EPA-OGWDW/TSC: 317.0: Oxyhalide DPBs and Bromide by IC

Summary
Analytes
Revision
Data and Sites

Official Method 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

Current Revision

Revision 1.0, May 2000

Media

WATER

Instrumentation

Ion Chromatography

Method Subcategory

Inorganic

Method Source

EPA-OGWDW/TSC

Citation

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

Brief Method 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 and Application

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

Applicable Concentration Range

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

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.

(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.

Quality Control 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.

Sample Handling

Samples should be collected in plastic or glass bottles that have been thoroughly cleaned and rinsed with reagent water. Sample bottles used for chlorite analysis must be opaque or amber. Preserve samples with 50 mg/L of ethylenediamine (EDA) and refrigerate at < 6^oC. When collecting a field sample from a treatment plant employing chlorine dioxide, the field sample must be sparged with an inert gas (helium, argon, nitrogen) prior to the addition of EDA preservative.

Maximum Holding Time

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

Relative Cost

$51 to $200

Sample Preparation Methods

This method has 4 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
Bromate(15541-45-4) Bromate	0.120 ug/L	100% Rec (SL)	10.80 % RSD (SL)	0.50 ug/L
Bromide(24959-67-9) Bromide Bromide (9CI) Bromide ion (-1)	0.540 ug/L	104% Rec (SL)	3.82 % RSD (SL)	20.00 ug/L
Chlorate(14866-68-3) Chlorate	0.620 ug/L	98% Rec (SL)	0.82 % RSD (SL)	100.00 ug/L
Chlorite(14998-27-7) Chlorite	0.450 ug/L	96% Rec (SL)	0.99 % RSD (SL)	100.00 ug/L

Precision Descriptor Notes:	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 Level Note:	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.

Precision Descriptor Notes:

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 Level Note:

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	PDF/Link
Revision 1.0, May 2000

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EPA-OGWDW/TSC: 317.0: Oxyhalide DPBs and Bromide by IC

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