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Combi-PAL OQ Document

LT 7.5.1 QF 018, REV. 1.2 / Document Serial Number: XXXXXX_XXX_XX

Combi-PAL Operational Qualification

Execution Approval Document

The signatures below represent approval of all interested parties for the

execution of the LEAP Technologies Combi-PAL Operational Qualification Protocol.

Company Name:______

Name: Signature: Title: Date:

LEAP Technologies Representative

Name: Signature: Title: Date:

Signature Page

The signatures below represent all those individuals who may have executed or assisted in the execution of the LEAP Combi-PAL Operational Qualification Protocol.

Company Name:______

Name: Signature/Title: Initials Date:

LEAP Technologies Representative:

Name: Signature/Title: Initials Date:

I.  Table of Contents

I.  Table of Contents

II.  Revision History

III.  PAL System Identification

IV.  Scope /Purpose

V.  Documentation

VI.  Procedure

VII.  General Considerations

VIII.  Laboratory Requirements

1.  Temperature

2.  Space Requirement

3.  Power Requirement

4.  Safety

5.  Accessories

IX.  Temperature Test

1.  Heated Headspace Syringe Holder

2.  Heated Agitator

X.  Injector Reproducibility Tests

1.  Preparation

2.  Testing with Headspace Syringe

3.  Testing with Liquid Syringe

4.  Calculation

XI.  Scope of OQ Test Acceptance Limits

XII.  Summary

XIII.  Certification

XIV.  Non-Conformance Record

  1. Addendum Tables
II.  Revision History
Revision / Date / Author / Reason for Changes
Rev A / July 16, 2001 / Ingo Christ
LEAP Technologies / Initial Protocol
Rev B / June 24, 2002 / Ingo Christ
LEAP Technologies / Syringe Accuracy is added for the 250mL syringe. Corrections to spelling errors and other inaccuracies were made.
1.0 / Jan. 22, 2004 / Eric Wethington and Michael Horton
LEAP Technologies / Format to conform to LEAP Quality System
1.1 / February 20, 2004 / Eric Wethington and Michael Horton
LEAP Technologies / Clarification of section titles IX and X.
Specification changes to reflect CTC specifications (for Agitator and HS syringe holder temperature).
III.  Combi-PAL System Identification
Serial Number:
Customer:
Address:
Building/Location:
Main Contact:
Distributor:
Cruise Control:
Date Install:
Warranty until:

IV. Scope / Purpose

The objective of this Document is to define Operational Qualification (OQ) requirements and acceptance criteria for the PAL System.

The Operational Qualification procedure is part of the validation process, which consists of Installation Qualification (IQ), OQ, Performance Qualification (PQ), Preventive Maintenance (PM), method validation and data validation to ensure compliance with products or method requirements.

Successful completion of this OQ Document will provide a high degree of assurance that the PAL System is performing throughout a representative operating range.

V.  Documentation

All qualification work will be performed as defined in the approved document (protocol), and all the documentation will be completed concurrently with the execution of the qualification studies. Data entries must be completed during the qualification testing.

Any deviation or exceptional case observed during the process of the OQ must be documented in the attached “OQ Non Conformance Record”.

If any point or section is not applicable for the specific PAL Autosampler System to be tested, it shall be marked with N/A (= not applicable).

All required documentation must be filed together in one location. To ease this process, LEAP provides the customer with a System Log book.

The documentation will be reviewed and approved by the lab management who initially approved the qualification studies.

A sign-off section is provided on each page of this document

Note: This page must be signed by both parties to confirm this agreement.

______

LEAP Representative Date Company Representative Date

VI.  Procedure

This is an overview of all action, which will take place. It is strongly recommended to perform an IQ on the system prior to the OQ or before a system inspection is necessary. For the system inspection, the following sections from the IQ are required:

Section VIII, IX, X and XI. Please consider a PM before doing the OQ Test.

These sections need to be attached to this record.

The OQ will verify that the PAL and Load System perform as intended throughout a representative operating range. Percent difference from the calculated value for each of 5 injections shall not exceed 2% for 250mL syringe. It is not useful to verify the accuracy of the 2500mL headspace syringe, since the syringe pulls a significant amount of liquid instead of gas. The result will always be lower when pulling liquids. The results will be determined by weighing each vial before and after the liquid is withdrawn. The operating range for the syringe will be 25%, 50% and 100%. The correlation coefficient must be 0.999 or higher.

The relative standard deviation (RSD) for five injections of each syringe type and amount shall be less than or equal to 1%. In total, there will be 30 injections. Since the Pal only measures the length of the syringe scale, the data for the 250mL liquid syringe is representative of all liquid syringes, and the 2500mL headspace syringe is representative of all headspace syringes.

Additionally, the OQ will determine whether the heated compartments of the syringe heater and sample incubator meet manufacturer’s specifications. Other tests address the operation of the sample agitator.

VII.  General Considerations

The PAL consists of a syringe-based X-Y-Z liquid, headspace and SPME handling system that can be adapted to a wide range of analytical instrumentation and sample formats. Common applications of the Combi-PAL are sample preparation of headspace or liquid samples for gas chromatography and mass spectroscopy. The Combi-PAL can be used in combination with almost any other equipment as part of a complete system.

From the point of view of LEAP Technologies, it is almost impossible to insist on one fixed OQ test. The following points shall give the customer and the certification engineer the flexibility, but also the guidance as to what is reasonable from the analytical point of view and what the limits are. The tests are described in detail. If one parameter has to be changed for any reason, consider the points below to make a decision.

The OQ test of choice from our point of view is:

·  Reproducibility testing via a certified balance

·  Temperature test via certified thermocouples

VIII.  Laboratory Requirements

1.  Temperature

Verify that the environmental requirements for safe operations are met for proper installation and use.

Temperature 10 °C to 30 °C Actual Temperature:______°C Pass ( )

______°F Fail ( )

2.  Space Requirements

The dimensions and weight of the PAL System allow the system to be placed on almost any laboratory bench. It is important to verify that the system can be placed in a horizontal position and that the bench is designed to carry the weight. Add a few centimeters to the minimum measurement around the system to allow space for cables and tubing.

GC PAL, DI PAL, Combi-PAL: Width: 830 mm

Depth: 390 mm

Height: 650 mm

3.  Power Requirements

Verify that the power supply is designed for the correct operating voltage of:

97.5 – 264 VAC

4.  Safety Measures / Precautions

The safety measures are outlined in the User Manual, page 2 and in any “Addendum to the User Manual,” e.g., the Fiber Bakeout Station, if applicable.

The Safety Guard must be installed. If the user declines the installation, it shall be noted in the “Non-Conformation Record”.

5.  Accessories

The customer is responsible for a properly maintained and functional chromatographic system. All supplies necessary to run or to maintain the instrument need to be available, such as headspace and direct liquid injection syringes, high purity gases for carrier gas and detector, wash solvents, deionized water, etc. During the procedure, a certified balance needs to be available for the validation engineer. LEAP will supply 250mL syringes and certified thermocouples.

IX.  Temperature Test

1.  Heated Headspace Syringe Holder

For the temperature check inside the Headspace syringe holder, please check that the batteries for the certified thermocouples are still working properly. Stick the front part of the multiplier into the bored-out plunger for the headspace syringe and insert it into the holder. Mount the holder with the testing equipment into the LEAP autosampler. Make sure that you don’t push the bored out plunger too far into the syringe.

Please go to the utility menu with the help of the hand-held remote. This enables you to set the temperature of the syringe and the heated agitator. Please set the “standby temp” for the heated syringe to 35° C and wait until the appropriate temperature is reached on the hand-held remote. Next, crosscheck it with the certified thermocouples. Expect approximately 0.5° C less than the actual temperature on the hand-held remote, since there is a distance of 0.5cm from the heater to the middle of the syringe.

The temperature specification is 33.5 - 36° C for the Combi-PAL readout. The actual temperature determined by the certified thermocouple must be ± 3° C of the readout value.

______

Combi-PAL Temp Readout Certified Thermocouple pass/fail

Now increase the “standby temp” to 100° C.

The Temperature specification is 98 - 101° C for the Combi-PAL readout. The actual temperature determined by the certified thermocouple must be ± 3° C of the readout value.

______

Combi-PAL Temp Readout Certified Thermocouple pass/fail

2.  Heated Agitator

For the temperature test of the heated agitator, fill a 10mL vial with deionized water and close it with a septum. Stick the thermocouple’s wire through the septum. Place the appropriate insert for 10mL vials into the agitator and add the prepared vial.

Now go to the utility menu and check the agitator in the tray holder menu option. Set the standby temperature at 35° C. Start the agitator by using the F1 key.

The Combi-PAL temperature readout specification is 34 - 36° C. The actual temperature as determined by the certified thermocouple must be ± 3° C of the readout temperature.

______

Combi-PAL Temp Readout Certified Thermocouple pass/fail

Now increase the “standby temp” to 80° C.

The Combi-PAL temperature readout specification is 79 - 81° C. The actual temperature as determined by the certified thermocouple must be ± 2% of the readout temperature.

______

Combi-PAL Temp Readout Certified Thermocouple pass/fail

X.  Injector Reproducibility Tests

1.  Preparation

Next, prepare some vials, 10 or 20mL headspace vials are suggested for the headspace syringe test, and 2mL vials are suggested for the liquid syringe test. Add deionized water until half full and crimp with standard septa and caps. Number them and weigh them on the certified balance provided by the customer. Plastic or Teflon septa are recommended for use with the 250mL and its #3 needle tip because GC style rubber septa are not compatible with that needle style. Instead, they are compatible with needle style #5, which is used for the headspace and typical 10mL GC syringes. Make sure that you wear gloves and that the vials are absolutely dry on the outside. Weigh each vial twice and record the data below. If the measurement during the second weighing changed more than 0.002g, please repeat this step until it’s constant. Enclose all balance print out sheets with the final validation report.

Every effort should be made to minimize bubble formation when withdrawing liquid from the sample vials. In this respect, the test differs from the intended application in which gas is withdrawn from the headspace vials, and smaller liquid volumes (typically 1 - 5mL compared to 62.5 - 250mL) are withdrawn for liquid GC injections. Larger volumes, however, are required for accurate and repeatable weight determinations.

2.  Testing with Headspace Syringe

Please program the following parameters for the PAL System:

·  Power on the PAL System and load it with 30 vials prepared prior to the test

·  Install a 2500mL syringe with the heated holder

·  Define the Start Signal as immediate

·  Fill Wash 1 with deionized water.

Create the following methods

Name: / HS25% / Name: / HS50%
Cycle: / GC Inj. / Cycle: / GC Inj.
Sample Volume: / 620mL / Sample Volume: / 1250mL
Air Volume: / 0 / Air Volume: / 0
Pre Cln Slv 1: / 3 / Pre Cln Slv 1: / 3
Pre Cln Slv 2: / 0 / Pre Cln Slv 2: / 0
Pre Cln Spl: / 0 / Pre Cln Spl: / 0
Fill Speed: / 50mL/s / Fill Speed: / 50mL/s
Fill Strokes: / 4 / Fill Strokes: / 4
Pullup Delay: / 5s / Pullup Delay: / 5s
Inject to: / Waste2 / Inject to: / Waste2
Inject Speed: / 500mL/s / Inject Speed: / 500mL
Pre Inj Delay: / 200ms / Pre Inj Delay: / 200ms
Pst Inj Delay: / 200ms / Pst Inj Delay: / 200ms
Pst Cln Slv 1: / 1 / Pst Cln Slv 1: / 1
Pst Cln Slv 2: / 0 / Pst Cln Slv 2: / 0
Name: / HS100%
Cycle: / GC Inj.
Sample Volume: / 2500mL
Air Volume: / 0
Pre Cln Slv 1: / 3
Pre Cln Slv 2: / 0
Pre Cln Spl: / 0
Fill Speed: / 50mL/s
Fill Strokes: / 4
Pullup Delay: / 5s
Inject to: / Waste2
Inject Speed: / 500mL/s
Pre Inj Delay: / 200ms
Pst Inj Delay: / 200ms
Pst Cln Slv 1: / 1
Pst Cln Slv 2: / 0

Now add the following jobs:

Tray: Tray 1 Tray 1: Tray 1:

First: 1 6 11

Last : 5 10 15

Increment: 1 1 1

Count: 1 1 1

Method: HS25% HS50% HS100%

Run the jobs. Weigh the vials and enter the weights into the following table. Make sure that you wear gloves and that the vials are absolutely dry on the outside. Weigh each vial twice and record the weights below. If the weight during the second weighing changed more than 0.002g, please repeat this step until it’s constant. Subtract the sampled weight from the previously measured vial weight (arithmetic means). Include all balance printouts with the final validations report.

Headspace Syringe (2.50mL)

Vial # / Sample
Vol (mL) / Vial Weight 1 (g) / Vial Weight 2 (g) / Vial Weight MEAN
(g) / Sampled Weight 1 (g) / Sampled Weight 2 (g) / Sampled MEAN
(g) / MEAN Difference
Vial wt. - Sampled wt. (g)
1 / 0.62
2 / 0.62
3 / 0.62
4 / 0.62
5 / 0.62
Control / N/A
6 / 1.25
7 / 1.25
8 / 1.25
9 / 1.25
10 / 1.25
Control / N/A
11 / 2.50
12 / 2.50
13 / 2.50
14 / 2.50
15 / 2.50
Control / N/A

3.  Liquid Syringe Testing

The autosampler only measures the distance from the highest point to the lowest point in the scale. This means a test with a 10mL syringe is equivalent to a 250mL syringe. The only physical difference is the inside diameter of different syringe sizes.