LABORATORY MANAGEMENT

and QUALITY ASSURANCE

Introduction
The analytical laboratory provides qualitative and
quantitative data for use in decision-making. To be valuable,
the data must accurately describe the characteristics and
concentrations of constituents in the samples submitted to the
laboratory. In many cases, because they lead to faulty
interpretations, approximate or incorrect results are worse
than no result at all.

HANDBOOK FOR ANALYTICAL QUALITY CONTROL IN WATER AND WASTEWATER

LABORATORIES, EPA 1979

Quality Assurance - Defined

Quality Assurance (QA) is a set of operating principles that,
if strictly followed during sample collection and analysis, will
produce data of known and defensible quality.
The Accuracy of the analytical result can be stated with a
high level of confidence.

STANDARD METHODS, 18th EDITION, 1992

Outline
Laboratory Management
Introduction to Quality Assurance Concepts

Laboratory Management
Who should be involved in laboratory management
and quality assurance?

Laboratory Management
Everyone involved with the lab:
Person sampling
Person running the test
Person washing the glassware
Person doing maintenance on the instruments
Person interpreting the results

Laboratory Management
Quality Assurance Program

Staff Organization and Responsibilities

Sample Control and Documentation
SOP for Analytical Methods & Procedures
Analyst Training Requirements
Equipment Preventative Maintenance
Calibration Procedures
Corrective Actions
Internal Quality Control Activities
Performance Audits
Data Assessment for Bias and Precision
Data Validation and Reporting

Laboratory Management
Keys to Quality Assurance Program:
Documentation
Communication
Training
Cross-Training
Updating

Sample Control and Documentation

A record keeping system (paper trail, chain of
custody) should track samples before, during, and
after analysis.
Everyone involved needs to understand and utilize
the system.

Sample Control and Documentation

Efficiently process information through lab system
while minimizing actual time spent recording data
Keep it simple!
Collect only the information you need

Suggested Information - Field

Site
Code

Hayfield Site
Influent
HS IN 1

Conditions
Comments:

Date 04-15-02 8am

Collected By Jim S.

Sunny, 75F
pH adjusted to <2 with
nitric acid
Grab sample

Suggested Information - Lab

Date of analysis
Laboratory technicians performing the analysis
Results (including units)
Analytical comments: based on need to know
Dilutions
Interferences encountered

SOP for Analytical Procedures

Describes method in enough detail that an
experienced analyst could obtain acceptable results.

SOP for Cleanliness

Labware cleaning procedures should be
documented and all persons involved should be
trained.

Routine Cleaning Procedure

Rinse glassware with tap water.
Clean glassware with a solution of water and
laboratory detergent.
Rinse the glassware with an acidic solution
1.0 N HCl
6N HNO3 for regulatory reporting of heavy metals

Rinse glassware at least 3X with DI water.

Routine Cleaning Procedure (cont.)

Glassware should be stored in a manner that
prevents contamination from dust particles.
Prior to analysis, rinse the glassware with sample to
prevent contamination or dilution.

SOP for Instrumentation Maintenance

Preventative maintenance is the key to optimal
instrument performance.
Follow any maintenance program and guidelines
suggested by the instrument manufacturer.
Instrument manual

Reduces instrument downtime

Service Contracts with Manufacturers

Analyst Training
Sample Logging and Preservation
Method SOPs
Measuring
Use of Volumetric glassware
(pipettes, graduated glassware)

Weighing / Use and care of

Analytical Balance
Washing and Care of Glassware

Operation of Analytical
Instrumentation
Data Handling and Reporting
Quality Control Activities
Safety

QUALITY ASSURANCE CONCEPTS

Quality Assurance
Quality Control
Certification of Analyst
Competence
Recovery of Known Additions
Analysis of Standards
Analysis of Reagent Blanks
Calibration with Standards
Analysis of Duplicates
Maintenance of Control Charts

Quality Assessment
Performance Evaluation Samples
Performance Audits

Quality Assurance
Quality Control
Certification of Analyst
Competence
Recovery of Known Additions
Analysis of Standards
Analysis of Reagent Blanks
Calibration with Standards
Analysis of Duplicates
Maintenance of Control Charts

Quality Assessment
Performance Evaluation Samples
Performance Audits

Certification of Analyst Competence

Demonstration of acceptable precision and accuracy
for each analyst
Minimum of four replicate analyses on a known
standard
Look for acceptable accuracy and precision
Acceptable limits vary per analytical method

Demonstration of Capability

What is Accuracy?
Accuracy is the nearness of a test result to the true
value.

What is Precision?
Precision is how closely repeated measurements
agree with each other.
Although good precision suggests good accuracy,
precise results can be inaccurate.

Imprecise and inaccurate

Accurate but imprecise

Precise but inaccurate

Precise and accurate

Quality Assurance
Quality Control
Certification of Analyst
Competence
Recovery of Known Additions
Analysis of Standards
Analysis of Reagent Blanks
Calibration with Standards
Analysis of Duplicates
Maintenance of Control Charts

Quality Assessment
Performance Evaluation Samples
Performance Audits

Standards
What is a standard?
Solution containing a known amount of a
specific substance
Example 1.00mg/L iron standard

Standards
How are standards used?
Instrument calibration
Instrument verification/accuracy check
Analyst training

Standards
Analysis of Known Standard Solutions Am I
running the test correctly?
Verifies instrument, technique, and reagents

Standards
Analysis of Known Standard Solutions
How often?
Daily, every Sample Batch?

National Institute of Standards and Technology

NIST

Standards
Recovery of Known Additions
Is my sample compatible with the test?
Identifies interferences and percent recovery

Standard Addition
Spiked sample

= 1.00 mg/L

Correct??
1.20 mg/L 1.39 mg/L 1.58 mg/L
1.20 mg/L

33

50 mg/L Iron
Standard

1.40 mg/L

1.60 mg/L

1.39 mg/L
1.58
mg/L
1.20
1.40 mg/L
1.60
mg/L
1.20
34

100==98.7
99 %
%
X 100
100
%

Calibration with Standards

Some instruments have built-in calibration curves,
not necessary to calibrate
Instrument without preprogrammed calibration
curves
Prepare curve daily - OR
Whenever a new lot of reagents is prepared

Calibrations

mg/L

ABS

pH Calibration Curve
+180
mV

-180
4

7
pH

10

Standards
Its what I always get
It meets the permit limit
I did:
what the manual said
what tech support said
what you told me

Its the same number the

City of ____ gets

I got what I expected

Ive run standards
Its a XXX brand
instrument, the best!
After 20 years you get a
feel for it
Im a chemist
Its the same answer the
lab got

Quality Assurance
Quality Control
Certification of Analyst
Competence
Recovery of Known Additions
Analysis of Standards
Analysis of Reagent Blanks
Calibration with Standards
Analysis of Duplicates
Maintenance of Control Charts

Quality Assessment
Performance Evaluation Samples
Performance Audits

Reagent Blanks
Some reagents contribute color to a sample
Quantifies amount of reagent contribution to color
formation
Monitors of purity of reagents

On each new lot of reagents

5% of samples (Standard Methods)

Reagent Blanks

Reagent Blanks

Quality Assurance
Quality Control
Certification of Analyst
Competence
Recovery of Known Additions
Analysis of Standards
Analysis of Reagent Blanks
Calibration with Standards
Analysis of Duplicates
Maintenance of Control Charts

Quality Assessment
Performance Evaluation Samples
Performance Audits

Analysis of Duplicates
Assesses precision
5% of sample need to be Duplicates
(Standard Methods)

Quality Assurance
Quality Control
Certification of Analyst
Competence
Recovery of Known Additions
Analysis of Standards
Analysis of Reagent Blanks
Calibration with Standards
Analysis of Duplicates
Maintenance of Control Charts

Quality Assessment
Performance Evaluation Samples
Performance Audits

What is a Control Chart?

Quality control (QC) measuring device that visually
represents the QC data
Information in a control chart can aid in
determining:
Probable source of measurement variability
Whether or not a process is in statistical control

How do Control Charts Work?

If the chart displays other than random variation
around the expected result, it suggests a problem
with the measurement process.
Control limits are plotted on the chart, to assess whether
this has happened. The measurement results are
expected to remain within these limits.

Normal Distribution
(Standard Deviation around the Mean)

-3s

-2s

-1s

MEAN

+1s

+2s

+3s

Confidence Limits

68%

-3s

-2s

-1s

10.00

+1s

+2s

+3s

Confidence Limits

95%

-3s

-2s

-1s

10.00

+1s

+2s

+3s

Confidence Limits

99%
-3s

-2s

-1s

10.00

+1s

+2s

+3s

Control Charts
A control chart is essentially a normal distribution
flipped on its side
A control chart is a plot of:
Test units on the vertical scale
Sequence of time on the horizontal scale

Control Chart
+3s
+2s
+1s
Mean
-1s
-2s
-3s

Control Chart
+3s
+2s

Upper Warning Limit

+1s
Mean
-1s
Lower Warning Limit

-2s
-3s

Control Chart
+3s

Upper Control Limit

+2s
+1s
Mean
-1s
-2s
Lower Control Limit

-3s

How do Control Charts Work?

Warning Limits
Set at 2s
Standard Methods suggests:
If 2 of 3 points are outside warning limits, analyze another
sample. If it is within warning limits, continue. If it is outside
warning limits, stop and troubleshoot.

How do Control Charts Work?

Control Limits
Set at 3s
Standard Methods suggests:
If any point is outside control limits, analyze another sample.
If it is within control limits, continue. If it is outside control
limits, stop and troubleshoot.

How do Control Charts Work?

A standard is measured regularly, and the results are
plotted on the control chart.
Control chart is a graph of concentration versus
time.

Control Chart
Iron Standard, FerroVer Procedure

UC L
UW L

+3s
+2s
+1s

Mean
-1s
-2s

LW L
LC L

Time

-3s

Constructing a Control Chart

A control chart can be constructed in a variety of
ways:
Graph paper
Spreadsheet problem, such as Excel

Constructing a Control Chart

Analyze 10-15 replicates of a standard.
Determine the mean and standard deviation.
Calculate 2s and 3s

Construct the control chart around the mean value

Use 2s as the warning limits
Use 3s as the control limits

Example Iron Standard Replicates

Sample

mg/L Iron

0.986

1.003

1.014

1.010

10

1.005

0.995

11

0.990

1.007

12

1.000

0.993

13

0.982

1.018

14

1.000

1.000

15

0.997

Example Iron Standard Replicates

Calculate:
Mean
Standard Deviation (1s)
2s
3s

Example Iron Standard Replicates

Calculate:
Mean
1.000
Standard Deviation (1s) 0.010 (0.990-1.010)
2s
0.020 (0.980-1.020)
3s
0.030 (0.970-1.030)

Control Chart
Iron Standard, FerroVer Procedure

1.03 mg/L
1.02 mg/L

UC L
UW L

+3s
+2s
+1s

Mean

1.00 mg/L

-1s
0.98 mg/L
0.97 mg/L

Time

-2s

LW L
LC L

-3s

Constructing a Control Chart

First, set up a
spreadsheet
with columns for
UWL, LWL, UCL,
LCL, and sample
results

Constructing a Control Chart

Fill in values for
UWL, LWL, UCL,
LCL, and sample
results

Control Chart
Iron Standard, FerroVer Procedure

1.03 mg/L
1.02 mg/L

UC L
UW L

+3s
+2s
+1s

Mean

1.00 mg/L

-1s
0.98 mg/L
0.97 mg/L

Time

-2s

LW L
LC L

-3s

Constructing a Control Chart

Fill in values for
UWL, LWL, UCL,
LCL, and sample
results

Constructing a Control Chart

Highlight data
and create a
graph

Constructing a Control Chart

mg/L Iron

Iron Control Chart

1.05

1.05

1.03

1.03

1.01

1.01

0.99

0.99

0.97

0.97

0.95

0.95
1

3
Sample

Format graph as
necessary
UWL
LWL
UCL
LCL
mg/L iron

Example Control Charts

Control Analysis Results Week 1
Sample

mg/L Iron

Thurs

0.988

Mon

1.003

Fri

0.992

Tues

0.995

Sat

0.992

Wed

1.006

Sun

1.004

Example Control Charts

mg/L Iron

Iron Control Chart - Week 1

1.05

1.05

1.03

1.03

1.01

1.01

0.99

0.99

0.97

0.97

0.95

0.95
1

4
Sample

UWL
LWL
UCL
LCL
mg/L iron

Week 1 results
display normal,
random variation
between the
UWL and LWL.

Example Control Charts

Control Analysis Results Week 2
Sample

mg/L Iron

Thurs

0.993

Mon

1.008

Fri

0.989

Tues

1.000

Sat

0.988

Wed

0.996

Sun

0.983

Example Control Charts

mg/L Iron

Iron Control Chart - Week 2

1.05

1.05

1.03

1.03

1.01

1.01

0.99

0.99

0.97

0.97

0.95

0.95
1

4
Sample

UWL
LWL
UCL
LCL
mg/L iron

Week 2 Three
or more points
in one direction
indicates a
possible bias in
analytical
results.
Investigate!

Example Control Charts

Control Analysis Results Week 3
Sample

mg/L Iron

Thurs

0.986

Mon

1.012

Fri

0.994

Tues

1.000

Sat

0.968

Wed

1.015

Sun

0.997

Example Control Charts

mg/L Iron

Iron Control Chart - Week 3

1.05

1.05

1.03

1.03

1.01

1.01

0.99

0.99

0.97

0.97

0.95

0.95
1

4
Sample

UWL
LWL
UCL
LCL
mg/L iron

Week 3 Data
has a high
degree of scatter
to the LCL.
Investigate!

Quality Assurance
Quality Control
Certification of Analyst
Competence
Recovery of Known Additions
Analysis of Standards
Analysis of Reagent Blanks
Calibration with Standards
Analysis of Duplicates
Maintenance of Control Charts

Quality Assessment
Performance Evaluation Samples
Performance Audits

Performance Evaluation Samples

Standards provided by an outside agency
Blind Samples

Performance Audits
Inspection to document sampling handling from
receipt to final reporting of results
To detect any variations from SOPs
Checklists developed for each analysis type

Sample entered in log book?

Meter calibrated?
Standard Analyzed?
Etc., etc..

LABORATORY MANAGEMENT
and QUALITY ASSURANCE

References
Standards Methods
Handbook for Analytical Quality Control in Water and
Wastewater Laboratories
EPA 1979

Hach Water Analysis Handbook

An Introduction to Standards and Quality Control for the
Laboratory
Barbara Martin, Hach Company