laboratory management and quality assurance
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LABORATORY MANAGEMENT LABORATORY MANAGEMENT and QUALITY ASSURANCEand 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
Date
Conditions
Collected By
Site
Code
Comments:
Hayfield Site Influent
04-15-02 8am
HS IN 1 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 QUALITY ASSURANCE CONCEPTSCONCEPTS
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
Precise but inaccurate
Accurate but imprecise
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’
33
= 1.00 mg/L
50 mg/L Iron Standard
1.20 mg/L 1.39 mg/L 1.58 mg/L
Correct??
1.20 mg/L 1.40 mg/L 1.60 mg/L
34
X 100 = 100 %1.20 mg/L
1.20 mg/LX 100 = 99 %
1.39 mg/L
1.40 mg/LX 100 = 98.7 %
1.58 mg/L
1.60 mg/L
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
mVmV
pHpH
0
+180
-1804 7 10
Standards
• “It’s what I always get”• “It meets the permit limit”• “I did”:
– what the manual said– what tech support said– what you told me
• “It’s the same number the City of ____ gets”
• “I got what I expected”• “I’ve run standards”• “It’s a XXX brand instrument,
the best!”• “After 20 years you get a feel
for it” • “I’m a chemist” • “It’s 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 DistributionNormal Distribution(Standard Deviation around the Mean)
+2s+2s +3s+3s+1s+1s-1s-1s-2s-2s-3s-3s MEAN
Confidence LimitsConfidence Limits
+2s+2s +3s+3s+1s+1s-1s-1s-2s-2s-3s-3s 10.00
68%
Confidence LimitsConfidence Limits
+2s+2s +3s+3s+1s+1s-1s-1s-2s-2s-3s-3s 10.00
95%
Confidence LimitsConfidence Limits
+2s+2s +3s+3s+1s+1s-1s-1s-2s-2s-3s-3s 10.00
99%
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+3s
+2s+2s
+1s+1s
Mean
-1s-1s
-2s-2s
-3s-3s
Control Chart
+3s+3s
+2s
+1s+1s
Mean
-1s-1s
-2s
-3s-3s
Upper Warning Limit
Lower Warning Limit
Control Chart
+3s
+2s+2s
+1s+1s
Mean
-1s-1s
-2s-2s
-3s
Upper Control Limit
Lower Control Limit
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.
+3s+3s
+2s+2s
+1s+1s
Mean
-1s-1s
-2s-2s
-3s-3s
UC L
LC LLW L
UW L
Control ChartControl ChartIron Standard, FerroVer ProcedureIron Standard, FerroVer Procedure
TimeTime
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
1 1.003
2 1.010
3 0.995
4 1.007
5 0.993
6 1.018
7 1.000
8 0.986
9 1.014
10 1.005
11 0.990
12 1.000
13 0.982
14 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)
+3s+3s
+2s+2s
+1s+1s
Mean
-1s-1s
-2s-2s
-3s-3s
UC L
LC LLW L
UW L
Control ChartControl ChartIron Standard, FerroVer ProcedureIron Standard, FerroVer Procedure
TimeTime
1.00 mg/L
1.02 mg/L
0.98 mg/L
1.03 mg/L
0.97 mg/L
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
+3s+3s
+2s+2s
+1s+1s
Mean
-1s-1s
-2s-2s
-3s-3s
UC L
LC LLW L
UW L
Control ChartControl ChartIron Standard, FerroVer ProcedureIron Standard, FerroVer Procedure
TimeTime
1.00 mg/L
1.02 mg/L
0.98 mg/L
1.03 mg/L
0.97 mg/L
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
0.95
0.97
0.99
1.01
1.03
1.05
1 2 3 4 5
Sample
mg
/L I
ron
0.95
0.97
0.99
1.01
1.03
1.05
UWL
LWL
UCL
LCL
mg/L iron
Format graph as necessary
Example Control Charts
• Control Analysis Results – Week 1
Sample mg/L Iron
Mon 1.003
Tues 0.995
Wed 1.006
Thurs 0.988
Fri 0.992
Sat 0.992
Sun 1.004
Example Control Charts
Iron Control Chart - Week 1
0.95
0.97
0.99
1.01
1.03
1.05
1 2 3 4 5 6 7
Sample
mg
/L I
ron
0.95
0.97
0.99
1.01
1.03
1.05
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
Mon 1.008
Tues 1.000
Wed 0.996
Thurs 0.993
Fri 0.989
Sat 0.988
Sun 0.983
Example Control Charts
Iron Control Chart - Week 2
0.95
0.97
0.99
1.01
1.03
1.05
1 2 3 4 5 6 7
Sample
mg
/L I
ron
0.95
0.97
0.99
1.01
1.03
1.05
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
Mon 1.012
Tues 1.000
Wed 1.015
Thurs 0.986
Fri 0.994
Sat 0.968
Sun 0.997
Example Control Charts
Iron Control Chart - Week 3
0.95
0.97
0.99
1.01
1.03
1.05
1 2 3 4 5 6 7
Sample
mg
/L I
ron
0.95
0.97
0.99
1.01
1.03
1.05
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 LABORATORY MANAGEMENT and QUALITY ASSURANCEand 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