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Determination of Perchlorate by U.S. EPA Method 332.0 Using a Compact Ion Chromatography System Coupled with Mass Spectrometry (IC-MS) John E. Madden 1 and Yukiko Kawahara 2 1 Thermo Fisher Scientific, Sunnyvale, CA, USA; 2 Thermo Fisher Scientific, San Jose, CA, USA Keywords: Integrion, Perchlorate in drinking water, Perchlorate in environmental water, RFIC system, Perchlorate, Drinking water, U.S. EPA Method 332.0 Introduction Perchlorate has been used as an oxidizer in rockets, munitions, and fireworks since the 1950s. It has been found to cause thyroid dysfunction, and has been linked to tumors in humans. Perchlorate is regulated under the Safe Drinking Water Act (2011). Additionally, numerous U.S. states have promulgated enforceable standards for the levels of perchlorate in drinking water. Massachusetts and California have established standards for drinking water of 2 µg/L and 6 µg/L respectively. More than 10 other states have also set advisory levels or health-based goals for perchlorate in drinking water ranging from 1 to 18 µg/L. U.S. EPA Method 332.0 — Ion Chromatography with Suppressed Conductivity and Electrospray Ionization/ Mass Spectrometry is one of the most sensitive and robust characterization methods available for perchlorate. Mass spectrometry (MS) provides lower detection limits in high-ionic-strength matrices than conductivity detection alone. The selectivity of the mass spectrometer allows the quantification of perchlorate in high-ionic strength matrices at well below currently enforced action levels. No. 203 APPLICATION PROOF NOTE This application proof note demonstrates the determination of perchlorate in environmental waters using the method published in Thermo Scientific Application Note 151 and U.S. EPA Method 332.0. Here, the method is performed using a Thermo Scientific Dionex Integrion HPIC system, a Thermo Scientific Dionex IonPac AS20 column set, and Thermo Scientific MSQ Plus Single Quadrupole Mass Spectrometer. Figure 1 shows the determination of 1.00 µg/L of perchlorate in a Laboratory Synthetic Sample Matrix (LSSM), which includes 250 mg/L each of chloride, bicarbonate, and sulfate.
Transcript

Determination of Perchlorate by U.S. EPA Method 332.0 Using a Compact Ion Chromatography System Coupled with Mass Spectrometry (IC-MS)John E. Madden1 and Yukiko Kawahara2 1Thermo Fisher Scientific, Sunnyvale, CA, USA; 2Thermo Fisher Scientific, San Jose, CA, USA

Keywords: Integrion, Perchlorate in drinking water, Perchlorate in environmental water, RFIC system, Perchlorate, Drinking water, U.S. EPA Method 332.0

IntroductionPerchlorate has been used as an oxidizer in rockets, munitions, and fireworks since the 1950s. It has been found to cause thyroid dysfunction, and has been linked to tumors in humans. Perchlorate is regulated under the Safe Drinking Water Act (2011). Additionally, numerous U.S. states have promulgated enforceable standards for the levels of perchlorate in drinking water. Massachusetts and California have established standards for drinking water of 2 µg/L and 6 µg/L respectively. More than 10 other states have also set advisory levels or health-based goals for perchlorate in drinking water ranging from 1 to 18 µg/L.

U.S. EPA Method 332.0 — Ion Chromatography with Suppressed Conductivity and Electrospray Ionization/Mass Spectrometry is one of the most sensitive and robust characterization methods available for perchlorate. Mass spectrometry (MS) provides lower detection limits in high-ionic-strength matrices than conductivity detection alone. The selectivity of the mass spectrometer allows the quantification of perchlorate in high-ionic strength matrices at well below currently enforced action levels.

No

. 203

APPLICATION PROOF NOTE

This application proof note demonstrates the determination of perchlorate in environmental waters using the method published in Thermo Scientific Application Note 151 and U.S. EPA Method 332.0. Here, the method is performed using a Thermo Scientific™ Dionex™ Integrion™ HPIC system, a Thermo Scientific™ Dionex™ IonPac™ AS20 column set, and Thermo Scientific™ MSQ Plus™ Single Quadrupole Mass Spectrometer. Figure 1 shows the determination of 1.00 µg/L of perchlorate in a Laboratory Synthetic Sample Matrix (LSSM), which includes 250 mg/L each of chloride, bicarbonate, and sulfate.

Method

ConditionsIC System: Dionex Integrion HPIC system

MS Detector: MSQ Plus Mass Spectrometer

Columns: Dionex IonPac AG20 (2 x 50 mm) Dionex IonPac AS20 (2 x 250 mm)

Eluent Source: Thermo Scientific™ Dionex™ EGC 500 KOH Eluent Generator Cartridge Thermo Scientific™ Dionex™ CR-ATC 600 Continuously Regenerated Anion Trap Column

Eluent: 55 mM KOH

Flow Rate: 0.3 mL/min

Column Temp: 35 °C

Inj. Volume: 200 µL via Thermo Scientific™ Dionex™ AS-AP AutoSampler

System Backpressure: ~2000 psi

Detection: Suppressed Conductivity, Thermo Scientific™ Dionex™ AERS™ 500e (2 mm) External Water Mode via Thermo Scientific™ AXP™ Pump, 41 mA

Mass Spectrometric Detection, details below

Divert Valve Switch Time: 6.0–14.0 min (0.0–6.0 min to waste, 6.0–14.0 min to MSQ Plus MS)

Desolvation Pump Flow Rate: 0.3 mL/min., 50:50 water:methanol via Thermo Scientific AXP Pump

Ionization: ESI Negative Mode

Needle Voltage: -3 kV

Cone Voltage: -70 V

Probe Temperature: 500 °C

Scan: SIM mode; 99, 101, 107, 191 m/z

Dwell Time: 0.3 s

Figure 1. 1.00 µg/L Perchlorate in Laboratory Synthetic Sample Matrix (250 mg/L Chloride, 250 mg/L Bicarbonate, and 250 mg/L Sulfate).

References1. Thermo Scientific Application Note 151: Determination

of Perchlorate in Environmental Waters by Ion Chromatography Coupled with Electrospray Mass Spectrometry (IC-MS). [Online] https://appslab.thermofisher.com/App/1949/an151-determination-perchlorate-environmental-waters-by-ion-chromatography-coupled-with-electrospray-mass-spectrometry-icms (accessed Aug. 1, 2016).

2. U.S. Environmental Protection Agency, Method 332, Determination of Perchlorate in Drinking Water by Ion Chromatography with Suppressed Conductivity and Electrospray Ionization Mass Spectrometry, Rev. 1.0, 2005. [Online]

Find out more at www.thermofisher.com/ICMS

©2017 Thermo Fisher Scientific Inc. All rights reserved. All trademarks are the property of Thermo Fisher Scientific and its subsidiaries. This information is presented as an example of the capabilities of Thermo Fisher Scientific products. It is not intended to encourage use of these products in any manners that might infringe the intellectual property rights of others. Specifications, terms and pricing are subject to change. Not all products are available in all countries. Please consult your local sales representatives for details. AB72127-EN 0317S

Peaks:

1. Perchlorate

1.000 µg/L

Counts

0 3 9 6

700

12 15 Minutes

14,000

1

SIM 191

SIM 101

SIM 99


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