title: US Environmental Protection Agency Method 314.1, an automated sample preconcentration/matrix elimination suppressed conductivity method for the analysis of trace levels (0.50 microg/L) of perchlorate in drinking water.
abstract: Since 1997 there has been increasing interest in the development of analytical methods for the analysis of perchlorate. The US Environmental Protection Agency (EPA) Method 314.0, which was used during the first Unregulated Contaminant Monitoring Regulation (UCMR) cycle, supports a method reporting limit (MRL) of 4.0 microg/L. The non-selective nature of conductivity detection, combined with very high ionic strength matrices, can create conditions that make the determination of perchlorate difficult. The objective of this work was to develop an automated, suppressed conductivity method with improved sensitivity for use in the second UCMR cycle. The new method, EPA Method 314.1, uses a 35 mm x 4 mm cryptand concentrator column in the sample loop position to concentrate perchlorate from a 2 mL sample volume, which is subsequently rinsed with 10 mM NaOH to remove interfering anions. The cryptand concentrator column is combined with a primary AS16 analytical column and a confirmation AS20 analytical column. Unique characteristics of the cryptand column allow perchlorate to be desorbed from the cryptand trap and refocused on the head of the guard column for subsequent separation and analysis. EPA Method 314.1 has a perchlorate lowest concentration minimum reporting level (LCMRL) of 0.13 microg/L in both drinking water and laboratory synthetic sample matrices (LSSM) containing up to 1,000 microg/L each of chloride, bicarbonate and sulfate.
authors.affiliation: Lakeshore Engineering Services, Inc., 26 W. Martin Luther King Drive, Cincinnati, OH 45219, USA. herb_wagner@hotmail.com
authors.forename: Herbert P
authors.initials: HP
authors.lastname: Wagner
authors.forename: B V
authors.initials: BV
authors.lastname: Pepich
authors.forename: C
authors.initials: C
authors.lastname: Pohl
authors.forename: D
authors.initials: D
authors.lastname: Later
authors.forename: R
authors.initials: R
authors.lastname: Joyce
authors.forename: K
authors.initials: K
authors.lastname: Srinivasan
authors.forename: D
authors.initials: D
authors.lastname: Thomas
authors.forename: A
authors.initials: A
authors.lastname: Woodruff
authors.forename: B
authors.initials: B
authors.lastname: Deborba
authors.forename: D J
authors.initials: DJ
authors.lastname: Munch
mesh_terms: D002853:Chromatography, Liquid / Q000295:instrumentation / Q000379:methods / Q000592:standards; D004988:Ethers, Cyclic / Q000737:chemistry; D017408:Guidelines as Topic; D010472:Perchlorates / Q000032:analysis* / Q000592:standards; D012015:Reference Standards; D015203:Reproducibility of Results; D012545:Schiff Bases / Q000737:chemistry; D017670:Sodium Compounds / Q000032:analysis; D012997:Solvents / Q000737:chemistry; D013696:Temperature; D014481:United States; D014484:United States Environmental Protection Agency; D014881:Water Supply / Q000032:analysis*
chemical_list: D004988:Ethers, Cyclic; D010472:Perchlorates; D012545:Schiff Bases; D017670:Sodium Compounds; D012997:Solvents; C444241:cryptand; C031068:sodium perchlorate; C494474:perchlorate