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
Hayfield Site
Site Date 04-15-02 8am
Influent
Code HS IN 1 Collected By Jim S.

Conditions Sunny, 75F

Comments: 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 • Operation of Analytical
• Method SOPs Instrumentation
• Measuring • Data Handling and Reporting
– Use of Volumetric glassware • Quality Control Activities
(pipettes, graduated glassware) • Safety
• Weighing / Use and care of
Analytical Balance
• Washing and Care of Glassware
QUALITY ASSURANCE
CONCEPTS
 Quality Assurance
Quality Control Quality Assessment
• Certification of Analyst • Performance Evaluation Samples
Competence • Performance Audits
• Recovery of Known Additions
• Analysis of Standards
• Analysis of Reagent Blanks
• Calibration with Standards
• Analysis of Duplicates
• Maintenance of Control Charts
 Quality Assurance
Quality Control Quality Assessment
• Certification of Analyst • Performance Evaluation Samples
Competence • Performance Audits
• Recovery of Known Additions
• Analysis of Standards
• Analysis of Reagent Blanks
• Calibration with Standards
• Analysis of Duplicates
• Maintenance of Control Charts
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 Quality Assessment
• Certification of Analyst • Performance Evaluation Samples
Competence • Performance Audits
• Recovery of Known Additions
• Analysis of Standards
• Analysis of Reagent Blanks
• Calibration with Standards
• Analysis of Duplicates
• Maintenance of Control Charts
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 1.40 mg/L 1.60 mg/L

50 mg/L Iron
33 Standard
 1.39 mg/L
1.58
1.20
X 100
100==98.7
99 %
100 %
%
1.40 mg/L
1.60
1.20
34
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 0

-180
4 7 10
pH
Standards
• “It’s what I always get” • “I got what I expected”
• “It meets the permit limit” • “I’ve run standards”
• “I did”: • “It’s a XXX brand instrument,
the best!”
– what the manual said
• “After 20 years you get a feel
– what tech support said
for it”
– what you told me
• “I’m a chemist”
• “It’s the same number the
• “It’s the same answer the lab
City of ____ gets” got”
 Quality Assurance
Quality Control Quality Assessment
• Certification of Analyst • Performance Evaluation Samples
Competence • Performance Audits
• Recovery of Known Additions
• Analysis of Standards
• Analysis of Reagent Blanks
• Calibration with Standards
• Analysis of Duplicates
• Maintenance of Control Charts
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 Quality Assessment
• Certification of Analyst • Performance Evaluation Samples
Competence • Performance Audits
• Recovery of Known Additions
• Analysis of Standards
• Analysis of Reagent Blanks
• Calibration with Standards
• Analysis of Duplicates
• Maintenance of Control Charts
Analysis of Duplicates
• Assesses precision
• 5% of sample need to be Duplicates
– (Standard Methods)
 Quality Assurance
Quality Control Quality Assessment
• Certification of Analyst • Performance Evaluation Samples
Competence • Performance Audits
• Recovery of Known Additions
• Analysis of Standards
• Analysis of Reagent Blanks
• Calibration with Standards
• Analysis of Duplicates
• Maintenance of Control Charts
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
Upper Warning Limit +2s
+1s
Mean
-1s
Lower Warning Limit -2s
-3s
Control Chart

Upper Control Limit +3s

+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 +3s
UW L +2s
+1s
Mean
-1s
LW L -2s
LC L -3s

Time
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 8 0.986
1 1.003 9 1.014
2 1.010 10 1.005
3 0.995 11 0.990
4 1.007 12 1.000
5 0.993 13 0.982
6 1.018 14 1.000
7 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
UC L +3s
1.02 mg/L UW L +2s
+1s
1.00 mg/L Mean
-1s
0.98 mg/L LW L -2s
0.97 mg/L LC L -3s

Time
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
UC L +3s
1.02 mg/L UW L +2s
+1s
1.00 mg/L Mean
-1s
0.98 mg/L LW L -2s
0.97 mg/L LC L -3s

Time
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
Iron Control Chart
Format graph as
1.05 1.05
necessary
1.03 1.03 UWL
mg/L Iron

LWL
1.01 1.01
UCL
0.99 0.99
LCL
0.97 0.97 mg/L iron
0.95 0.95
1 2 3 4 5
Sample
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
Iron Control Chart - Week 1 Week 1 results
1.05 1.05
display normal,
1.03 1.03 UWL
random variation
between the UWL
mg/L Iron

LWL
1.01 1.01
UCL and LWL.
0.99 0.99
LCL
0.97 0.97 mg/L iron

0.95 0.95
1 2 3 4 5 6 7
Sample
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
Iron Control Chart - Week 2
Week 2 – Three
1.05 1.05 or more points in
1.03 1.03 UWL
one direction
indicates a
mg/L Iron

LWL
1.01 1.01
UCL possible bias in
0.99 0.99
LCL analytical results.
0.97 0.97 mg/L iron
Investigate!
0.95 0.95
1 2 3 4 5 6 7
Sample
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
Iron Control Chart - Week 3
Week 3 – Data
1.05 1.05 has a high degree
1.03 1.03 UWL
of scatter to the
LCL. Investigate!
mg/L Iron

LWL
1.01 1.01
UCL
0.99 0.99
LCL
0.97 0.97 mg/L iron
0.95 0.95
1 2 3 4 5 6 7
Sample
 Quality Assurance
Quality Control Quality Assessment
• Certification of Analyst • Performance Evaluation Samples
Competence • Performance Audits
• Recovery of Known Additions
• Analysis of Standards
• Analysis of Reagent Blanks
• Calibration with Standards
• Analysis of Duplicates
• Maintenance of Control Charts
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