ZEMC-3008
Document No.
SHIMADZU GAS CHROMATOGRAPH CHROMATOGRAPH SYSTEM GC-2010 Series
Operational Qualification Operational Qualification Report System Name System ID No. Installation Site The undersigned performer reports that the Operational Qualification Protocol has been successfully completed for the system stated above.
• Performer
Signature
Date
Print
/
/
Title Company
The undersigned reviewer and manager report that the performer has completed the Operational Qualification Protocol successfully.
• Reviewer
Signature
Date
Print
/
/
/
/
Title Company
• Manager
Signature Print Title Company
Date
Operation Qualification
Table of Contents
Table of Contents 1.
DEFINITIONS .................. ..................... .................... ..................... .................... .......................... ....... 3 1-1 1-2 1-3
2.
Documentation...............................................................................................................................3 Scope.............................................................................................................................................4 Entries and Revisions ................... .................... ..................... .................... .......................... .......... 5
PRELIMINARY CHECKS....................................................................................................................6 2-1 2-2 2-3 2-4 2-5
Designation and Recording of Reviewer .................... .................... ..................... .................... ....... 6 Performer Identification & Approval..................... Approval ..................... .................... ..................... .................... .............. 7 Planning Items to be Evaluated in Operational Qualification........... ..................... ..................... ..... 9 Calibration Certification and Instruments Used ................... ..................... ..................... ............... 14 Other Tools Used ................... .................... ..................... .................... ..................... .................... 16
3.
OPERATIONAL OPERATIONAL QUALIFICATION QUALIFICATION RECORD .................. .................... ..................... .................... .... 17
4.
CHANGE LIST..................................................................................................................................34
5.
ATTACHED TTACHED DOCUMENTS ..................... .................... ..................... .................... ..................... ........ 37
Operation Qualification
Table of Contents
Table of Contents 1.
DEFINITIONS .................. ..................... .................... ..................... .................... .......................... ....... 3 1-1 1-2 1-3
2.
Documentation...............................................................................................................................3 Scope.............................................................................................................................................4 Entries and Revisions ................... .................... ..................... .................... .......................... .......... 5
PRELIMINARY CHECKS....................................................................................................................6 2-1 2-2 2-3 2-4 2-5
Designation and Recording of Reviewer .................... .................... ..................... .................... ....... 6 Performer Identification & Approval..................... Approval ..................... .................... ..................... .................... .............. 7 Planning Items to be Evaluated in Operational Qualification........... ..................... ..................... ..... 9 Calibration Certification and Instruments Used ................... ..................... ..................... ............... 14 Other Tools Used ................... .................... ..................... .................... ..................... .................... 16
3.
OPERATIONAL OPERATIONAL QUALIFICATION QUALIFICATION RECORD .................. .................... ..................... .................... .... 17
4.
CHANGE LIST..................................................................................................................................34
5.
ATTACHED TTACHED DOCUMENTS ..................... .................... ..................... .................... ..................... ........ 37
Operation Qualification
Definitions
1. Definitions 1-1
Documentation
1.
The purpose of this document is to record the results of the Operational Qualification (OQ) (OQ) implemented implemented on the Shimadzu Gas Chromatograph GC-2010. If the inspections pass the criteria and the results have been approved, it has been verified that th e instruments operate properly in accordance with their intended purpose.
2.
The following are established as the responsible parties 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 either 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; Department; or, an individual recognized by the Manager to be equipped with 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 GC system being inspected. As well as verifying the contents of the Installation Qualification Protocol and Operational Qualification Protocol documentation, the Manager shall also grant final approval to the inspection procedures.
3.
The Performer shall check each instrument and execute inspections in accordance with the procedures described in the Operational Qualification Protocol (Document No. ). After checking all items, the Performer shall sign and date the cover sheet of this document and submit this document as a 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 inspecting all items and checking their results, the Reviewer shall sign and date the cover sheet of this document as approval of the Operational Qualification.
5.
The Manager shall first check the contents of this document. After all inspections in the Operational Qualification Protocol have been implemented, the Manager shall check their results. The Manager shall then enter a unique document control No. in the Document No. column at the top right of the cover sheet, and then sign and date th e cover sheet of this document as final approval of the Operational Qualification.
6.
This document is comprised of 1. Definitions, Definitions, 2. Preliminary Preliminary Checks, 3. Operational Qualification Qualification Record, 4. Change List and 5. Attached Documents. All of these sections must be included.
7.
This document contains contains important information information and any form of duplication, photography, photography, or reproduction reproduction without the permission of the General Manager of the Quality Assurance Department, Analytical & Measuring Instruments Division, Shimadzu Corporation, is prohibited. However, the records of the inspections conducted using this document may be duplicated at the discretion of the Manager. Manager.
Operational Qualification 1-2
Definitions
Scope
This Operational Qualification shall apply to the equipment installed at the following site. (Address): (Company): (Department): (Installation Site): (Equipment ID No.): (Product Model Name)
Performer (signature):
Date:
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Reviewer
Date:
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(signature):
Operational Qualification 1-3
Definitions
Entries and Revisions
1.
Making entries Use a 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 has 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 pass criteria, round off the final answer to bring it in line with the number of figures required for the pass criteria. For example, if the pass criterion is defined down to 0.1, but the answer is given down to 0.01, round off the answer.
3.
Deletion and correction of mistakenly filled items To correct mistaken entries such as inspection results, delete the entire entry by drawing a diagonal line through it and enter the correction in the margins. To correct numerical values or symbols (checkmarks), 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 parts 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 d ocument. When making a change, delete the existing description as explained above, enter the change point, and then write down 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.
6.
Handling problems Any problems identified in 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 t he 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. If necessary, pages can be added. To add a page, record the “Change List No. ” on the page and date/ sign it. Add an alphabetical letter (starting from A) to the page number (e.g., 5-A), and insert the added page after the relevant page. Add the page number of the added page to the Table of Contents and record it in the Change List.
8.
Attaching data Attached data are added by assigning page nu mbers 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 “37-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.
Operational Qualification
Preliminary Checks
2. Preliminary Checks 2-1
Designation and Recording of Reviewer
Before conducting this inspection, enter the name of the Reviewer designated by the Manager.
Reviewer
Name: Title:
Date:
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Use the spaces below if more than one Reviewer is to be set. If the spaces are not used, place a checkmark in the “Not Applicable” checkbox. Reviewer 2 ( Not applicable)
Name: Title:
Date:
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Date:
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Reviewer 3 ( Not applicable)
Name: Title:
Operational Qualification 2-2
Preliminary Checks
Performer Identification & Approval
Identify and approve the Performer. Choose the entry section according to the way in which the Performer is selected. If
the Performer is a service technician authorized by Shimadzu Corporation, complete the following.
This is to certify that the below-signed person has received training in the Quality Assurance Department of the Analytical & Measuring Instruments Division of Shimadzu Corporation. The person has been certified by the General Manager of the Quality Assurance Department as a qualified IQ/OQ Inspector, as proven by the certificate. The person performs the Installation Qualification Protocol as the Performer. Performer
Name:
Date:
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Title: Company name: Certificate No.: Signature: Use the spaces below if more than one Performer is to be set. If the spaces are not used, place a checkmark in the “Not Applicable” checkbox. Performer 2 ( Not applicable)
Name:
Date:
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Date:
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Title: Company name: Certificate No.: Signature: Performer 3 ( Not applicable)
Name: Title: Company name: Certificate No.: Signature:
The above-signed persons are hereby recognized as Certified IQ/OQ Inspectors and approved to perform the Operational Qualification Protocol as the Performer. Reviewer
Signature:
Date:
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Date:
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Manager
Signature:
Operational Qualification If
Preliminary Checks
the Performer has been appointed by the Manager, complete the following.
Performer
Name:
Date:
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Title: Company name: Signature: The above-signed person is hereby recognized as a Certified IQ/OQ Inspector and approved to perform the Operational Qualification Protocol as the Performer. Reviewer
Signature:
Date:
/
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Date:
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Manager
Signature:
Operational Qualification 2-3
Preliminary Checks
Planning Items to be Evaluated in Operational Qualification
Prior to implementing this operational qualification, check the system configuration, determine the component and system items to be evaluated and have them approved by signing the signature column at the end o f this section.
2-3-1
Checking Equipment Configuration
The units and special accessories comprising this system are listed below. If the unit is included in the system, place a checkmark in the “Applicable” box. If the unit is not included in the system, place a checkmark in the “Not Applicable” box. No signature or date entry is required for units or systems with a checkmark in the “Not Applicable” box on the Implementation Record page. Applicable
Not Applicable
• Gas Chromatograph • Auto Injector
Model Name
GC-2010A
AOC-20i AOC-20i
AOC-20s
SPL-2010 (Addition) WBI-2010 OCI/PTV-2010
without power supply
• Auto Sampler
• Injection Unit
• Detector
• Data processing unit
FID-2010 (Addition 1) FID-2010 (Addition 2) FID-2010 (Addition 3) FTD-2010 (Addition 1) FTD-2010 (Addition 2) FPD-2010 ECD-2010 (Addition 1) ECD-2010 (Addition 2) ECD-2010 (Addition 3) ECD-2010 (Addition 4)
Computer GCsolution CLASS-Agent C-R7A plus C-R8A
FLM-2/FLM-17
• Other options
We hereby approve the system configuration specified above.
Performer (signature):
Date:
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Reviewer
Date:
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(signature):
Operational Qualification 2-3-2
Preliminary Checks
Planning Component Evaluation Items
Prior to implementing this operational qualification, confirm which items to be evaluated for components comprising the system. Place a checkmark in the “Applicable” box for items to be evaluated, and “Not Applicable” for items not to be evaluated. Enter a diagonal line in the Pass/Fail checkbox for “Not applicable” items. 1. GC-2010 Gas Chromatograph No. 1 2 3 4 5 6 7 8 9 10
Item Display/LED Test Standard Self-diagnostic Test Firmware Verification Temperature Test Column Inlet Pressure Test Column Inlet Pressure Test Flow Rate Accuracy Test Column Oven Test Temperature Program Test Sensitivity Test
Outline
Item
1 2 3 4
Display, LED Test ROM,RAM self-diagnostic Test Firmware Verification Basic operation test
1 2
Outline Verify the display and LED operation. Verify that ROM and RAM memory operates normally. Verify the program version. Verify that the auto injector basic operation is correct.
Outline Verify that the auto sampler basic operation is correct. Verify the program version.
4. SPL-2010 Split/Splitless Injection unit No. 1 2 3
Item Column Inlet Pressure Test Pressure Program Test Flow Rate Test
1 2 3
Item Column Inlet Pressure Test Pressure Program Test Flow Rate Test
Not Applicable
Applicable
Not applicable
Not Applicable Applicable
Not applicable
Applicable Outline
Verify the accuracy of the column inlet pressure. Verify that the pressure program operates normally. Verify the accuracy of the full-flow and septum purging.
5. WBI-2010 Direct Injection Unit No.
Applicable
Item Initial Operation Test Firmware Version Check
Applicable
3. AOC-20s Auto Sampler No.
Not applicable
Verify the operation of displays and LEDs Verify. the status and operation of all parts Verify the version number of software Verify that the temperature control is normal Verify the accuracy of the column inlet pressure Verify the function of the column inlet pressure program. Verify the flow rate accuracy of full-flow and septum purging. Verify the accuracy of the column oven temperature. Verify the function of the column temperature program. Verify the detector sensitivity.
2. AOC-20i Auto Injector No.
Applicable
Not Applicable Applicable
Not applicable
Applicable Outline Verify the accuracy of the column inlet pressure Verify that the pressure program operates normally Verify the total flow rate and septum purge accuracy
Not Applicable Applicable
Not applicable
6. OCI/PTV-2010 On-column/Programmable Temperature Injection Unit Applicable No. 1 2 3 4
Item Temperature Test Column Inlet Pressure Test Pressure Program Test Flow Rate Test
Outline Verify that temperature control is normal. Verify the accuracy of the column inlet pressure. Verify that the pressure program operates normally. Verify the accuracy of the full-flow and septum purging.
Not Applicable Applicable
Not applicable
Operational Qualification
Preliminary Checks
7. FID-2010 Flame Ionization Detector No. 1
Item Sensitivity test
Applicable Outline
Verify the detector sensitivity.
8. FTD-2010 Flame Thermionic Detector No. 1
Item Sensitivity test
Outline Verify the detector sensitivity.
1
Item Sensitivity test
Outline Verify the detector sensitivity.
1
Item Sensitivity test
Outline Verify the detector sensitivity.
1
Item Basic Operation Test
Item
Personal Computer 1-1 Computer boot-up test 1-2 Time and date check 1-3 Hard disk drive test 1-4 Print driver check 1-5 Network connection test GCsolution 2-1
Software version check
2-2
Program alteration check
2-3
Shimadzu User Authentication Tool connection check
2-4
Security function tests
2-4-3
Password log management function check Number of password characters check Failed login detection
2-4-4
User lockout function check
2-4-5
Failed login log
2-4-1 2-4-2
2-5
User access rights check
2-6 2-7 2-8
System policy function check Audit trail check Screen lock function check Test of function to prevent duplicate user registration
2-9
Not Applicable Applicable
Not applicable
Not Applicable Applicable
Not applicable
Not Applicable Applicable
Not applicable
Applicable Outline
Verify that the basic operation is correct..
12. Data Processing Unit GCsolution/CLASS-Agent No.
Applicable
11. FLM-2/FLM-17 Flame Warning Unit No.
Not applicable
Applicable
10. ECD-2010 Electron Capture Detector No.
Applicable
Applicable
9. FPD-2010 Flame Photometric Detector No.
Not Applicable
Not Applicable Applicable
Not applicable
Applicable Outline
Checks that the computer boots up and runs normally. Checks that the PC time and date are correct. Checks that the hard disk operates correctly. Checks the print driver test page and the version number. Checks that the network connection is normal. Checks that the software is not changed to an inappropriate version. Conducts the program alteration check. Checks the Shimadzu User Authentication Tool connection using database access and log registration. (This test is conducted only if the Shimadzu User Authentication Tool is used with GCsolution.) Checks that the security functions operate, including restrictions on the number of password characters. Checks that a duplicated password cannot be used. Checks that the restriction on the minimum number of password operates. Confirms that a failed login is detected. Confirms that a user is locked out when the designated number of login failures is exceeded. Confirms that a failed login attempt is registered in the log. Confirms that software use is restricted according to differences in registered user access rights. Checks the GCsolution system policy function. Checks the audit trail functions. Checks the screen lock function. Confirms that a duplicate user name cannot be registered.
Not Applicable Applicable
Not applicable
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Operational Qualification
No.
2-10
Item
Software function checks
2-10-1
Peak integration
2-10-2
Peak area percentage method
2-10-3
Internal standard method
2-10-4
External standard method
Preliminary Checks
Applicable
Not applicable
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Checks that correct data is registered by GCsolution automatic registration to the database.
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Checks that correct data is registered by GCsolution manual registration to the database.
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Checks the CLASS-Agent Manager electronic signature function.
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Checks that the changes to the CLASS-Agent Manager system setting conditions are recorded to the system log.
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Outline Checks the GCsolution peak integration, peak identification from retention times, quantitative calculations using peak areas and peak heights, column performance parameter calculations for each Pharmacopoeia, and the output of data information, calibration curve information, and set parameters. Checks the peak integration functions. Checks the quantitation calculation functions using the peak area percentage method. Checks the quantitation calculation functions using the internal standard method. Checks the quantitation calculation functions using the external standard method.
CLASS-Agent 3-1
Software version check
3-2
Program alteration check Shimadzu User Authentication Tool connection check
3-3 3-4
Security function tests
3-4-3
Password log management function check Number of password characters check Failed login detection
3-4-4
User lockout function check
3-4-5
Failed login log
3-4-1 3-4-2
3-5
User access rights check
3-6
Test of function to prevent duplicate user registration
3-7
Data display, search, and sort
3-8
Data recovery
GCsolution automatic registration GCsolution automatic 4 registration function check (Data integrity check) GCsolution manual registration GCsolution manual registration 5 function check Electronic signature 6
Electronic signature check
Checks that the software is not changed to an inappropriate version. Conducts the program alteration check. Checks the Shimadzu User Authentication Tool connection using database access and log registration. Checks that the security functions operate, including restrictions on the number of password characters. Checks that a duplicated password cannot be used. Checks that the restriction on the minimum number of password operates. Confirms that a failed login is detected. Confirms that a user is locked out when the designated number of login failures is exceeded. Confirms that a failed login attempt is registered in the log. Confirms that software use is restricted according to differences in registered user access rights. Confirms that a duplicate user name cannot be registered. Checks that the sample search and sort work correctly and that the data is displayed normally. Checks that the data files registered in a database can be correctly recovered.
System log 7
System log recording check
4. Data Processing Unit Chromatopac C-R7A plus/C-R7Ae plus/C-R8A Applicable No. 1
Item Memory self-diagnostic test
2-1 2-2
Zero point Span
2-3
Zeroing
2-4 2-5 2-6
Linearity Slope test Accuracy
2-7
Range
2-8
Repeatability
Outline Checks that the result of the ROM/RAM self-diagnostic check is normal. Checks the measured voltage value at 0 V analog input. Checks the measured voltage value at 1 V analog input. Checks the difference between measured voltage values in two measuring ranges. Checks the linearity between 0 V and 1 V input voltages. Slope test at fixed input voltage (0 V). Checks the accuracies for peak area, height, and retention time. Checks the range (discrepancy from maximum to minimum) for peak area, height, and retention time. Checks the repeatability (coefficient of variance) for peak area, height, and retention time.
Not Applicable Applicable
Not applicable
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Operational Qualification 2-3-3
Preliminary Checks
Planning System Evaluation Items
Prior to implementing this operational qualification, confirm which items to be evaluated for t he system. Place a checkmark in the “Applicable” box for items to be evaluated, and “Not Applicable” for items not to be evaluated. Enter a diagonal line in the Pass/Fail checkbox for “Not applicable” items. 1. GC-2010 Analysis System No. 1
Applicable
Item Repeatability tests
Outline Verify the repeatability for the peak area and retention time.
Not Applicable Applicable
Not applicable
Execution purpose of this Qualification New
installation
Periodic check
Component
addition
Repair
Others(
)
We hereby approve that the Operational Qualification will be implemented by evaluating the items specified in section 2-3 of this document.
Performer (signature):
Date:
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Reviewer
Date:
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(signature):
Operational Qualification 2-4
Preliminary Checks
Calibration Certification and Instruments Used
The instruments and reagents used in the inspections are listed below. When instruments controlled by the Shimadzu service company 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) Items prepared by the Shimadzu Service Company (1) Instruments for which the traceability certificate will be submitted Certificates of traceability are attached to the following instruments controlled by the Shimadzu service company. *
Pressure gauge For the assured performance specifications of the pressure gauge used to measure the column inlet pressure accuracy and for the pressure program operational check, a precision of ±6 kPa shall be required in the pressure range (200 kPa and 250 kPa) required for the equipment inspections. Instrument name: Digital pressure gauge Inspection date:
Instrument name: Digital pressure gauge Inspection date:
Instrument name: Inspection date:
*
Expiry date: ; Model: MT10
Control No:
Expiry date: ; Model
Control No:
Expiry date:
Instrument name: Precision membrane flow meter; Model: SF-1
Instrument name: Digital flow meter Inspection date:
Control No:
Flow meter For the assured performance specifications of the flow meter used for the full-flow and septum purge accuracy checks and for TCD sensitivity measurements, a precision of ±3% shall be required in the flow rate range (3, 20, and 200 mL/min) required for the equipment inspections.
Inspection date:
; Model: POP-612
Instrument name: Inspection date:
Control No:
Expiry date: ; Model: DFM-1000
Control No:
Expiry date: ; Model
Control No:
Expiry date:
* Digital temperature indicator For the assured performance specifications of the recorder used to measure the column oven temperature accuracy, a precision of ±0.5°C shall be required at the 150°C temperature required for the equipment inspections.
Instrument name: Hybrid recorder Inspection date:
Instrument name: Digital thermometer Inspection date:
Instrument name: Inspection date:
*
; Model: RD2212
Control No:
Expiry date: ; Model:ND522-3LP
Control No:
Expiry date: ; Model
Control No:
Expiry date:
Resistance temperature sensor
For the assured performance specifications of the resistance temperature sensor used to measure the column oven temperature accuracy, a precision of ±0.5°C shall be required in the temperature range (150 °C) required for the equipment inspections.
Instrument name: Sheathed resistance temperature sensor; NRHS1-0 Inspection date:
Instrument name: Inspection date:
Control No:
Expiry date: ; Model Expiry date:
Control No:
Operational Qualification
Preliminary Checks
* Thermocouple For the assured performance specifications of the thermocouple used to measure the column oven temperature accuracy, a precision rating of ±0.6°C shall be required in the temperature range (150 °C) required for the equipment inspections.
Instrument name: K-sheath thermocouple Inspection date:
Instrument name: Inspection date:
; Model: SCH S1-0
Control No:
Expiry date: ; Model
Control No:
Expiry date:
* DC voltage/current generator The DC voltage/current generator used for the Chromatopac Hardware Validation check shall have a precision rating of ±0.15% at the test point as a guaranteed performance specification.
Instrument name:
; Model: R6142
Control No:
Programmable DC voltage/current generator Inspection date:
Instrument name: Inspection date:
(2)
Expiry date: ; Model
Control No:
Expiry date:
Instrument/reagents whose Quality Assurance sheet is submitted upon request For the following equipment and reagents, the quality assurance sheet can be submitted upon request from a customer.
* Standard reagents for performance inspection n-C12, 14, 16/n-heptane solution 100ng/µL 2mL x 5 Ampoules［221-44247-08］ For the detector sensitivity test and the system repeatability test of FID Lot No.: Expires: n-decane/n-hexane solution 1000ng/µL 2mL x 5 Ampoules［221-44247-11］ For the detector sensitivity test and system repeatability test of TCD Lot No.: Expires: Azobenzene/n-hexane solution 1ng/µL 2mL x 5 Ampoules［221-44247-07］ For the detector sensitivity test and the system repeatability test of FTD (N compounds) Lot No.: Expires: Malathion/n-hexane solution 100pg/µL 2mL x 5 Ampoules［221-44247-14］ For the detector sensitivity test and the system repeatability test of FTD (P compounds) Lot No.: Expires: Tributyl phosphate/n-hexane solution 1ng/µL 2mL x 5 Ampoules［221-44247-15］ For the detector sensitivity test and the system repeatability test of FTD (P compounds) Lot No.: Expires: Tributyl phosphate/n-hexane solution 10ng/µL 2mL x 5 Ampoules［221-44247-12］ For the detector sensitivity test and the system repeatability test of FPD (P compounds) Lot No.: Expires: Dodecanethiol/n-hexane solution 10ng/µL 2mL x 5 Ampoules［221-44247-13］ For the detector sensitivity test and the system repeatability test of FPD (S compounds) Lot No.: Expires: γ-BHC/n-hexane solution 0.1ng/µL 2mL x 5 Ampoules［221-44247-03］ For the detector sensitivity test and the system repeatability test of ECD Lot No.: Expires:
Operational Qualification 2-5
Preliminary Checks
Other Tools Used
Tools, solvents, etc. used in this inspection are shown below. These are classed as customer-supplied items or Shimadzu service company-supplied items.
(1) Items prepared by the customer * Carrier gas * Detector gas * Hexane * Glass insert for split * Glass insert for splitless, WBI
[221-41444-01] [221-48335-01]
; when using SPL for inspection ; when using WBI for inspection
(2) Items prepared by the Shimadzu Service Company * Devices Glass
vial 1.5mL Vial cap 1.5mL Vial septum 1.5mL Glass vial 4 mL Vial cap 4 mL Vial septum 4 mL
[221-34272-92] [221-34273-92] [221-41239-91] [221-34267-92] [221-34268-92] [221-34266-92]
Columns (To test GC unit. Select from following four types.) CBP1-M25-025 [221-28635-25] DB-1-30N-STD [J&W P/N ：122-1032] ZB-1 (30m x 0.25mmID, 0.25 µm) Rtx-1 (30m x 0.25mmID, 0.25 µm)
; for AOC-20i/s ; for AOC-20i/s ; for AOC-20i/s ; for AOC-20i/s ; for AOC-20i/s ; for AOC-20i/s
; for sensitivity, repeatability tests ; for sensitivity, repeatability tests ; for sensitivity, repeatability tests ; for sensitivity, repeatability tests
Columns (For OCI/PTV temperature test; for sensitivity test and system check using WBI. Select from following two types.) CBP1-W12-100 ；for OCI/PTV and WBI tests [221-28647-12] DB-1-15M-STD ；for OCI/PTV and WBI tests [J&W P/N ：125-1032] Pressure measurement Pipe
adaptor
MF-MF Column holder Microsyringe MS-G10AC Microsyringe (CAL)10F-RA6
[221-42686-91] [201-48555-**] [221-31567-91] [221-45169-01] [221-45170-01]
; for pressure test ; to connect adapter and pressure gauge ; to fix temperature sensor ; for manual injection ; for manual injection
* Others Vulcanized
tape
Cable
[018-21330] [223-06064-90]
； for pressure measurement adapter ； to connect voltage / current generator
The equipment, reagents, tools, and misc. items described in Sections 2.4 and 2.5 are approved for use in the inspections.
Performer (signature):
Date:
/
/
Reviewer
Date:
/
/
(signature):
Operational Qualification
Operational Qualification Record
3. Operational Qualification Record If the unit is included in the system to be inspected, place a checkmark in the “Applicable” box. If the unit is not included in the system, place a checkmark in the “Not Applicable” box. Enter a diagonal line in the Pass/Fail checkbox for “Not applicable” items. Here, Inspection results are recorded along the procedure of Chapter 4 in Operational Qualification Protocol.
3-1
Gas Chromatograph GC-2010
Applicable
Not Applicable
GC-2010 ＿＿
Model Name Component ID Serial Number (S/N) No. 1
2
____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____
Item isplay, LED est
Standard self-diagnostic est irmware ersion check
3
Temperature est
Criteria Verify the display and LED operation. Verify the status and operation of all parts. Verify the program version.
Verify that temperature control is normal.
4
Column inlet pressure test
Verify the accuracy of the column inlet pressure.
Results
All LEDs light. Screen contrast possible.
adjustment
"Good" displayed self-diagnostic test.
as
result
Fail
LED
□
□
Display
□
□
□
□
□
□
□
□
□
□
□
□
of
the
ersion number and build number are displayed.
Ver.
The version No. and build No. atches the controlled version umber.
Controled Ver. No.
Version: Build No.: Version: Build No.:
TEMP LED lights green. Displayed actual values agree to the set values within ±1°C.
Temperature controller
(Name)
Set value
Measured value
COL
__ __.__ °C
__ __.__ °C
INJ1
__ __.__ °C
__ __.__ °C
INJ2
__ __.__ °C
__ __.__ °C
DET1
__ __.__ °C
__ __.__ °C
DET2
__ __.__ °C
__ __.__ °C
AUX3
__ __.__ °C
__ __.__ °C
AUX4
__ __.__ °C
__ __.__ °C
AUX5
__ __.__ °C Pressure gauge correction value
__ __.__ °C
Inspection pressure gauge reading 10.0± 3.0ｋPa Inspection pressure gauge reading 200.0± 20.0ｋPa
5
the
is
Pass
Inspection pressure gauge reading 500.0± 35.0ｋPa
__.__ ｋPa
Pressure gauge reading
__ __.__ ｋPa
Post-correction reading
__ __.__ ｋPa
Pressure gauge correction value Pressure gauge reading
__ __ __.__ ｋPa
Post-correction reading
__ __ __.__ ｋPa
__.__ ｋPa
Pressure gauge correction value
__.__ ｋPa
Pressure gauge reading
__ __ __.__ ｋPa
Post-correction reading
__ __ __.__ ｋPa
Performer (signature):
Date:
/
/
Reviewer
Date:
/
/
(signature):
Operational Qualification No.
Item Pressure program test
6
Flowrate test
Operational Qualification Record Criteria
Verify that the pressure program operates normally. Verify the accuracy of the full-flow and septum purging.
7
Results
Monitored pressure 6 minutes after start 250.0 ± 5.0 kPa
__ __ __.__ ｋPa
Inspection pressure gauge reading 8 minutes after start 250.0 ± 20.0 kPa
__ __ __.__ ｋPa
Septum purge vent measured flow rate 3.0± 1.0mL/min
Septum purge __.__ mL/min
Pass
Fail
□
□
□
□
□
□
□
□
□
□
□
□
□
□
Split vent ______. __mL/min
Total of septum purge and split vent flow rate values
10.0± 3.0mL/min
Total ______. __mL/min Split vent _________mL/min
Total of septum purge and split vent flow rate values
Total
200± 20mL/min
_________mL/min Split vent _________mL/min Total
Total of septum purge and split vent flow rate values
500± 35mL/min
_________mL/min
Column oven test
Verify the accuracy of the column oven temperature.
8
Temperature program test 9
Sensitivity test
Inspection temperature sensor displayed value 50.0±3.2℃
Temp. correction value
Inspection temperature sensor displayed value 150.0±4.2℃
Temp. correction value
Inspection temperature sensor displayed value 280.0±5.7℃ 280±4℃
Temp. correction value
__.__ °C
Temp. sensor reading
___ __.__ °C
Corrected temp. value
___ __.__ °C __.__ °C
Temp. sensor reading
__ __ __.__ °C
Corrected temp. value
__ __ __.__ °C __.__ °C
Temp. sensor reading
__ __ __.__ °C
Corrected temp. value
__ __ __.__ °C
Verify that the onitored temperature 6 minutes after start 200 ± 1°C column temperature Inspection temperature reading 8 minutes after start program 200.0 ± 4.7°C operates Using a temperature sensor with 1 °C minimum normally. display increment 200 ±3°C Verify the detector sensitivity.
10
FID ( Applicable Not Applicable) Calculated S value Inj. unit ( ) Make-up gas: N2 10.0 x 10-3 C/g min. Make-up gas: He 7.00 x 10-3 C/g min. TCD ( Applicable Not Applicable) Calculated S value Inj. unit ( ) 3 4.00 x 10 mV･ml/mg min.
__ __ __ °C __ __ __.__ °C __ __ __ °C
C16AREA value
μV･s Calculated S value
__ __.__ __x 10-3C/g
C10AREA value
μV･s
Flowrate at vent
__ __.__ __mL/min __ __.__ __x103ｍV･ mL/mg
Calculated S value
Performer (signature):
Date:
/
/
Reviewer
Date:
/
/
(signature):
Operational Qualification AOC-20i Auto Injector
3-2 Single
Operational Qualification Record
Applicable
Not Applicable
Dual system, main injector Model Name
AOC-20i
Component ID Serial No. (S/N)
No.
Item Display, LED test
1
____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ Criteria Verify the display and LED operation. Verify that ROM and RAM memory operates normally.
ROM ， RAM self diagnosis Firmware Verify version check program version.
2
3
Basic operation test
4
Not Applicable
the
All LEDs light, except decimal point. Display shows "000".
Version number is displayed. The version number matches the controlled version number.
Verify that the auto injector basic operation is correct.
Results
Display: Version No. Controled Ver. No.
Sample injected into the GC and GC operation starts.
Pass
Fail
□
□
□
□
□
□
□
□
Dual system, sub injector
Model Name
AOC-20i
Component ID Serial No. (S/N)
No.
1 2
3
____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____
Item
Criteria
Results
Display, LED Verify the display and LED All LEDs light, except decimal point. test operation. ROM ， RAM Verify that ROM and RAM Display shows "000". memory operates normally. self diagnosis Firmware version check Basic operation test
4
Verify program version.
the Version number is displayed.
Pass
Display:
□
□
□
□
□
□
□
□
Version No.
The version number matches the Controled controlled version number. Ver. No. Verify that the auto injector Sample No.1 transferred to the main basic operation is correct. injector, sample No. 2 transferred to the sub-injector. Sub-injector injects into the GC simultaneously with the main AOC.
Performer (signature):
Date:
/
/
Reviewer
Date:
/
/
(signature):
Fail
Operational Qualification
3-3
Operational Qualification Record
AOC-20s Auto Sampler Model Name
Applicable
Not Applicable
AOC-20s
Component ID Serial No. (S/N)
No.
____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____
Item
Criteria
1
Initial operation test
Verify that the auto sampler basic operation is correct.
2
Firmware version check
Verify the program version.
Results
Fail
□
□
□
□
LED lights green, not red.
Version number is displayed.
Version No.
The version number matches the controlled version number.
Controled Ver. No.
Performer (signature):
Date:
/
/
Reviewer
Date:
/
/
(signature):
Pass
Operational Qualification 3-4
Operational Qualification Record
SPL-2010 Split/Splitless Injection Unit Model Name
Applicable
Not Applicable
SPL-2010
Component ID Serial No. (S/N)
No.
____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____
Item Column inlet pressure test
Criteria Verify the accuracy of the column inlet pressure.
Inspection pressure gauge reading 10.0± 3.0ｋPa Inspection pressure gauge reading 200.0±20.0ｋPa
1
Inspection pressure gauge reading 500.0±35.0ｋPa
2
Pressure program test
Flowrate test
Verify that the pressure program operates normally. Verify the accuracy of the full-flow and septum purging.
Results Pressure gauge correction value
__ __.__ ｋPa
Post-correction reading
__ __.__ ｋPa
Pressure gauge correction value
□
□
□
□
□
□
□
□
__.__ ｋPa
Pressure gauge reading
__ __ __.__ ｋPa
Post-correction reading
__ __ __.__ ｋPa
Pressure gauge correction value
__.__ ｋPa
Pressure gauge reading
__ __ __.__ ｋPa
Post-correction reading
__ __ __.__ ｋPa
Monitored pressure 6 minutes after start 250.0 ± 5.0 kPa
__ __ __.__ ｋPa
Inspection pressure gauge reading 8 minutes after start 250.0 ± 20.0 kPa
__ __ __.__ ｋPa
Septum purge vent measured flow rate 3.0±1.0mL/min
Septum purge __.___mL/min
Total of septum purge and split vent flow rate values
Split vent __.__ mL/min Total ____. __mL/min
3 Total of septum purge and split vent flow rate values
200±20mL/min
Total of septum purge and split vent flow rate values
500±35mL/min
Split vent ________mL/min Total ________mL/min Split vent ________mL/min Total ________mL/min
Performer (signature):
Date:
/
/
Reviewer
Date:
/
/
(signature):
Fail
__.__ ｋPa
Pressure gauge reading
10.0±3.0mL/min
Pass
Operational Qualification
3-5
Operational Qualification Record
Applicable
WBI-2010 Direct Injection Unit Model Name
Not Applicable
WBI-2010
Component ID Serial No. (S/N)
No.
____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____
Item Column inlet pressure test
Criteria Verify the accuracy of the column inlet pressure.
Inspection pressure gauge reading 10.0± 3.0ｋPa Inspection pressure gauge reading 50.0± 10.0ｋPa
1
Inspection pressure gauge reading 200.0±20.0ｋPa
2
Results Pressure gauge correction value
__ __.__ ｋPa
Post-correction reading
__ __.__ ｋPa
Pressure gauge correction value
□
□
□
□
□
□
□
□
__.__ ｋPa
Pressure gauge reading
__ __.__ ｋPa
Post-correction reading
__ __.__ ｋPa
Pressure gauge correction value Pressure gauge reading
__ __ __.__ ｋPa
Post-correction reading
__ __ __.__ ｋPa
__.__ ｋPa
Pressure program test
Verify that the pressure program operates normally.
Monitored pressure 6 minutes after start 250.0 ± 5.0 kPa
__ __ __.__ ｋPa
Inspection pressure gauge reading 8 minutes after start 250.0 ± 20.0 kPa
__ __ __.__ ｋPa
Flowrate test
Verify total flow (column outlet flow) and septum purge accuracy.
Septum purge vent measured flow rate 3.0 ± 1.0mL/min
Septum purge __.__ mL/min
Column outlet measured flow rate 5.0± 1.5mL/min
Measured flow __.__ mL/min
Column outlet measured flow rate 20.0± 5.0mL/min
Measured flow ____. __mL/min
Column outlet measured flow rate 100 ± 15mL/min
Measured flow ______mL/min
Performer (signature):
Date:
/
/
Reviewer
Date:
/
/
(signature):
Fail
__.__ ｋPa
Pressure gauge reading
3
Pass
Operational Qualification 3-6
Operational Qualification Record
OCI/PTV-2010 On-column/Programmable Temperature Injection Unit
Applicable Model Name
Not Applicable
OCI/PTV-2010
Component ID Serial No. (S/N) No.
____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____
Item Temperature test
1
Criteria Verify that temperature control is normal.
Results
Measured temperature value displayed immediately after start: 50 ± 5°C Measured temperature value displayed 8 minutes after start: 250 ± 5°C
Pass
Fail
__ __.__ ℃
□
□
__ __ __.__℃
□
□
□
□
□
□
□
□
□
□
□
□
Fan operation begins 10 minutes after start. Column inlet pressure test
Verify column inlet pressure accuracy.
Inspection pressure gauge reading 10.0 ± 3.0ｋPa Inspection pressure gauge reading 50.0 ± 10.0ｋPa
2 Inspection pressure gauge reading 200.0 ± 20.0ｋPa Inspection pressure gauge reading 500.0 ± 35.0ｋPa Pressure program test 3
Verify that the pressure program operates normally. Flow rate test Verify Used for accuracy of OCI, so not total flow and septum conducted. purge.
4
Pressure gauge correction value
__.__ｋPa
Pressure gauge reading
__ __.__ｋPa
Post-correction reading
__ __.__ｋPa
Pressure gauge correction value
__.__ｋPa
Pressure gauge reading
__ __.__ｋPa
Post-correction reading
__ __.__ｋPa
Pressure gauge correction value
__.__ｋPa
Pressure gauge reading
__ __ __.__ｋPa
Post-correction reading
__ __ __.__ｋPa
Pressure gauge correction value
__.__ｋPa
Pressure gauge reading
__ __ __.__ｋPa
Post-correction reading
__ __ __.__ｋPa
Monitored pressure 6 minutes after start 250.0 ± 5.0 kPa
__ __ __.__ｋPa
Inspection pressure gauge reading 8 minutes after start 250.0 ± 20.0 kPa
__ __ __.__ｋPa
Septum purge vent measured flow rate 3.00± 1.00mL/min
Septum purge __.___mL/min
Total of septum purge and split vent flow rate values
Split vent __.__ mL/min
10.0± 3.0mL/min
Total ____. __mL/min
Total of septum purge and split vent flow rate values
200± 20mL/min
Total of septum purge and split vent flow rate values
500± 35mL/min
Split vent _________mL/min Total __________mL/min Split vent _________mL/min Total _________mL/min
Performer (signature):
Date:
/
/
Reviewer
Date:
/
/
(signature):
Operational Qualification 3-7
Operational Qualification Record
FID-2010 Flame Ionization Detector
Applicable
Not Applicable
Addition 1
FID-2010
Model Name Component ID Serial No. (S/N) No.
____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____
Item
Criteria
Sensitivity test 1
Verify detector sensitivity
Injection unit ( )
Addition 2
Applicable
Not
Sensitivity S calculated value Make-up gas ： N2 ≥10.0x10 -3C/g Make-up gas ：He ≥7.00x10 -3C/g
Results C16AREA value
μV･s
Sensitivity S calculated value
Pass
Fail
□
□
Pass
Fail
□
□
Pass
Fail
□
□
__ __.__ __x 10-3C/g
Applicable
FID-2010
Model Name Component ID Serial No. (S/N) No.
____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____
Item
Criteria
Sensitivity test 1
Verify detector sensitivity
Injection unit ( )
Addition 3
Applicable
Sensitivity S calculated value Make-up gas ： N2 ≥10.0x10 -3C/g Make-up gas ：He ≥7.00x10 -3C/g
Not
Model Name
Results C16AREA value
μV･s
Sensitivity S calculated value
__ __.__ __x 10-3C/g
Applicable
FID-2010
Component ID Serial No. (S/N) No.
Item Sensitivity test
1
____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ Criteria Verify detector sensitivity
Injection unit ( )
Sensitivity S calculated value Make-up gas ： N2 ≥10.0x10 -3C/g Make-up gas ：He ≥7.00x10 -3C/g
Results
C16AREA value Sensitivity S calculated value
μV･s __ __.__ __x 10-3C/g
Performer (signature):
Date:
/
/
Reviewer
Date:
/
/
(signature):
Operational Qualification 3-8
Operational Qualification Record
FTD-2010 Flame Thermionic Detector
Applicable
Not Applicable
Addition 1
FTD-2010
Model Name Component ID Serial No. (S/N)
No.
____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____
Item
Criteria Verify the detector sensitivity.
Sensitivity test
Results
N (Applicable N/A) Azobenzen MDQ ≦ -12 2.00 x 10 gN/s
Injection unit ( ) 1
P (Applicable N/A) Malathion Tributyl phosphate MDQ ≦ 0.900 x 10-12 gP/s
Addition 2
Applicable
Not
AREA value
µV･s
Pass
Fail
□
□
□
□
Pass
Fail
□
□
□
□
__.__ __ x 10-12gN/s
MDQ
AREA value
µV･s __.__ __ __ x 10-12gP/s
MDQ
Applicable
FTD-2010
Model Name Component ID Serial No. (S/N)
No.
____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____
Item
Criteria Verify the detector sensitivity.
Sensitivity test Injection unit ( ) 1
N (Applicable N/A) Azobenzen MDQ ≦ 2.00 x 10 -12 gN/s P (Applicable N/A) Malathion Tributyl phosphate MDQ ≦ 0.900 x 10 -12 gP/s
Results
AREA value
µV･s __.__ __ x 10-12gN/s
MDQ
AREA value
µV･s -12
MDQ
__.__ __ __ x 10 gP/s
Performer (signature):
Date:
/
/
Reviewer
Date:
/
/
(signature):
Operational Qualification 3-9
Operational Qualification Record
FPD-2010 Flame Photometric Detector
Applicable
Not Applicable
FPD-2010
Model Name Component ID Serial No. (S/N)
No.
____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____
Item
Criteria Verify the detector sensitivity.
Sensitivity test Injection unit ( )
Results
S (Applicable N/A) Dodecane thiol MDQ ≦ 40.0 x 10 -12 gS/s
AREA value
P (Applicable N/A) Tributyl phosphate MDQ ≦2.00x10 -12gP/s
AREA value
µV･s
Pass
Fail
□
□
□
□
__ __.__ x 10-12gS/s
MDQ
1
3-10
µV･s -12
MDQ
ECD-2010 Electron Capture Detector
__.__ __ x 10 gP/s
Applicable
Not Applicable
Addition 1
ECD-2010
Model Name Component ID Serial No. (S/N)
No.
____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____
Item
Criteria Verify the detector sensitivity.
Sensitivity test
1
γ -BHC MDQ ≦ 80.0 x 10-15 g/s
Injection unit ( )
Addition 2
Applicable
Results
Not
Model Name
AREA value
µV･s
MDQ
-1５
__ __.__ x 10
Pass
Fail
□
□
Pass
Fail
□
□
g/s
Applicable
ECD-2010
Component ID Serial No. (S/N)
No.
1
____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____
Item
Criteria
Sensitivity test
Verify the detector sensitivity.
Injection unit ( )
Results
γ -BHC MDQ ≦ 80.0 x 10-15 g/s
AREA value
µV･s
MDQ
-1５
__ __.__ x 10
g/s
Performer (signature):
Date:
/
/
Reviewer
Date:
/
/
(signature):
Operational Qualification Addition 3
Applicable
Not
Operational Qualification Record
Applicable
ECD-2010
Model Name Component ID Serial No. (S/N)
No.
____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____
Item
Criteria Verify the detector sensitivity.
Sensitivity test
1
Applicable
Pass
Not
Fail
µV･s
AREA value γ -BHC MDQ ≦ 80.0 x 10-15 g/s
Injection unit ( )
Addition 4
Results
□
□
Pass
Fail
□
□
__ __.__ x 10-1５g/s
MDQ
Applicable
ECD-2010
Model Name Component ID Serial No. (S/N)
No.
____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____
Item
Criteria Verify the detector sensitivity.
Sensitivity test
1
Injection unit ( )
Results
γ -BHC MDQ ≦ 80.0 x 10-15 g/s
AREA value
µV･s
MDQ
-1５
3-11 FLM-2/FLM-17 Flame Warning Unit Model Name
__ __.__ x 10
Applicable
g/s
Not Applicable
FLM-2/FLM-17
Component ID No.
1
Item Basic operation test
Criteria
Results
Verify that the basic The FLM (amplifier unit) lamp goes out correctly. operation is correct.
Performer (signature):
Date:
/
/
Reviewer
Date:
/
/
(signature):
Pass
Fail
□
□
Operational Qualification 3-12
Operational Qualification Record
GCsolution /CLASS-Agent
Applicable Workstation GCsolution
Model Name Serial Number (S/N) No.
____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ Item
1-1 1-2
Criteria
Computer boot-up test
Windows starts up normally.
Time and date check
Date and time are correct. Permitted range
Inspection results Computer
/
/
/
：
：
：
：
□ Hard disk drive test
No error detected for any drive.
Pass
Fail
□
□
□
□
□
□
□
□
□
□
□
□
Basic
/
Drive
1-3
Not Applicable
Error detection
C
□ □ □
Test page printed correctly. 1-4
The driver version number matches the controlled version number.
Print driver check
Network connection test Not implemented because not connected to network
1-5
No packets lost.
Ver. Controled Ver. Designated IP address
GCsolution 2-1
Software version check
The version number matches the controlled version number.
2-2
Program alteration check
“OK” is displayed for every item.
Applicable
Not
Applicable
Ver. Control ed Ver.
□
□
□
□
Server name for the connected database is correct.
□
□
Login possible from [View event log].
□
□
Lockout by GCPrun.exe is registered.
□
□
□
□
□
□
□
□
Server name: Shimadzu Authentication Tool connection check Not implemented because not used with GCsolution
2-3
2-4
Security function test
Password log management Duplicated passwords cannot be used. function check Number of password characters A password shorter than the minimum length is not accepted while a 2-4-2 check password satisfying the minimum length is accepted. Login is not possible with an incorrect password but possible with the 2-4-3 Failed login detection correct password. 2-4-1
2-4-4 2-4-5
User lockout function check
The user is locked out for the specified lockout time.
□
□
Failed login log
The login lockout is registered in the log.
□
□
Performer (signature):
Date:
/
/
Reviewer
Date:
/
/
(signature):
Operational Qualification
No.
Item
Operational Qualification Record
Criteria
2-5
User access rights check
2-6
System policy function check
Inspection results
Pass
Fail
OQ_USER_2 can edit Instrument Parameters but OQ_USER_1 cannot edit them.
□
□
A check mark appears for the audit trail settings in a newly created method file.
□
□
Overwriting other method files is prohibited.
□
□
Audit trail details (Date&Time, Modification, Reason) are displayed correctly.
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The Screen lock function operates.
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2-7
Audit trail check
2-8
Screen lock function check
2-9
Test of function to prevent duplicate user registration
"OQ_USER_1" cannot unlock the screen but "OQ_USER_2" can unlock the screen. A message indicates that “This user ID is already registered.” Duplicate user registration is not possible.
2-10
Software function checks
Registration to Agent database
Database name
Peak tailing is conducted in the "Demo_Data-IT01.gcd" report. Peak vertical splitting is conducted in the "Demo_Data-IT02.gcd" report. Peak baseline processing is conducted in the "Demo_Data-IT03.gcd" report.
2-10-1 Peak integration
2-10-2 Peak area percentage method
The results match.
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2-10-3 Internal standard method
The results match.
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The results match.
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Operator name (Acquired by), analysis date (Data Acquired), processed date (Data Processed), and name of data file (Data File Name) used are printed as sample information.
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Calibration curve information is printed.
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Unit Parameters and Peak Integration, peak Identification, and Quantitative parameters and Compound Table are printed.
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2-10-4 External standard method
CLASS-Agent Software
Applicable
The version number matches controlled version number.
the
Ver.
Not
Applicable
Controled Ver.
CLASS-Agent manager Shimadzu User Authentication Tool
3-1
Software version check
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3-2
Program alteration check
"Total: Pass" appears for all software. Server name for the connected database is correct.
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3-3
Shimadzu User Authentication Tool connection check Not implemented because already implemented in Test 2-3
Login possible from [View event log].
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Lockout by AgentMan2.exe is registered.
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Server name:
Performer (signature):
Date:
/
/
Reviewer
Date:
/
/
(signature):
Operational Qualification
No.
Item
Security function tests Not implemented because already implemented in Test 2-4 Password log management 3-4-1 function check Number of password characters 3-4-2 check
Operational Qualification Record
Criteria
Inspection results
Pass
Fail
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Samples are displayed in correct sequence after a sort.
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Displayed sample and data information matches the GCsolution report.
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Correct files exist in folder.
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Printed report is identical to GCsolution Test 2-10-4.
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Re-registered without overwriting. Data registered, without overwriting.
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Three sets of data are identical.
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3-4
Duplicated passwords cannot be used.
3-4-3
Failed login detection
3-4-4
User lockout function check
A password shorter than the minimum length is not accepted while a password satisfying the minimum length is accepted. Login is not possible with an incorrect password but possible with the correct password. The user is locked out for the specified lockout time.
3-4-5
Failed login log
The login lockout is registered in the log.
3-5
3-6
3-7 3-8 4
User access rights check Test of function to prevent duplicate user registration Data display, search, and sort Data recovery GCsolution automatic registration function check (Data integrity check)
Login prohibited with an incorrect password but possible with the correct password. “User Administration" item is enabled for OQ_USER_2 but disabled for OQ_USER_1. Duplicate user cannot be registered and the message “Unable to set the Login ID or User Name. It has been already used” appears. Samples are searched correctly.
5
GCsolution manual registration function check
6
Electronic signature check
Electronic signature information is printed correctly.
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7
System log recording check
Change to configuration settings is registered in the System Log.
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Performer (signature):
Date:
/
/
Reviewer
Date:
/
/
(signature):
Operational Qualification 3-13
Chromatopac C-R7A plus/C-R7Ae C-R7
Model Name Component ID Serial Number (S/N) No.
1
Operational Qualification Record
____
____
____
Item
Memory self-diagnost ic test
Applicable
plus ____
____
____
____
Initialization completes without error.
ROM VRAM RAM Power LED lights Keyboard LEDs light BOOT Version Program Version The version number matches the controlled version number.
Span Zeroing
Area
± 2 %
Height
± 1 % ±1% 1% 1% 2% 0.1 % 0.5 % 0.8 %
Retention time Range "PASS" is displayed for all results falling within the specified tolerances
Repeatability
Zero point
C H 2
Span
____
____
Area Height Retention time Area Height Retention time
Pass
Fail
µV
µV
µV
%FS
µV/min %
%
%
% % % % % % µV
µV
µV
%FS
µV/min %
Ver. Controled Ver.
± 0.1%FS 1 to 70µV/min
Slope test Accuracy
____
± 750 µV 992000 to 1008000µV ± 96µV
Linearity
Hardware validation
____
Inspection results
Zero point
2
____
Criteria
C H 1
Not Applicable
± 750µV 992000 to 1008000µV
Zeroing
± 96µV
Linearity Area
± 0.1%FS 1 to 70µV/min ± 2 %
Height
± 1 %
%
Retention time Area Height Retention time Area Height Retention time
±1% 1% 1% 2% 0.1 % 0.5 % 0.8 %
% % % % % % %
Slope test Accuracy
Range
Repeatability
Performer (signature):
Date:
/
/
Reviewer
Date:
/
/
(signature):
Operational Qualification 3-14
Operational Qualification Record
Chromatopac C-R8A
No.
Item
1
Memory self-diagnost ic test
____
____
____
____
____
____
Span
____
Zeroing Linearity
Height Retention time
Range
Repeatability
Zero point
C H 2
Span
Area Height Retention time Area Height Retention time
Linearity
Accuracy
µV %FS
± 2 %
µV/min %
± 1 %
%
±1% 1% 1% 2% 0.1 % 0.5 % 0.8 %
%
% % % % % % µV
µV
%FS
µV/min %
%
%
% % % % % %
Area
± 2 %
Height
± 1 % ±1% 1% 1% 2% 0.1 % 0.5 % 0.8 %
Retention time Range
Repeatability
Area Height Retention time Area Height Retention time
Controled Ver. µV µV
µV
Performer (signature):
Date:
/
/
Reviewer
Date:
/
/
(signature):
Fail
± 0.1%FS 1 to 70µV/min
Slope test
____
Ver.
± 750µV 992000 to 1008000µV ± 96µV
Zeroing
____
Inspection results Pass
± 0.1%FS 1 to 70µV/min Area
Accuracy
____
992000 to 1008000µV ± 96µV
Slope test
Hardware validation
____
Program Version Memory Check Status Diagnostic Status The version number matches the controlled version number. Zero point ± 750 µV
Initialization completes without error.
C H 1
2
____
Criteria
"PASS" is displayed for all results falling within the specified tolerances
Not Applicable
C-R8A
Model Name Component ID Serial Number (S/N)
Applicable
Operational Qualification 3-15
Operational Qualification Record
GC-2010 Gas Chromatograph Analysis System
Applicable
Not Applicable
Gas Chromatograph Analysis System No. 1
Item Repeatability test
Criteria Verify the repeatability for the peak, area and retention
Auto injector not used
time.
AREA value CV < 1.00% (FID, TCD) < 8.00%（FTD） < 3.00%（FPD） < 5.00%（ECD） Retention time CV < 0.30%
AREA value CV < 10.00% Retention time CV < 2.00% Auto injector used
Inspection result Injection unit ＿＿＿＿ Detector ＿＿＿＿ N/A
AREA value __ __.__ __ %
Injection unit ＿＿＿＿ Detector ＿＿＿＿ N/A
AREA value __ __.__ __ %
Injection unit ＿＿＿＿ Detector ＿＿＿＿ N/A
AREA value __ __.__ __ %
Injection unit ＿＿＿＿ Detector ＿＿＿＿ N/A
AREA value __ __.__ __ %
Injection unit ＿＿＿＿ Detector ＿＿＿＿ N/A
AREA value __ __.__ __ %
Injection unit ＿＿＿＿ Detector ＿＿＿＿ N/A
AREA value __ __.__ __ %
Injection unit ＿＿＿＿ Detector ＿＿＿＿ N/A
AREA value __ __.__ __ %
Injection unit ＿＿＿＿ Detector ＿＿＿＿ N/A
AREA value __ __.__ __ %
Retention time __ __.__ __%
Retention time __ __.__ __%
Retention time __ __.__ __%
Retention time __ __.__ __%
Retention time __ __.__ __%
Retention time __ __.__ __%
Retention time __ __.__ __%
Retention time __ __.__ __%
Performer (signature):
Date:
/
/
Reviewer
Date:
/
/
(signature):
Pass
Fail
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Operational Qualification
Change List
4. Change List When changing or deleting the contents of this document, or adding new information to this document, record the revision letter, 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. Revision letter: Assign an alphabetical letter for each revision, starting from A. Give the same revision letter for changes made at the same time. Change No: Enter the change number assigned in sequence from 1 onwards in accordance with “1-3 Entries and Revisions”. Increase this number over different revision letters (do not revert the Change No. to 1 when the revision letter proceeds from A to B, for example). 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. Revision letter
Change No.
Page
Reason
Date
Performer
Reviewer
Manager
Operational Qualification Revision letter
Change No.
Page
Change List Reason
Date
Performer
Reviewer
Manager
Operational Qualification Revision letter
Change No.
Page
Change List Reason
Date
Performer
Reviewer
Manager
