Chromatographic Peak Integration

The NELAC Institute
Manual Integration
Assessment Forum
January, 2008
Bob Di Rienzo
DataChem Laboratories, Inc.
Melinda Jacobson
City of Phoenix
Discussion Topics
9 What Is It
9 Why Do We Need It with Examples
9 Areas of Concern
9 Requirements
9 Documentation
What is Manual Integration?
Peak integration is the process used by
chromatographic software to determine
peak area or height used for quantitation.
The software may be configured to perform
“Automatic Integration” through
defined integration parameters.
“Manual Integration” is the process employed by the
data user to integrate peak height or area by manually
setting the baseline using chromatographic software.
Why Do We Need To Do It?
Manual integration is performed by the

data user when the automatic integration
performed by the data system is in error:
9Software integration limitations;

9Complicated chromatography due to sample
matrix interferences; or
9Poor resolution or response.
Software Error: Peak is Not Integrated
Software Error: Wrong Peak Identified

Chromatography Problem 1: Split Peaks

Chromatography Problem 2:
Coelution of Target Compounds/Shoulders
Chromatography Problem 3: Baseline Noise

Negative Peaks
Rising or Falling Baselines
Excessive Peak Tailing
Integration of Hydrocarbons
Areas of Concern
Manual integration is a perfectly acceptable,

and expected procedure to be performed
on chromatographic data that has not been
integrated appropriately using the
software’s automatic integration
procedures.
Areas of Concern
A “No Manual Integration” Policy is a problem…
Computers aren’t always right!

Areas of Concern
Consistent and appropriate integrations are
scientifically defensible…inconsistent or
inappropriate integrations are difficult to defend.
All standards, samples and QC samples must be

integrated in the same manner.
Areas of Concern
Manual integrations should NEVER be performed in an
attempt to make the data meet method acceptance criteria:
Removing Area from the Peak a.k.a. “Peak Shaving”

Areas of Concern
Adding Area to the Peak a.k.a. “Peak Enhancing”

Areas of Concern
Changing Peak Height

Areas of Concern
Corrective or Preventative Actions, not manual
integration, should be performed when poor
resolution or response is the problem.
Enlarged chromatograms must be used to

discern the baseline noise.
Always review hard copy data against

electronic data.
NELAC 2003 Requirements
On-Site Assessment
Chapter 3, Appendix C,
Section C.4.1.7.8
Procedures for allowing manual

correction of raw data (e.g. manual
integration) and for overriding
instrument qualitative results.
Quality Systems
Chapter 5, Control of Records
Section 5.4.12.1.5
The laboratory shall establish a record

keeping system that allows the history of
the sample and associated data to be
readily understood through the
documentation. This system shall
produce unequivocal, accurate records
that document all laboratory activities….
Quality Systems
Chapter 5, Analytical Records
Section 5.4.12.2.2
Observations, data and calculations

shall be recorded at the time they
are made and shall be identifiable to
the specific task.
Quality Systems
Chapter 5, Analytical Records
Section 5.4.12.2.5.3 e)
The essential information to be

associated with the analysis….. shall
be included
all manual calculations, e.g., manual
integrations; and ,
Quality Systems
Chapter 5, Data Integrity Training
Section 5.5.2.7
Specific examples of breaches of

ethical behavior should be
discussed including improper data
manipulations…………
Quality Systems
Chapter 5, Control of Data
Section 5.5.4.7
Calculations and data transfers shall

be subject to appropriate checks in
a systematic manner.
Quality Systems
Section 5.5.4.7.1 c)
The laboratory shall establish SOPs

addressing manual calculations
including manual integrations.
Quality Systems
Section 5.5.4.7.2.b)
procedures are established and

implemented for protecting the data;
such procedures shall include, but not be
limited to, integrity and confidentiality of
data entry or collection, data storage,
data transmission and data processing;
TNI Volume 1, Module 2
General Requirements
Volume 1, Module 2
Control of Records (4.13.2.2)
Observations, data and calculations

shall be recorded at the time they
are made and shall be identifiable to
the specific task.
Volume 1, Module 2
Control of Records (4.13.3 a)
The laboratory shall establish a record

keeping system that allows the history of
the sample and associated data to be
readily understood through the
documentation. This system shall
produce unequivocal, accurate records
that document all laboratory activities….
Volume 1, Module 2
Control of Records (4.13.3 f)
All information necessary for the

historical reconstruction of data
must be maintained by the
laboratory.
vii. all manual calculations;

Volume 1, Module 2
Data Integrity Training (5.2.7 e)
Specific examples of breaches of

ethical behavior such as improper
data manipulations……..
Volume 1, Module 2
Control of Data (5.4.7.1)
Calculations and data transfers shall

be subject to appropriate checks in
a systematic manner.
Volume 1, Module 2
Control of Data (5.4.7.2 b)
procedures are established and

implemented for protecting the data;
such procedures shall include, but not be
limited to, integrity and confidentiality of
data entry or collection, data storage,
data transmission and data processing;
Documentation
Procedures for All Manual Calculations

9 (Manual Integrations)
Training
9 (Manual Calculations, Peer Review, and Data Integrity)
Analytical Records – All Manual Calculations

9 (Manual Integrations)
Manual Integration Documentation
Include both the original and manually
9 integrated chromatograms
(NELAC 2003 Analytical Records - historical reconstruction)
9 Analyst’s Initials and Date and Reason

(NELAC 2003 Analytical Records – all lab activities)
9 Reviewer’s Initials and Date

(NELAC 2003 Control of Data – appropriate checks / systematic manner)
9 Review electronic data against hard copy

(NELAC 2003 Control of Data – protecting the data)
FINALLY…
Manual Integrations are necessary for the

generation of data of known and
documented quality.
Just because a manual integration has been

documented does not mean it’s acceptable
and/or appropriate.
References
9EPA Region 9 SOP #835, “Chromatographic Integration
Procedures”
9Florida Department of Health SOP CM-018-1.5, “Laboratory

Policy Regarding Manual Chromatographic Peak Integration”
9EPA OIG Report No. 2006-P-00036, “Promising Techniques

Identified to Improve Drinking Water Laboratory Integrity and
Reduce Public Health Risks”
9“Chromatographic Integration Methods”, Second Edition,

Norman Dyson, 1996
Thank You
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The NELAC Institute

9 Why Do We Need It with Examples

Manual integration is performed by the

9Software integration limitations;

Software Error: Peak is Not Integrated

Software Error: Wrong Peak Identified

Chromatography Problem 1: Split Peaks

Chromatography Problem 3: Baseline Noise

Manual integration is a perfectly acceptable,

A “No Manual Integration” Policy is a problem…

Computers aren’t always right!

All standards, samples and QC samples must be

Removing Area from the Peak a.k.a. “Peak Shaving”

Adding Area to the Peak a.k.a. “Peak Enhancing”

Changing Peak Height

Enlarged chromatograms must be used to

Always review hard copy data against

Procedures for allowing manual

The laboratory shall establish a record

Observations, data and calculations

The essential information to be

Specific examples of breaches of

Calculations and data transfers shall

The laboratory shall establish SOPs

procedures are established and

Observations, data and calculations

The laboratory shall establish a record

All information necessary for the

vii. all manual calculations;

Specific examples of breaches of

Calculations and data transfers shall

procedures are established and

Procedures for All Manual Calculations

Analytical Records – All Manual Calculations

9 Analyst’s Initials and Date and Reason

9 Reviewer’s Initials and Date

9 Review electronic data against hard copy

Manual Integrations are necessary for the

Just because a manual integration has been

9Florida Department of Health SOP CM-018-1.5, “Laboratory

9EPA OIG Report No. 2006-P-00036, “Promising Techniques

9“Chromatographic Integration Methods”, Second Edition,

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