STANDARD METHODS 22 EDITION 5000 METHODS … · Methods for the Examination of Water and Wastewater 22nd edition 2012, available from American Public Health ... the Standard Methods

STANDARD METHODS 22ND

EDITION 5000 METHODSBy City of Phoenix

5020 QUALITY ASSURANCE/QUALITY CONTROL

INITIAL QUALITY CONTROL

Initial Demonstration Of Capability (IDC)*

Method Detection Limit *Operational Range*Refer to Section 1020 for specifics

ONGOING QUALITY CONTROL

Calibration Calibration Verification

+/-10 % unless otherwise specified in method

Quality Control Sample Method Blank

When appropriate (Table 5020:I) include at least one Method Blank daily or with each batch of 20 or fewer.

Laboratory Fortified Blank If the LFB is not prepared from a second source to confirm method accuracy,

(unless the method specifies otherwise) the laboratory must also verify the accuracy of its standard preparation by analyzing a mid-level second-source calibration standard whenever a new initial calibration curve is prepared. Results must agree within 15% unless otherwise specified in a method.

ONGOING QUALITY CONTROL

Duplicates When appropriate (Table 5020:I), run either a sample duplicate or an

LFMD per batch. It is not necessary to perform both. (For basic guidance on duplicates, see Section 1020B.)

Laboratory Fortified Matrix Include at least one LFM/LFMD daily or with each batch of 20 or fewer

samples. (Some regulatory programs require more frequent use of LFMs.

Section 1020 currently specifies that LFBs and LFMs be made from a second source. However, as long as each initial calibration solution is verified via a second source (5020B.2b), the LFB/LFM need not be from a second source (unless the method specifies otherwise).

Section Analyte Method Blank

LFB* LFM+ &LFMD‡ Other

5210B BOD ‐ ‐ ‐ 1,2,35210C ‐ ‐ ‐ 1,2,35210D ‐ ‐ ‐ 1,2,3

5220B COD X X X 1,2,35220C X X X 1,2,35220D X X X 1,2,3

Table 5020:I MINIMUM QUALITY CONTROL FOR METHODS IN PART 5000

5310B TOC X X X 1,2,35210C X X X 1,2,35210D X X X 1,2,35320B Dissolved Organic

HalogenX X X 1,2,3

5510B Aquatic HumicSubstances

X X X 1,2,3

5510C X X X 1,2,3

5520B Oil and Grease X X X 1,2,35520C X X X 1,2,35520D X X X 1,2,35520E X X X 1,2,35520F X X X 1,2,35520G X X X 1,2,3

5530B Phenols X X X 1,2,35530C5530D X X X 1,2,3

5540B Surfactants X X X 1,2,35540C X X X 1,2,35540D X X X 1,2,3

5550B Tannin and Lignin X X X 1,2,3

Section Analyte Method Blank

LFB* LFM+ &LFMD+

5560B § Organic/Volatile Acids X X X 1,2,3

5560C § X X X 1,2,3

5560D X X X 1,2,3

5710B THMs and DBPs ‐ ‐ ‐ 1,2,3

5710C ‐ ‐ ‐ 1,2,3

5710D ‐ ‐ ‐ 1,2,3

5910B UV‐Absorbing Organic Constituents

X ‐ ‐ 1,2,3

* Laboratory-fortified blank.† Laboratory-fortified matrix.‡ Laboratory-fortified matrix duplicate.§ A sample preparation technique that is normally combined with a subsequent determinative techniqueX indicates that a QC type is mandatory for the method.

- indicates that a QC type is not mandatory for the method.1. Additional QC guidelines in method.2. Duplicates or LFMD of the sample will be run.3. Refer to 5020B for further QC requirements.This table is not comprehensive; refer to the specific method and 5020B for further details.

SM 5210 B TRANSITIONING FROM 20TH EDITION TO 22ND EDITION

All changes noted reference 22nd

Edition Section Reference


3g(2) adds ATU solution as an optional Nitrification Inhibitor 3h Regarding GGA, the following was added: Prepare fresh

immediately before use “unless solution is maintained in a sterile condition. Store all glucose-glutamic mixtures at 4⁰C or lower. Commercial preparations may be used but concentrations may vary.”

4b (1) Check pH: if it is not between 6.0 - 8.0, adjust sample temperature to 20+/-3⁰C, then adjust pH to 7.0 to 7.2

4b (4) and 5b allows sample temperature prior to dilution to be 20+/-3⁰C rather than +/-1⁰C (but the incubation temperature remains 20+/-1⁰C). Also note that the “prior to dilution” is new.


4b(5) adds pretreatment procedures for samples containing hydrogen peroxide

4c expands guidance on selection and storage of source water and pinpoints the maximum allowed blank depletion at 0.20 mg/L rather than 0.2 mg/L.

4d and 5d “Do not filter seed sources; filtering removes the seed microorganisms.”

5a Dilution water should be at least 7.5mg/L DO before use 5c(1) For dilutions greater than 1:100 make a primary

dilution before making final dilution in the bottle.


5g “After preparing dilution, measure initial DO within 30 minutes.”

5c “make at least 3 dilutions of prepared sample…..”

5e “Seed all samples to which nitrification inhibitor has been added”

5i allows a +/- 6 hour variance in the “5 day” incubation period (5days +/- 6 hrs.)


6b Prepare 3 test bottles of GGA per batch of samples 6d “Ideally, make 3 dilutions of seed such that……” 7a(2) (and 6a) For bottles with 300mL of sample (100%

concentration), DO depletion may be reported as the BOD even if it is less than 2.0 mg/L . No K1 qualifier needed.

7b All test results that meet depletion criteria must be averaged within each dilution series. (results cannot be omitted for presence of toxicity, statistical outliers, etc)


7b Test replicates within a dilution series that show more than 30% differencebetween high and low values must be qualified with K9.

8b Detection limits were added for seeded vs. unseeded samples with and without dilutions.


Reporting: Average the test results for all qualified bottles within each dilution series. Report the result as BOD5 if nitrification is not inhibited. Report results as CBOD5 if nitrification is inhibited. Samples showing large differences between the computed BOD for different dilutions, for example, greater than 30%, may indicate the presence of a toxic substance or analytical problems. When the effect becomes repetitive, investigate to identify the cause. Identify results in the test reports when any of the following quality control parameters is not met:

• Dilution water blank exceeds 0.20 mg/L (5210B.6c),

• Glucose-glutamic acid check falls outside acceptable limits (5210B. 6b),

• Test replicates show more than 30% difference between high and low values,

• Seed control samples do not meet the above criteria in all dilutions (5210B.6d), or

• Minimum DO is less than 1.0 mg/L [5210B.7a3)].

SM 5310 B, C, D TRANSITIONING FROM 20TH EDITION TO 22ND EDITION

Throughout 5310, when making internal method references, the format "5310 C or D" is used rather than "Method C or D."

Some of the verbiage is different but the intent is the same


5310B.6 Quality Control - "The quality control practices considered to be an integral part of each method are summarized in Table 5020:I." was added.

The rest of this section goes on to require a blank & a 2nd source laboratory control sample after every 10th analysis, or to make periodic known additions to samples. It is worded exactly the same as the 20th edition.

Table 5020:I lists Method Blank, LFB, and LFM & LFMD as the minimum quality control requirements for 5310B, C & D.

Both 5310C.6 & 5310D.6 refer to 5310B.6, as they did in the 20th edition.


5310C.1b Interferences - Gives slightly more detail using "See 5310B.1b" rather than "See Section 5310B.1."

5310D.1b Interferences - Again gives more detail using "See 5310B.1b and C.1.b" rather than "See Section 5310B.1 and C.1."


The biggest change is not within the method, but in the ADHS method reference. The Standard Methods reference for TOC in the new Rules will be “C (2011).” AAR R9-14-610 Approved Methods and References Key Reference C American Public Health Association et al., Standard Methods for the Examination of Water and Wastewater 22nd edition 2012, available from American Public Health Association, 800 I Street, NW, Washington, DC 20001 or at http://www.standardmethods.org, with the approved method having the same last two digits in the method number as the year in which the method was approved by the Standard Methods Committee, as published for the individual methods in the 22nd edition."


The previous Standard Methods reference was “C2,” which included some ADHS specifications. C2 American Public Health Association et al., Standard Methods for the Examination of Water and Wastewater 20th ed. 1998, available from American Public Health Association, 800 I St., NW, Washington, DC 20001, modified to require: a. For drinking water TOC testing: 1. That inorganic carbon be removed from each TOC sample before analysis,

ii. That each TOC sample not be filtered before analysis, iii. That the pH of each TOC sample be checked an documented before analysis and

that the test result be qualified in the final report if the sample pH was >2, and iv. That each acidified TOC sample be analyzed within 28 days."

(Followed by ADHS requirements for drinking water (b.) DOC, (c.) UV and (d.) disinfection byproducts testing as well.)

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STANDARD METHODS 22 EDITION 5000 METHODS … · Methods for the Examination of Water and Wastewater 22nd edition 2012, available from American Public Health ... the Standard Methods