check
2-4-2 Number of password characters check
2-4-3 Failed login detection
2-4-4 User lockout function check
2-4-5 Failed login record
(Outline) Checks that the security functions operate, including restrictions on the number of password
characters.
Before conducting this test, verify that the configuration settings of Shimadzu User
(Preparation)
Authentication Tool are as listed below. Change the settings for items (3) and (4) as indicated
below.
Item Setting
(1) Minimum password length (Check only; set to non-zero value)
(2) Permission to use previous No check
password
(3) User lockout time 1 minute
(4) User login failures (Check only; set to non-zero value)
(5) PC Login failures Value the same as or larger than
“User login failures” setting
(Procedure) 1) Start up UVProbe, and log in as the “OQ_USER_1” test user.
2) Select [Security] in the [Edit] menu.
3) Enter the current password, and also enter the same password as the new password.
4) Confirm that the new password is not accepted.
5) Enter the current password and enter a new password that is shorter than the minimum
number of characters set for the Shimadzu User Authentication Tool software.
6) Confirm that the change is not accepted, as the password is too short.
7) Enter a password equal in length to the minimum number of characters and confirm that the
change is accepted.
8) Close UVProbe.
9) Start up UVProbe again, and enter “OQ_USER_1” as the test user ID.
10) Enter a password that is not set and click [OK].
11) Confirm that login is not permitted and a message is displayed warning that the password is
incorrect.
12) Repeat steps 9) to 11) for the number of times designated for “User login failures”.
13) After the designated numbers of login failures, confirm that the “OQ_USER_1” is locked
out and cannot log in for the designated lockout time.
14) After the designated lockout time elapses, start up UVProbe again. Enter “OQ_USER_1” as
the login ID and correctly enter the set password.
15) Confirm that login is possible.
16) Close UVProbe, and then log in again as the “OQ_USER_2” test user.
17) Select [Security] in the [Edit] menu.
18) Select the [Event Log] tab, and confirm that the login failures in the procedure above and
the corresponding times appear in the displayed log. Close UVProbe.
19) If any settings in the Shimadzu User Authentication Tool configuration were changed in the
Preparation above, return them to their original values.
(Criteria) 2-4-1 Duplicate password is not accepted.
2-4-2 Change to a password shorter than the minimum number of characters is not
accepted.
Change to a password with the minimum number of characters is accepted.
2-4-3 Login prohibited with an incorrect password but possible with the correct
password.
2-4-4 User locked out after the designated number of login failures.
Login prohibited for the designated lockout time.
2-4-5 Login failures recorded in the log.
Rev 3. 10 Page 19 of 120

Test 2-5
(Item) User access rights check
(Outline) Confirms that software use is restricted according to differences in registered user access rights.
This procedure is performed only when UVProbe is run in Security or GLP mode.
(Procedure)
1) Start UVProbe.
2) Log in with the user ID “OQ_USER_2”
3) Select [Method] from the [Edit] menu, and confirm that the content of the analysis method
can be changed. Close UVProbe.
4) Start UVProbe again, and log in as “OQ_USER_1”.
5) Confirm that the [Method] command in the [Edit] menu is disabled (grayed out).
(Criteria) OQ_USER_2 can edit the analysis method, but it is disabled for OQ_USER_1.
Test 2-6
(Item) Lock function check
(Outline) Checks that during UVProbe startup, the manual access lock function operates normally. This
procedure is performed only when UVProbe is run in GLP mode.
(Procedure)
Perform this procedure as described below. For detail on operation, refer to the UVProbe
Instruction Manual (Tutorial).
1) Start up UVProbe
2) Select [Lock] from the [Window] menu.
3) The Login screen is displayed. Confirm that the UVProbe menus cannot be accessed.
4) Log in using the “OQ_USER_2” password to close the Login screen, and confirm that the
UVProbe menus have become accessible.
(Criteria) Login screen is displayed.
UVProbe can be used after entering password.
Page 20 of 120 Rev 3. 10

Test 2-7
If data from this computer is being registered to the CLASS-Agent database, certain check and implementation
items must be performed beforehand. Refer to cautions described below.
(Item) Software function check

(Outline) Checks that the software functions operate normally by actually processing some UVProbe
data and verifying the results.
(Preparation) 1) Prepare the UVProbe software Install disk for the test.
2) Run the file “Check_Data.EXE” in the folder ¥English¥UVProbe¥Disk1 on the Install
disk.
3) The following file is copied to the folder
“C:¥ProgramFiles¥Shimadzu¥UVProbe¥Test”.
Data Name Date / Time

For Test 7-1 Anthracene.spc 2002.9.25 2:15
Note 1: The data used here is overwritten each time the check is conducted. Each time
the test is performed, install the file to the hard drive from the CD-ROM.
Note 2: Always check the date and time of the data used with Explorer.
Note 3:The location of English is selected in the Control Panel.
(Cautions when registering to Agent Database)

(Cautions) When registering to the Agent database, make the following preparations before the test.
1) Start UVProbe automatic registration if it is not running, or if it is already running,

double-click it in the task tray and verify the settings. If it is in the task tray due to the
autostart function, it is necessary to enter a password to open it. In this case, a system
administrator must enter the password.
2) Note the existing settings. Register the re-analysis data from the Analytical Instrument 1
to the normally used database using the UVProbe analyst name.
Perform as follows after completion of the test.
1) Close all of the data loaded in UVProbe, and delete the data file copied in “Preparation”
above using Explorer. In addition, if any of the UVProbe automatic registration settings
were changed, return the settings to their original values.
Rev 3. 10 Page 21 of 120

Test 2-7-1
(Item) Peak detection / point pick check
(Outline) Checks that peak detection and peak pick functions of the Spectrum module operate normally.
(Procedure)
1) Start up UVProbe. (Spectrophotometer need not be connected to PC.)
2) Using the [Open] command in the [File] menu of the Spectrum module, load the
following data.
C:¥ProgramFiles¥Shimadzu¥UVProbe¥Test¥Anthracene.spc
3) Using the [Save As] command in the [File] menu, save the data to the same folder as
“Anthra.spc”.
4) Select [Peak Detection] from the [Data Processing] menu.
5) Display the shortcut menu by right-clicking on the peak detection table, select
[Properties], and in the [General] page, set the peak detection parameters as follows
Threshold value : 0.2 Interpolation : no check

Number of points :4 Averaging : no check
6) Select [Settings] in the [View] menu, and for the number of decimal places to be
displayed for the X and Y axes, set 1 place and 4 places, respectively.
7) Using [Save As] in the [File] menu, save the data as “Anthra1.spc”.
8) Confirm that the detected peaks and valleys match those shown below.
Wavelength (nm) Abs Wavelength (nm) Abs

(Peak) 376.0 0.5569 (Valley) 365.5 0.1461
(Peak) 356.5 0.5884 (Valley) 346.5 0.2224
(Peak) 339.5 0.4169
9) Select [Point Pick] in the [Data Processing] menu.

10) Enter “330” and “350” in the Point Pick table wavelength column, and confirm that the
absorbance values for these wavelengths are as follows.
No. Wavelength (nm) Abs

1 330.0 0.1891
2 350.0 0.3023
11) Using [Save As] in the [File] menu, save the data as “Anthra2.spc”.
12) Print the report using the report template (OQ_ProbeTest3.rpt) copied to the same folder
at step 2). If the point pick table or spectrum data set log object is not contained in
“OQ_ProbeTest3.rpt”, insert them using the report generator.
13) Verify that the report records the file name changes from steps 3), 5), 7), 10) and 11), as
well as the detection parameter changes, date and user name in the data set log.
(Criteria) Peak detection and point pick results match in confirmation steps 8) and 10).
File name changes in steps 3), 5), 7), 10) and 11) and the peak detection parameter
changes are recorded in the data log along with the date and user name*1.
*1) The user name of the user logged into UVProbe is recorded as the data set log user name.
Therefore, if the UVProbe application mode is Normal, the user name is left blank.
Page 22 of 120 Rev 3. 10

Test 2-7-2
(Item) Quantitation function check
(Outline) Checks that the quantitation function in the Photometric module operates normally.
(Procedure)
1) Start up UVProbe. (Spectrophotometer need not be connected to PC.)
2) Select [Photometric] in the [Window] menu.
3) Select [Method] in the [Edit] menu, in the [Wavelengths] page, register Measurement
Wavelength: 452 nm, and in the [Calibration] page, select WL1:WL452.0. (Leave the
other settings at their default values.)
4) In the [Measurement Parameters (Standard)] page, change the [Data Acquired By] setting
to “User Entry”. (Leave the other settings at their default values.)
5) Complete the measurement method editing, leaving the file name as the default name.
6) Select [Settings] in the [View] menu, and for the number of decimal places to be
displayed in the Standard Sample and Sample tables, set 5 places and 3 places,
respectively.
7) Enter the sample IDs, concentrations and absorbances in the Standard Sample table as
follows.
Sample ID Concentration Absorbance(WL452.0)
Std_1 1 0.03314
Std_2 2 0.06407
Std_3 4 0.12666
Std_4 10 0.33617
8) Select [Standard Curve Statistics] in the [Graph] menu, and place check marks for
“Equation” and “Correlation Coefficient”.
9) Verify that the calibration curve function and correlation coefficient displayed at the
bottom of the calibration curve graph match the values shown below.
Calibration curve function : Y=0.03383x - 0.00379
Correlation coefficient r2 : 0.99935
10) Select [Save As] in the [File] menu, and after selecting [Standard file (*.std)] as the file
type, save the file as “OQ_Test1-3-2.std”.
11) Load the following file using the [Open] command in the [File] menu.
C:¥ProgramFiles¥Shimadzu¥UVProbe¥Data¥Ver2Data¥B-carotene.unk
12) Import the standard sample file created in step 10) using the [Open] command in the
[File] menu.
13) Change the file name as follows, and save it as a photometric file.
C:¥ProgramFiles¥Shimadzu¥UVProbe¥Test¥OQ_Test1-3-2.Pho
14) Verify that the sample concentrations in the sample table match those listed below.
Sample ID Concentration Sample ID Concentration

S1 6.526 S6 6.000
S2 5.892 S7 4.764
S3 5.555 S8 4.791
S4 5.505 S9 2.867
S5 5.607 S10 3.560
15) Open the following file using the Report Generator, and print the report after inserting the
photometric log and photometric summary objects on the second page (Add New).
C:¥ProgramFiles¥Shimadzu¥UVProbe¥Reports¥Standard Curve.rpt
16) Verify that the printed report records the standard sample file importation, file save
content, date and user name implemented in steps 12 and 13) above.
17) Return the settings and objects that were changed in steps 6) and 15) to their original
state.
(Criteria) The calibration curve function and correlation coefficient, and quantitation results
match in steps 9) and 14).
The standard sample file importation and file save content of steps 12) and 13) are
recorded in the photometric log along with the date and user name.
Rev 3. 10 Page 23 of 120

Test 2-8
(Item) Communication check
(Outline)
Checks that spectrophotometer initialization settings are performed using UVProbe, and that
communication operates normally.
(Procedure)
Perform the procedure as described below.
For details on operation, refer to the UVProbe Instruction Manual (Tutorial).
1) Turn on the spectrophotometer.

2) Start up the UVProbe software, and select the Spectrum module.
3) Click the [Connect] button to start control of the spectrophotometer.
4) Confirm that the spectrophotometer initialization screen is displayed, and that the settings
and diagnostics start automatically for each item.
(Criteria) The spectrophotometer initialization screen is displayed.
Page 24 of 120 Rev 3. 10

Operational Qualification UV-1700 Protocol
4-2 Spectrophotometer
4-2-1 UV-1700 UV-VIS Spectrophotometer
1. Introduction
This section presents the standard operating procedure (SOP) for Operational Qualification of the UV-1700
Ultraviolet-Visible Spectrophotometer. The procedures shown here employ the Validation functions provided
as standard with the UV-1700. Refer to the Instruction Manual for details about the operation procedure and to
clarify uncertain points.
The UV-1700 incorporates a standard semi/full-automatic inspection validation function for checking the
instrument performance. Using that validation function, the procedures for performing tests 1 - 11 are shown
here.
The following Validation function test items are used for performing the tests.
Test 1: Firmware version check ….Checks the ROM version printed in results printout.
Test 2: Initial setup check …. Full-automatic test “7. Initialization results record”
Test 3: Wavelength accuracy check …. Full-automatic test “1. Wavelength accuracy”
Test 4: Wavelength setting repeatability check …. Full-automatic test “2. Wavelength repeatability”
Test 5: Photometric accuracy check …. Semi-automatic test “1. Photometric accuracy”
Test 6: Photometric repeatability check …. Semi-automatic test “2. Photometric repeatability”
Test 7: Baseline flatness check …. Full-automatic test “5. Baseline flatness”
Rev 3. 10 Page 25 of 120

(1) Test Preparation

(Item) Printer selection : Select the printer to be used for printing the results.
Detailed printout settings : Set detailed printout to “Yes”
(Outline) Printer selection : In the UV-1700 instrument conditions setting mode, select and set the
printer to be used for printing the test results.
Detailed printout settings : Make settings so that the test results and spectrum/time course
curve are automatically printed out after each test is completed.
(Procedure) Perform the procedure as described below.
For details on operation, refer to the UV-1700 Instruction Manual (Operation Guide).
1) Turn on the UV-1700.

2) The spectrophotometer initialization screen is displayed on the LCD and the settings and
diagnostics start automatically for each item.
3) When the initialization is completed normally, the UV-1700 mode selection screen is
displayed on the LCD.
<Printer Selection>
4) Select [9. Utilities].

5) Select [5. Printer] to select the printer connected to the UV-1700.
6) Perform the settings as directed by the messages on the screen.
7) After completing the printer settings, press the [RETURN] key to return to the UV-1700
mode selection screen.
8) Set the connected printer to the ON LINE state.
<Detailed Printout Settings>
9) In the UV-1700 mode selection screen, press the [F3] key (Mainte.).
10)In the instrument’s Maintenance screen, select [1. Validation].
11)In the Validation menu screen, press the [F4] key (Test Settings).
1) When the test settings screen is displayed, press the [2] key, to set [2. Auto print] to
“ON”.
2) Press the [RETURN] key to return to the Validation menu screen.
Page 26 of 120 Rev 3. 10

(2) Test Conditions Setting Procedure

No. Setting Outline
Test 3 To check the accuracy of the displayed wavelength value, set it so that the D2 emission lines
656.1nm and 486.0nm are used, and enter the pass criteria value (standard value).
Test 4 Enter the pass criteria value (standard value) for the wavelength setting repeatability.
Test 5 Enter the information for the filter for transmittance calibration to be used for checking the
photometric value accuracy, and set the measurement conditions.
photometric repeatability, and set the measurement conditions.
Test 7 Set the measurement range for checking the baseline flatness, and enter the pass criteria value
(standard value).
(Criteria)
Test 1: The version number matches the controlled version number.
Test 2: Each item of the initial settings is completed as “OK”.
Test 3: Measurement deviation of D2 emission lines 656.1nm and 486.0nm is within
±0.3nm.
Test 4 :
Instrument specifications …. Deviation from average of 3 values is within ±0.1nm
Pharmacopoeia …. Deviation from average of 3 values is within ±0.2nm
Test 5:
Instrument specifications
Absorbance near 1Abs : Deviation from reference value is within ±0.004 Abs
Absorbance near 0.5Abs: Deviation from reference value is within ±0.002 Abs
Note) The instrument specifications apply only to specifications determined with a
NIST-traceable visible region filter, or a semi-standard optical filter whose value is
calibrated to a NIST filter.
Pharmacopoeia….Deviation from standard value is within ±0.008 Abs
Test 6:
Absorbance near 1Abs : Deviation from average of 3 values is within ±0.002 Abs
Absorbance near 0.5Abs : Deviation from average of 3 values is within ±0.001 Abs
Pharmacopoeia
Test 7: Baseline flatness is within ±0.002 Abs
* For the measurement methods and pass criteria values in Tests 3 - 11, refer to Additional
Information from page 31.
Rev 3. 10 Page 27 of 120

<Semi-auto items setting>
2) In the instrument Maintenance screen, select [1. Validation].
3) In the Validation menu screen, press the [1] key (Semi-auto Items).
4) Enter the set password.
5) The Semi-auto items setting menu screen is displayed, and the items that are set for
inspection will all be highlighted. At this time, if [3. Stray light] inspection is set to be
performed, perform steps 6) - 8).
6) In the Semi-auto items setting menu screen, press the [3] key (Stray Light).
7) In the Stray Light conditions setting screen, press the [1] key (Inspection) to toggle the
setting to “No”.
8) Press the [RETURN] key to return to the Semi-auto items setting menu screen.
< Test 5 Conditions Setting >

9) In the Semi-auto items setting menu screen, press the [1] key (Photometric Accuracy).
10) In the Photometric Accuracy conditions setting screen, press the [1] key (Inspection), to
toggle it to “Yes”.
11) Press the [2] key (Measurement mode), and select “Abs”.
12) Press the [3] key (Check λ), and enter 635.0, 590.0, 546.1, 456.0 and 440.0nm as the
measurement wavelengths.
13) Press the [4] key (10% filter) to display the 10% Filter conditions setting screen.
14) In the 10% Filter conditions setting screen, press the [1] key (Serial Number) and enter the
serial number of the 10% ND optical filter to be used.
15) Press the [2] key (Good THRU), and enter the valid period of the calibration values for the
10% ND optical filter to be used.
16) Press the [3] key (Tolerance), and set the tolerance value to ±8mAbs (or ±4mAbs).
17) Press the [4] key (Calibration values), and enter the calibration values for the 10% ND
optical filter to be used.
18) Press the [RETURN] key to return to the Photometric Accuracy conditions settings screen.
19) Press the [5] key (30% Filter) to display the 30% Filter conditions setting screen.
20) In the 30% Filter conditions setting screen, press the [1] key (Serial Number) and enter the
serial number of the 30% ND optical filter to be used.
21) Press the [2] key (Good THRU), and enter the valid period of the calibration values for the
30% ND optical filter to be used.
22) Press the [3] key (Tolerance), and set the tolerance value to ±8mAbs (or ±2mAbs).
23) Press the [4] key (Calibration values), and enter the calibration values for the 30% ND
optical filter to be used.
24) Press the [RETURN] key twice to return to the Semi-auto items setting screen.

25) In the Semi-auto items setting menu screen, press the [2] key (Photometric Repeatability).
26) In the Photometric Repeatability conditions setting screen, press the [1] key (Inspection) to
toggle it to “Yes”.
27) Press the [2] key (Measurement Mode), and select “Abs”.
28) Press the [3] key (Check λ), and enter 635.0nm as the measurement wavelength.
29) Press the [4] key (10% filter), and enter the serial number of the 10% ND optical filter and
the valid period of the calibration values, and set the tolerance value to ±4mAbs (or
±2mAbs).
30) Press the [5] key (30% filter), and enter the serial number of the 30% ND optical filter and
the valid period of the calibration values, and set the tolerance value to ±2mAbs (or
±1mAbs).
31) Press the [RETURN] key 3 times to return to the Validation menu screen.
Page 28 of 120 Rev 3. 10

< Full-automatic Test Conditions Setting >
(Procedure) 32) In the Validation menu screen, press the [2] key (Auto items).
33) Enter the set password.
34) The Full-automatic test conditions setting menu screen is displayed, and the items that are
set for inspection are all highlighted. At this time, if [3. Resolution], [4. Baseline stability]
and [6. Noise level] are set for testing, perform steps 35) - 38).
35) In the Full-automatic test conditions setting menu screen, press the [3] key (Resolution).
36) In the Resolution conditions setting screen, press the [1] key (Inspection) to toggle the
setting to “No”.
37) Press the [RETURN] key to return to the Full-automatic test conditions setting menu
screen.
38) In the same way, select [4. Baseline Stability] and [6. Noise Level], and toggle their [1.
Inspection] settings to “No”.

39) In the Full-automatic test conditions setting menu screen, press the [7] key (Initialization
Record) to highlight the item (to be executed).
40) Press the [RETURN] key to return to the Validation screen.

41) In the Full-automatic test conditions setting menu screen, press the [1] key (Wavelength
accuracy).
42) In the Wavelength Accuracy conditions setting screen, press the [1] key (Inspection) to
toggle the setting to “Yes”.
43) Press the [2] key (Method” and select “D2 Lamp.
44) Press the [3] key (Check λ), and select “Both λ”.
45) Press the [4] key (Tolerance), and set the tolerance value to ±0.3nm.
screen.

Repeatability).
48) In the Wavelength repeatability conditions setting screen, press the [1] key (Inspection) to
toggle the setting to “Yes”.
49) Press the [2] key (Tolerance), and set the tolerance value to ±0.2nm (or ±0.1nm).
screen.

51) In the Full-automatic test conditions setting menu screen, press the [5] key (Baseline
Flatness).
52) In the Baseline Flatness conditions setting screen, press the [1] key (Inspection) to toggle
the setting to “Yes”.
53) Press the [2] key (Scanning Range), and set the starting and ending wavelengths as 1100nm
and 190nm, respectively.
54) Press the [3] key (Tolerance), and set the tolerance value to ±2mAbs.
screen.
Rev 3. 10 Page 29 of 120

(3) Test Procedure

When using the validation functions, the tests proceed in order from <Semi-auto test items> -> <Full-auto test
items>.

1) In the Validation menu screen, verify that the following items are highlighted, indicating
that they are set for inspection.
2) Install the CPS-240A in the UV-1800 sample compartment, and set the temperature
controller temperature to that specified in the filter transmittance calibration test results
document.
3) Set the ND optical filter into the CPS-240A cell holder.
Cell holder 1 : None
Cell holder 2 : 10% ND optical filter
* To stabilize the ND optical filter temperature, keep the sample compartment lid closed for at least 10
minutes before starting the measurements.
4) After verifying that the CPS-240A cell position is “Cell 1” (Controller “CELL POSITION”
“1” LED is illuminated), press the [START/STOP] key to start the validation operation.
5) The semi-automatic test [1. Photometric Accuracy] starts, and baseline correction is
performed. When a message appears on the screen requesting that the 10% ND filter be set
in place, using the CPS-240A controller (press the [STEP] button), set the cell position to
“Cell 2”. Press the [START/STOP] key to perform measurement of the 10% ND filter.
6) When a message appears on the screen requesting that the 30% ND filter be set in place,
using the CPS-240A controller (press the [STEP] button), set the cell position to “Cell 3”.
Press the [START/STOP] key to perform measurement of the 30% ND filter.
7) When the [1. Photometric Accuracy] measurement is completed, the measurement and
Pass/Fail judgment results are printed out.
8) The [2. Photometric Repeatability] test starts, and a message appears requesting
confirmation that there is nothing in the sample compartment. Remove the CPS-240A and
replace it with the standard sample compartment. Press the [START/STOP] key to start the
auto zero operation.
9) Following the on-screen messages, repeat the indicated photometric measurements while
removing and inserting the filters.
10) When the [2. Photometric Repeatability] measurement is completed, the measurement and
11) The full-automatic test [1. Wavelength Accuracy] starts, and following the message that
appears on the screen, check that there is nothing in the sample compartment, and press the
[START/STOP] key.
12) When the full-automatic tests are completed, the measurement results and Pass/Fail
judgment results are printed out for each of the tests, and the display returns to the
Validation screen.
13) Attach the measurement results for each of the test items to this document.
Page 30 of 120 Rev 3. 10

<Additional Information>
· About Displayed Wavelength Value Accuracy, and Wavelength Setting Repeatability
The pass criteria and procedures used for the displayed wavelength value accuracy and
wavelength setting repeatability inspections of Test 3 and Test 4, respectively, are derived from
the Japanese Pharmacopoeia Fifteenth Edition.
Japanese Pharmacopoeia Fifteenth Edition - General Test Methods
2.24. UV-VIS Spectrophotometer Measurement Methods
Wavelength, transmittance, or absorbance calibration
After pre-adjusting the spectrophotometer, confirm that the wavelength and transmittance comply with
the following tests.
Using optical filters, the wavelength is within ... Testing can be conducted using a low-pressure
mercury lamp ... or deuterium discharge tube 486.00 nm and 656.10 nm emission lines. The
measured wavelength and emission line wavelength shall differ by no more than ±0.3 nm. When
conducting three measurements, all measured values shall be within ± 0.2 nm of the average value.
Rev 3. 10 Page 31 of 120

· Photometric accuracy check

The display of the photometric accuracy is defined in the JIS standards, as follows:
JIS K0115-2004 Rules for absorbance analysis
4.2 Displaying unit performance
(e) Photometric accuracy
Measure the percentage transmittance or absorbance of a standard substance (4). Display the
measured value and its difference from the standard value.
The measurement method for photometric accuracy conforms with the 15th Japanese
Pharmacopoeia:
Transmittance and absorbance are measured using optical filters for transmittance calibration.
When testing is conducted under the test conditions in the test report attached to each filter in
order to read the transmittance at the reference wavelength value indicated in the test report, the
displacement between the measured transmittance and reference transmittance shall lie within
1% of the upper and lower limits of the relative accuracy indicated in the test report… .
(Explanation)
The actual transmittance tolerance at the wavelength of each optical filter for transmittance
calibration can be determined, as described below. The actual transmittance tolerance at the
wavelength of each optical filter for transmittance calibration can be determined, as described
below.
Example: For a 30% ND optical filter with reference value and guaranteed accuracy as follows:
Wavelength (nm) 440 465 546.1 590 635

Transmittance (%) 23.92 29.17 29.91 27.99 28.50
Absorption (Abs) : 0.621 0.535 0.524 0.553 0.545
Guaranteed calibration accuracy: ±1% (relative value with respect to
transmittance)
The Japanese Pharmacopoeia prescribes a transmittance tolerance relative value of ±2% (1%
added to the guaranteed accuracy upper and lower limits), such that the transmittance tolerance at
440 nm is:
23.92 x (2/100) ≈ 0.48
Thus, the transmittance tolerance is 23.92 ± 0.48% (23.44% to 24.40%). Converting this to
absorbance using absorbance = log10 (100/transmittance), gives an absorbance tolerance range of
0.613 to 0.630 Abs.
Based on the above information, the Test 5 Pass Criteria/ (Pharmacopoeia ) are defined as
follows:
The tolerance range is 29.40% to 30.60% at 30% transmittance (0.523 Abs absorbance).
Converting this to absorbance gives 0.514 to 0.532 (0.523 ± 0.009). However, due to the rounding
errors during conversion, a pass criterion of (reference value ± 0.008 Abs) is adopted for the
photometric accuracy near 0.5 Abs.
Similarly, as the tolerance range is 0.991 to 1.009 Abs at 10% transmittance, a pass criterion of
(reference value ± 0.008 Abs) is adopted.
Page 32 of 120 Rev 3. 10

<Additional Information> (Measurement Methods and Criteria)
· Photometric repeatability check

The display of the photometric repeatability is defined in the JIS standards, as follows:
JIS K0115 Rules for absorbance analysis
(f) Photometric repeatability
Load a sample that does not change over time into the sample compartment and measure the
percentage transmittance or absorbance. Next, remove the sample and load it again. The
photometric repeatability expresses the discrepancies in measured values when this
operation is repeated several times.
The number of measurements and the measurement method for Test 6 conforms with the 15th
Japanese Pharmacopoeia:
When testing is conducted under the test conditions in the test report attached to each filter in order
to read the transmittance at the reference wavelength value indicated in the test report, the
displacement between the measured transmittance and reference transmittance shall lie within 1%
of the upper and lower limits of the relative accuracy indicated in the test report. Additionally,
after the measurement is conducted three times, all measured absorbance values (or
measured transmittance values converted to absorbance values) shall lie within ±0.002 of the
average value for absorbance up to 0.500 and ±0.004 for absorbance over 0.500.
· Test method and evaluation criteria for baseline flatness

The test method for spectrophotometer baseline flatness is defined in the Japan Analytical
Instruments Manufacturers Association standards, as follows:
JAIMAS 0001 Displaying UV-VIS spectrophotometer performance
3.7 Baseline flatness
(3) Test method
With the sample compartment empty, set the absorbance to zero (or 100%T transmittance). Scan
the wavelengths across the guaranteed wavelength range and record the absorbance (or
transmittance) with a recorder. Determine the maximum and minimum absorbance values,
after eliminating recognized noise.
In the UV-1700, from the viewpoint of noise exclusion, the measured baseline is subjected to
smoothing, and the absorbance difference with the 0 Abs line is set as the baseline curvature
(flatness).
Rev 3. 10 Page 33 of 120

1. Introduction
This section presents the standard operating procedure (SOP) for Operational Qualification of the UV-1800
Ultraviolet-Visible Spectrophotometer. The procedures shown here employ the Validation functions provided
as standard with the UV-1800. Refer to the Instruction Manual for details about the operation procedure and to
The UV-1800 incorporates a standard semi/full-automatic inspection validation function for checking the
instrument performance. Using that validation function, the procedures for performing tests 1 - 11 are shown
here.
The following Validation function test items are used for performing the tests.
Test 1: Firmware version check ….Checks the ROM version printed in results printout.
Test 2: Initial setup check …. Validation Settings “3. Print init. status”
Test 3: Wavelength accuracy check …. Full-automatic test “WL accuracy D2”
Test 4: Wavelength setting repeatability check …. Full-automatic test “WL repeatability D2”
Test 5: Photometric accuracy check …. Semi-automatic test “Photo accuracy”
Test 6: Photometric repeatability check …. Semi-automatic test “Photo repeatability”
Test 7: Baseline flatness check …. Full-automatic test “Baseline flatness”
Page 34 of 120 Rev 3. 10

(1) Test Preparation

(Item) Printer selection : Select the printer to be used for printing the results.
Detailed printout settings : Set detailed printout to “Yes”
(Outline) Printer selection : In the UV-1800 instrument conditions setting mode, select and set the
printer to be used for printing the test results.
Detailed printout settings : Make settings so that the test results and spectrum/time course
curve are automatically printed out after each test is completed.
1) Turn on the UV-1800.

2) The spectrophotometer initialization screen is displayed on the LCD and the settings and
diagnostics start automatically for each item.
3) When the initialization is completed normally, the UV-1800 mode menu screen is
displayed on the LCD. When the security functions are enabled, only a user with
authority to change instrument validation conditions can log in.
<Printer Selection>
4) Select [8. Utilities] in the mode menu screen.

5) Select [5. Printer] to select the printer connected to the UV-1800.
6) Perform the settings as directed by the messages on the screen.
7) After completing the printer settings, press the [RETURN] key to return to the UV-1800
mode menu screen.
8) Set the connected printer to the ON LINE state.
10) In the instrument’s Maintenance screen, select [1. Validation].
11) In the Validation menu screen, press the [F4] key (Settings).
12) When the settings screen is displayed, press the [1] key, to set [1. Auto print] to “ON”.
13) Press the [3] key to set [3. Print init. status ] to “ON”.
14) Press the [RETURN] key to return to the Validation menu screen.
Rev 3. 10 Page 35 of 120

(2) Test Conditions Setting Procedure

No. Setting Outline
Test 3 To check the accuracy of the displayed wavelength value, set it so that the D2 emission lines
656.1nm and 486.0nm are used, and enter the pass criteria value (standard value).
Test 4 Enter the pass criteria value (standard value) for the wavelength setting repeatability.
photometric value accuracy, and set the measurement conditions.
photometric repeatability, and set the measurement conditions.
Test 7 Set the measurement range for checking the baseline flatness, and enter the pass criteria value
(standard value).
(Criteria)
Test 1: The version number matches the controlled version number.
Test 2: Each item of the initial settings is completed as “OK”.
Test 3:
Instrument specifications Measurement deviation of D2 emission lines 656.1nm is
within ±0.1nm.
Measurement deviation of D2 emission lines 486.0nm is
within ±0.3nm.
Pharmacopoeia Measurement deviation of D2 emission lines 656.1nm
and 486.0nm is within ±0.3nm.
Test 4 :
Instrument specifications …. Deviation from average of 3 values is within ±0.1nm
Pharmacopoeia …. Deviation from average of 3 values is within ±0.2nm
Test 5:
Absorbance near 1Abs : Deviation from reference value is within ±0.004 Abs
Absorbance near 0.5Abs: Deviation from reference value is within ±0.002 Abs
NIST-traceable visible region filter, or a semi-standard optical filter whose value is
calibrated to a NIST filter.
Pharmacopoeia….Deviation from standard value is within ±0.008 Abs
Test 6:
Pharmacopoeia
Test 7: Baseline flatness is within ±0.0010 Abs
* For the measurement methods and pass criteria values in Tests 3 - 11, refer to Additional
Information from page 41.
Page 36 of 120 Rev 3. 10

<Semi-auto items setting>
15) In the Validation Function Settings screen, press the [1] key (Semi-auto Items).

16) In the Semi-auto items setting menu screen, press the [1] key (Photometric accuracy).
17) The standard filter selection screen is displayed.
Here, enter the 30% ND filter for [1. Standard filter 1] and the 10% ND filter for [2.
Standard filter 2], and enter the test conditions.
18) In the standard filter selection screen, select the [1] key (Standard filter 1).
19) In the Standard filter 1 test setting conditions screen, set the conditions as follows.
1. Inspection : Yes
2. Meas. Mode : Abs
3. Standard values
Measurement wavelength : 635.0/ 590.0/ 546.1/ 456.0/ 440.0 (nm)
Test value (Absorbance specified in test result document using 30% ND
filter)
4. Serial number : (Serial number of 30% ND filter)
5. Good THRU : (Expiration date of 30% ND filter)
6. Tolerance : (Test 5: Criteria value for absorbance near 0.5 Abs)
20) Press the [RETURN] key to return to the standard filter selection screen.
1. Inspection : Yes
2. Meas. Mode : Abs
3. Standard values
Measurement wavelength : 635.0/ 590.0/ 546.1/ 456.0/ 440.0 (nm)
Test value (Absorbance specified in test result document using 10% ND
filter)
24) Verify that [1. Standard filter 1] and [2. Standard filter 2] only are highlighted (Test
execution).
Rev 3. 10 Page 37 of 120


26) In the Semi-auto items setting menu screen, press the [2] key (Photometric repeatability).
27) The standard filter selection screen is displayed.
Here, enter the 30% ND filter for [1. Standard filter 1] and the 10% ND filter for [2.
Standard filter 2], and enter the test conditions.
1. Inspection : Yes
2. Meas. Mode : Abs
3. Wavelength : 635.0 (nm)
1. Inspection : Yes
2. Meas. Mode : Abs
3. Wavelength : 635.0 (nm)
34) Verify that [1. Standard filter 1] and [2. Standard filter 2] only are highlighted (Test
execution).
36) Verify that [1. Photometric accuracy] and [2. Photometric repeatability] only are highlighted
(Test execution).
37) Press the [RETURN] key to return to the Validation function settings screen.
< Full-automatic Test Conditions Setting >

(Procedure) 38) In the Validation Function Settings screen, press the [2] key (Full-auto Items).

accuracy D2).
40) In the Wavelength Accuracy D2 conditions setting screen, set the conditions as follows.
1. Inspection : Yes
2. Wavelength : 656.1 nm, 486.0 nm
3. Tolerance 656.1: (Test 3: Criteria value for 656.1 nm)
4. Tolerance 486.0: (Test 3: Criteria value for 486.0 nm)
41) Press the [RETURN] key to return to the Full-automatic test conditions setting menu screen.

repeatability D2).
43) In the Wavelength repeatability D2 conditions setting screen, set the conditions as follows.
1. Inspection : Yes
2. Tolerance : (Criteria value for Test 4)
Page 38 of 120 Rev 3. 10


45) In the Full-automatic test conditions setting menu screen, press the [2] key (Baseline
flatness).
46) In the Baseline flatness conditions setting screen, set the conditions as follows.
1. Inspection : Yes
2. Scan range : 1100 - 190 nm
3. Tolerance : (Criteria value for Test 7)
Rev 3. 10 Page 39 of 120

(3) Test Procedure

When using the validation functions, the tests proceed in order from <Semi-auto test items> -> <Full-auto test
items>.

< Test 5 Photometric accuracy >
48) In the Validation menu screen, verify that the following items are highlighted, indicating
that they are set for inspection.
49) Install the CPS-240A in the UV-1800 sample compartment, and set the temperature
document.
50) Set the ND optical filter into the CPS-240A cell holder.
Cell holder 1 : None
* To stabilize the ND optical filter temperature, keep the sample compartment lid closed for at least 10
minutes before starting the measurements.
51) After verifying that the CPS-240A cell position is “Cell 1” (Controller “CELL POSITION”
“1” LED is illuminated), press the [START/STOP] key to start the validation operation.
52) Check that there is nothing in the sample compartment, and press the [START/STOP] key.
The semi-automatic test [1. Photometric Accuracy] starts, and baseline correction is
performed. When a message appears on the screen requesting that the ND filter be set in
place, using the CPS-240A controller (press the [STEP] button), set the cell position to
“Cell 2”. Press the [START/STOP] key to perform measurement of the 30% ND filter.
53) Check that there is nothing in the sample compartment, and press the [START/STOP] key,
then the baseline correction is performed. When a message appears on the screen requesting
that the ND filter be set in place, using the CPS-240A controller (press the [STEP] button),
set the cell position to “Cell 3”. Press the [START/STOP] key to perform measurement of
the 10% ND filter.
54) When the [1. Photometric Accuracy] measurement is completed, the measurement and
< Test 6 Photometric repeatability >

55) The [2. Photometric Repeatability] test starts, and a message appears requesting
confirmation that there is nothing in the sample compartment. Remove the CPS-240A and
replace it with the standard sample compartment. Press the [START/STOP] key to start the
auto zero operation.
56) Following the on-screen messages, repeat the indicated photometric measurements while
removing and inserting the filters.
57) When the [2. Photometric Repeatability] measurement is completed, the measurement and
< Test 3, 4, 7 >

58) The full-automatic test [2. Baseline flatness] starts, and following the message that appears
on the screen, check that there is nothing in the sample compartment, and press the
[START/STOP] key.
59) When the full-automatic tests are completed, the measurement results and Pass/Fail
judgment results are printed out for each of the tests, and the display returns to the
Validation screen.
60) In case of the wavelength accuracy using D2 light beam, the test starts automatically.
Attach the measurement results for each of the test items to this document.
Page 40 of 120 Rev 3. 10

<Additional Information>
· About Displayed Wavelength Value Accuracy, and Wavelength Setting Repeatability
The pass criteria and procedures used for the displayed wavelength value accuracy and
wavelength setting repeatability inspections of Test 3 and Test 4, respectively, are derived from
the Japanese Pharmacopoeia Fifteenth Edition.
After pre-adjusting the spectrophotometer, confirm that the wavelength and transmittance comply with
the following tests.
Using optical filters, the wavelength is within ... Testing can be conducted using a low-pressure
mercury lamp ... or deuterium discharge tube 486.00 nm and 656.10 nm emission lines. The
measured wavelength and emission line wavelength shall differ by no more than ±0.3 nm. When
conducting three measurements, all measured values shall be within ± 0.2 nm of the average value.
Rev 3. 10 Page 41 of 120

· Photometric accuracy check

The display of the photometric accuracy is defined in the JIS standards, as follows:
Pharmacopoeia:
(Explanation)
below.
Example: For a 30% ND optical filter with reference value and guaranteed accuracy as follows:
Wavelength (nm) 440 465 546.1 590 635

Transmittance (%) 23.92 29.17 29.91 27.99 28.50
Absorption (Abs) : 0.621 0.535 0.524 0.553 0.545
transmittance)
added to the guaranteed accuracy upper and lower limits), such that the transmittance tolerance at
440 nm is:
23.92 x (2/100) ≈ 0.48
absorbance using absorbance = log10 (100/transmittance), gives an absorbance tolerance range of
0.613 to 0.630 Abs.
follows:
Converting this to absorbance gives 0.514 to 0.532 (0.523 ± 0.009). However, due to the rounding
errors during conversion, a pass criterion of (reference value ± 0.008 Abs) is adopted for the
photometric accuracy near 0.5 Abs.
Similarly, as the tolerance range is 0.991 to 1.009 Abs at 10% transmittance, a pass criterion of
(reference value ± 0.008 Abs) is adopted.
Page 42 of 120 Rev 3. 10


JIS K0115 Rules for absorbance analysis
(f) Photometric repeatability
The number of measurements and the measurement method for Test 6 conforms with the 15th
Japanese Pharmacopoeia:
When testing is conducted under the test conditions in the test report attached to each filter in order
to read the transmittance at the reference wavelength value indicated in the test report, the
measured transmittance values converted to absorbance values) shall lie within ±0.002 of the
average value for absorbance up to 0.500 and ±0.004 for absorbance over 0.500.
· Test method and evaluation criteria for baseline flatness

3.7 Baseline flatness
(3) Test method
With the sample compartment empty, set the absorbance to zero (or 100%T transmittance). Scan
the wavelengths across the guaranteed wavelength range and record the absorbance (or
In the UV-1800, from the viewpoint of noise exclusion, the measured baseline is subjected to
smoothing, and the absorbance difference with the 0 Abs line is set as the baseline curvature
(flatness).
Rev 3. 10 Page 43 of 120

Operational Qualification UV-1601PC/1650 Protocol
4-2-3 UV-1601PC/UV-1650 UV-VIS Spectrophotometer
1. Introduction
Ultraviolet-Visible Spectrophotometer UV-1601PC/UV-1650 (main unit).
Refer to the Instruction Manual for details about the operation procedure and to clarify uncertain points.
Test 1
(Item) Firmware version check
(Outline) Checks the program version.
(Procedure) Follow the procedure below.

Refer to the UVProbe Instruction Manual (Tutorial) for details about these operations.
2) Start the UVProbe software and select the Spectrum module.
3) Click the [Connect] button to start spectrophotometer control.
4) The spectrophotometer initial setup screen is displayed. Automatic setting and diagnosis
starts for each item in sequence.
5) The checksum value for the program is displayed at the top-left of the initial setup screen.
6) Enter this value in the results checksum value box below. Enter the corresponding version
from the table of checksum values and versions in Additional Information below.
(Criteria) Version number matches the version number on record.
<Additional · Relationship between the firmware version and checksum value

Information>
The checksum value for the UV-1601PC/UV-1600 UV-VIS Spectrophotometer firmware
appears at the top-left of the screen displayed during instrument setup. The relationship
between the checksum values and versions is listed below.
Checksum value Version
RevA(** **)
0E D3 : Ver 1.70
C8 0A : Ver 1.81
DE E6 : Ver 1.83
1E E6 : Ver 1.84
E4 CE : Ver 2.20
E4 5E : Ver 2.30
AF A7 : Ver 2.40
5A 7B : Ver 2.60
Page 44 of 120 Rev 3. 10

Test 2
(Item) Initial setup check
(Outline) Checks that the instrument initial setup was completed correctly.


5) Click the [OK] button when all initial setup is completed and then close the initial setup
screen.
* The O mark by each item changes color when the initial setup and diagnosis is complete. Green
indicates normal; red indicates abnormal.
6) Display the unit history in the output window on the UVProbe screen.
* The initial setup items are displayed in this window in a different order from the setting and
diagnosis procedure.
7) The initial setup information appears in the output window. Select all this information and
copy it to the Clipboard.
8) Paste and print the initial setup information using the Report Generator or another
software application.
(Criteria) All initial setup items ended as “Pass.”
Rev 3. 10 Page 45 of 120

Test 3
(Item) Wavelength accuracy check
(Outline) Uses the emission-line wavelengths (486.0, 656.1 nm) of the internal D2 lamp to check the
accuracy of the displayed wavelengths.

1) Check that the spectrophotometer initial setup is completed normally.

2) Select the UVProbe Spectrum module.
[Measurement at D2 lamp 656.1 nm emission line]

3) Select [Method] from the [Edit] menu.
4) Set the following parameters
[Measurement]
Wavelength range : 650 nm to 660 nm
Scan speed : Medium
Autosampling pitch : Check mark
[Unit parameters]
Photometry type : Energy
Light source : D2
PM GAIN :3
* During measurement in the Energy mode, the instrument detector gain (PM gain) must be set to match
the lamp energy intensity. Here, the PM gain is set to 3. However, the peak height may vary between
individual lamps and due to the time the lamp has been used. Change the PM gain setting if the peak
cannot be detected due to the peak being too high or too low.
5) Click the [OK] button to complete the measurement method settings.

6) Click the [Start] button to start the measurement.
7) When the measurement is complete, enter the file name and click [OK].
* The data is still unsaved at this time (it exists in the computer memory only). To save this data to disk
using the input file name, select [Save] from the [File] menu. To change the file name, select [Save
As] from the [File] menu.

8) Change the wavelength range to 480 nm to 490 nm in the measurement method and
repeat steps 5) to 7).
9) Select [Peak Pick] from the [Operations] menu to detect the peaks in the D2 lamp 486.0
nm and 656.1 nm emission line spectra measured at steps 7) and 8).
10) Print the measurement results (peak detect table) and check the accuracies of the
wavelengths.
(Criteria) At D2 lamp 486.0 nm and 656.1 nm emission lines, measurement error ≤ ± 0.3 nm
Page 46 of 120 Rev 3. 10

Test 4
(Item) Wavelength setting repeatability check
(Outline) Measures the wavelength of the D2 lamp emission lines three times each and then compares
the average value against each measured value to check the repeatability of the wavelength
setting.


3) Repeat the measurement in Test 3 three times and detect the peak value in each spectrum.
4) Print the peak detect tables and then check the repeatability using each measured peak
value and the average value.
(Criteria) Instrument specification: Deviation from average of three measurements ≤ ± 0.1 nm

Pharmacopoeia: Deviation from average of three measurements ≤ ± 0.2 nm
<Additional Information> (Measurement Methods and Pass Criteria)
The pass criteria (Pharmacopoeia) for the wavelength accuracy check and the pass criteria
and measurement methods for the wavelength setting repeatability check (Test 3 and Test
4) are prescribed in the 15th Japanese Pharmacopoeia.
After pre-adjusting the spectrophotometer, confirm that the wavelength and transmittance
comply with the following tests.
Using optical filters, the wavelength is within ... Testing can be conducted using a
low-pressure mercury lamp ... or deuterium discharge tube 486.00 nm and 656.10 nm
emission lines. The measured wavelength and emission line wavelength shall differ by no
more than ±0.3 nm. When conducting three measurements, all measured values shall be
within ±0.2 nm of the average value.
Rev 3. 10 Page 47 of 120

Test 5
(Item) Photometric accuracy check
(Outline) Uses filter for transmittance calibration to check the photometric accuracy.


2) Install the CPS-240A in the spectrophotometer sample compartment, and set the
document.
3) Mount the filter for transmittance calibration indicated below into the CPS-240A cell
holder:
Cell 1 : None
Cell 2 over : Filter for transmittance calibration
* To allow the ND optical filter temperature to stabilize, leave the sample compartment door closed for
about 10 minutes.
4) Select the photometric module and open the measurement method.
5) Click the [Wavelengths] tab and set the following parameters:
Measurement method : Point
Data acquisition method : Instrument
6) For the measurement wavelengths, registered the wavelengths specified in the optical
filter test results document.
7) Set the other parameters, as follows:
[Calibration]
Calibration curve method : Photometric measurement
[Instrument parameters]
Photometry type : Absorbance or transmittance (According to pass
criteria)
Slit width (nm) : (Slit width used in optical filter test results document)
8) Click the [Attachments] tab, set the following parameters, and click the [Initialize] button:
Attachments : CPS
Number of cells : (1 + number of set filters)
* The operations above are necessary for the UVProbe software to recognize that the CPS-240A
accessory is connected. The CPS-240A does not operate when the [Initialize] button is clicked.
9) Click the [Close] button to close the measurement method.

10) Enter the sample names in the [Sample ID] column of the sample table.
(For example, line 1: blank; line 2: 10%filterA; line 3: 30%filterA)
11) Select [Blank Subtraction] from the [Operations] menu to add Cell 1 of the cell positioner
to the blank setting list.
12) Click the [Baseline] button to conduct baseline compensation over a range including all of
the measurement wavelengths.
13) Click the [Read Unk] button to start the measurement.
14) Print the measurement results (sample table) and check the photometric accuracy.
(Criteria) Instrument specification

Absorbance near 1 Abs: Deviation from reference value ≤ ± 0.004 Abs
Absorbance near 0.5 Abs: Deviation from reference value ≤ ± 0.002 Abs
Note) The instrument specification applies only to specifications determined with a
NIST-traceable visible region filter.
Pharmacopoeia
Deviation from reference value ≤ ± 0.008 Abs
Page 48 of 120 Rev 3. 10


Pharmacopoeia:
(Explanation)
below.
Example: For a 30% ND optical filter with reference value and guaranteed accuracy as
follows:
Wavelength (nm) 440 465 546.1 590 635

Transmittance (%) 23.92 29.17 29.91 27.99 28.50
Absorption (Abs) : 0.621 0.535 0.524 0.553 0.545
transmittance)
added to the guaranteed accuracy upper and lower limits), such that the transmittance
tolerance at 440 nm is:
23.92 x (2/100) ≈ 0.48
absorbance using absorbance = log10 (100/transmittance), gives an absorbance tolerance
range of 0.613 to 0.630 Abs.
follows:
Converting this to absorbance gives 0.514 to 0.532 (0.523 ± 0.009). However, due to the
rounding errors during conversion, a pass criterion of (reference value ± 0.008 Abs) is adopted
for the photometric accuracy near 0.5 Abs.
Similarly, as the tolerance range is 0.991 to 1.009 Abs at 10% transmittance, a pass criterion
of (reference value ± 0.008 Abs) is adopted.
Rev 3. 10 Page 49 of 120

Test 6
(Item) Photometric repeatability check
(Outline) Uses filter for transmittance calibration to check the photometric accuracy over three repeated
measurements.


4) Register 635 nm as the measurement wavelength.

[Calibration]
Photometry type : Absorbance
Slit width (nm) : (Slit width used in optical filter test results
document)
[Attachments]
Attachments : None
- Repeatability Measurement at Absorbance near 1.0 Abs -

7) Enter the sample names (6 lines) in the Sample ID column of the sample table
(For example, line 1: 10%Rep1; line 2: 10%Rep2; … line 6: 30%Rep3)
8) Verify that the standard sample compartment is set and that the cell holder is empty. Click
the [Baseline] button to conduct baseline compensation over a range including all of the
9) Set a transmittance optical filter having an absorbance near 1.0Abs in the
spectrophotometer sample compartment.
11) Remove the optical filter from the spectrophotometer sample compartment.
12) Repeat steps 9) to 12) two more times (making a total of three measurements).

(For example, line 4: 30%A_REP1; line 5: 30%A_Rep2; line 6: 30%A_Rep3)
14) Verify that the cell holder is empty, and click the [Baseline] button to conduct baseline
compensation over a range including all of the measurement wavelengths.
19) Print the measurement results (sample table) and check the photometric repeatability.

Absorbance near 1 Abs: Deviation from average of three measurements ≤ ±0.002 Abs
Absorbance near 0.5 Abs: Deviation from average of three measurements ≤ ±0.001 Abs
Pharmacopoeia
Page 50 of 120 Rev 3. 10


(f) Photometric repeatability check
The number of measurements and the measurement method for Test 6 conforms with the
15th Japanese Pharmacopoeia:
measured transmittance values converted to absorbance values) shall lie within ±0.002 of
the average value for absorbance up to 0.500 and ±0.004 for absorbance over 0.500.
Rev 3. 10 Page 51 of 120

Test 7
(Item) Baseline flatness check
(Outline) Checks the baseline flatness in the range from 190 nm to 1100 nm.


4) Set the following parameters as follows.
[Measurement]
Wavelength Range : 190 nm to 1100 nm
Scan Speed : Slow
Autosampling Interval : ON (Check mark)
[Unit parameters] 1

6) Click the [Baseline] button to conduct baseline compensation in the 190 nm to 1100 nm
range.
7) Click the [Go TO WL] button and set the wavelength to 750 nm.
8) Click the [Auto Zero] button to autozero.
* The data is still unsaved at this time (it exists in the computer memory only). To save this data to
disk using the input file name, select [Save] from the [File] menu. To change the file name, select
[Save As] from the [File] menu.
11) Print the measurement results. Check the maximum and minimum values, using the
central value of the noise level (excluding shock noise due to light-source or filter
switching) as the baseline absorbance.
(Criteria) Baseline max. value & min. value ≤ ± 0.002 Abs
<Additional · Test method and evaluation criteria for baseline flatness

Information>
3.7 Baseline flatness check (Baseline flatness)
(3) Test method
With the sample compartment empty, set the absorbance to zero (or 100%T transmittance).
Scan the wavelengths across the guaranteed wavelength range and record the absorbance (or
For a Shimadzu UV-VIS Spectrophotometer, from the viewpoint of noise elimination, the
switching) is defined as the baseline absorbance and the maximum and minimum values
define the baseline deflection.
Page 52 of 120 Rev 3. 10

1. Introduction
Test 1



Information> The checksum value for the UV-2401PC/UV-2450 UV-VIS Spectrophotometer firmware

RevA(** **)
13 00 ; Ver 1.00
E0 00 ; Ver 1.10
BE 00 ; Ver 1.30
0F 00 ; Ver 1.40
30 00 ; Ver 2.00
4F 00 ; Ver 2.20
1F 00 ; Ver 2.30
67 00 ; Ver 2.40
BB 00 ; Ver 2.50
FD 00 ; Ver 2.60
Rev 3.10 Page 53 of 120

Test 2


screen.
* The ○ mark by each item changes color when the initial setup screen and diagnosis is complete.
Green indicates normal; red indicates abnormal.
* The initial setup screen items are displayed in this window in a different order from the setting and
7) The initial setup screen information appears in the output window. Select all this
information and copy it to the Clipboard.
Page 54 of 120 Rev 3. 10

Test 3
(Procedure)
Follow the procedure below.


[Measurement]
Scan speed : Medium
Autosampling Interval : Check mark
[Unit parameters]
Slit width : 0.2 nm
Light source : D2
PM GAIN :3
* During measurement in the Energy mode, the instrument detector gain (PM gain) must be set to
match the lamp energy intensity. Here, the PM gain is set to 3. However, the peak height may vary
between individual lamps and due to the time the lamp has been used. Change the PM gain setting
if the peak cannot be detected due to the peak being too high or too low.


10) Print the measurement results (peak detect table) and check the accuracy of the
wavelengths.
Rev 3. 10 Page 55 of 120

Test 4
setting.


4) Print the three peak detect tables and then check the repeatability using each measured
peak value and the average value.


Page 56 of 120 Rev 3. 10

Test 5


document.
holder:
Cell 1 : None
about 10 minutes.
Measurement method: Point
Data acquisition method: Instrument
6) For the measurement wavelengths, register the wavelengths specified in the optical filter
test results document.
[Calibration]
Photometry type: Absorbance or transmittance (According to pass criteria)
Attachments: CPS
Number of cells: (1 + number of set filters)


Note) The instrument specifications apply only to specifications determined with a NIST-traceable
visible region filter, or an optical filter whose value is calibrated to a NIST filter.
Pharmacopoeia
Rev 3. 10 Page 57 of 120


Pharmacopoeia:
(Explanation)
below.
follows:
Wavelength (nm) 440 465 546.1 590 635

Transmittance (%) 23.92 29.17 29.91 27.99 28.50
Absorption (Abs) : 0.621 0.535 0.524 0.553 0.545
transmittance)
23.92 x (2/100) ≈ 0.48
follows:
Page 58 of 120 Rev 3. 10

Test 6
measurements.



[Calibration]
Calibration curve method: Photometric measurement
Photometry type: Absorbance
[Attachments]
Attachments: None



Pharmacopoeia
Rev 3. 10 Page 59 of 120


Page 60 of 120 Rev 3. 10

Test 7


[Measurement]
Scan Speed : Slow
[Unit parameters] 1
Slit width (nm) : 2.0

range.

Information>
(3) Test method
Rev 3. 10 Page 61 of 120

1. Introduction
Test 1



Information> The checksum value for the UV-2501PC/UV-2550 UV-VIS Spectrophotometer firmware
RevA(** **)
13 00 ; Ver 1.00
E0 00 ; Ver 1.10
BE 00 ; Ver 1.30
0F 00 ; Ver 1.40
30 00 ; Ver 2.00
4F 00 ; Ver 2.20
1F 00 ; Ver 2.30
67 00 ; Ver 2.40
BB 00 ; Ver 2.50
FD 00 ; Ver 2.60
Page 62 of 120 Rev 3. 10

Test 2


screen.
Rev 3. 10 Page 63 of 120

Test 3
(Procedure)


[Measurement]
Scan speed : Medium
Autosampling Interval : Check mark
[Unit parameters]
Slit width : 0.2 nm
Light source : D2
PM GAIN :3
* During measurement in the Energy mode, the instrument detector gain (PM gain) must be set to
match the lamp energy intensity. Here, the PM gain is set to 3. However, the peak height may vary
between individual lamps and due to the time the lamp has been used. Change the PM gain setting
if the peak cannot be detected due to the peak being too high or too low.


wavelengths.
Page 64 of 120 Rev 3. 10

Test 4
setting.




Rev 3. 10 Page 65 of 120

Test 5


document.
holder:
Cell 1 : None
Cell 2or later : Filter for transmittance calibration
about 10 minutes.
[Calibration]
Slit width (nm): (Slit width used in optical filter test results document)
Attachments: CPS
Number of cells: (1 + number of set filters)


NIST-traceable visible region filter, or an optical filter whose value is calibrated to a
NIST filter.
Pharmacopoeia
Page 66 of 120 Rev 3. 10


Pharmacopoeia:
(Explanation)
below.
follows:
Wavelength (nm) 440 465 546.1 590 635

Transmittance (%) 23.92 29.17 29.91 27.99 28.50
Absorption (Abs) : 0.621 0.535 0.524 0.553 0.545
transmittance)
23.92 x (2/100) ≈ 0.48
follows:
Rev 3. 10 Page 67 of 120

Test 6
measurements.



[Calibration]
Photometry type: Absorbance
[Attachments]
Attachments: None

7) Enter the sample names (6 lines) in the Sample ID column of the sample table.


Pharmacopoeia
Page 68 of 120 Rev 3. 10


Rev 3. 10 Page 69 of 120

Test 7


4) Set the following parameters as follows
[Measurement]
Scan Speed : Slow
[Unit parameters]

range.

Information>
(3) Test method
Page 70 of 120 Rev 3. 10

1. Introduction
Ultraviolet-Visible Spectrophotometer UV-3600.
Test 1


5) Close the initial setup screen, click [Configure] in the [Instrument] menu and select the
[Maintenance] tab.
6) Record and confirm the Firmware Version displayed in this tab.
Rev 3. 10 Page 71 of 120

Test 2


screen.
Page 72 of 120 Rev 3. 10

Test 3


3) Confirm that at least 2 hours have elapsed since the instrument has been switched ON.
Select [Instrument] / [Configure], and in the [Initialize] tab, click [Perform] to execute the
[System Initialization] (standard initialization).
[Measurement]
Wavelength range: (6nm width with standard measurement wavelength
approximately centered)
Scan speed: Medium
Autosampling Interval: (UV/VIS area: 0.01nm, NIR area: 0.05nm)
[Unit parameters]
Photometry type: Energy
Slit width: (UV/VIS area: 0.2nm, NIR area: 2nm)
Light source: D2
Detector lock: PM
* At wavelengths greater than 800nm, it is necessary to remove the stray light cut-off filter from
the optical path in the monochromator before conducting measurement. This setting is
performed by placing a check mark in the [Filter Lock (No Filter)] check box in the
[Maintenance] tab, accessed after selecting [Configure] in the UVProbe [Instrument] menu.
* During measurement in the Energy mode, the instrument detector gain (PM gain) must be set
to match the lamp energy intensity. Here, the PM gain is set to 3. However, the peak height
may vary between individual lamps and due to the time the lamp has been used. Change the
PM gain setting if the peak cannot be detected due to the peak being too high or too low.

wavelengths.
UV/VIS Area NIR Area

Standard Wavelength Standard Wavelength
486.0 nm 972.0 nm
656.1 nm 1312.2 nm
1458.0 nm
1968.3 nm
2624.4 nm
(Criteria) UV/VIS area : Standard wavelength within ±0.2nm

NIR area : Standard wavelength within ±0.8nm
Rev 3. 10 Page 73 of 120

Test 4
setting.


3) Repeat the measurement in Test 3 three times (only for standard wavelengths listed below)
and detect the peak value in each spectrum.
UV/VIS Area NIR Area

Standard Wavelength Standard Wavelength
486.0 nm 1312.2 nm
656.1 nm
(Criteria) UV/VIS area - Deviation from average of three measurements ≤ ± 0.08 nm

NIR area - Deviation from average of three measurements≤ ± 0.32 nm
Page 74 of 120 Rev 3. 10

Test 5


document.
holder:
Cell 1 : None
about 10 minutes.
[Calibration]
Time constant (sec) : 1.0
Attachments : CPS
Number of cells : (1 + number of set filters)


NIST-traceable visible region filter, or an optical filter whose value is calibrated to a
NIST filter.
Pharmacopoeia
Rev 3. 10 Page 75 of 120


Pharmacopoeia:
(Explanation)
below.
follows:
Wavelength (nm) 440 465 546.1 590 635

Transmittance (%) 23.92 29.17 29.91 27.99 28.50
Absorption (Abs) : 0.621 0.535 0.524 0.553 0.545
transmittance)
23.92 x (2/100) ≈ 0.48
follows:
Page 76 of 120 Rev 3. 10

Test 6
measurements.



[Calibration]
Slit width (nm) : (Slit width used in optical filter test results
document)
[Attachments]
Attachments: None

7) Enter the sample names in the Sample ID column of the sample table.

13) Enter the sample names in the Sample ID column of the sample table.

Absorbance near 1 Abs: Deviation from average of three measurements ≤ ± 0.0016 Abs
Pharmacopoeia
Rev 3. 10 Page 77 of 120


Page 78 of 120 Rev 3. 10

Test 7


[Measurement]
Scan Speed : Middle
Autosampling Interval : 1 nm
[Unit parameters]

6) Confirm that at least 2 hours have elapsed since the instrument has been switched ON,
and then perform baseline compensation.
9) Click the [Start] button to start the measurement
11) To eliminate fluctuations such as noise in the above measurement results, perform
smoothing using the parameters displayed below.
12) Print out the measurement results, record the maximum and minimum values of the
processed peaks, and verify that the respective values are within the criteria standard.
Wavelength Range Smoothing

185 nm to 200 nm Delta Lambda 10
(Criteria) Specifications at Installation

Baseline max. value & min. value ≤ ±0.004 Abs (185 nm to 200 nm)
≤ ± 0.001 Abs (200 nm to 3000 nm)
≤ ±0.005 Abs (3000 nm to 3300 nm)
Specifications at Inspection
Baseline max. value & min. value ≤ ±0.008 Abs (185 nm to 200 nm)
≤ ±0.002 Abs (200 nm to 3000 nm)
≤ ±0.01 Abs (3000 nm to 3300 nm)
Rev 3. 10 Page 79 of 120


Information>
(3) Test method
Page 80 of 120 Rev 3. 10

Operational Qualification Syringe Sipper N/CN Protocol
4-3 Syringe Sipper N/CN
1. Introduction
This section presents the standard operating procedure (SOP) for Operational Qualification of the Syringe
Sipper N/CN. Tests 1 to 4 are conducted for an N-type syringe sipper; tests 1 to 5 are conducted for a CN-type
syringe sipper. However, Test 4 (Carry-over check) applies only to units using a flow-through cell recommended
for a Shimadzu syringe sipper. In addition, no pass criterion applies to Test 5; the measured value is noted as a
verification item. Refer to the Instruction Manual for details about the operation procedure and to clarify
uncertain points.
Test 1
(Item) Initial operation check
(Outline) Checks that the syringe pump unit initial operation is correct.
(Procedure) If UVProbe is not used with the UV-1700, perform the test using the following
procedure.
For details on operation, refer to the UV-1700 Spectrophotometer instruction manual
(Operation Guide) and the syringe sipper instruction manual.
2) Select [1. Photometric] from the Mode selection screen.
3) Press the [F2] key (Sample Control).
4) Select the Syringe Sipper as an accessory, and when the [F1] key (Initial) is pressed,
verify that the syringe sipper initialization operation is conducted.
If UVProbe is used for instrument control, perform the test using the following
procedure.
Refer to the Syringe Sipper Instruction Manual and UVProbe Instruction Manual (Tutorial)
for details about these operations.
1) Check that the system is running.

2) Select the syringe sipper as an accessory in the UVProbe software. Check that the syringe
sipper conducts its initialization movements when the [Reset] button on the Method
Setting screen is clicked.
(Criteria) Initial movements complete normally.
Rev 3. 10 Page 81 of 120

Test 2 & 3
(Item) Test 2: Intake volume accuracy check
Test 3: Intake volume repeatability check
(Outline) Test 2: Conducts three intake operations on distilled water in a beaker and determines the
actual intake volume by weighing the beaker before and after.
Test 3: Conduct three intake operations on distilled water in a beaker. Determine the intake
repeatability from the discrepancy with the average intake volume.
procedure.
1) Prepare the following devices and sample.
a) Container : beaker
b) Sample : distilled water
c) Balance : Calibrated balance capable of measurement to 0.001g

4) Select the Syringe Sipper as an accessory, and set the parameters as follows.
Pump speed : 0.6 mL/sec
Sip volume : 1.00 mL
Dwell time : 1.0 sec
Purge volume : 0.00 mL/sec
Sample recovery : waste
5) Press the [F1] key (Initial) to conduct the sipper initialization operation.
6) Fill the beaker half-way with distilled water, weigh the beaker and its contents and record
the weight.
7) Take the sipper nozzle that is installed in the spectrophotometer sample compartment, and
insert it into the distilled water in the beaker.
8) Press the [F4] key (Manual sip) to begin sipping the distilled water.
9) When the sipping operation is completed, weigh the beaker on the balance and record the
weight.
10) Repeat steps 7) – 9) three times, and confirm the sip volume accuracy.
11) Take the average value of the 3 sipping operation results, and determine the deviation of
each sipping value from the average value to verify the sip volume repeatability.
Page 82 of 120 Rev 3. 10

(Procedure) If UVProbe is used for instrument control, perform the test using the following
procedure.
Refer to the Syringe Sipper Instruction Manual and UVProbe Instruction Manual (Tutorial)
for details about these operations.
1) Provide the following items:

a) Container : Beaker
b) Sample : Distilled water
c) Electronic balance : A calibrated balance able to weigh down to 0.001g.

4) Select the syringe sipper as an accessory in the UVProbe software. Set the following
parameters;
Sip rate : 0.6 mL/sec
Sip volume : 1.00 mL
Dwell time : 2 sec
Sample Recovery : No check mark
5) Click the [Reset] button on the Method Setting screen to conduct the syringe sipper initial
operation.
6) Half fill the beaker with distilled water. Weigh the beaker on the electronic balance and
record the weight.
7) Insert the intake nozzle mounted to the spectrophotometer sample compartment into the
distilled water.
8) Click on the [Sip] button to take in distilled water.
9) After taking in the sample, weigh the beaker on the electronic balance again and record
the weight.
10) Repeat steps 7) to 9) three times to determine the intake volume accuracy.
11) Determine the average of the three measured results. Determine the deviation of each
measured value from the average value to confirm the intake volume repeatability.
(Criteria) Test 2: Deviation from set value ≤ ±0.10 mL

Test 3: Deviation from average of three measurements ≤ ±0.03 mL
Rev 3. 10 Page 83 of 120

Test 4
(Item) Carry-over check
(Outline) Checks the carry-over value using an aqueous solution of potassium dichromate.
procedure.
a) Container : 2 beakers
b) Sample : distilled water and potassium dichromate aqueous solution (diluted to
obtain absorbance near 0.5 Abs at 350 nm)

4) Press the [GOTO WL] key, and set the wavelength to 350 nm.
5) Press the [F1] key (T%/ABS) to select the absorbance mode (ABS).
6) Press the [F2] key (Sample Control), select the Syringe Sipper as an accessory, and set the
parameters as follows.
Pump speed : 0.6 mL/sec
Sip volume : Normally required sample volume (differs depending on flow cell)
Dwell time : 2.0 sec
No. of Rinses : 0 times
Sample recovery : waste
7) Press the [F1] key (Initial) to conduct the sipper initialization operation.
8) Press the [F4] key (Manual sip), sip distilled water from the sample compartment nozzle,
and press the [RETURN] key to return to the Measurement screen.
9) Press the [AUTO ZERO] key to perform the auto zero operation.
10) After measuring the distilled water 3 times, measure the potassium dichromate aqueous
solution 3 times.
11) Repeat step 10) two more times.
12) Print the measurement results, and check the carryover.
Page 84 of 120 Rev 3. 10

procedure.

a) Container : 2 beakers
b) Sample : Aqueous solution of potassium dichromate (diluted to achieve
approximately 0.5 Abs at 350 nm)

4) Set the following parameters and click the [Reset] button in the [Attachments] tab to start
syringe sipper initialization operation.
[Wavelength]
Register 350.0 nm as the measurement wavelength.
[Calibration]
Slit width : 2.0(nm)
[Attachments]
Attachments : Syringe sipper
Sip rate : 0.6 mL/sec
Sip volume : Standard required sample volume (differs according to
flow-through cell)
Dwell time : 2 sec
Rinses :0
Sample Recovery : No check mark
5) After the initialization operation is complete, click the [Sip] button to take distilled water
into the sample compartment intake nozzle. Click the [Close] button to close the
measurement method.
6) Click the [Go TO WL] button and set the wavelength to 350.0 nm.
8) Enter the numbers 1 to 18 in the Sample ID column to create an 18-line sample table.
9) Measure distilled water three times and then measure the potassium dichromate aqueous
solution three times.
10) Repeat step 9) two more times.
11) Print the measurement results (sample table) and check the carry-over value.
(Criteria) Carry over ≤ 1.0%
<Additional Preparation procedure for weakly acidic aqueous solution of potassium dichromate
Information> (1) Dilute 167 mg HClO4 (60%) in 1L distilled water to create a 0.001 mol/L (0.001N)
perchloric acid solution.
(2) Dissolve 47 mg potassium dichromate (K2Cr2O7) to the 0.001N perchloric acid solution
created at step (1) above to create 1L solution.
Rev 3. 10 Page 85 of 120

Test 5
(Item) Temperature control accuracy check
(Outline) Checks the difference between the circulating water and cell holder temperatures.
1) Set the water circulating device water temperature to 37°C.

2) Mount a semimicro cell filled with distilled water in the sample cell holder installed in the
3) Insert the temperature sensor approximately 2 cm into the distilled water in the cell.
4) After checking that the piping connections have been made between the water circulating
device and cell holder unit, start water circulation.
5) When the cell internal temperature deviation drops below ±1°C, read the temperature and
enter it in the sheet.
Page 86 of 120 Rev 3. 10

Operational Qualification ASC-5 Protocol
4-4 Automatic Sample Changer ASC-5
1. Introduction
This section presents the standard operating procedure (SOP) for Operational Qualification of the Automatic
Sample Changer ASC-5. Refer to the Instruction Manual for details about the operation procedure and to
Test 1 & 2
(Item) Test 1: Firmware version check
Test 2: Initial operation check
(Outline) Test 1: Checks the program version.
Test 2: Checks that the initial operation is correct.
Refer to the ASC-5 Instruction Manual for details about these operations.
1) Turn on the ASC-5.
2) The LEDs display the program checksum value (flashing). Record the checksum value
and use it to confirm the version number from the table in Additional Information below.
3) Confirm that the intake nozzle automatically returns to the home position and the ASC-5
reverts to its initial status (TEACHING and READY LEDs not lit).
(Criteria) Test 1: The program checksum value is displayed and matches the version number on
record.
Test 2: Initial movements complete normally with no error displayed.
Information>
The relationship between the ASC-5 firmware checksum values and version numbers is
listed below.
02A ; Ver 1.00
Rev 3. 10 Page 87 of 120

Operational Qualification ASC-5 Protocol
Test 3
(Item) Manual operation check
(Outline) Uses ASC-5 manual key operation to check that the intake nozzle moves smoothly in the X
and Y directions one pitch at a time.
(Procedure)
Refer to the ASC-5 Instruction Manual for details about these operations.
1) Turn on the ASC-5.
2) After the initial movements are complete, press the HOME key to set the ASC-5 into
ready status (READY LED lit).
3) Mount the standard test-tube rack (ASC-5 accessory) to the ASC-5 sample stage.
4) Insert standard test-tubes (ASC-5 accessory) into the four corners of the standard
test-tube rack.
5) Press the down-arrow key while holding down the [FILE] key and set “F-0” (File 0).
6) Press the [START/STOP] key while holding down the [FILE] key and load “F-0”.
7) Confirm that the intake nozzle is at the #1 test-tube position (X:1, Y:1).
8) Press the arrow keys repeatedly to move the intake nozzle one pitch at a time and check
that the nozzle moves to each test-tube position.
(Criteria) The intake nozzle moves smoothly to each test-tube position.
Page 88 of 120 Rev 3. 10

Operational Qualification DIS-1200 Protocol
4-5 Elution Test 6-Cell Holder DIS-1200
1. Introduction
This section presents the standard operating procedure (SOP) for Operational Qualification of the Elution Test
6-Cell Holder DIS-1200. Refer to the Instruction Manual for details about the operation procedure and to
Test 1 & 2
(Item) Test 1: Initial operation check
Test 2: Cell position check
(Outline) Test 1: Checks that the cell holder home position is correctly detected when the Initialize
command is used.
Test 2: Conduct three transmittance measurements at each cell position to verify that the
optical beam is not obstructed.
(Procedure) Perform the operations described in the procedure below.
For details on operation, refer to the DIS-1200 instruction manual and UV-1700 Instruction
Manual (Operation Guide).
1) Verify that the spectrophotometer initialization process is completed normally.

2) Check that the DIS-1200 is set in the spectrophotometer sample compartment.
4) Press the [GOTO WL] key, and set the wavelength to 550nm.
5) In the measurement conditions setting screen, press the [F2] key (Sample Control).
6) Select [1. Sample Module], and select “Standard (Multicell [6])” from the list of
displayed accessories.
7) Press the [F1] key (Initial), and verify that the DIS-1200 initialization operation is
performed and that cell holder 1 moves to the optical beam position.
8) Set the other parameters as follows.
2. Number of cells used :6
3. Reagent blank correction (cell 1) : None
4. Cell blank correction : None
9) Press the [RETURN] key to return to the measurement conditions setting screen.
10) Press the [AUTO ZERO] key to perform auto zero correction (100% correction).
11) Press the [START/STOP] key to start transmittance measurement of cell holders 1 – 6.
12) Repeat step 11) two more times, for a total of 3 measurements.
13) Print the measurement results, and verify that the values are within the standard value.
(Criteria) Test 1: Initialization causes cell holder 1 to move to the optical beam position.
Test 2: Transmittance at each cell position is 100.0 ±1.0%.
Rev 3. 10 Page 89 of 120

Operational Qualification DIS-8 Protocol
4-6 Elution Test 8-Cell Holder DIS-8
1. Introduction
This section presents the standard operating procedure (SOP) for Operational Qualification of the Elution Test
8-Cell Holder DIS-8. Refer to the Instruction Manual for details about the operation procedure and to clarify
uncertain points.
2. Inspection Outline
# (Item) (Outline)
1 Initial operation check Checks that the cell holder home position is correctly detected when
the Initialize command is used.
Test 1 & 2
(Outline) Test 1: Checks that the cell holder home position is correctly detected when the Initialize
command is used.
Test 2: Conduct three transmittance measurements at each cell position to verify that the
optical beam is not obstructed.
For details on operation, refer to the DIS-8 instruction manual and UV-1700 Instruction
Manual (Operation Guide).
1) Verify that the spectrophotometer initialization process is completed normally.

2) Check that the DIS-8 is set in the spectrophotometer sample compartment.
4) Press the [GOTO WL] key, and set the wavelength to 550nm.
5) In the measurement conditions setting screen, press the [F2] key (Sample Control).
6) Select [1. Sample Module], and select “Standard (Microcell [8])” from the list of
displayed accessories.
7) Press the [F1] key (Initial), and verify that the DIS-8 initialization operation is performed
and that cell holder 1 moves to the optical beam position.
13) Print the measurement results, and verify that the values are within the standard value.
(Criteria) Test 1: Initialization causes cell holder 1 to move to the optical beam position.
Test 2: Transmittance at each cell position is 100.0 ±1.0%.
Page 90 of 120 Rev 3.10

Operational Qualification CPS-240A/B Protocol
4-7 Cell Positioner CPS-240A/B
1. Introduction
This section presents the standard operating procedure (SOP) for Operational Qualification of the Cell
positioner CPS-240A/B. Refer to the Instruction Manual for details about the operation procedure and to clarify
uncertain points.
# (Item) (Outline)
1 Initial operation check Checks that the cell holder home position is correctly detected when
the power is turned on.
2 Cell position check Conducts three transmittance measurements at each cell position to
confirm that the optical beam is not interrupted by thermal insulation,
etc.
3 Temperature accuracy check Checks the cell holder base temperature accuracy with respect to the
set temperature.
Rev 3. 10 Page 91 of 120

Test 1 & 2
(Outline) Test 1: Confirms that the cell holder home position is correctly detected when the power is
turned on.
Test 2: Conducts three transmittance measurements at each cell position to confirm that the
optical beam is not interrupted by thermal insulation, etc.
procedure.
For details on operation, etc., refer to the UV-1700 instruction manual (Operation Guide).
1) Verify that the UV-1700 initialization process is completed normally.

2) Verify that the CPS-240A (or CPS-240B) is set in the UV-1700 sample compartment, and
that the wiring and other installation items are completed.
4) In the measurement conditions setting screen, press the [F1] key (T%/ABS) to select the
transmittance mode.
5) Press the [GOTO WL] key, and set the wavelength to 550 nm.
6) Verify that when the controller is turned on, cell holder 1 moves to the optical beam
position.
7) Press the [F2] key (Sample Control).
8) Press [1. Sample Module], and select “CPS-240” from the displayed accessories
9) Press the [F1] key (Initial), and verify that the UV-1700 recognizes that the CPS-240 is
connected as an accessory.
* The operations above are required in order for the CPS-240A/B to be recognized as an accessory. Even
if the [Initial] button is clicked, the CPS-240A/B will not operate.

Print the measurement results, and verify that the values are within the standard value.
Page 92 of 120 Rev 3. 10

(Procedure) If UVProbe is used for instrument control, perform the test using the following
procedure.
Refer to the CPS-240 Instruction Manual and UVProbe Instruction Manual (Tutorial) for
details about these operations.

16) Mount the CPS-240A (or CPS-240B) cell holder in the spectrophotometer sample
compartment and check that all wiring is connected.
17) Select the UVProbe photometric module and open the measurement method.
18) Set the following parameters and then click the [Initialize] button in the [Attachments]
tab.
[Wavelengths]
Register 550.0 nm as the measurement wavelength.
[Calibration]
Photometry type : Transmittance
[Attachments]
Attachments : CPS
Number of cells :6
* The operations above are required in order for the CPS-240A/B to be recognized as an accessory. Even
if the [Initial] button is clicked, the CPS-240A/B will not operate.

20) Click the [Go TO WL] button and set the wavelength to 550.0 nm.
21) Turn on the CPS-240A/B controller and confirm that Cell 1 moves to the optical beam
position.
22) Click the [Auto Zero] button to autozero (100% compensation).
23) Enter the numbers 1 to 18 in the Sample ID column to create an 18-line sample table.
25) Repeat step 10) two more times (making a total of three measurements).
26) Print the measurement results (sample table) and check that the values meet the pass
criteria.
(Criteria) Test 1: Cell 1 automatically moves to the optical beam position when CPS-240A/B is
turned on.
±1.0%.
Test 2: Transmittance at each cell position is within 100.0±
Rev 3. 10 Page 93 of 120

Test 3
(Item) Temperature accuracy check
(Outline) Checks the cell holder base temperature accuracy with respect to the set temperature.

Refer to the CPS-240 Instruction Manual for details about these operations.
Mount the CPS-240A (or CPS-240B) in the spectrophotometer sample compartment and
check that all wiring is connected.
1) Place the temperature sensor against the base of the CPS-240A (or CPS-240B) Cell 6
holder.
2) Set the cell holder to 16°C at the CPS temperature controller.
3) While watching the thermometer connected to the sensor, wait until the sensor temperature
stabilizes.
4) Once the sensor’s temperature stabilizes, record the temperature read from the
thermometer.
Also record the actual measurement temperature obtained by subtracting the temperature
deviation (correction value), which is determined by the measurement value (Ω) specified
in the temperature sensor inspection report and the JIS table, from the thermometer
reading.
5) Determine the deviation of the actual measurement temperature from the set temperature
(16°C), and verify that it falls within the criteria.
6) Repeat steps 2) to 5) to determine the deviation at set temperatures of 37°C and 60°C.
(Criteria) The deviation from the set temperatures (16°°C, 37°°C, 60°°C) is within ±(0.5+A+B) °C
A: Thermocouple test accuracy
B: Thermometer accuracy rating*
* Use the accuracy rating recorded in the thermometer inspection report.
Example) If the temperature rating is ± (0.1% of rdg + 0.3°C), the accuracy rating for the set
temperatures 16°C and 37°C is ±0.3°C, and ±0.4°C for 60°C.
Page 94 of 120 Rev 3. 10

Operational Qualification TCC-240A Protocol
4-8 Thermoelectrically Temperature Controlled Cell Holder TCC-240A
1. Introduction
Thermoelectrically Temperature Controlled Cell Holder TCC-240A. Refer to the Instruction Manual for
details about the operation procedure and to clarify uncertain points.
# (Item) (Outline)
1 Temperature accuracy check Checks the cell holder base temperature accuracy with respect to the
set temperature.
Test 1
(Item) Temperature accuracy check
(Outline) Checks the cell holder base temperature accuracy with respect to the set temperature.

Refer to the TCC-240 Instruction Manual for details about these operations.
1) Mount the TCC-240A in the spectrophotometer sample compartment and check that all
wiring is connected.
2) Place the temperature sensor against the base of the TCC-240A cell holder.
3) Set the cell holder to 10°C at the TCC temperature controller.
4) While watching the thermometer connected to the sensor, wait until the sensor temperature
stabilizes.
5) Once the sensor’s temperature stabilizes, record the temperature read from the
thermometer.
Also record the actual measurement temperature obtained by subtracting the temperature
deviation (correction value), which is determined by the measurement value (Ω) specified
in the temperature sensor inspection report and the JIS table, from the thermometer
reading.
6) Determine the deviation of the actual measurement temperature from the set temperature
(10°C), and verify that it falls within the criteria.
7) Repeat steps 3) to 6) to determine the deviation at set temperatures of 37°C and 60°C.
(Criteria) The deviation from the set temperatures (10°°C, 37°°C, 60°°C) is within ±(0.5+A+B) °C
A: Thermocouple test accuracy
B: Thermometer accuracy rating*
* Use the accuracy rating recorded in the thermometer inspection report.
Example) If the temperature rating is ± (0.1% of rdg + 0.3°C), the accuracy rating for the set
temperatures 10°C and 37°C is ±0.3°C, and ±0.4°C for 60°C.
Rev 3. 10 Page 95 of 120

Operational Qualification HCP-1C Protocol
4-9 Screen Copy Printer HCP-1C
1. Introduction
This section presents the standard operating procedure (SOP) for Operational Qualification of the Screen Copy
Printer HCP-1C. Refer to the Instruction Manual for details about the operation procedure and to clarify
uncertain points.
# (Item) (Outline)
1 Printing test Performs test printout, and checks control circuit operation, print
head/printer mechanism functions and print quality.
Test 1
(Item) Printing test
(Outline) Performs test printout, and checks control circuit operation, print head/printer mechanism
functions and print quality.
For details on operation, refer to the HCP-1C instruction manual.
1) Set recording paper in the HCP-1C, and position the recording paper set lever at [Print].
2) Turn on the HCP-1C and UV instrument, and wait for the initialization process to be
completed.
3) At the UV instrument, select the [9. Utilities] menu.
4) Select [5. Printer], and select HCP-IC.
5) Following the on-screen messages, set the conditions to the desired values.
6) When the printer settings are completed, press the [RETURN] key to return to the mode
selection screen.
7) Set the HCP-1C to the ON LINE state.
8) Press the [PRINT] key to print out a hard copy of the mode selection screen.
(Criteria) No problems with printing condition.
Page 96 of 120 Rev 3.10

Operational Qualification DUP-414 Protocol
4-10 Screen Copy Printer DPU-414
1. Introduction
Printer DPU-414. Refer to the Instruction Manual for details about the operation procedure and to clarify
uncertain points.
# (Item) (Outline)
Test 1

For details on operation, refer to the DPU-414 instruction manual.
1) Verify that recording paper is set in the DPU-414.
2) Turn on the DPU-414 and UV instrument, and wait for the initialization process to be
completed.
4) Select [5. Printer], and select DPU-414.
selection screen.
7) Set the DPU-414 to the ON LINE state.
Rev 3. 10 Page 97 of 120

Operational Qualification MPU Protocol
4-11 Screen Copy Printer MPU
1. Introduction
Printer MPU. Refer to the Instruction Manual for details about the operation procedure and to clarify uncertain
points.
# (Item) (Outline)
Test 1

For details on operation, refer to the MPU instruction manual.
1) Verify that recording paper is set in the MPU.
2) Turn on the MPU and UV-1800, and wait for the initialization process to be completed.
3) At the UV-1800, select the [9. Utilities] menu.
4) Select [5. Printer], and select MPU.
selection screen.
7) Set the MPU to the ON LINE state.
Rev 3. 10 Page 98 of 120

Operational Qualification ESC/P Compatible Copy Printer Protocol
4-12 ESC/P Compatible Screen Copy Printer
1. Introduction
This section presents the standard operating procedure (SOP) for Operational Qualification of the ESC/P
Compatible Screen Copy Printer. Refer to the Instruction Manual for details about the operation procedure
and to clarify uncertain points.
# (Item) (Outline)
Test 1

For details on operation, refer to the printer instruction manual.
1) Verify that recording paper is set in the printer.
2) Turn on the printer and UV instrument, and wait for the initialization process to be
completed.
3) Using the printer panel settings, set the printer mode to “ESC/P”.
5) Select [5. Printer], and select ESC/P24.
selection screen.
8) Set the printer to the ON LINE state.
Page 99 of 120 Rev 3. 10

Operational Qualification PCL Compatible Copy Printer Protocol
4-13 PCL Compatible Screen Copy Printer
1. Introduction
This section presents the standard operating procedure (SOP) for Operational Qualification of the PCL
Compatible Screen Copy Printer. Refer to the Instruction Manual for details about the operation procedure
# (Item) (Outline)
Test 1

For details on operation, refer to the printer instruction manual.
1) Verify that recording paper is set in the MPU.
2) Turn on the printer and UV-1800, and wait for the initialization process to be completed.
3) At the UV-1800, select the [9. Utilities] menu.
4) Select [5. Printer], and select PCL.
selection screen.
7) Set the MPU to the ON LINE state.
Page 100 of 120 Rev 3. 10

Operational Qualification Time Course (Multi λ) Program Pack Protocol
4-14 Time Course (Multi λ) Program Pack
1. Introduction
This section presents the standard operating procedure (SOP) for Operational Qualification of the Time Course
(Multi λ) Program Pack. Refer to the Instruction Manual for details about the operation procedure and to
# (Item) (Outline)
the program.
Test 1&2
(Item) Test 1: Program version check
Test 2: Checksum value check
(Outline) Test 1: Checks the program version using the spectrophotometer IC card check function.
Test 2: Verifies that the program’s check sum value matches the original value using the
spectrophotometer IC card check function.
For details on operation, refer to the UV-1700 instruction manual (Installation/Maintenance
and Operation Guides).
1) Check that the spectrophotometer is turned on.
2) Insert the program pack in the slot on the right side of the spectrophotometer.
3) In the mode selection screen, press the [F2] key (IC card).
4) In the data/program pack management screen, select [3. Program pack check].
5) Check that the check sum value matches, and check the version number.
6) Press the [PRINT] key to print the results screen (hard copy).
(Criteria) Test 1 : Program version number matches the controlled version number.
Test 2 : Checksum value matches.
Rev 3.10 Page 101 of 120

Operational Qualification DNA Protein quantitation P.P. Protocol
4-15 DNA/Protein Quantitation Program Pack
1. Introduction
DNA/Protein Quantitation Program Pack. Refer to the Instruction Manual for details about the operation
# (Item) (Outline)
the program.
Test 1 & 2
Page 102 of 120 Rev 3. 10

Operational Qualification Protein Quantitation P.P. Protocol
4-16 Protein Quantitation Program Pack
1. Introduction
This section presents the standard operating procedure (SOP) for Operational Qualification of the Protein
Quantitation Program Pack. Refer to the Instruction Manual for details about the operation procedure and to
# (Item) (Outline)
the program.
Test 1 & 2

Rev 3. 10 Page 103 of 120

Operational Qualification CLASS-Agent Protocol
4-17 CLASS-Agent
1. Introduction
This section presents the standard operating procedure (SOP) for Operational Qualification of the Class-Agent.
User Registration of Performer
The system administrator must complete user registration for the Performer who conducts the work (OQ User)
before this Operational Qualification is conducted. Simultaneously, register the Windows user ID to allow the
OQ User to log in to Windows as a normal operator.
Disable the Performer's user registration when all operations are complete.
● CLASS-Agent User Registration

A user with [User Administration] authority starts the CLASS-Agent Manager and logs in. Click [Tools] ->
[User Administration] to open the [User Administration] screen. If the OQ User is already created but
disabled (displayed gray), select the required user and click [Valid/Invalid] to validate this user. Click [Edit]
and check that the authority shown below is set for the user. To register a new user, click [New] and register
the user as shown in the table below.
<OQ User Registration> * ( ) Indicates name used with UVProbe
Login ID UVProbe
User name Password CLASS-Agent Authority Group
(User ID) Authority Group
Operator,
OQ_USER_1 OQ_Operator ******* Operator
but with additional “Approval”
authority for Agent Manager
OQ_USER_2 OQ_Approver ******* Administrator Administrator
The administrator should issue the initial user password and inform the user.
Page 104 of 120 Rev 3. 10

Test 1-1
(Outline) Checks that the software is not changed to an inappropriate version.
(Procedure) 1) Check the version number printed in the test results from the alteration test in Test 1-2.
2) Check that the version number matches the version number on record.
Test 1-2
(Outline) Conducts the program alteration check.
(Procedure) 1) Click on the Windows [Start] button and select [Programs] -> [Class-Agent Software] ->
[Program Files Check] to run the alteration check program.
2) A login window is displayed. Login using the test user ID “OQ_USER_2”.
3) The Program Alteration Check screen is displayed. After selecting a program to be
checked (it becomes highlighted), click the [Check] button.
4) Click the [Run] button. File comparison is conducted and the results indicate whether
program alteration has occurred.
5) Click the [Notepad] button.
7) Similarly, check other installed programs (not Shimadzu User Authentication Tool).
(Criteria) “Pass” is displayed for all software.
Test 1-3
(Item) Shimadzu User Authentication Tool connection check
(Outline) Checks the Shimadzu User Authentication Tool connection using database access and log
registration.
(Procedure) 1) Open the Windows Control Panel and double-click on the Shimadzu User Authentication
Tool icon to open the main menu.
2) Record the server name displayed at the bottom of the main menu and confirm that the
connected database is correct.
* Conduct steps 3) and 4) below after conducting Test 3-4-4.
3) Log in to [Log Display] as “OQ_USER_2” from the main menu. Set the test date and test
computer name in [Search Conditions]. Search the log and print out the results.
4) Confirm that the user lockout generated in Test 3-4-4 is registered and that the software
name is AgentMan2.exe.
Server name for the connected database is correct.

(Criteria)
Login possible from [Log Display].
Lockout by AgentMan2.exe is registered.
Rev 3. 10 Page 105 of 120

Test 1-4
(Item) 1-4-1 Password log management function check
1-4-2 Number of password characters check
1-4-3 Failed login detection
1-4-4 User lockout function check
1-4-5 Failed login record
(Outline) Checks that the security functions operate, including restrictions on the number of password
characters.
(Preparations) Before conducting this test, verify that the configuration settings in the Shimadzu User
Authentication Tool are set as shown below. Be sure to change items (3) and (4) to the settings
shown below.
Item Setting
(1) Minimum password length (Verify only; set to non-zero value)
(2) Previous password is permitted No check mark
(3) User lockout duration 1 minute
(4) User lockout after # bad logon attempts Check only; set to non-zero value
(5) PC lockout after # bad logon attempts The same number as the user logon
attempts, or higher
(Procedure) 1) Run CLASS-Agent Manager, and log on as test user “OQ_USER_1”.
2) Select [Change Password] in the [Tools] menu.
3) Enter the current password and enter the same password as the new password.
4) Confirm that the new password is not accepted.
5) Enter the current password and enter a new password that is shorter than the minimum number
of characters set in the Shimadzu User Authentication Tool.
6) Confirm that the change is not accepted, as the password is too short.
7) Enter a password equal in length to the minimum number of characters and confirm that the
change is accepted.
8) Log out.
9) Click [Login] in the [File] menu, and log in using the test user ID “OQ_USER_1”.
10) Enter a password that is not set and click OK.
11) Check that login is not permitted and a message is displayed warning that the password is
incorrect.
12) Repeat steps 9) to 11) for the number of times designated for “User logon attempts”.
13) After the designated numbers of login failures, confirm that a message indicates that the current
user is locked out and confirm that the user cannot log in for the designated lockout time.
14) After the designated lockout time elapses, select [File] -> [Login]. Enter “OQ_USER_1” as the
login ID and correctly enter the set password.
15) Confirm that login is possible.
16) Click [SYSTEM] -> [SYSTEM LOG] -> [LOG2.MDB] in the CLASS-Agent Manager
database tree.
17) Click [OK] on the “Search Log Information” screen.
18) Confirm that the login failures in the procedure above and the corresponding times appear in
the displayed log.
19) If any settings were changed in the Configuration settings of the User Authentication Tool as
indicated in (Preparations), return the settings to their original values.
(Criteria)
1-4-1 Duplicate password is not accepted.
1-4-2 Change to a password shorter than the minimum number of characters is not
accepted.
Change to a password with the minimum number of characters is accepted.
1-4-3 Login prohibited with an incorrect password but possible with the correct password.
1-4-4 User locked out after the designated number of login failures.
Login prohibited for the designated lockout time.
1-4-5 Login failures are recorded in the log.
Page 106 of 120 Rev 3. 10

Test 1-5
(Item) User access rights check
(Outline) Checks that software use is restricted according to differences in registered user access rights.
(Procedure) 1) Run CLASS-Agent Manager.
2) Enter “OQ_USER_2” as the login ID, and correctly enter the set password.
3) Select [Tools] and check that the “User Administration” item is enabled (displayed as
solid black characters).
4) Log out of CLASS-Agent Manager.
5) Select [File] -> [Login] once more. Enter “OQ_USER_1” as the login ID. Correctly enter
the set password.
6) Select [Tools] and check that the “User Administration” item is disabled (displayed as
gray characters).
(Criteria) “User Administration” item is enabled for OQ_USER_2 but disabled for OQ_USER_1.
Test 1-6
(Item) Test of function to prevent duplicate user registration
(Outline) Checks that a duplicate user name cannot be registered.
2) Log in by entering the user ID “OQ_USER_2” and the corresponding password.
3) Select [Tools] -> [User Administration].
4) Select “OQ_USER_1” and click [Active/Invalid].
5) A message indicates that Login ID: OQ_USER_1 is invalidated. Click [OK].
6) Enter “OQ Test” in the Reasons column and click [OK].
7) Click the [New] button.
8) Enter the following information and click [OK].
Login ID OQ_USER_1
User name OQ_Operator
9) Confirm that a message indicates that the user cannot be registered because the Login ID
or User Name already exists.
10) After this test, select “OQ_USER_1” and click [Active /Invalid] to validate this user.
(Criteria) Duplicate user cannot be registered and a message indicates that the setting is not possible
because the Login ID or User Name already exists.
Rev 3. 10 Page 107 of 120

Test 1-7
(Item) Data display, search, and sort check
(Outline) Checks that the sample search and sort work correctly and that the data is displayed normally.
(Procedure) 1) Run CLASS-Agent Manager. Login by entering the user ID “OQ_USER_1” and the
corresponding password.
2) Display the contents of the database registered in UVProbe Test 2-7-1.
3) Click in the sample display area, select [Edit] -> [Filter Database] and perform a search
using the following conditions:
(1) Reg. date (from): Date that UVProbe Test 2-7-1 was implemented
(2) Reg. date (to): Date that UVProbe Test 2-7-1 was implemented
(3) PC name: Computer name used for Test 1-5.
Name of the inspected computer if UVProbe Test 2-7-1 was implemented with the
inspected computer. Otherwise, designate the name of the computer used to register
data to the displayed database for the UVProbe OQ.
(4) File information 1: Anthra
4) Check that the samples registered during UVProbe Test 2-7-1 are found and displayed.
5) Click in the sample information display area. Select [Edit] -> [Sort]. Enter “File
information 1” for [Sort Item 1] and select “Ascending.”
6) Confirm that the samples are displayed in File Information 1 in the sample information
display area in the sequence: “Anthra.scp”, “Anthra1.scp”, “Anthra2.scp”.
7) Double-click on “Link file 1” for the data “Anthra2.scp” registered in the UVProbe Test
2-7-1, display the peak detection and point pick results, and print them out. Confirm that
the printed output content is identical to that in the report printed in UVProbe Test 2-7-1.
8) Duble-click on “Link file 3” for the same data, display the data set log and print it out.
Confirm that the print contnet is identical to that in the report printed in UVProbe Test
2-7-1.
Samples are searched correctly.

(Criteria)
Samples are displayed in correct sequence after a sort.
Link file 1 peak detection/point pick table contents are identical to those of the UVProbe
report.
Link file 3 data set log display is identical to that of the UVProbe report.
Test 1-8
(Item) Data recovery
(Outline) Checks that the data files registered in a database can be correctly recovered.
(Procedure) 1) Conduct this test while logged in for Test 1-7.
2) Select the data (Anthra2.spc) registered during UVProbe Test 2-7-1 and select
[Operations] -> [Browse Compressed File].
3) Click [Select All] and then click [Extract]. When a message prompts whether to
overwrite files, click [Overwrite All].
4) Using Explorer, check that the following file is saved in the folder in
C:¥ProgramFiles¥Shimadzu¥UVProbe¥Test:
C:¥ProgramFiles¥Shimadzu¥UVProbe¥Test¥Anthra2.spc
(Criteria) File is saved correctly.
Page 108 of 120 Rev 3. 10

Test 2
This test uses data registered in the database during UVProbe Test 2-7-1 and data recovered in CLASS-Agent
Manager Test 1-8.
(Item) UVProbe auto registration check

(Outline) Checks that data is correctly registered by UVProbe automatic registration to the database.
(Procedure) 1) Run UVProbe. Login as the test user “OQ_USER_2.”
2) Run UVProbe-Agent automatic registration if it is not running. If UVProbe-Agent
automatic registration is already running, double-click the task tray and check the
settings. A password is required if automatic registration was saved to the task tray by
automatic startup. The system administrator should enter the password.
3) Make a note of the existing settings. Register the re-analysis data under the name of the
UVProbe operator to the database to which data was recovered in Test 1-8.
4) Open the Anthra2.spc file recovered in Test 1-8. Select [Peak Pick] from the
[Operations] menu to display the peak detect table.
5) Enter “Re-registered” in the comment column of line 1 of the peak detect table and then
select [Save] from the [File] menu to conduct database auto registration.
6) Print out the peak detect table using the report template “OQ_ProbeTest3.rpt.” If the
point pick table or spectral data set log is not present in the template, insert it from the
report generator.
7) Check that the contents of the report is the same as the report printed during UVProbe
Test 2-7-1.
8) Run CLASS-Agent Manager and log in as test user “OQ_USER_2”.
9) Display the database where the data is registered and click the sample display area.
Select [Edit] -> [Filter Database] to search under the following conditions.
(1) Reg. date (from): Date that UVProbe Test 2-7-1 was conducted.
(2) Reg. date (to): Date that Test 2 (this test) was conducted.
(3) PC name: Computer name used for Spectrophotometer (UVProbe) Test 2-7-1.
Name of the inspected computer if UVProbe Test 2-7-1 was
implemented with the inspected computer. Otherwise, designate the
name of the computer used to register data to the displayed
database for the UVProbe OQ.
(4) File information 1: Anthra2
10) Check that the data registered during UVProbe Test 2-7-1 is not overwritten by the data
registered by this procedure.
11) Double-click on “Link file 3” for the sample registered in this procedure, display the
data log, and print it out. Confirm that the content of the printed output is identical to
that of the report output in step 6) of this procedure.
Peak detection/point pick results and the contents of the data set log are identical to
(Criteria)
those of UVProbe Test 2-7-1.
Re-registration is accomplished without overwriting
Data set log displayed content is identical to that of the UVProbe report.
Rev 3. 10 Page 109 of 120

Test 3
This test uses data recovered in CLASS-Agent Manager Test 1-8.
(Item) UVProbe manual registration check

(Outline) Checks that data is correctly registered by UVProbe manual registration to the database.
(Procedure) 1) Run UVProbe manual registration. Login as the test user “OQ_USER_2”.
2) Choose [Select Database] from the [File] menu and then select the database that was
selected for UVProbe Test 2-7-1.
3) Select [Tools] -> [Configuration] -> [Select Compression File] and confirm that there is a
check mark in the “File1” checkbox.
4) Select Spectral File (*.spc) as the file type.
5) Select “C:¥-ProgramFiles¥Shimadzu¥UVProbe¥Test” in the Folder window and select
“Anthra2.spc” in the File window.
6) Select [Entry] from the [Entry] menu.
7) Click [Yes] when the prompt appears.
8) Check that “OK” is displayed as the selected data [Results].
9) Run CLASS-Agent Manager and log in as test user “OQ_USER_2”.
10) Display the database where the data is registered and click the sample display area.
Select [Edit] -> [Filter Database] to search under the following conditions.
(1) Reg. date (from): Date that UVProbe Test 2-7-1 was conducted.
(2) Reg. date (to): Date that Test 3 (this test) was conducted.
(3) PC name: Computer name used for UVProbe Test 2-7-1.
Name of the inspected computer if UVProbe Test 2-7-1 was
implemented with the inspected computer. Otherwise, designate the
name of the computer used to register data to the displayed
database for the UVProbe OQ.
11) Select the data registered by UVProbe Test 2-7-1, UVProbe auto registration Test 2, and
this manual registration procedure and run [View] -> [Show Multi Samples].
12) Click the data display area.
13) Select [File] -> [Print]. A screen displays the printed image. Check that the data
information table contents are displayed. Adjust the column widths and enable the check
for vertical lines, horizontal lines, header, and footer.
14) Click [Printing]. On the print confirmation screen, select the required printer, set paper
orientation to landscape, and click on the [Print] button.
15) Check that the data registered by the three registration operations matches, with the
exception of the registration dates.
(Criteria) Data registered, without overwriting.

Data matches in printed results with the exception of the registration dates.
Page 110 of 120 Rev 3. 10

Test 4
(Item) Electronic signature check
(Outline) Checks the CLASS-Agent Manager electronic signature function.
2) Login as the “OQ_USER_2” test user.
3) Select [Tools] -> [Configuration] and open the [Approval Settings] tab. If the approvals
level is not set to 1, set it to 1, click [Save Settings], and click [Close] to exit
CLASS-Agent Manager. Proceed to step 6).
4) If the approval level is already set to 1, set it to 3 and click [Save]. Next, revert the setting
to 1, click [Save] again, and then click [Close].
Note: This step is required for Test 7 System Log Recording Check.
5) Exit CLASS-Agent Manager.
6) Run CLASS-Agent Manager and log in as “OQ_USER_1”.
7) Click in the sample display area, Select [Edit] -> [Filter Database] and perform a search
using the following conditions:
(1) Reg. date (from): Date that UVProbe Test 2-7-1 was implemented
(2) Reg. date (to): Date that Test 3 was implemented
(3) PC name: Computer name used for UVProbe Test 2-7-1.
Name of the inspected computer if UVProbe Test 2-7-1 was implemented with
the inspected computer. Otherwise, designate the name of the computer used to
register data to the displayed database for the UVProbe OQ.
8) Click one of the displayed data files and click [Approve] to approve it.
9) Click the sample information display area. Select [File] -> [Print]. Confirm that a print
preview window showing the printed image opens and that the printed image shows the
details of the sample information table. Adjust the column widths, if necessary, and print.
10) Confirm that “OQ_USER 1” is printed in the Approver cell and that the correct date and
time are printed in the Approval Date cell.
11) Log off and then log in as “OQ_USER_2”.
12) Select the data file approved at step 8) and click [Reject]. Enter the comment “Data was
invalidated due to the OQ Test data.” in the Comment field and click [OK].
13) If the Approval level was changed at step 3), return it to the original level.
(Criteria) Electronic signature information is printed correctly.
Test 5
(Item) System log recording check
(Outline) Checks that the changes to the CLASS-Agent Manager system setting conditions are recorded to
the system log.
(Procedure)
1) Run CLASS-Agent Manager.
2) Login as the “OQ_USER_2” test user.
3) Select the “SYSTEM LOG” database.
4) Select [Filter of Log Info.], enter the date that Test 4 was implemented for [DATE (from)]
and [DATE (to)], enter the name of the inspected computer as the [PC name], and enter
“Config” for [Operation]. Click [OK].
5) Select [File] -> [Print]. Place a check at all options and then click [Printing]. If necessary,
adjust the column widths.
6) Check that the change to the approval level in Test 4 is correctly recorded.
(Criteria) Change to configuration settings is registered in the System Log.
Rev 3. 10 Page 111 of 120

Operational Qualification Validation Software Protocol
4-18 Validation Software Package
1. Introduction
This section presents the standard operating procedure (SOP) for Operational Qualification of the Validation
Software Package. Refer to the Instruction Manual for details about the operation procedure and to clarify
uncertain points.
2 Inspection Procedures
Test 1
(Outline)
Checks the version number of the validation software package.
(Procedure)
1) Check the version number printed in the program alteration check results from Test 2.
2) Check that the version number matches the controlled version number.
Test 2
(*.dll, *.exe) in the validation software folder.
(Procedure) 1) Click on the Windows [Start] button and select [Programs] -> [Shimadzu] -> [UVPC
Perfval - Alteration Check Software] to run the alteration check program.
2) When the Login screen opens, log in using the login ID and password of Admin.
3) The Program Alteration Check screen is displayed. Select (highlight) “UVPC Validation
Software” and click the [Check] button.
4) Click the [Execute] button to run the program alteration check.
Page 112 of 120 Rev 3. 10

Operational Qualification COL-UVPC Protocol
4-19 Color Measurement Software COL-UVPC
1. Introduction
This section presents the standard operating procedure (SOP) for Operational Qualification of the Color
Measurement Software COL-UVPC. Refer to the Instruction Manual for details about the operation procedure
Test 1
(Outline) Checks the version number of the color measurement software package.
(Procedure)
1) Check the version number printed in the program alteration check results from Test 2.
Test 2
(*.dll, *.exe) in the color measurement software folder.
(Procedure)
1) Click on the Windows [Start] button and select [Programs] -> [Shimadzu] -> [UVPC
Perfval - Alteration Check Software] to run the alteration check program.
2) When the Login screen opens, log in using the login ID and password shown below, as
appropriate.
UVProbe installed in “Normal” mode

Login ID : Admin
Password : None (blank)
UVProbe installed in “Security” or “GLP” mode

Login ID : OQ_USER_2 (Test user ID registered in section 4-1)
Password : ******* (password used when above user registered)
3) When the [Program Alteration Check] screen is displayed, select (highlight) “UVColor”,
4) Click the [Run] button to execute the Program Alteration Check program.
Rev 3. 10 Page 113 of 120

Operational Qualification COL-UVPC Protocol
Test 3
(Item) Function check
(Outline) Checks the results of running the color measurement software data calculation functions to
ensure that the software functions operate normally.
(Procedure)
1) Run COL-UVPC.
2) Select [Illuminant/Obs Parameters] from the [Configure] menu and set the following
parameters:
Illuminant :C
Std Observer : 2°
Sample ID repeat :1
Hitch Std : NO
3) Select [Color Scales] from the [Configure] menu and select the [CIE XYZ…] X, Y and Z
calculation items.
4) Read the following installed file as sample data:
Data name Date and time
Silcon.spc 93/03/04 11:30
5) Automatic calculation is conducted and the results are displayed in a table on the screen.
Confirm that the values match the values below and print out the table.
X Y Z
24.52 35.56 65.34 (when the version is over 3.00)
24.52 35.56 65.33 (when the version is under 2.70)
(Criteria) Steps 1) to 4) run correctly using the file in Step 4) and the results match the values
shown in Step 5).
Page 114 of 120 Rev 3. 10

Operational Qualification FLM-UVPC Protocol
4-20 Film Thickness Measurement Software FLM-UVPC
1. Introduction
This section presents the standard operating procedure (SOP) for Operational Qualification of the Film
Thickness Measurement Software FLM-UVPC. Refer to the Instruction Manual for details about the
operation procedure and to clarify uncertain points.
Test 1
(Outline) Checks the version number of the film thickness measurement software package.
(Procedure) 1) Check the version number printed in the program alteration check results from Test 2.
Test 2
(Outline) Uses the alteration check software to check that no modifications have occurred to the
contents, date, or checksum of the files (*.dll, *.exe) in the film thickness measurement
software folder.
(Procedure) 1) From the Windows Start menu, select [Programs] -> [Film Thickness Measurement] ->
[Program Alteration Check] to run the Program Alteration Check program.
2) When the Login screen opens, log in using the login ID and password shown below, as
appropriate
UVProbe installed in “Normal” mode

Login ID : Admin
Password : None (blank)
UVProbe installed in “Security” or “GLP” mode

Login ID : OQ_USER_2 (Test user ID registered section 4-1)
Password : ******* (password used when above user registered)
3) When the [Program Alteration Check] screen is displayed, select (highlight) “UVFilm”,
4) Click the [Run] button to execute the Program Alteration Check program.
Rev 3. 10 Page 115 of 120

Operational Qualification FLM-UVPC Protocol
Test 3
(Item) Function check
(Outline) Checks the results of running the film thickness measurement software data calculation
functions to ensure that the software functions operate normally.
(Procedure)
1) Run FLM-UVPC.
2) Select [Calculating Parameters] from the [Configure] menu and set the following
parameters:
Wavelength (nm) : 400.0 to 800.0
Refractive index : 1.500
Incident Angle : 5.0
Smoothing dWL : Enable
Delta lambda (interval x) : 10
Threshold of Peak : 0.1000
Repetition :1
Auto Plot Out : Disable
3) Read the following installed file as sample data:

Data name Date and time
Silcon1.spc 91/06/18 02:30
4) Automatic calculation is conducted and the results are displayed in a table on the screen.
Confirm that the values match the values below and print out the table.
Film thickness Peak SD
2.397 15.87
(Criteria) Steps 1) to 3) run correctly using the file in Step 3) and the results match the values
shown in Step 4).
Page 116 of 120 Rev 3. 10

Operational Qualification Invalidating Inspection Data
4-21 Invalidating Inspection Data
1. Introduction
This section presents the standard operating procedure (SOP) to invalidate the inspection data stored in the
database using the CLASS Agent Manager. Refer to the Instruction Manual for details about the operation
Uses the CLASS-Agent Manager to invalidate inspection data stored in the CLASS-Agent database.
# (Item) (Outline)
1 Invalidating Inspection Data Uses the CLASS-Agent Manager to invalidate inspection data stored
in the CLASS-Agent database.
Test 1
(Item) Invalidating Inspection Data
(Outline) Uses the CLASS-Agent Manager to invalidate inspection data stored in the CLASS-Agent
database.
(Procedure) 1) Run CLASS-Agent Manager and log in as “OQ_USER_2”.
2) Display the database where the data is registered and click the sample information display
area. Select [Edit] -> [Search] and search for the following data conditions.
(1) Reg. date (from): Date that the test was implemented.
(2) Reg. date (to): Date that the test was implemented.
(3) PC name: Computer name used for the test.
The inspected computer is the same as the computer used to conduct
this procedure.
(4) Instrument name : Name of analytical instrument inspected here.
3) Select all displayed data.
4) Click [Reject] in Agent Manager and enter the comment “Data was invalidated after the
OQ Test.” in the Comment row to invalidate the data.
Rev 3. 10 Page 117 of 120

Operational Qualification Change List
5. Change List
When changing or deleting the contents of this document, or adding new information to this document, record
change list number, page number, reason, date, and name of the Performer in the Change List below, and obtain
the approval of the Reviewer and the Manager.
Change No: Enter the change number assigned in sequence from 1 onwards in accordance with
“1.3 Entries and Revisions”.
Page: Enter the page number in which the change, deletion or addition was made.
Reason: Enter the reason for the change, deletion or addition.
Date: Enter the date on which the change, deletion or addition was made.
Change
Page Reason Date Performer Reviewer Manager
No.
Page 118 of 120 Rev 3. 10

Change
No.
Rev 3. 10 Page 119 of 120

Change
No.
Page 120 of 120 Rev 3. 10

UV OQP ZEMA-2004B Rev310 1600

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SHIMADZU UV-VIS SPECTROPHOTOMETER

Operational Qualification Protocol

Performer Signature Date

Reviewer Signature Date

Manager Signature Date

Page 2 of 120 Rev 3.10

6. This document is comprised of 1. Definitions, 2. Preliminary Checks, 3. Operational Qualification Outline, 4.

Rev 3.10 Page 3 of 120

1-3 Entries and Revisions

2. Rounding of numeric values

3. Deletion and correction of mistakenly filled items

4. Changing or deleting steps, procedures or acceptance criteria

Page 4 of 120 Rev 3. 10

7. In the event of a Fail

<Additional Information> Significant Figures

<What are Significant Figures?>

<Calculating Significant Figures>

Rev 3. 10 Page 5 of 120

<Format for Clearly Stating the Number of Significant Digits>

Page 6 of 120 Rev 3. 10

2-1 Reviewer Confirmation

2-2 Performer Identification & Approval

2-3 Planning Items to be Evaluated in Operational Qualification

Rev 3.10 Page 7 of 120

2-4 Calibration Certificate and Instruments Used

(1) Instruments supplied by Shimadzu Representative

(1) Instruments for which traceability certification will be submitted

* Temperature-controlled cell holder

* Resistance temperature sensor

(2) Items to be supplied by customer

Page 8 of 120 Rev 3. 10

2-5 Other Tools Used

(1) Customer-supplied items

(2) Items supplied by the Shimadzu Representative

Rev 3. 10 Page 9 of 120

3. Operational Qualification Outline

3-1 Outline of Inspection Procedures

No. Item Outline

Page 10 of 120 Rev 3. 10

No. Item Outline

3. Syringe Sipper N/CN

No. Item Outline

No. Item Outline

No. Item Outline

No. Item Outline

Rev 3. 10 Page 11 of 120

No. Item Outline

No. Item Outline

No. Item Outline

No. Item Outline

No. Item Outline

12. ESC/P Compatible Printer

No. Item Outline

13. PCL Compatible Printer

No. Item Outline

14. Time Course (Multi λ) Program Pack

No. Item Outline

15. DNA/Protein Quantitation Program Pack

No. Item Outline

Page 12 of 120 Rev 3. 10

No. Item Outline