EPA Method 317

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EPA Method 317:
Oxyhalide DPBs and Bromide by IC. Official Name: Determination of Inorganic Oxyhalide Disinfection By-Products in Drinking Water Using Ion Chromatography with the Addition of a Postcolumn Reagent for Trace Bromate Analysis

Summary:
The concentrations of anions in a 225-uL are determined using an ion chromatography (IC) system equipped with an ultraviolet/visible (UV/Vis) detector or a conductivity detector (CD).

Scope:
This method determines inorganic oxyhalide disinfection by-product anions in reagent water, surface water, ground water, and finished drinking water.

Citation:
Methods for the Determination of Organic and Inorganic Compounds in Drinking Water, Volume 1 (EPA/815-R-00-014)

Interferences:
(A) Co-elution: Modifying the eluent with organic solvents, changing the detection system, or pretreating the sample can reduce co-elution.(B) Pretreatment cartridges: Use of a pretreatment cartridge can lead to artifacts in the sample; use with caution.(C) Turbidity: Remove turbidity using filtration.(D) Weakly-bound anions: Anions which are weakly retained by the column interfere with fluoride determination at > 1.5 mg/L.(E) Carryover effects: There are some compounds in ozonated and chlorine dioxide matrices which will elute well after sulfate. These may carry over in later runs.(F) Chlorine dioxide. Chlorine dioxide can form chlorite. Remove chlorine dioxide by purging the sample with inert gas.(G) Chlorite: Chlorite interferes with the quantitation of low-concentration bromate on the post-column UV/Vis detector, and should be removed.

QC Requirements:
Initial demonstration of laboratory capability (IDC), and subsequent analysis in each analysis batch of a Laboratory Reagent Blank (LRB), Initial Calibration Check Standard (ICCS), Laboratory Fortified Blank (LFB), Instrument Performance Check Standard (IPC), Continuing Calibration Check Standards (CCCS), Laboratory Fortified Sample Matrix (LFM), and either a Field, Laboratory, or LFM duplicate sample analyses.

Maximum Holding Time:
28 days for bromate, chlorate, bromide (source/raw water only)14 days for chlorite.

Media:
WATER

Subcategory:
Inorganic

Concentration:
Bromide, Chlorite, Chlorate: 5-500 ug/L and Bromate: 0.5-15 ug/L

Precision:
Precision and accuracy were determined using data from eight to nine replicate analyses of fortified reagent water samples. Samples for bromide, chlorate, and chlorite were analyzed using ion chromatography followed by conductivity detection. Samples for bromate were analyzed using ion chromatography followed by post-column UV/Vis detection (which provides high sensitivity). Additional precision and accuracy values are available in the method, characterizing method performance in various fortified matrices (chlorinated drinking water, high ionic water, high organic water), and using different detectors and instrument set-ups.

Detection:
Multiple MDLs were determined using different instrumenation and conditions; consult the method for more information. MDL procedure is equivalent to the procedure at 40 CFR part 136, Appendix B. MDLs were determined using the standard deviation of 7 or 8 replicate analyses of an analyte-fortified reagent water sample multiplied by the t-value for (# of samples -1) degrees of freedom at the 99% confidence level. Detailed instructions for how MDLs are determined are found in Section 9.2.6 of the Method.

Revision Number:
Revision 1.0, May 2000