2020

QUALITY ASSURANCE/QUALITY CONTROL

Reviewed by Standard Methods Committee, 2010. Editorial revisions, 2021. Terry E. Baxter (chair), Rodger B. Baird.

2020  A. Introduction

Quality control (QC) is an important attribute of any labora- evaluating the test’s accuracy and precision. Laboratories should
tory’s quality assurance (QA) program. Without QC, there is no generate method-specific acceptance criteria for precision or bias
confidence in the results of analytical tests. As described in Part (or both) using control-charting techniques.
1000, essential QC measures include method calibration, reagent Evaluate precision by analyzing duplicate samples. However, if
standardization, assessment of each analyst’s capabilities, anal- these results are “nondetect” or “invalidated,” precision cannot be
ysis of blind check samples, determination of the method’s sen- calculated. Laboratory-fortified matrices (LFMs) are not appli-
sitivity [method detection level (MDL) or quantification limit], cable to methods currently in Part 2000, so Table 2020:2 has no
and regular evaluation of bias, precision, and the presence of entry in the LFM column.
laboratory contamination or other analytical interference. The Evaluate bias by analyzing standards or samples with known
details of these procedures, their performance frequency, and or certifiable parameter values. If a known or certifiable standard
expected ranges of results should be formalized in a written QA analyte cannot be prepared or is otherwise unavailable, then bias
manual and standard operating procedures. In addition, it is the cannot be calculated.
laboratory’s responsibility to qualify and report data values not To help verify the accuracy of calibration standards and over-
meeting QC or other method-defined requirements with sufficient all method performance, participate in an annual or preferably
information so the client or end user can determine the usability semi-annual program of analysis of single-blind QC check sam-
of the qualified data. ples (QCS)—ideally provided by an external entity. Such pro-
While general information on QC procedures is provided in Part grams are sometimes called proficiency testing (PT)/performance
1000 and specific procedures are typically outlined in individual evaluation (PE) studies. An unacceptable result on a PT sample is
methods, some of the methods in Part 2000 are not amenable to often a strong indication that a test protocol is not being followed
standard QC procedures; they have procedures considered unique to successfully. Investigate circumstances fully to find the cause. In
the method that do not necessarily apply to other more conventional many jurisdictions, participation in PT studies is a required part
analytical methods. For some methods, such as oxygen-consumption of laboratory certification and accreditation.
rate, bias is not applicable. Several methods in this part do not Laboratories may save time and money by purchasing premade
have acceptance-criteria guidance for either precision or bias of test standards, titrants, and reagents, but they still must perform the
results. This does not, however, relieve analysts of the responsibility for QC checks on these materials required by the analytical methods.

2020  B. Quality Control Practices

1. Initial Quality Control where:

5.84 = the two-sided Student t factor for 99% confidence limits and
a. Initial demonstration of capability (IDC): Analysts must
3 degrees of freedom.1
demonstrate their capability to use a method before analyzing
any samples for the first time using that method. For methods Also, verify that the method is sensitive enough to meet mea-
in which bias is applicable (see Table 2020:1), run a laboratory- surement objectives for detection and quantitation by determining
fortified blank (LFB) (2020 B.2e), performance evaluation sample, the lower limit of the operational range. (For basic guidance on
or standard with a known or otherwise certifiable concentration at demonstrating capability, see Sections 1020 B.1 and 2)
least 4 times and compare results to the limits listed in the method b. Method detection level (MDL): Before analyzing samples,
or those established by the laboratory. If no limit is specified, use determine the MDL for each analyte or method parameter in
the following procedure to establish limits: accordance with Section 1020 B.4. Part 2000 methods considered
Calculate the standard deviation of the 4 samples. The LFB’s amenable to MDL determination are indicated in Table 2020:1.
recovery limits are Determine MDL at least annually for each analyte or parameter
in a method and major matrix category. The laboratory should
LFB s initial recovery limits = mean ± (5.84 ×standard deviation) define all matrix categories in its QA manual.
Ideally, use pooled data from several analysts rather than data
from one analyst. (For specific information on MDLs and pooled
MDLs, see Section 1020 B.4.)

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 2020 QUALITY ASSURANCE/QUALITY CONTROL - B. Quality Control Practices

c. Operational range: Before using a new method or instrument, acceptance criteria for the operational range, including MRL, in
determine its operational range (upper and lower limits), or at least the QA/QC documentation. In Part 2000, only salinity suggests an
verify that the intended range of use is within the operational range. initial operating range (see Table 2020:1).
For each analyte, use standard concentrations that provide increas-
ing instrument or other test response. The minimum reporting level 2. Ongoing Quality Control
(MRL) is set to a concentration at or above the lowest standard used
in the analysis. Quantitation at the MRL must be verified initially a. Calibration or standardization: Calibrate the method or
and at least quarterly (preferably daily) by analyzing a QC sam- standardize titration reagents using the directions in the proce-
ple (where applicable to the method). Laboratories should define dure. Methods in Part 2000 that require calibration or titration
Table 2021:1. Methods in Part 2000 Indicating or Amenable to Initial Quality Control
Section Bias Precision MDL Operational Range
2120 B Color – • – –
2120 C – • • –
2120 D – • • –
2120 E – • • –
2120 F – • • –

2130 B Turbidity – – • –

2170 B Flavor Profile Analysis – • – –

2310 B Acidity – • – –

2320 B Alkalinity • • – –

2340 C Hardness • • – –

2350 B Oxidant Demand/Requirement – – • –

2350 C – – • –
2350 D – – • –
2350 E – – • –

2510 B Conductivity – • – –

2520 B Salinity – • – •
2520 C – • – –

2530 C Floatables • • • –

2540 B Solids – • – –
2540 C – • – –
2540 D – • – –
2540 E – • – –

2560 B Particle Counting and Size Distribution – • • –

2560 C – • • –
2560 D – • • –

2570 B Asbestos • • – –

2580 B Oxidation–Reduction Potential • • – –

2710 G Tests on Sludges – • – –

2710 H – • – –

2720 B Anaerobic Sludge Digester Gas Analysis • • – –

2720 C • • • –

2810 B Dissolved Gas Supersaturation • • – –

• indicates that the QC type is considered applicable or amenable to the method.
– indicates that the QC type is neither applicable or amenable to the method.
Note: This table is not comprehensive; refer to the specific method for details.

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 2020 QUALITY ASSURANCE/QUALITY CONTROL - B. Quality Control Practices

Table 2020:2. Summary of Ongoing Quality Control for Methods in Part 2000
Calibrate or
Section Standardize QCS MB LFB Duplicates LFM
2120 B Color • • – – • –
2120 C • • – – • –
2120 D • • – – • –
2120 E • • – – • –
2120 F • • – – • –

2130 B Turbidity • • – – – –

2150 B Odor – – • – – –
2150 C – – • – • –

2160 B Taste – – • – – –

2170 B Flavor Profile Analysis – – • – • –

2310 B Acidity • • • • • –

2320 B Alkalinity • • – • • –

2340 C Hardness • • • • • –

2350 B Oxidant Demand/Requirement – – • – – –

2350 C – – • – – –
2350 D – – • – – –
2350 E – – • – – –

2510 B Conductivity • • – • • –

2520 B Salinity • • – • • –
2520 C • • – – • –

2540 B Solids – – • • • –
2540 C – – • • • –
2540 D – – • • • –
2540 E – – • • • –
2540 F – – – – • –
2540 G – – – – • –

2550 B Temperature • – – – – –

2560 B Particle Counting and Size • • • • • –

2560 C Distribution • • • • • –
2560 D • • • • • –

2570 B Asbestos • – • – • –

2580 B Oxidation–Reduction Potential • – – – • –

2710 B Tests on Sludges • – – – – –

2710 G – – – – • –
2710 H – – – – • –

2720 B Anaerobic Sludge Digester Gas – – – – • –

2720 C Analysis • • – – • –

2810 B Dissolved Gas Supersaturation • – – – • –

• indicates that the QC type is considered applicable or amenable to the method.
– indicates that the QC type is neither applicable or amenable to the method.
Note: This table is not comprehensive; refer to the specific method for details.

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 2020 QUALITY ASSURANCE/QUALITY CONTROL - B. Quality Control Practices

reagent standardization are indicated in Table 2020.2. (For basic demonstrate ongoing capability. Some methods may have spe-
calibration guidance, see Section 1020 B.11.) cific limits to use in lieu of plotting control charts. In those cases,
b. Calibration or standardization verification: Verify calibra- control charts may still be useful in identifying potential prob-
tion by periodically analyzing a calibration standard and calibra- lems. Ensure that the LFB meets the method’s performance crite-
tion blank during a run—typically, after each batch of 10 samples ria when such criteria are specified. Establish corrective actions to
and at the end of the run. The calibration verification standard’s be taken if the LFB does not satisfy acceptance criteria.
analyte or parameter concentration should be varied over the cal- Include at least one LFB daily or per each batch of 20 or fewer
ibration range to determine detector response. samples. Some regulatory programs require a higher frequency of
For the calibration verification to be valid, check standard LFBs. If the sample results are often “nondetect,” consider using
results must not exceed ±10% of its true value, and calibration duplicate LFBs to assess precision.
blank results must not be greater than one-half the reporting level f. Duplicates: When appropriate (Table 2020:2), randomly select
(unless the method specifies otherwise). routine samples to be analyzed twice. Independently prepare and
If a calibration verification fails, immediately cease analyzing analyze duplicate samples. Include at least one duplicate for each
samples and initiate corrective action. The first step may be to matrix type daily or with each batch of 20 or fewer samples. Calcu-
reanalyze the calibration verification. If the calibration verifica- late control limits for duplicates when method-specific limits are not
tion passes, continue the analysis. Otherwise, repeat the initial provided. (For basic guidance on duplicates, see Section 1020 B.7.)
calibration and reanalyze the samples run since the last accept- Some regulatory programs require more frequent use of duplicates.
able calibration verification.
If the LFB is not prepared from a second source to confirm method 3. Calculations
accuracy, the laboratory must also verify the accuracy of its standard
preparation by analyzing a midlevel second-source calibration stan- a. LFB recovery:
dard whenever a new initial calibration curve is prepared. Results
must agree within 15% (unless otherwise specified in a method).  measured conc 
LFB % Recovery =   ×100
Verify standardized titration reagents by periodically re-standard-  spiked conc 
 
izing. Method parameters in Part 2000 that are determined using
standardized titration reagents are acidity, alkalinity, and hardness.
b. Relative percent difference:
Typically, the standardized reagents are stable for several months
when sealed to avoid evaporation and stored properly. Re-standard-  
ize reagents once a month or when improper storage occurs. If the  
 D1 − D2 
titration reagent’s normality (titer value) has changed, then use the % RPD =   ×100
  D1 + D2  
measured value, adjust the normality (titer value) as the procedure    
  2  
describes, or prepare and standardize fresh titration reagent as needed.
c. Quality control sample (QCS): Analyze an externally gen-
erated, blind QCS (unknown concentration) at least annually where:
(preferably semi-annually or quarterly). Obtain this sample from
a source external to the laboratory, and compare results to that D1 = concentration determined for first duplicate, and
D2 = concentration determined for second duplicate.
laboratory’s acceptance results. If testing results do not pass
acceptance criteria, investigate why, take corrective action, and c. Relative standard deviation (% RSD):
analyze a new QCS. Repeat this process until results meet the
acceptance criteria. Methods in Part 2000 considered amenable to s
% RSD = ×100
QCS determination are indicated in Table 2020.2. x
d. Method blank (MB): Include at least one MB daily or with
each batch of 20 or fewer samples, whichever is more frequent. n
Any constituents recovered must generally be less than or equal ∑ ( xi − x )2
i =1
to one-half the reporting level (unless the method specifies oth- s=
(n −1)
erwise). If any MB measurements are at or above the reporting
level, take immediate corrective action as outlined in Section
1020 B.5. This may include reanalyzing the sample batch. where:
e. Laboratory-fortified blank (LFB): If each initial calibration s = standard deviation,
solution is verified via a second source (2020 B.2b), the LFB n = total number of values from replicate analyses,
need not be from a second source (unless otherwise specified in a xi = each individual value used to calculate mean, and
method). Table 2020:2 indicates methods in Part 2000 where the x = mean of the total number (n) of values.
use of LFB is considered appropriate.
Using stock solutions preferably prepared with the second References
source, prepare fortified concentrations so they are within the
calibration curve. Ideally, vary LFB concentrations to cover the 1. Meier PC, Zund EE. Statistical methods in analytical chemistry,
range from the midpoint to the lower part of calibration curve, 2nd ed. New York, (NY): Wiley Interscience; 2000.
including the reporting limit. 2. U.S. Environmental Protection Agency. Definition and procedure for
Calculate percent recovery, plot control charts, and determine the determination of the method detection limit, rev. 1.11, 1995. 40
control limits (Section 1020 B.13) for these measurements to CFR Part 136, Appendix B. Fed Reg. 5:23703.
Published online: August 27, 2018
Revised: January 11, 2022
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