ZEMC-3008_Eng_GC2010_OQR0725

ZEMC-3008

Document No.

SHIMADZU GAS 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.

Signature Date

Print / /

Title

Performer

Company

The undersigned reviewer and manager report that the performer has completed the Operational Qualification Protocol successfully.

Signature Date

Print / /

Title

Reviewer

Company

Signature Date

Print / /

Title

Manager

Company

Rev. 3.00 Page 2 of 37

Operation Qualification Table of Contents

1. DEFINITIONS .....................................................................................................................................3 1-1 Documentation ...............................................................................................................................3 1-2 Scope.............................................................................................................................................4 1-3 Entries and Revisions ....................................................................................................................5

2. PRELIMINARY CHECKS....................................................................................................................6 2-1 Designation and Recording of Reviewer ........................................................................................6 2-2 Performer Identification & Approval................................................................................................7 2-3 Planning Items to be Evaluated in Operational Qualification..........................................................9 2-4 Calibration Certification and Instruments Used ............................................................................14 2-5 Other Tools Used .........................................................................................................................16

3. OPERATIONAL QUALIFICATION RECORD ...................................................................................17

4. CHANGE LIST..................................................................................................................................34

5. ATTACHED DOCUMENTS...............................................................................................................37

Table of Contents


Operation Qualification Definitions

1. Definitions

1-1 Documentation 1. The purpose of this document is to record the results of the Operational Qualification (OQ) 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 the instruments operate properly in accordance with their intended purpose.

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 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; 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 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 the cover sheet of this document as final approval of the Operational Qualification.

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

Change List and 5. Attached Documents. 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. However, the records of the inspections conducted using this document may be duplicated at the discretion of the Manager.


Operational Qualification Definitions

1-2 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: / /

Reviewer (signature): Date: / /


Operational Qualification Definitions

1-3 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 document. 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 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. 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 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 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: / / 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: / /

Reviewer 3 (Not applicable)

Name: Title: Date: / /



2-2 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:

Title:

Company name:

Certificate No.:

Signature:

Date: / /

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:

Title:

Company name:

Certificate No.:

Signature:

Date: / /

Performer 3 (Not applicable) Name:

Title:

Company name:

Certificate No.:

Signature:

Date: / /

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:

Manager

Signature:

Date: / /

Date: / /



If the Performer has been appointed by the Manager, complete the following.

Performer

Name:

Title:

Company name:

Signature:

Date: / /

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:

Manager

Signature:

Date: / / Date: / /



2-3 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 of 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 Model Name Gas Chromatograph GC-2010A

Auto Injector AOC-20i AOC-20i without power supply

Auto Sampler AOC-20s

Injection Unit SPL-2010 (Addition) WBI-2010 OCI/PTV-2010

Detector 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)

Data processing unit Computer GCsolution CLASS-Agent C-R7A plus C-R8A

Other options FLM-2/FLM-17

We hereby approve the system configuration specified above.

Performer (signature): Date: / / Reviewer (signature): Date: / /

Rev. 3.00 Page 10 of 37


2-3-2 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. Item Outline Applicable Not applicable1 Display/LED Test Verify the operation of displays and LEDs 2 Standard Self-diagnostic Test Verify. the status and operation of all parts 3 Firmware Verification Verify the version number of software 4 Temperature Test Verify that the temperature control is normal 5 Column Inlet Pressure Test Verify the accuracy of the column inlet pressure 6 Column Inlet Pressure Test Verify the function of the column inlet pressure program. 7 Flow Rate Accuracy Test Verify the flow rate accuracy of full-flow and septum purging. 8 Column Oven Test Verify the accuracy of the column oven temperature. 9 Temperature Program Test Verify the function of the column temperature program.

10 Sensitivity Test Verify the detector sensitivity.

2. AOC-20i Auto Injector Applicable Not Applicable

No. Item Outline Applicable Not applicable1 Display, LED Test Verify the display and LED operation. 2 ROM,RAM self-diagnostic Test Verify that ROM and RAM memory operates normally. 3 Firmware Verification Verify the program version. 4 Basic operation test Verify that the auto injector basic operation is correct.

3. AOC-20s Auto Sampler Applicable Not Applicable

No. Item Outline Applicable Not applicable1 Initial Operation Test Verify that the auto sampler basic operation is correct. 2 Firmware Version Check Verify the program version.

4. SPL-2010 Split/Splitless Injection unit Applicable Not Applicable

No. Item Outline Applicable Not applicable1 Column Inlet Pressure Test Verify the accuracy of the column inlet pressure. 2 Pressure Program Test Verify that the pressure program operates normally. 3 Flow Rate Test Verify the accuracy of the full-flow and septum purging.

5. WBI-2010 Direct Injection Unit Applicable Not Applicable

No. Item Outline Applicable Not applicable1 Column Inlet Pressure Test Verify the accuracy of the column inlet pressure 2 Pressure Program Test Verify that the pressure program operates normally 3 Flow Rate Test Verify the total flow rate and septum purge accuracy

6. OCI/PTV-2010 On-column/Programmable Temperature Injection Unit

Applicable Not Applicable

No. Item Outline Applicable Not applicable1 Temperature Test Verify that temperature control is normal. 2 Column Inlet Pressure Test Verify the accuracy of the column inlet pressure. 3 Pressure Program Test Verify that the pressure program operates normally. 4 Flow Rate Test Verify the accuracy of the full-flow and septum purging.

Rev. 3.00 Page 11 of 37


7. FID-2010 Flame Ionization Detector Applicable Not Applicable

No. Item Outline Applicable Not applicable1 Sensitivity test Verify the detector sensitivity.

8. FTD-2010 Flame Thermionic Detector Applicable Not Applicable


9. FPD-2010 Flame Photometric Detector Applicable Not Applicable


10. ECD-2010 Electron Capture Detector Applicable Not Applicable


11. FLM-2/FLM-17 Flame Warning Unit Applicable Not Applicable

No. Item Outline Applicable Not applicable1 Basic Operation Test Verify that the basic operation is correct..

12. Data Processing Unit GCsolution/CLASS-Agent Applicable Not Applicable

No. Item Outline Applicable Not applicablePersonal Computer

1-1 Computer boot-up test Checks that the computer boots up and runs normally. 1-2 Time and date check Checks that the PC time and date are correct. 1-3 Hard disk drive test Checks that the hard disk operates correctly. 1-4 Print driver check Checks the print driver test page and the version number. 1-5 Network connection test Checks that the network connection is normal.

GCsolution

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 connection 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.)

2-4 Security function tests Checks that the security functions operate, including restrictions on the number of password characters.

2-4-1 Password log management function check Checks that a duplicated password cannot be used.

2-4-2 Number of password characters check Checks that the restriction on the minimum number of password 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 log 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 System policy function check Checks the GCsolution system policy function. 2-7 Audit trail check Checks the audit trail functions. 2-8 Screen lock function check Checks the screen lock function.

2-9 Test of function to prevent duplicate user registration Confirms that a duplicate user name cannot be registered.

Rev. 3.00 Page 12 of 37


No. Item Outline Applicable Not applicable

2-10 Software function checks

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.

2-10-1 Peak integration Checks the peak integration functions.

2-10-2 Peak area percentage method Checks the quantitation calculation functions using the peak area percentage method.

2-10-3 Internal standard method Checks the quantitation calculation functions using the internal standard method.

2-10-4 External standard method Checks the quantitation calculation functions using the external standard method.

CLASS-Agent

3-1 Software version check Checks that the software is not changed to an inappropriate version.

3-2 Program alteration check Conducts the program alteration check.

3-3 Shimadzu User Authentication Tool connection check Checks the Shimadzu User Authentication Tool connection using database access and log registration.

3-4 Security function tests Checks that the security functions operate, including restrictions on the number of password characters.

3-4-1 Password log management function check Checks that a duplicated password cannot be used.

3-4-2 Number of password characters check Checks that the restriction on the minimum number of password operates.

3-4-3 Failed login detection Confirms that a failed login is detected.

3-4-4 User lockout function check Confirms that a user is locked out when the designated number of login failures is exceeded.

3-4-5 Failed login log Confirms that a failed login attempt is registered in the log.

3-5 User access rights check Confirms that software use is restricted according to differences in registered user access rights.

3-6 Test of function to prevent duplicate user registration Confirms that a duplicate user name cannot be registered.

3-7 Data display, search, and sort Checks that the sample search and sort work correctly and that the data is displayed normally.

3-8 Data recovery Checks that the data files registered in a database can be correctly recovered.

GCsolution automatic registration

4 GCsolution automatic registration function check (Data integrity check)

Checks that correct data is registered by GCsolution automatic registration to the database.

GCsolution manual registration

5 GCsolution manual registration function check Checks that correct data is registered by GCsolution manual registration to the database.

Electronic signature

6 Electronic signature check Checks the CLASS-Agent Manager electronic signature function.

System log

7 System log recording check Checks that the changes to the CLASS-Agent Manager system setting conditions are recorded to the system log.

4. Data Processing Unit Chromatopac C-R7A plus/C-R7Ae plus/C-R8A


No. Item Outline Applicable Not applicable

1 Memory self-diagnostic test Checks that the result of the ROM/RAM self-diagnostic check is normal.

2-1 Zero point Checks the measured voltage value at 0 V analog input. 2-2 Span Checks the measured voltage value at 1 V analog input.

2-3 Zeroing Checks the difference between measured voltage values in two measuring ranges.

2-4 Linearity Checks the linearity between 0 V and 1 V input voltages. 2-5 Slope test Slope test at fixed input voltage (0 V). 2-6 Accuracy Checks the accuracies for peak area, height, and retention time.

2-7 Range Checks the range (discrepancy from maximum to minimum) for peak area, height, and retention time.

2-8 Repeatability Checks the repeatability (coefficient of variance) for peak area, height, and retention time.

Rev. 3.00 Page 13 of 37


2-3-3 Planning System Evaluation Items Prior to implementing this operational qualification, confirm which items to be evaluated for 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 Analysis System Applicable Not Applicable

No. Item Outline Applicable Not applicable1 Repeatability tests Verify the repeatability for the peak area and retention time.

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.



Rev. 3.00 Page 14 of 37


2-4 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 ; Model: POP-612 Control No: Inspection date: Expiry date: Instrument name: Digital pressure gauge ; Model: MT10 Control No: Inspection date: Expiry date: Instrument name: ; Model Control No: Inspection date: Expiry date: * 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.

Instrument name: Precision membrane flow meter; Model: SF-1 Control No: Inspection date: Expiry date: Instrument name: Digital flow meter ; Model: DFM-1000 Control No: Inspection date: Expiry date: Instrument name: ; Model Control No: Inspection date: Expiry date: * Digital temperature indicator For the assured performance specifications of the recorder used to measure the column oven temperature accuracy, a precision of 0.5C shall be required at the 150C temperature required for the equipment inspections. Instrument name: Hybrid recorder ; Model: RD2212 Control No: Inspection date: Expiry date: Instrument name: Digital thermometer ; Model:ND522-3LP Control No: Inspection date: Expiry date: Instrument name: ; Model Control No: Inspection date: 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 0.5C shall be required in the temperature range (150 C) required for the equipment inspections. Instrument name: Sheathed resistance temperature sensor; NRHS1-0 Control No: Inspection date: Expiry date: Instrument name: ; Model Control No: Inspection date: Expiry date:

Rev. 3.00 Page 15 of 37


* Thermocouple

For the assured performance specifications of the thermocouple used to measure the column oven temperature accuracy, a precision rating of 0.6C shall be required in the temperature range (150 C) required for the equipment inspections. Instrument name: K-sheath thermocouple ; Model: SCH S1-0 Control No: Inspection date: Expiry date: Instrument name: ; Model Control No: Inspection date: 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: Expiry date: Instrument name: ; Model Control No: Inspection date: Expiry date:

(2) 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/L 2mL x 5 Ampoules221-44247-08 For the detector sensitivity test and the system repeatability test of FID

Lot No.: Expires: n-decane/n-hexane solution 1000ng/L 2mL x 5 Ampoules221-44247-11

For the detector sensitivity test and system repeatability test of TCD Lot No.: Expires:

Azobenzene/n-hexane solution 1ng/L 2mL x 5 Ampoules221-44247-07 For the detector sensitivity test and the system repeatability test of FTD (N compounds)

Lot No.: Expires: Malathion/n-hexane solution 100pg/L 2mL x 5 Ampoules221-44247-14

For the detector sensitivity test and the system repeatability test of FTD (P compounds) Lot No.: Expires:

Tributyl phosphate/n-hexane solution 1ng/L 2mL x 5 Ampoules221-44247-15 For the detector sensitivity test and the system repeatability test of FTD (P compounds)

Lot No.: Expires: Tributyl phosphate/n-hexane solution 10ng/L 2mL x 5 Ampoules221-44247-12

For the detector sensitivity test and the system repeatability test of FPD (P compounds) Lot No.: Expires:

Dodecanethiol/n-hexane solution 10ng/L 2mL x 5 Ampoules221-44247-13 For the detector sensitivity test and the system repeatability test of FPD (S compounds)

Lot No.: Expires: -BHC/n-hexane solution 0.1ng/L 2mL x 5 Ampoules221-44247-03

For the detector sensitivity test and the system repeatability test of ECD Lot No.: Expires:

Rev. 3.00 Page 16 of 37


2-5 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 [221-41444-01] ; when using SPL for inspection * Glass insert for splitless, WBI [221-48335-01] ; when using WBI for inspection

(2) Items prepared by the Shimadzu Service Company

* Devices Glass vial 1.5mL [221-34272-92] ; for AOC-20i/s Vial cap 1.5mL [221-34273-92] ; for AOC-20i/s Vial septum 1.5mL [221-41239-91] ; for AOC-20i/s Glass vial 4 mL [221-34267-92] ; for AOC-20i/s Vial cap 4 mL [221-34268-92] ; for AOC-20i/s Vial septum 4 mL [221-34266-92] ; for AOC-20i/s Columns (To test GC unit. Select from following four types.) CBP1-M25-025 [221-28635-25] ; for sensitivity, repeatability tests DB-1-30N-STD [J&W P/N122-1032] ; for sensitivity, repeatability tests ZB-1 (30m x 0.25mmID, 0.25 m) ; for sensitivity, repeatability tests Rtx-1 (30m x 0.25mmID, 0.25 m) ; 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 [221-28647-12] for OCI/PTV and WBI tests DB-1-15M-STD [J&W P/N125-1032] for OCI/PTV and WBI tests Pressure measurement adaptor [221-42686-91] ; for pressure test Pipe MF-MF [201-48555-**] ; to connect adapter and pressure gauge Column holder [221-31567-91] ; to fix temperature sensor Microsyringe MS-G10AC [221-45169-01] ; for manual injection Microsyringe (CAL)10F-RA6 [221-45170-01] ; for manual injection

* Others Vulcanized tape [018-21330] for pressure measurement adapter Cable [223-06064-90] 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.



Rev. 3.00 Page 17 of 37

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 Model Name GC-2010

Component ID

Serial Number (S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ No. Item Criteria Results Pass Fail

All LEDs light. LED 1

Display, LED test

Verify the display and LED operation.

Screen contrast adjustment is possible. Display

2

Standard self-diagnostic test

Verify the status and operation of all parts.

"Good" displayed as the result of the self-diagnostic test.

Version: Version number and build number are displayed. Ver. Build No.:

Version: 3

Firmware version check

Verify the program version. The version No. and build No.

matches the controlled version number.

Controled Ver. No. Build No.:

TEMP LED lights green. 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

4

Temperature test

Verify that temperature control is normal.

Displayed actual values agree to the set values within 1C.

AUX5 __ __.__C __ __.__C

Pressure gauge correction value __.__Pa

Pressure gauge reading __ __.__Pa

Inspection pressure gauge reading 10.0 3.0Pa

Post-correction reading __ __.__Pa Pressure gauge correction value __.__Pa

Pressure gauge reading __ __ __.__Pa


Post-correction reading __ __ __.__Pa Pressure gauge correction value __.__Pa


5

Column inlet pressure test

Verify the accuracy of the column inlet pressure.


Post-correction reading __ __ __.__Pa



Rev. 3.00 Page 18 of 37


No. Item Criteria Results Pass Fail

Monitored pressure 6 minutes after start 250.0 5.0 kPa __ __ __.__Pa

6

Pressure program test

Verify that the pressure program operates normally.

Inspection pressure gauge reading 8 minutes after start250.0 20.0 kPa __ __ __.__Pa

Septum purge vent measured flow rate 3.0 1.0mL/min

Septum purge __.__ mL/min

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

200 20mL/min Total _________mL/min Split vent _________mL/min

7

Flowrate test Verify the accuracy of the full-flow and septum purging.

Total of septum purge and split vent flow rate values500 35mL/min Total

_________mL/min

Temp. correction value __.__C Temp. sensor reading ___ __.__C

Inspection temperature sensor displayed value 50.03.2 Corrected temp. value ___ __.__C

Temp. correction value __.__C Temp. sensor reading __ __ __.__C

Inspection temperature sensor displayed value 150.04.2 Corrected temp. value __ __ __.__C

Temp. correction value __.__C

Temp. sensor reading __ __ __.__C

8

Column oven test

Verify the accuracy of the column oven temperature.

Inspection temperature sensor displayed value 280.05.7 2804 Corrected temp. value __ __ __.__C

Monitored temperature 6 minutes after start 200 1C

__ __ __C Inspection temperature reading 8 minutes after start 200.0 4.7C __ __ __.__C 9

Temperature program test

Verify that the column temperature program operates normally. Using a temperature sensor with 1C minimum

display increment 200 3C __ __ __C

C16AREA value

Vs

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.

Calculated S value __ __.__ __x10

-3C/g

C10AREA value Vs Flowrate at vent __ __.__ __mL/min

10

Sensitivity test

Verify the detector sensitivity.

TCD ( Applicable Not Applicable) Calculated S value Inj. unit ( ) 4.00 x 103mVml/mg min.

Calculated S value

__ __.__ __x103VmL/mg



Rev. 3.00 Page 19 of 37


3-2 AOC-20i Auto Injector Applicable Not Applicable

Single Dual system, main injector Model Name AOC-20i

Component ID

Serial No. (S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____


1 Display, LED test Verify the display and LED operation.

All LEDs light, except decimal point.

2 ROM RAM self diagnosis Verify that ROM and RAM memory operates normally.

Display shows "000". Display:

Version number is displayed. Version No. 3


Verify the program version. The version number matches the

controlled version number. Controled Ver. No.

4 Basic operation test

Verify that the auto injector basic operation is correct.

Sample injected into the GC and GC operation starts.

Not Applicable Dual system, sub injector Model Name AOC-20i

Component ID

Serial No. (S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____


1 Display, LED test Verify the display and LED operation.

All LEDs light, except decimal point.

2 ROM RAM self diagnosis Verify that ROM and RAM memory operates normally.

Display shows "000". Display:





4

Basic operation test

Verify that the auto injector basic operation is correct.

Sample No.1 transferred to the main injector, sample No. 2 transferred to the sub-injector. Sub-injector injects into the GC simultaneously with the main AOC.



Rev. 3.00 Page 20 of 37


3-3 AOC-20s Auto Sampler Applicable Not Applicable

Model Name AOC-20s Component ID

Serial No. (S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____


1 Initial operation test

Verify that the auto sampler basic operation is correct.

LED lights green, not red.







Rev. 3.00 Page 21 of 37


3-4 SPL-2010 Split/Splitless Injection Unit Applicable Not Applicable

Model Name SPL-2010 Component ID

Serial No. (S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____







Inspection pressure gauge reading 200.020.0Pa



1






2



Inspection pressure gauge reading 8 minutes after start 250.0 20.0 kPa __ __ __.__Pa

Septum purge vent measured flow rate 3.01.0mL/min

Septum purge __.___mL/min

Split vent __.__ mL/min Total of septum purge and split vent flow rate values

10.03.0mL/min Total ____. __mL/min Split vent ________mL/min Total of septum purge and split vent flow rate values

20020mL/min Total ________mL/min Split vent ________mL/min

3

Flowrate test

Verify the accuracy of the full-flow and septum purging.

Total of septum purge and split vent flow rate values 50035mL/min Total

________mL/min



Rev. 3.00 Page 22 of 37


3-5 WBI-2010 Direct Injection Unit Applicable Not Applicable

Model Name WBI-2010 Component ID

Serial No. (S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____










1






2



Inspection pressure gauge reading 8 minutes after start250.0 20.0 kPa __ __ __.__Pa


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 3

Flowrate test

Verify total flow (column outlet flow) and septum purge accuracy.

Column outlet measured flow rate 100 15mL/min Measured flow ______mL/min



Rev. 3.00 Page 23 of 37


3-6 OCI/PTV-2010 On-column/Programmable Temperature Injection Unit


Model Name OCI/PTV-2010 Component ID

Serial No. (S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____


Measured temperature value displayed immediately after start: 50 5C __ __.__

Measured temperature value displayed 8 minutes after start: 250 5C __ __ __.__

1

Temperature test

Verify that temperature control is normal.

Fan operation begins 10 minutes after start.












2


Verify column inlet pressure accuracy.




3



Inspection pressure gauge reading 8 minutes after start 250.0 20.0 kPa __ __ __.__Pa


Septum purge __.___mL/min

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

200 20mL/min Total __________mL/min Split vent

_________mL/min

4

Flow rate test Used for OCI, so not conducted.

Verify accuracy of total flow and septum purge.

Total of septum purge and split vent flow rate values 500 35mL/min Total

_________mL/min



Rev. 3.00 Page 24 of 37


3-7 FID-2010 Flame Ionization Detector Applicable Not Applicable Addition 1

Model Name FID-2010 Component ID

Serial No. (S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____


C16AREA valueVs

1

Sensitivity test Injection unit ( )

Verify detector sensitivity

Sensitivity S calculated value Make-up gasN2 10.0x10-3C/g Make-up gasHe 7.00x10-3C/g

Sensitivity S calculated value __ __.__ __x10

-3C/g

Addition 2 Applicable Not Applicable


Serial No. (S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____


C16AREA valueVs

1





-3C/g

Addition 3 Applicable Not Applicable


Serial No. (S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____


C16AREA valueVs

1





-3C/g



Rev. 3.00 Page 25 of 37


3-8 FTD-2010 Flame Thermionic Detector Applicable Not Applicable Addition 1 Model Name FTD-2010

Component ID

Serial No. (S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____


AREA value Vs N (Applicable N/A)

Azobenzen MDQ 2.00 x 10-12 gN/s MDQ __.__ __ x 10-12gN/s

AREA value Vs

1



P (Applicable N/A) Malathion Tributyl phosphate MDQ 0.900 x 10-12 gP/s

MDQ __.__ __ __ x 10-12gP/s

Addition 2 Applicable Not Applicable Model Name FTD-2010

Component ID

Serial No. (S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____


AREA value Vs N (Applicable N/A)

Azobenzen MDQ 2.00 x 10-12 gN/s MDQ __.__ __ x 10-12gN/s

AREA value Vs

1



P (Applicable N/A) Malathion Tributyl phosphate MDQ 0.900 x 10-12 gP/s

MDQ __.__ __ __ x 10-12gP/s



Rev. 3.00 Page 26 of 37


3-9 FPD-2010 Flame Photometric Detector Applicable Not Applicable Model Name FPD-2010

Component ID

Serial No. (S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____


AREA value Vs S (Applicable N/A) Dodecane thiol MDQ

40.0 x 10-12 gS/s MDQ __ __.__ x 10-12gS/s

AREA value Vs

1



P (Applicable N/A) Tributyl phosphate MDQ2.00x10-12gP/s MDQ __.__ __ x 10-12gP/s

3-10 ECD-2010 Electron Capture Detector Applicable Not Applicable Addition 1 Model Name ECD-2010

Component ID

Serial No. (S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____


AREA value Vs 1


Verify the detector sensitivity. -BHC MDQ 80.0 x

10-15 g/s MDQ __ __.__ x 10-1g/s

Addition 2 Applicable Not Applicable Model Name ECD-2010

Component ID

Serial No. (S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____


AREA value Vs 1



10-15 g/s MDQ __ __.__ x 10-1g/s



Rev. 3.00 Page 27 of 37

Operational Qualification Operational Qualification Record Addition 3 Applicable Not Applicable Model Name ECD-2010

Component ID

Serial No. (S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____


AREA value Vs 1



10-15 g/s MDQ __ __.__ x 10-1g/s

Addition 4 Applicable Not Applicable Model Name ECD-2010

Component ID

Serial No. (S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____


AREA value Vs 1



10-15 g/s MDQ __ __.__ x 10-1g/s

3-11 FLM-2/FLM-17 Flame Warning Unit Applicable Not Applicable

Model Name FLM-2/FLM-17 Component ID


1

Basic operation test

Verify that the basic operation is correct.

The FLM (amplifier unit) lamp goes out correctly.



Rev. 3.00 Page 28 of 37


3-12 GCsolution /CLASS-Agent Applicable Not Applicable



Model Name Workstation GCsolution Serial Number (S/N)

____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____

No. Item Criteria Inspection results Pass Fail

1-1 Computer boot-up test Windows starts up normally. Computer Basic / / / / 1-2 Time and date check Date and time are correct. Permitted range

Drive Error detection

C

1-3 Hard disk drive test No error detected for any drive.

Test page printed correctly. Ver. 1-4 Print driver check The driver version number

matches the controlled version number. Controled Ver.

1-5 Network connection test Not implemented because not connected to network

No packets lost. Designated IP address

GCsolution Applicable Not Applicable

Ver. 2-1 Software version check The version number matches the controlled version number. Control ed Ver.

2-2 Program alteration check OK is displayed for every item.

Server name for the connected database is correct.

Server name:

Login possible from [View event log].

2-3

Shimadzu Authentication Tool connection check Not implemented because not used with GCsolution

Lockout by GCPrun.exe is registered. 2-4 Security function test

2-4-1 Password log management function check Duplicated passwords cannot be used.

2-4-2 Number of password characters check A password shorter than the minimum length is not accepted while a password satisfying the minimum length is accepted.

2-4-3 Failed login detection Login is not possible with an incorrect password but possible with the correct password.

2-4-4 User lockout function check The user is locked out for the specified lockout time. 2-4-5 Failed login log The login lockout is registered in the log.

Rev. 3.00 Page 29 of 37





2-5 User access rights check 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. 2-6 System policy function check Overwriting other method files is prohibited.

2-7 Audit trail check Audit trail details (Date&Time, Modification, Reason) are displayed correctly.

The Screen lock function operates. 2-8 Screen lock function check "OQ_USER_1" cannot unlock the screen but "OQ_USER_2" can

unlock the screen.

2-9 Test of function to prevent duplicate user registration 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. 2-10-1 Peak integration

Peak baseline processing is conducted in the "Demo_Data-IT03.gcd" report.

2-10-2 Peak area percentage method The results match. 2-10-3 Internal standard method The results match.

The results match. 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.

Calibration curve information is printed. 2-10-4 External standard method

Unit Parameters and Peak Integration, peak Identification, and Quantitative parameters and Compound Table are printed.

CLASS-Agent Software Applicable Not Applicable

The version number matches the controlled version number. Ver.

Controled Ver.

CLASS-Agent manager Shimadzu User Authentication Tool

3-1 Software version check

3-2 Program alteration check "Total: Pass" appears for all software.

Server name for the connected database is correct.

Server name:

Login possible from [View event log].

3-3

Shimadzu User Authentication Tool connection check Not implemented because already implemented in Test 2-3

Lockout by AgentMan2.exe is registered.

Rev. 3.00 Page 30 of 37





3-4 Security function tests Not implemented because already implemented in Test 2-4

3-4-1 Password log management function check Duplicated passwords cannot be used.

3-4-2 Number of password characters check A password shorter than the minimum length is not accepted while a password satisfying the minimum length is accepted.

3-4-3 Failed login detection Login is not possible with an incorrect password but possible with the correct password.

3-4-4 User lockout function check The user is locked out for the specified lockout time. 3-4-5 Failed login log The login lockout is registered in the log.

Login prohibited with an incorrect password but possible with the correct password. 3-5 User access rights check User Administration" item is enabled for OQ_USER_2 but disabled for OQ_USER_1.

3-6 Test of function to prevent duplicate user registration 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. Samples are displayed in correct sequence after a sort. 3-7 Data display, search, and sort Displayed sample and data information matches the GCsolution report.

3-8 Data recovery Correct files exist in folder.

Printed report is identical to GCsolution Test 2-10-4. 4 GCsolution automatic registration function check (Data integrity check) Re-registered without overwriting.

Data registered, without overwriting. 5 GCsolution manual registration function check Three sets of data are identical. 6 Electronic signature check Electronic signature information is printed correctly. 7 System log recording check Change to configuration settings is registered in the System Log.

Rev. 3.00 Page 31 of 37


3-13 Chromatopac C-R7A plus/C-R7Ae Applicable Not Applicable



Model Name C-R7 plus Component ID Serial Number

(S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____


ROM VRAM RAM Power LED lights Keyboard LEDs light BOOT Version Program Version Ver.

1 Memory self-diagnostic test

Initialization completes without error.

The version number matches the controlled version number.

Controled Ver.

Zero point 750 V V Span 992000 to

1008000V V

Zeroing 96V V Linearity 0.1%FS %FS Slope test 1 to 70V/min V/min

Area 2 % % Height 1 % % Accuracy Retention time 1 % % Area 1 % % Height 1 % % Range Retention time 2 % % Area 0.1 % % Height 0.5 % %

CH1

Repeatability

Retention time 0.8 % % Zero point 750V V Span 992000 to

1008000V V


Area 2 % % Height 1 % %

Accuracy

Retention time 1 % % Area 1 % % Height 1 % %

Range

Retention time 2 % % Area 0.1 % % Height 0.5 % %

2 Hardware validation

"PASS" is displayed for all results falling within the specified tolerances

CH2

Repeatability

Retention time 0.8 % %

Rev. 3.00 Page 32 of 37


3-14 Chromatopac C-R8A Applicable Not Applicable



Model Name C-R8A Component ID Serial Number

(S/N) ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____


Program Version Ver. Memory Check Status Diagnostic Status 1

Memory self-diagnostic test

Initialization completes without error. The version number matches the controlled version

number. Controled Ver.

Zero point 750 V V Span 992000 to

1008000V V



CH1

Repeatability

Retention time 0.8 % % Zero point 750V V Span 992000 to

1008000V V



2 Hardware validation

"PASS" is displayed for all results falling within the specified tolerances

CH2

Repeatability

Retention time 0.8 % %

Rev. 3.00 Page 33 of 37


3-15 GC-2010 Gas Chromatograph Analysis System


Gas Chromatograph Analysis System

No. Item Criteria Inspection result Pass Fail

AREA value __ __.__ __ %

Injection unit Detector N/A

Retention time __ __.__ __%

AREA value __ __.__ __ %



AREA value __ __.__ __ %



AREA value __ __.__ __ %



AREA value __ __.__ __ %



AREA value __ __.__ __ %



AREA value __ __.__ __ %



AREA value __ __.__ __ %

1 Repeatability test

Verify the repeatability for the peak, area and retention time.

Auto injector not used AREA value CV < 10.00% Retention time CV < 2.00% Auto injector used AREA value CV < 1.00% (FID, TCD) < 8.00%FTD < 3.00%FPD < 5.00%ECD Retention time CV < 0.30%





Rev. 3.00 Page 34 of 37

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

Rev. 3.00 Page 35 of 37


Revision letter


Rev. 3.00 Page 36 of 37


Revision letter


Rev. 3.00 Page 37 of 37

Operational Qualification Attached Documents

5. Attached Documents

* Appended data shall be numbered by adding letters in sequence from A to the final page number of this document (e.g.

37-A1/3 - A3/3) and appended to this document after entry in the list above.



Attached Item Description Page 2-4 Calibration Certificates Pressure gauge Certificate of traceability Flow meter Certificate of traceability Digital temperature indicator Certificate of traceability Resistance temperature sensor Certificate of traceability Thermocouple Certificate of traceability Programmable DC

voltage/current generator Certificate of traceability

Standard reagents for performance inspections

Certificate

3-1 GC-2010 Gas Chromatograph Test 10 FID Sensitivity test Verification Data Appendix 37- TCD sensitivity test Verification Data Appendix 37-

3-7 FID-2010 Flame Ionization Detector Verification Data Appendix 37- Test 10 FID Sensitivity test Verification Data Appendix 37-

3-8 FTD-2010 Flame Thermionic Detector Verification Data Appendix 37- 3-9 FPD-2010 Flame Photometric Detector Verification Data Appendix 37- 3-10 ECD-2010 Electron Capture Detector Verification Data Appendix 37- 3-12 GCsolution/Class-Agent Workstation Test 1-3 Hard disk drive check results Verification data Appendix 37- Test 1-4 Printer driver test page Verification data Appendix 37- Test 1-5 Network connection test results Verification data Appendix 37- Test 2-2 GCsolution program alteration check results Verification data Appendix 37- Test 2-3 Lockout log Verification data Appendix 37- Test 2-7 Audit trail Verification data Appendix 37- Test 2-10 GCsolution function check results Verification data Appendix 37- Test 3-2 CLASS-Agent program alteration check

results Verification data Appendix 37-

Test 3-3 Lockout log Verification data Appendix 37- Test 3-7 Data display, search, and sort Verification data Appendix 37- Test 4 Automatic database registration function

check results Verification data Appendix 37-

Test 5 Manual database registration function check results

Verification data Appendix 37-

Test 6 Electronic signature check Verification data Appendix 37- Test 7 System log recording check Verification data Appendix 37- Appendix 37- 3-13 Chromatopac C-R7Aplus/C-R7Aeplus Verification data Appendix 37- 3-14 Chromatopac C-R8A Verification data Appendix 37- 3-4-1 GC-2010 Analysis System Test 1 Repeatability Test Verification data Appendix 37-