EPA Method 317.0REV2.0


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EPA Method 317.0REV2.0:
Inorganic Oxyhalide DBPs in Drinking Water By Ion Chromatography With Conductivity Detection and Trace Bromate Using Post Column Reagent Colorimetry. 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:
About a quarter of a milliliter of sample is introduced directly into an ion chromatograph equipped with a guard column and a suppressor device. The target anions are separated and measured using an analytical column and a conductivity detector. In addition trace bromate analysis is achieved using a postcolumn reagent delivery system, a heated postcolumn reaction coil, and a ultraviolet/visible (UV/VIS) absorbance detector. Bromide should not be determined in finished water because its concentration can differ significantly between preserved and unpreserved samples and there are too many variables that influence measured concentrations. The target anions include chlorite, chlorate, bromate, and bromide by conductivity detection and bromate anions by postcolumn UV/VIS absorbance detection. The ion chromatographic system must utilize suppressed conductivity detection. The postcolumn reagent must be delivered pneumatically and some form of software signal filtering or smoothing of the absorbance signal must be incorporated.

Scope:
This method determines oxyhalide disinfection by-product anions in reagent water, surface water, ground water, and finished drinking water. In addition, bromide can be accurately determined in source or raw water.

Citation:
EPA Web site for Analytical Methods for Drinking Water

Interferences:
(A) Coelution: Direct chromatographic coelution, concentration dependent coelution, and ionic displacement effects (which can shift rentention times) can all cause interferences by coelution. It may be possible to overcome by adjusting chromatographic conditions (e.g., changing columns), diluting the sample, or using pretreatment cartridges. Care must be taken when using these steps to ensure that analyses are not adversely affected.(B) Contamination: Interferences may be caused by contaminants in the reagent water, reagents, glassware, and other sample processing apparatus that lead to discrete artifacts or elevated baselines.(C) Particulate: Samples containing particles > 0.45 um, and reagents containing particles > 0.20 um can damage chromatography columns and flow systems. Filtration should be use to prevent damage.(D) Carry over: Carry over peaks from one analysis to another may also cause interferences as false positives.(E) Chlorine dioxide: Sample matrices with residual chlorine dioxide will result in the formation of additional chlorite prior to analysis.(F) Chlorite: The presence of chlorite can interfere with the quantitation of low concentrations of bromate on the postcolunn UV/VIS absorbance detector.

QC Requirements:
Initial Demonstration of Capability must show acceptable Demonstration of Accuracy (IDA) and Precision (IDP) and the Method Detection Limit (MDL) must be determined. Recovery for Laboratory Fortified Blanks (LFB) must be 75 - 125% from the Minimum Reporting Level (MRL) to 5X MRL. Recovery should be 75 - 125% for Laboratory Fortified Sample Matrix (LFM). Dichloroacetate is added as a surrogate and surrogate recovery must be 90 - 115%. Relative Percent Difference (RPD) for field or laboratory duplicates must be + or - 20% for concentrations ranging between the MRL to 5X the MRL. Peak Gaussian Factor (PGF) must fall between 0.80 and 1.15 Retention Time (RT) and the surrogate RT must remain 80% of the initial RT when the column was new.

Maximum Holding Time:
14 days for chlorite; 28 days for chlorate, bromide and bromate

Media:
WATER

Subcategory:
Inorganic

Concentration:
5 - 100 ug/L (conductivity detector); 0.5-15 ug/L (bromate; post-column reactor)

Sample Prep:
None

Precision:
Precision and accuracy values were determined by analyzing nine replicates of fortified reagent water (see Table 3 of the method), using the conditions specified in Table 1 of the method. Values for all analytes were determined using conductivity detection. Additional data are available in the method.

Detection:
MDL values listed are for conductivity detection with post column reagent (PCR) online. Other values without PCR online and for bromate using the UV/VIS detector are in the method (and can provide for a lower level of detection). The MDL for a specific matrix may differ from those listed, depending on the nature of the sample and the specific instrumentation used.

Revision Number:
Revision 2.0, July 2001

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