EQUIPMENT QUALIFICATION PLAN
(EQP)
Agilent Enterprise Edition Compliance Services
Qualification of GC Systems
Agilent 7890/7820 Series with Liquid or Headspace Samplers (Including CTC) and
Agilent 6890/6850/5890 Models and Select Non-Agilent GC Models
REVIEW DOCUMENT NAME:
Agilent_Recommended_EQP_GC
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Agilent_Recommended_EQP_GC
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Enterprise Edition Compliance Services
How to Use This Document
This document is an Equipment Qualification Plan (EQP). It covers Design Qualification (DQ), Installation Qualification (IQ),
Operational Qualification (OQ), scheduled repeat OQ, and Re-Qualification after Repair (RQ). It contains information on how
Enterprise Edition Compliance Services work, and also provides a full list of the tests and checks performed as part of Agilent’s
standard Enterprise Edition IQ and OQ services.
The hardware IQ and OQ procedures listed in this document include fixed tests and checks at Agilent recommended criteria and
limits.
All tests in this document exist in all Agilent delivery tools. However, customer-selectable variance to the standard hardware
OQ setpoints is possible to enable testing of chromatography system(s) over their intended range of use. All setpoint menu
selections in the Variance Section are with the validated range of Enterprise Edition.
The inventory of systems covered by the EQP will be maintained as a separate record.
To facilitate the EQP review and approval process, this document is best viewed on-screen using Adobe ®. There are also three
pdf file attachments included with this document: (i) Question and Answer document (ii) 21 CFR Part11 Conformance Checklist
for the Agilent Compliance Engine (ACE) - the Enterprise Edition delivery tool, (iii) EE 1.76 EQR Comparison with previous
versions.
To approve this EQP simply print to paper and sign. To add variances see instructions below. Keep copies for your own records.
Verbal confirmation of approval is sufficient for Agilent service to proceed with scheduling and delivery.
To make variances to the standard hardware OQ setpoints:
[1] Use the pull-down button to select the alternative approval statement “shall follow...the standard specifications with
VARIANCES to OQ setpoints...”; [2] Complete the “EQP Record of Variances to Setpoints from Standard OQ Specifications”
later in this document; [3] Print EQP to paper and [4] ENSURE THE VARIANCE REQUEST IS COMMUNICATED to Agilent service
engineer BEFORE first OQ delivery starts. Do not e-mail/FAX/post copies of your approved EQP to Agilent. BUT CUSTOMER
MUST PROVIDE A COPY OF ANY EQP WITH VARIANCES TO AGILENT OPERATOR ON-SITE TO ENSURE THE VARIANCES ARE
ENTERED INTO DELIVERY TOOL. NO EXTRA FEE TO DELIVER SETPOINT VARIANCES.
For a full process description, click here to go to the EQP Record of Variances section.
Approval of EQP
The undersigned person(s) approve the following:
[1] the use of Enterprise Edition Compliance Services and delivery of the IQ and/or OQ and/or RQ checks and tests appropriate
to the actual configuration, make, and model of those systems covered by the service;
[2] the specifications described in this Standard EQP Review Document where the tests, setpoints, and limits shall follow...
the
FIXEDAgilent
Agilentrecommended
recommended
specifications
theSTANDARD
STANDARD FIXED
specifications.
Name and Role
Signature and Date
[You cannot save form entries with Adobe Reader. Typed entries and menu selections are printed on your official paper copy when you print]
DO NOT SEND AGILENT A COPY OF YOUR APPROVED EQP. THIS DOCUMENT IS YOUR OWN RECORD OF APPROVAL.
© Agilent Technologies, Inc. 2014
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Enterprise Edition Compliance Services
Contents
To go to a section, click on one of the section titles below.
SectionsPage
How Enterprise Edition Compliance Services Work.................................................................................................. 4
Design Qualification (DQ)............................................................................................................................................... 5
Installation Qualification (IQ) Hardware...................................................................................................................... 6
Operational Qualification (OQ) Hardware.................................................................................................................... 7
Standard OQ Test Specifications for GC Systems...................................................................................................... 7
OQ Test Design and Rationale for GC Systems.......................................................................................................... 9
EQP Record of Variances to Setpoints from Standard OQ Specifications............................................................... 15
Re-Qualification after Repair (RQ) Hardware............................................................................................................ 16
Legal, Endorsement, and Revision History................................................................................................................ 17
PDF file attachments to this electronic EQP (open the attachments folder for this document in Adobe):
Why Has Agilent Introduced the New
Compliance Service, Called Enterprise Edition?
Introduction
Table of contents: [click on title for fast navigation]
What Are The High Level Changes In Enterprise Edition
And What Were The Drivers For These Changes?
Any Other Practical Or Process Changes In
Enterprise Edition?
Let’s Dive Into The Details – How Do The Protocols And
Tests In Enterprise Edition Compare To Classic Edition?
List Of Enterprise Edition OQ Tests Versus
Classic OQPV Tests For LC:
What About The Reports, How Are These Different
To OQPV Reports?
What Would I Have To Do If I Wanted To Move My
Annual OQ Service From Classic To Enterprise Edition?
What Are The Main Risks To Migrating To
Enterprise Edition And How To Avoid Them?
Finally, Can You Summarize The High Level
Comparison Of Enterprise Edition Versus
Classic Edition Compliance Services?
EE 1.76 Comparison
Document
© Agilent Technologies, Inc. 2014
Part 11 Checklist (ACE)
Agilent (then we were HP Analytical) introduced
OQPV for our own LC and GC instruments in the early
1990’s and since then we have delivered well over
100,000 OQPV reports to customers around the world.
Despite the undoubted success and acceptance of our
old OQPV (now called Classic Edition to distinguish
from the new Enterprise Edition service) times have
changed. Expectations and requirements of an
OQ have slightly shifted. The number and type of
instruments and software used by our customers has
increased. And of course we are truly in the new world
of computers and electronic media.
So Agilent set out with a team of international experts
3 years ago to create an upgraded compliance service
that would meet the new demands but crucially
maintain the fundamental requirements:
• Always pass FDA and national agency audits
without over-testing or under-testing;
• Challenge the LC or GC system with a scientifically
sound methodology that provides valuable
performance data.
• Meet the quality needs of customers and the spirit &
intention of the GLP & GMP laws.
• Offer this service at a cost-effective price that
makes it more than just worthwhile – we hope it
is the simplest & best qualification choice that a
customer can make.
What Are The High Level Changes In
Enterprise Edition And What Were The
Drivers For These Changes?
The first big driver was the software environment.
A greatly increased number of chromatography data
system (CDS) products are available to control
LC and GC systems. Agilent has ChemStation,
Cerity, EZChrom, OpenLab and some specialist
LCMS/GCMS software. Our customers also use
Empower, Chromeleon, Atlas, Turbochrom and many
others. Classic OQPV was built into ChemStation
software. The Classic OQPV is a miracle of validated
and almost fully automated OQ testing. But these
benefi ts are therefore limited to Agilent instruments
running on ChemStation. To provide all our customers,
and customers of non-Agilent instruments, a single
OQ solution as good as (or better than) OQPV – it
was clear we had to develop an automation tool
independent of ChemStation and any other CDS.
The Agilent Compliance Engine (ACE) is our new
software tool that manages the workflow and
protocols, calculates results and produces the
reports. Naturally it is fully validated and tested.
Our service engineers carry “ACE laptops” in the
same way as they carry “ChemStation laptops”.
Alternatively our contract customers can have the
ACE software on their own laptops or installed with
Agilent OpenLab networked CDS.
Q & A: Why Change?
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Enterprise Edition Compliance Services
How Enterprise Edition Compliance Services Work
Enterprise Edition is designed to fit the traditional quality systems used by firms and recognized by regulatory agencies
worldwide.
How Enterprise Edition aligns with a traditional, paper-based methodology is described below:
[i] Policy documents dictate the need for validation & qualification of GMP/GLP systems and usually mention the DQ/IQ/OQ/
PQ model. The precise procedures for IQ & OQ for each type of equipment are prescribed in an approved SOP, perhaps called
SOP #123: Qualification of GC Systems. In Enterprise Edition, the EQP has the same role as the traditional Qualification SOP.
[ii] The traditional SOP provides lists of tests & limits for the range of system configurations found in the lab or department. The
EQP follows this concept. The inventory of systems covered by an SOP or EQP changes over time - so this is kept as a separate
record.
[iii] The traditional Qualification SOP typically has blank results forms as attachments to be photocopied for each IQ or OQ event
- the results recorded in ink with manual calculations. In Enterprise Edition this execution process is streamlined and automated
by use of Adobe forms and the Agilent Compliance Engine (ACE) delivery tool. It provides reports with no hand-writing errors;
validated calculations; automated pass/fail report; traceability to raw data and a count of number of times a test was run. This
automation provides efficiency and enforces compliance to procedure.
[iv] The traditional Qualification SOP is approved and released only once - replacing need to author individual protocols for
each chromatography system. This is the same concept for the EQP. The appropriate tests for each individual configuration
are automatically selected by ACE from the list in the approved EQP - at time of delivery. The final reports are unique for each
system and each qualification event - but the single approved EQP can cover a lab, department or as wide a scope as desired.
(v) In the traditional qualification methodology there is no convenient provision to record the actual workflow of the tests
execution and results. In the event that a test is repeated during the Enterprise Edition delivery, ACE maintains a counter per
test which is automatically incremented for GxP compliant work, and the engineer should generate a deviation note within the
ACE report.
Figure 1:
This EQP Review Document is the record of IQ checks and OQ / RQ tests, setpoints, and limits for GC systems. The tests already exist in the automation tool called ACE and
are ready to run after the EQP is approved. ACE holds the test forms applicable to the full range of GC configurations plus a validated calculation and report generator engine.
At time of delivery, a record of individual system configuration is made by the operator and entered into ACE. The correct test forms are automatically selected by ACE from
its internal catalog of test designs. Each test in the catalog has a blank results template form. The appropriate setpoints and limits for the individual GC system are added by
ACE to the forms according to the approved EQP. When each test is run, the results are calculated and forms completed and then collated to make a single final report called
an Equipment Qualification Report (EQR), which is provided in secure PDF format or optional CD disk – printable to paper and stored in a binder and/or customers’ network
storage system.
© Agilent Technologies, Inc. 2014
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Enterprise Edition Compliance Services
Design Qualification (DQ)
Design Qualification (DQ) for commercial lab instruments is recommended by some, but not all, guidances and procedures.
Defintions of DQ found in guidances and firm-specific validation procedures vary widely around the world. Some firms require
nothing more than a record (such as certificate) from the instrument manufacturer demonstrating that the lab system has
been designed for purpose and manufactured to a quality standard. Others treat DQ as the development of a user requirement
specification document (URS) which can be matched to the IQ and OQ specifications for a manufacturer. Other firms consider
DQ as including the vendor selection activities.
USP Chapter <1058> pre-published in USP 31/Supplement defines DQ:
Design qualification (DQ) is the documented collection of activities that define the functional and operational specifications of
the instrument and criteria for selection of the vendor, based on the intended purpose of the instrument. Design qualification
(DQ) may be performed not only by the instrument developer or manufacturer but also may be performed by the user. The
manufacturer is generally responsible for robust design and maintaining information describing how the analytical instrument
is manufactured (design specifications, functional requirements, etc.) and tested before shipment to users. Nonetheless, the
user should ensure that commercial off-the-shelf (COTS) instruments are suitable for their intended application and that the
manufacturer has adopted a quality system that provides for reliable equipment. Users should also determine capability of the
manufacturer for support installation, services, and training.
For your reference, Agilent provides the following statements for DQ purposes:
1. All Agilent LC, LCMS, GC, GCMS, UV-Vis and Dissolution hardware and software laboratory products including the ACE
software used to deliver qualification services, are designed, manufactured, and tested according to Agilent internal Quality
Life-Cycle Development Procedures.
2. Certificates of Agilent testing, validation, and conformance to standards are provided with new Agilent instruments
and similar certification is provided for ACE software. These documents are checked and recorded in Enterprise Edition
Compliance Services IQ.
3. Agilent maintains information describing how products are manufactured and maintains a problem and bug reporting
program as required by international software quality guidelines.
4. The OQ specifications in this EQP can be used, as appropriate, by the user to prepare URS. The OQ specifications in this EQP
represent the levels of performance acceptable to regulatory agencies for the technique; conform to typical specifications
found in Validation literature; are equally suitable for OQ at installation and on-going OQ throughout operational lifetime; are
equivalent to the OQ specifications published in the legacy Agilent Classic OQPV protocols; and are suitable for most user
requirements.
5. Agilent Technologies is capable of installation, support, preventive maintenance, on-going qualification and re-qualification
after repair and user training worldwide.
© Agilent Technologies, Inc. 2014
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Enterprise Edition Compliance Services
Installation Qualification (IQ) Hardware
Hardware IQ checks and tests for Agilent software products include the following:
1. Purchase Order Documents:
Allows the customer to verify that the instrument being qualified matches their design requirements (if available) and
purchase order.
2. Preparation and Installation Documents:
Gathers and records information about preparation and installation documents.
3. System and Installation Documentation:
Gathers and records information about reference and user manuals for initial installations.
4. Product Quality Assurance Documents:
Collects and records certificates and other forms that verify that the vendor has developed and built the product according to
internal standards.
5. Start Up Test:
Verifies that all modules start up properly.
6. Instrument Check:
Demonstrates that all modules of the instrument are correctly installed and connected. It does not test instrument
performance as fully as OQ. This test is not necessary and therefore skipped if an OQ is to be performed by Agilent operator
at installation after IQ.
.
© Agilent Technologies, Inc. 2014
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Enterprise Edition Compliance Services
Operational Qualification (OQ) Hardware
Standard OQ Test Specifications for GC Systems
Test Name
Setpoints and Parameters
Limits
System Inspection and Basic
Safety and Operation
N/A
Gases, chassis electric grounding, interlocks,
hydrogen shutdown, and so on all correct.
GC Oven Temperature Accuracy
and Stability
Temperature 1 = 230.0 °C
Temperature 2 = 100.0 °C
(Stability measured at Temperature 2)
Accuracy ≤ 1.0 % of setpoint (in °K)
Stability ≤ 0.5 °C
Headspace Vent and
Pressurization Valve Integrity
N/A
Valve functions properly.
Headspace Heated Zones
Temperature Accuracy
Zone 1: 100.0 °C
Zone 2: 110.0 °C
Zone 3: 115.0 °C*
Accuracy ≤ 4.0 °C on G1888A and 7697
Accuracy ≤ 6.0 °C on 7694 (Zone 1)
Accuracy ≤ 2.0 °C on CTC
Vial Heater Temperature Accuracy
Temperature 1: 60.0 °C
Setpoints for temperature 2 and 3 are
variable.
Diff. from setpoint ≥ –2.0 °C, ≤ 2.0 °C
Inlet Pressure Decay
Inlet gas flow control
Pressure change / 5 minutes ≥ -2.0 psi, ≤ 0.5 psi
Inlet Pressure Accuracy
Inlet pressure = 25.0 psi
Accuracy ≤ 1.2 psi
Detector Flow Accuracy
Flow rate varies by detector type (Test is
N/A for NPD)
Accuracy ≤ 10.0 % of setpoint (or 0.5 ml/minute,
whichever is larger)
Signal Noise and Drift (FID)
Detector signal
Initial signal ≤ 25 pA
Noise ≤ 0.10 pA
Drift ≤ 2.50 pA/hour
Signal Noise and Drift (TCD)
Detector signal
Initial signal ≤ 35 DU (1 DU = 25 uV)
Noise ≤ 0.15 DU
Drift ≤ 2.20 DU/hour
Signal Noise and Drift (NPD)
Initial signal
(Test N/A to 5890)
Initial signal = 30 – 50 DU (1 DU = 1 pA)
Noise ≤ 0.15 DU
Drift ≤ 3.50 DU/hour
Signal Noise and Drift (ECD)
Initial signal
(Test N/A to 5890)
Initial signal ≤ 70 DU (1 DU = 5 Hz)
Noise ≤ 0.15 DU
Drift ≤ 1.00 DU/hour
Signal Noise and Drift (uECD)
Initial signal
(Test N/A to 5890)
Initial signal ≤ 400 DU (1 DU = 1 Hz)
Noise ≤ 3.00 DU
Drift ≤ 15.00 DU/hour
Signal Noise and Drift
(FPD new style)
Initial signal
Sulfur
(Test N/A to 5890)
Initial signal ≤ 70 DU (1 DU = 150 pA)
Noise ≤ 5.00 DU
Drift ≤ 5.00 DU/hour
Signal Noise and Drift (FPD+)
Initial signal
Sulfur
(Test N/A to 5890)
Initial signal ≤ 70 DU (1 DU = 150 pA)
Noise ≤ 4.00 DU
Drift ≤ 3.00 DU
Signal Noise and Drift
(FPD new style)
Initial signal
Phosphorous
(Test N/A to 5890)
Initial signal ≤ 80 DU (1 DU = 150 pA)
Noise ≤ 5.00 DU
Drift ≤ 5.00 DU/hour
Signal Noise and Drift (FPD+)
Initial signal
Phosphorous
(Test N/A to 5890)
Initial signal ≤ 20 DU (1 DU = 150 pA)
Noise ≤ 2.00 DU
Drift ≤ 1.50 DU
© Agilent Technologies, Inc. 2014
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Document Released: April 2014
Enterprise Edition Compliance Services
Operational Qualification (OQ) Hardware (continued)
Standard OQ Test Specifications for GC Systems (continued)
Test Name
Setpoints and Parameters
Limits
Signal to Noise
(FID/SS/ALS/MMI)
Signal height divided by ASTM baseline
noise for known concentration and
conditions.
Signal to noise ≥ 300,000 (nitrogen makeup gas)
Signal to noise ≥ 240,000 (helium makeup gas)
Signal to Noise
(FID/SS/HSS/MMI)
Signal height divided by ASTM baseline
noise for known concentration and
conditions.
Signal to noise ≥ 5,000 (nitrogen makeup gas)
Signal to noise ≥ 4,000 (helium makeup gas)
Signal to Noise (FID/VI/HSS)
Signal height divided by ASTM
baseline noise for known
concentration and conditions.
Signal to noise ≥ 4,000 (nitrogen makeup gas)
Signal to noise ≥ 3,200 (helium makeup gas)
Signal to Noise
(FID/non-SS/using 18710-60170)
Signal height divided by ASTM baseline
noise for known concentration and
conditions.
Signal to noise ≥ 800 (nitrogen makeup gas)
Signal to noise ≥ 600 (helium makeup gas)
Signal to Noise
(FID/non-SS/using 5188-5372)
Signal height divided by ASTM baseline
noise for known concentration and
conditions.
Signal to noise ≥ 300 (nitrogen makeup gas)
Signal to noise ≥ 240 (helium makeup gas)
Signal to Noise (NPD)
Signal height divided by ASTM baseline
noise for known concentration and
conditions.
Signal to noise ≥ 300
Signal to Noise
(TCD/SS/ALS/MMI)
Signal height divided by ASTM baseline
noise for known concentration and
conditions.
Signal to noise ≥ 5,000
Signal to Noise (TCD/non-SS)
Signal height divided by ASTM baseline
noise for known concentration and
conditions.
Signal to noise ≥ 100
Signal to Noise (uECD)
Signal height divided by ASTM baseline
noise for known concentration and
conditions.
Signal to noise ≥ 1,500
Signal to Noise (FPD new style)
Signal height divided by ASTM baseline
noise for known concentration and
conditions.
Signal to noise ≥ 700 (sulfur)
Signal to noise ≥ 1,000 (phosphorous)
Signal to noise (FPD+)
Signal height divided by ASTM baseline
noise for known concentration and
conditions.
Signal to noise ≥ 1,400 (sulfur)
Signal to noise ≥ 2,400 (phosphorous)
Injection Precision
Injection volume on column: 1/1000/250 ul
(ALS/Agilent HSS/CTC HSS with
split/splitless FID)
Injection time: 0.2 minutes
(pressure-balanced HSS only)
Retention time RSD ≤ 1.00 %
Area RSD ≤ 3.00 % (ALS & Agilent HSS)
Area RSD ≤ 4.00 % (CTC HSS)
Area RSD ≤ 5.00 % (Packed Inlet & Special detectors)
Injection Carry Over
Injection Volume on column: 1000/250 ul
(Agilent HSS/CTC)
Area carry over ≤ 1.00 %
* for 7697 HSS model only
Key:
Fixed setpoints/limits
Variance allowed for setpoint(s)
End of Section - Standard OQ Test Specifications for Agilent GC Systems
© Agilent Technologies, Inc. 2014
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Operational Qualification (OQ) Hardware (continued)
OQ Test Design and Rationale for GC Systems
Many GMP/GLP enforcement agency inspectors now ask firms to provide a risk assessment of their equipment and computer
systems plus a science-based rationale for subsequent validation and qualification testing.
GENERAL RISK STATEMENT: Any LC, LCMS, UHPLC, UHPLC_MS, GC, or GCMS system used for raw material testing or final
drug product / medical device testing in GMP or used in formal GLP studies will likely fall into a HIGH RISK category. This risk
assessment will imply the need for IQ & OQ & on-going qualification. ANY USER SPECIFIC RISK ANALYSIS SUPERCEDES THIS
GENERAL RISK STATEMENT.
This section outlines the science-based rationale for each test in the Agilent hardware OQ plus a brief test design and procedure
description.
The recommended set of hardware OQ tests described in this EQP derives from Agilent’s intepretation of FDA, USP, and GAMP4
guidelines and other authoritative expert literature.
The OQ test design incorporates modular and holistic testing which is a proven and regulatory acceptable approach. Direct
metrology is used to test the inlet integrity (pressure decay and pressure accuracy), detector flow accuracy and temperature
accuracy of the GC (oven, oven ramp, inlet/detector) and headspace heated zones. Holistic chemical testing is used for the
evaluation of the following critical instrument characteristics: precision, signal to noise, and carry over. Certified reference
standards and calibrated traceable thermometers and manometers are used. Considering the number of setpoints, parameters,
and conditions of each recommended OQ test, the proven concepts of worst case, range, and representative have been applied.
If a property or characteristic is known to have its worst performance at one end of a range of use, that end is the setpoint that
should be tested and other setpoints are not required. If a property or characteristic has no known worst case, testing at the
high and low points of the range of use is required. If there are too many possible use cases and conditions to realistically test
and none is a worst case, a representative sample for test is the best approach.
The following OQ tests for GC Systems (with FID, ECD, TCD, NPD, FPD, but NOT MSD) will be performed as appropriate for the
configuration of the individual GC system.
1. System Inspection and Basic Safety and Operation [core GC OQ test]
Rationale: System must be in safe and operational condition before starting the OQ tests.
Procedure: The instrument is given a general inspection and its basic safety features are challenged to ensure proper operation.
2. GC Oven Temperature Accuracy and Stability [core GC OQ test]
Rationale: Oven temperature accuracy is important for comparability between systems and transferring methods. Oven
temperature stability is critical for qualitative and quantitative analysis.
Procedure: At two different temperatures, accuracy is measured using an external calibrated thermometer. At one of these,
a statistically significant number of additional readings are taken during the total duration of the test to calculate the oven
stability. Accuracy is the difference between found and setpoint values.
3. Headspace Vent and Pressurization Valve Integrity [core GC OQ test if headspace sampler is integral part of system]
Rationale: Proper operation of the valves is critical for repeatable peak areas and carry over.
Procedure: This test verifies that the valves operate properly: with no excessive leaks or restricted internal flow paths.
© Agilent Technologies, Inc. 2014
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Operational Qualification (OQ) Hardware (continued)
OQ Test Design and Rationale for GC Systems (continued)
4. Headspace Heated Zones Temperature Accuracy [core GC OQ test if headspace sampler is integral part of system]
Rationale: Temperature accuracy of the heated zones is important for comparing systems and transferring methods. Oven
accuracy is critical to quantitative headspace methods.
Procedure: The temperature is measured using an external calibrated thermometer with appropriate probe design. Accuracy is
determined as the difference between found and setpoint values.
5. Inlet Pressure Decay [core GC OQ test]
Rationale: Pressure integrity of the inlet is critical for repeatable injection and retention times. The pressure decay and pressure
accuracy tests combine to demonstrate pressure integrity.
Procedure: The inlet is capped, a pressure applied, and inlet flow is turned off. The pressure decay is recorded over a specified
time range.
6. Inlet Pressure Accuracy [core GC OQ test]
Rationale: Pressure integrity of the inlet is critical for repeatable injection and retention times. The pressure decay and pressure
accuracy tests combine to demonstrate pressure integrity. This test checks for accurate pressure to the head of the column.
Column flow is achieved by maintaining a constant pressure against a known restriction. Because the restriction is a function of
the column geometry, measuring pressure in the inlet is the most accurate way to determine flow.
Procedure: The inlet is capped, a pressure is applied and the inlet pressure is recorded using an external calibrated manometer
connected to the inlet.
7. Detector Flow Accuracy [core GC OQ test]
Rationale: Detector flow accuracy is critical for a stable detector signal. Incorrect flows may have an impact on detector
performance.
Procedure: Flow accuracy is determined by measuring the flows with a calibrated mass flowmeter and comparing them to the
test setpoints and the values displayed by the GC.
8. Signal to Noise [core GC OQ test]
Rationale: Sensitivity of GC detection is a critical performance feature in quantitative and qualitative analysis. A signal-to-noise
value of a representative compound at known concentration provides sensitivity statistics.
Procedure: A traceable standard is injected and signal to noise is calculated.
9. Injection Precision [core GC OQ test]
Rationale: System precision is critical for quantitative analysis.
Procedure: An initial stabilizing injection followed by six repeat injections of a traceable standard followed by a final blank
injection is made. The %RSD of the six injections is calculated to provide precision statistics. There are separate dedicated
instrument parameters and reference standards applicable to each inlet/detector combination. This test is performed with liquid
and headspace sampler configurations.
© Agilent Technologies, Inc. 2014
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Operational Qualification (OQ) Hardware (continued)
OQ Test Design and Rationale for GC Systems (continued)
10.Carry Over [core OQ test for headspace but optional extra fee test for liquid samplers]
Rationale: Low carry over from a previous injection is critical for accuracy of quantitative and reliability of qualitative analysis.
For headspace samplers, the engineering condition contributes to carry over performance, so this is a core OQ test for these
samplers.
Procedure: The blank injection after the six repeat injections of the precision test is evaluated for carry over, and the result is
expressed as a percentage.
11.Vial Heater Temperature Accuracy [core GC OQ test if sampler tray has the heater option installed]
Rationale: The 7693A vial heater option can be used during sample preparation. This test verifies that it heats accurately.
Procedure: The temperature of the heater (using an external thermometer) is recorded and accuracy is calculated as the
difference between the recorded value and setpoint. A single temperature is tested by default, but it is possible to add two more
setpoints.
12.Signal Noise and Drift [core GC OQ test]
Rationale: This test gives an indication of detector sensitivity and stability.
Procedure: The signal is monitored at specified conditions appropriate to the type of detector over a twenty-minute period.
The signal noise is calculated based on ASTM E594-96 as the average peak-to-peak noise in a number of signal segments.
The drift is calculated as the slope of the linear regression for the signal. Detector type and the gases used all contribute to
different performance and therefore different limits for each configuration.
© Agilent Technologies, Inc. 2014
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Operational Qualification (OQ) Hardware (continued)
OQ Test Design and Rationale for GC Systems (continued)
The following tests are NOT INCLUDED in the standard OQ for GC but can be ordered as EXTRA COST TESTS.
Test Name
Setpoints and Parameters
Limits
Include
Response Linearity
(FID, TCD)
Certified reference standard with multiple peaks
known concentration
Coefficient of determination (r2) = 0.99900
R/F Precision ≤ 10.00 % RSD
GC Heated Zones
Temperature
Accuracy (uECD /
MSD not supported)
Inlet temp. 1 = 200.0 °C / 250.0 °C (OC / all others)
Detector temp. 1 = 200.0 °C / 300.0 °C
Setpoints for temperature 2 are variable.
Inlet accuracy ≤ 15 °C / 10 °C (OC / all others)
Detector accuracy ≤ 15 °C
GC Oven Temp.
Ramp: Accuracy,
Linearity, Precision
Initial temperature: 50.0 °C
Ramp 30.0 °C/minute
Final temperature: 280.0 °C
Ramp accuray: ≤ 1.0 °C/minute
Ramp linearity ≥ 0.99990
Ramp precision ≤ 2.0 %
LTM Basic Operation
N/A
Self test completes w/o errors
Ref. voltage = 794 ± 10 mV
Transferlines 1, 2 = 794 ± 50 mV
Column temperature = 784 ± 10 mV
LTM Oven
Temperature Acc.
and Stability
Temperature 1 = 230.0 °C
Temperature 2 = 100.0 °C
Stability measured at temperature 2
Diff. from setpoint ≤ 1.0 % of setpoint (in °K)
Stability ≤ 0.5 °C
LTM Oven Temp.
Ramp: Accuracy,
Linearity, Precision
Initial temperature: 50 °C
Ramp 100 °C/minute
Final temperature: 280 °C
Ramp accuray: ≤ 2.0 °C/minute
Ramp linearity ≥ 0.9990
Ramp precision ≤ 2.0 %
Injection Carry Over
Injection volume on column: 1.0 ul
(ALS split/splitless FID)
Area carry over ≤ 1.00 %
Key:
Fixed setpoints/limits
Variance allowed for setpoint(s)
Extra Test 1. FID Response Linearity [NOT CORE OQ TEST: additional extra fee test]
Rationale: Response linearity is critical for quantitative analysis. It is often demonstrated in user applications and analytical
methods typically using multi-level calibration standards and internal standards. Therefore, this is an optional extra fee OQ test.
The FID response linearity test uses a certified chemical reference test mix that is validated to be challenging and representative
of many applications.
Procedure: The response linearity test is executed using a single injection from a standard containing a number of n-alkanes
with increasing concentrations. Response linearity can be calculated with just one injection of a standard for the following
reasons.
• The difference in length of the n-alkanes (boiling-point increases) separates these components on the column.
• The increasing concentration gives an increasing detector response.
• GC theory states (and experiment confirms) that the response factors for these compounds are the same (within a very small
variance). Therefore, a single injection of this multi-component /multi-level concentration sample can be used to calculate the
response linearity of the detector.
• The single injection test design eliminates the contribution of injector precision to the linearity statistics evaluation.
© Agilent Technologies, Inc. 2014
Page 12 of 18
No reproduction, translation, or use without permission
Agilent_Recommended_EQP_GC
Document Released: April 2014
Enterprise Edition Compliance Services
Operational Qualification (OQ) Hardware (continued)
OQ Test Design and Rationale for GC Systems (continued)
Extra Test 2. GC Heated Zones Temperature Accuracy [NOT CORE OQ TEST: additional extra fee test]
Rationale: The precise temperature of the heated zones is not critical to quantitative or qualitative analysis. When the inlet
zones are hot enough to vaporize but not so hot as to thermally decompose sample, this is adequate. When the detector zones
are hot enough to evaporate sample and prevent condensation, this is adequate. Temperature accuracy of the heated zones may
be important for comparing systems and transfer methods. Therefore, this is an optional test.
Procedure: This test demonstrates that the inlet and detector show an accurate temperature using proprietary novel design
to overcome the inherent difficulties in gaining accurate and meaningful readings. The temperature is measured using an
external thermometer. The probe is inserted as if it is a column with a pre-defined length above the column nut to get consistent
measurements between different instruments. Two setpoints (high and low) are measured. (Note: Due to the possible risk of
radioactive contamination, ECDs are excluded from this service).
Extra Test 3. GC Oven Temperature Ramp: Accuracy, Linearity, and Precision [NOT CORE OQ TEST: additional extra fee test]
Rationale: Most GC analyses use a temperature program instead of an isothermal oven temperature program to complete the
separation of the compounds in the sample. For retention time reproducibility, it is important that the temperature program is
always executed in the same way.
This test uses a calibrated digital thermometer to determine the accuracy, linearity, and precision of the GC oven temperature
program. Linearity is defined as the coefficient of determination (r2) and uses data points that are part of the ramp. Ramp
accuracy is defined as the slope of the linear curve fit through the same data points used for linearity calculations. Precision is
calculated as the RSD over three temperatures in the slope over three different runs.
Procedure: In this test, a linear oven temperature profile is collected three times in a row using a digital thermometer and a data
logger. For each run, the oven ramp accuracy and oven ramp linearity are calculated. After all three runs are completed, the oven
ramp precision is calculated. The ramp in use is a steep slope that challenges the GC to deliver high power in a reproducible
way.
Extra Test 4-6. LTM Tests [NOT CORE OQ TEST: additional extra fee test]
Rationale: The RTD is a column packed in a heating foil. Although columns are generally considered to be consumables and not
part of a hardware qualification, in this case the “oven” includes the column so tests are required to evaluate its functionality.
A direct temperature measurement (vs. indirect) is preferred but not feasible in this case given the LTM design: adding a
temperature sensor to the metal foil introduces a cold spot and adversely affects temperature, and inserting a probe into the
RTD requires taking the column apart.
One indirect temperature measurement is a direct measurement of the return voltage from the RTD, which can be converted to
temperature using a known equation.
Another indirect temperature measurement would be chemical tests. If the system is not able to heat up in a reproducible
way, you might see a shift in retention times. Because this kind of measurement is used by Agilent (and many other vendors)
to evaluate system performance, it would be difficult for LTM to rework the complete chemical test suite: especially detectorspecific tests like Signal to Noise and Signal Noise and Drift. The RTD can be any column and noise, in particular, is influenced
by the column type.
© Agilent Technologies, Inc. 2014
Page 13 of 18
No reproduction, translation, or use without permission
Agilent_Recommended_EQP_GC
Document Released: April 2014
Enterprise Edition Compliance Services
Operational Qualification (OQ) Hardware (continued)
OQ Test Design and Rationale for GC Systems (continued)
Based on the above, the following qualification is executed when an LTM is installed:
1. A complete GC qualification without Injection Precision (IP) is run with standard oven procedures. An LTM Basic Operation
test is scheduled to show the LTM is functional.
2. An LTM Oven Temperature Accuracy and Stability test is executed. This test is similar to the standard GC Oven Temperature
Accuracy and Stability.
3. An LTM Oven Temperature Ramp test is executed, similar to the standard GC Oven Temperature Ramp test, but it uses a
much higher ramp.
4. The IP test is run using the LTM module. Inlet, detector, and RTD modules are tested separately in steps 1-3, but this test
verifies that all components work together. LTM runs in general are very short due to the high oven ramp and very fast cool
down rate.
Procedure for LTM Basic Operation: After completing the self test, four different temperatures (voltages) are measured:
reference voltage (setpoint), return voltage (column temperature), and both transfer lines. This assures that all zones are
functional, correctly installed, and connected.
Procedure for LTM Oven Temperature Accuracy and Stability: This test uses a calibrated voltmeter to determine temperature
accuracy and stability of the LTM oven. (Voltages are measured and then converted to temperatures using a known relation. The
converted temperatures are used in all calculations and limit comparisons.)
Procedure for LTM Oven Temperature Ramp: This test uses a calibrated voltmeter to determine the accuracy, linearity, and
precision of the LTM oven temperature program. (Temperatures cannot be measured directly for LTM ovens, so voltages are
measured and then converted to temperatures using a known relation. The converted temperatures are used in all calculations
and limit comparisons.) Linearity is defined as the coefficient of determination (r2) and uses data points that are part of the
ramp. Ramp accuracy is defined as the slope of the linear curve fit through the same data points used for linearity calculations.
Precision is calculated as the RSD over three temperatures in the slope over three different runs.
Extra Test 7. Carry Over [NOT CORE TEST: additional extra fee test for liquid samplers]
Rationale: For liquid samplers, carry over performance is contingent on many variable factors independent of the engineering
condition of the GC system. Many different syringe wash programs are available that can eliminate carry over. These are user
selectable and may be application specific. The condition of the injection syringe is the only controllable engineering factor.
Procedure: The blank injection after the six repeat injections of the precision test is evaluated for carry over, and the result is
expressed as a percentage. For liquid samplers, carry over performance is contingent on many variable factors independent of
the engineering condition of the GC system.
© Agilent Technologies, Inc. 2014
Page 14 of 18
No reproduction, translation, or use without permission
Agilent_Recommended_EQP_GC
Document Released: April 2014
Enterprise Edition Compliance Services
Operational Qualification (OQ) Hardware (continued)
EQP Record of Variances to Setpoints from Standard OQ Specifications
IGNORE THIS SECTION IF YOU ACCEPT AND APPROVE THE FIXED STANDARD QUALIFICATION TESTS AND SETPOINTS
RECORDED IN THE PRECEDING PAGES OF THIS STANDARD EQP.
-EQP with Variance Approval Process: Customer Actions: (1) View in Adobe®; select required setpoint variances below; select
the alternative approval statement on page 2; (2) Print to paper to save the selections; sign page 2 of this EQP; (3) Ensure the
approved EQP with Variances is provided to Agilent operator on the day of the first delivery before start of OQ; counter-sign
and date the Agilent operator signature on this page. [End of EQP with Variance approval process. Next step: wait for your
qualification reports.] -Agilent Operator Actions: (1) Enter and save the customer change requests on this page into the ACE
tool; (2) Sign and date this page on the customer copy to verify that you made the changes in ACE; return signed copy to
customer for counter-signature; (3) Deliver the qualification by following this EQP and any setpoint variances. (Note: Once the
EQP Variances are entered into ACE these are saved for all future OQ/RQ events where applicable.)
Test Name
Setpoint
Standard Value
GC Heated Zones Temperature Accuracy
(Inlet temp. default varies by OC/others; detector
temp. default varies by FPD/others except MSD and
uECD [test does not apply]
Inlet temp. 1
Inlet temp. 2
Variance
Units
200.0/250.0
No variance
°C
Not applicable
No variance
°C
Detector temp. 1
200.0/300.0
No variance
°C
Detector temp. 2
Not applicable
No variance
°C
Temperature 1
230.0
No variance
°C
Temperature 2
100.0
No variance
°C
Zone 1 temperature
100.0
No variance
°C**
Zone 2 temperature
110.0
No variance
°C**
Zone 3 Temperature (7697)
110.0
No variance
°C
Temperature 1
60.0
No variance
°C
Temperature 2
Not applicable
No variance
°C
Temperature 3
Not applicable
No variance
°C
Injection Precision, Injection Carry Over (ALS)
Injection volume on column
1.0
No variance
ul
Injection Precision, Injection Carry Over (Agilent HSS)
Injection volume on column
1000
No variance
ul
Injection Precision, Injection Carry Over (HSS*)
Injection time*
0.02
No variance
minutes
GC Oven Temperature Ramp: Accuracy, Linearity,
and Precision
Initial temperature
50.0
No variance
°C
Ramp
30.0
No variance
°C/minute
Final temperature
280.0
No variance
°C
Temperature 1
230.0
No variance
°C
Temperature 2
100.0
No variance
°C
Initial temperature
50.0
No variance
°C
Ramp
100.0
No variance
°C/minute
Final temperature
280.0
No variance
°C
GC Oven Temperature Accuracy and Stability
Headspace Heated Zones Temperature Accuracy
Vial Heater Temperature Accuracy
LTM Oven Temperature Accuracy and Stability
LTM Oven Temperature Ramp: Accuracy, Linearity,
and Precision
* Pressure-balanced HSS
** Temperatures over 150 °C only applicable to 7697 HSS
For a fully tailored operational qualification program using all the flexibility of Enterprise Edition, contact your local Agilent representative and/or e-mail Enterprise_edition@agilent.com
with your OQ test specification requirements. Fees may apply.
© Agilent Technologies, Inc. 2014
Page 15 of 18
No reproduction, translation, or use without permission
Agilent_Recommended_EQP_GC
Document Released: April 2014
Enterprise Edition Compliance Services
Re-Qualification after Repair (RQ) Hardware
In the event of a hardware breakdown followed by an engineering repair of a qualified instrument, it is necessary to re-qualify
the system to an appropriate level before release back into operational use.
Agilent offers a service contract to repair and re-qualify an instrument during the period between scheduled annual OQs.
The level of re-testing is prescribed in the RQ section of ACE: a form is displayed for the operator showing all types of repair
possible and the re-testing required. Part of an example form is shown below.
Re-Qualification After Repair
Mainframe Strategies
Repair/Replace Strategy
OQ/PV Testing
Main board
System Insp. & Basic Safety & Op.
GC Oven Temp. Acc. & Stability
Inlet Pressure Accuracy
Detector Flow Accuracy
GC Oven Temp. Ramp
Keyboard
System Insp. & Basic Safety & Op.
EPC board
Inlet Pressure Accuracy
Detector Flow Accuracy
The full list of repair and re-test guidance is available for review by customers of the RQ service.
The RQ form in ACE prescribes which tests the operator must perform for each repair circumstance. The test procedure,
setpoints, and limits will be an exact repeat of the previous OQ test (a so called regression testing strategy).
Dual-Acceptance Limits
Within the Equipment Qualification Plan (EQP) of the Agilent Enterprise Edition, each of the tests final result can be compared
against two different limits if required. This allows customer-configured OQ to report against a User Limit (limit1) and the Agilent
Recommended Limit (limit2) simultaneously.
The Standard_EQP documents have both Limit1 & Limit2 values set the same – effectively de-activating this feature. Custom_
EQP’s can also be prepared on request, making effective use of the Two-Limit feature of the Agilent Compliance Engine (ACE).
In those cases, “Limit2” will always be the Agilent Recommended limit, and “Limit1” will be the limit requested by the user.
Agilent will not be under any obligation regarding the OQ testing results against User-requested limits that are more stringent
than the Agilent Recommended ones.
Customer:
Agilent Operator (verifies variances are entered into ACE):
Name:
Name:
Signature, Date:
Signature, Date:
© Agilent Technologies, Inc. 2014
Page 16 of 18
No reproduction, translation, or use without permission
Agilent_Recommended_EQP_GC
Document Released: April 2014
Enterprise Edition Compliance Services
Legal, Endorsement, and Revision History
Enterprise Edition and its primary components (ACE software tool, procedures, test design, metrology tools, chemical reference
standards, operator training materials) has been designed, developed, tested, validated, and released for commercial use
following Agilent’s Life-Cycle Development Quality Assurance methodology.
Date: April 2014
Services R&D Manager: Michael F. Pope. Santa Clara, California USA
Services Quality Manager: Julio Hector. Santa Clara, California USA
Enterprise Edition is endorsed by Dr. Ludwig Huber on behalf of labcompliance.com.
ACE software is patented. Copyright is claimed by this statement for all original work comprising Enterprise Edition. Any
unauthorized use, reproduction, or translation will be prosecuted to the maximum extent possible by law. All customer copies of
EQP approval, final qualification reports, and raw data provided to customer at delivery of the service become the property of
the customer.
Revision History of GC Enterprise Edition Protocols.
A.01.83 April 2014
A.01.82 September 2013
A.01.81 April 2013
A.01.80. December 2012
A.01.79. July 2012
A.01.78. April 2012
A.01.77. February 2012
A.01.76. August 2011
A.01.75. March 2011
A.01.74. September 2010
A.01.73. June 2010
A.01.72. January 2010
A.01.71. October 2009
A.01.70. May 2009
A.01.60. May 2008
A.01.53. August 2007
A.01.50. March 2007
A.01.40. December 2006
Added support for TCD with hydrogen or nitrogen carrier/makeup configurations.
Area RSD limit in the Injection Precision test updated to 5% for packed inlets combined with special
detectors (ECD, uECD, NPD, FPD, FPD+, DFPD+)
Added support for (1) Agilent 7890B Series GC; (2) Agilent 7890 FPD+ and DFPD+ detectors. Enhanced
flexibility in set-points and limits with individual settings per inlet and detector type. No regulatory
impact for previously approved EQP’s.
Added support for General-Purpose GC systems. Enhanced scheduling of response Linearity test for
independent FID and TCD testing if both are present. Added Injection Carry Over Optional test for liquid
injectors (ALS).
Added support for Agilent 7650A Sampler. Updated ASTM noise algorithm for the Signal-to-Noise and
Noise & Drift calculations. Enhanced graphical representation. Enhanced integration and compatibility
with HSS for the FID Response Linearity test.
Added support for PTV inlet in Inlet Temperature Accuracy test. No regulatory impact for previously
approved EQP’s.
Added support for: (1) Agilent Ion Trap 220 and 240. (2) Varian/Bruker GC 430 and 450. No regulatory
impact for previously-approved Standard_EQP documents.
No changes to GC. Protocol revision made independent from ACE revisions. No regulatory impact.
No changes to GC. Added HSS third heated zone Temp Accuracy for model 7696.
No changes to GC.
(1): Added selection boxes for Optional Tests.(No regulatory impact).
Added support for Perkin Elmer HS40XL and TurboMatrix 40 headspace samplers.
Added E-signature fields (NO REGULATORY IMPACT)
(1) Added Response Linearity (FID) test; (2) added GC Oven Temperature Ramp: Accuracy, Linearity, and
Precision test; (3) added 7693 ALS and Vial Heater Temperature Accuracy test; (4) added Agilent 7820
Series and Varian GC support; (5) updated noise and drift calculation. (NO REGULATORY IMPACT)
(1) Changed test spec (NO REGULATORY IMPACT): (a) Injection Precision for FID, CTC HSS limit now
3 % to 4 % after evaluating world-wide data; (b) Inlet Pressure Decay limit now dual with existing
pressure decrease unchanged and new pressure increase at < 0.5 psi/5 minutes; (c) added Headspace
Vent and Pressurization Valve Integrity test; (d) updated noise and drift oven setpoint to 100 C, same
limit; (2) added G1883A HSS support; (3) added Japanese FPD standard (P/N 5188-5245) support;
(4) added forms: Certificate of System Qualification at end of EQR, Chromatography Report after each
applicable test, Errors and Corrections for operator and customer to record any corrections to EQR,
Data Transfer Audit Log for complete traceability.
Added kPa units for pressure tests.
Initial GC – Operational Qualification
End of EQP Review Document
© Agilent Technologies, Inc. 2014
Page 17 of 18
No reproduction, translation, or use without permission
www.agilent.com/chem/enterprise
Information, descriptions and specifications in this
publication are subject to change without notice.
© Agilent Technologies, Inc. 2014
Published in USA, April 22, 2014
Page 18 of 18