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Determination of Haloacetic Acids in Water Using IC-ESI-MS/MS

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Determination of Haloacetic Acids in Water Using IC-ESI-MS/MS Application Note 217 Note Application Determination of Haloacetic Acids in Water Using IC-ESI-MS/MS Rosanne Slingsby, Charanjit Saini, and Chris Pohl Thermo Fisher Scientific, Sunnyvale, CA, USA Introduction The determination of the chloro-, bromo-, and mixed This method allows separation and detection of sub-µg/L haloacetic acids in waters destined for human consump- levels of nine haloacetic acids (HAAs) in high-ionic tion, including drinking water and swimming pool water, strength matrices. Using this method, the analytes are has been reported using a variety of analytical techniques.3 separated from chloride, sulfate, nitrate, bromide, and U.S. EPA Methods 552.2 and 552.3 use acidic methanol bicarbonate, and detected using a triple quadrupole mass derivatization followed by gas chromatography with spectrometer with an electrospray interface. Quantifica- electron capture detection.4 This method is both labor- tion is achieved using internal standards. intensive and time-consuming. Bruzzoniti5 recently published a table summarizing the existing IC columns Haloacetic acids occur in drinking water during the and methods used for HAAs analysis, including this disinfection process as a result of the reaction between method, which uses the Thermo Scientific™ Dionex™ chlorine and natural organic materials such as humic and IonPac™ AS24 column. Asami6 used offline sample fulvic acids.1,2 The iodoacids (for example, iodoacetic pretreatment with external standard calibration and acid) are much less stable and are not included in this MS/MS detection for calibration of haloacetic acids and analysis. When bromide is present in the water, bromoace- oxyhalides, using perchlorate as an internal standard. tic acids and mixed chloro- and bromoacetic acids can Only the method using the Dionex IonPac AS24 column also be generated. Haloacetic acids have been linked to addresses the issue of high-ionic strength matrices. All the possible threats to human health. Monitoring for mono- IC methods take advantage of the low pKa values of chloroacetic acid (MCAA), monobromoacetic acid HAAs (~ 0.7–2.8) by using anion-exchange separation (MBAA), dichloroacetic acid (DCAA), trichloroacetic acid mode. Hydroxide-based eluents are used in conjunction (TCAA), and dibromoacetic acid (DBAA) has been in with chemical suppression, so the background signal effect since they were first regulated under the Stage I entering the mass spectrometer is as low as that of water. Disinfection Byproducts (DBP) Rule, Dec. 16, 1998, with When mass spectrometric detection is used, the matrix a minimum contamination level (MCL) set at 60 µg/L. ions are typically diverted to waste during the analytical Stage II DBP Rule, Jan. 4, 2006, maintained the MCL but run to avoid contamination of the detector. EPA Method also instituted minimum reporting limits (MRL) require- 332.07 uses the same configuration as discussed in this ments of 2 µg/L for MCAA and 1 µg/L for the other paper for the determination of perchlorate in drinking HAAs. The remaining four HAAs that may be present in water; namely, ion chromatography with matrix diversion drinking water are: chlorobromoacetic acid (CBAA), and detection using suppressed conductivity followed by chlorodibromoacetic acid (CDBAA), dichlorobromoacetic electrospray mass spectrometry. The selectivity of the acid (DCBAA), and tribromoacetic acid (TBAA). analytical column in a method using matrix diversion must be designed such that the matrix ions are sufficiently resolved from target analytes. 2 Four internal standards are used in our method for the Dionex ASRS 300 nine target analytes. These were chosen because they elute Suppressor 1 MD 2 throughout the chromatographic run, thus allowing easy Valve 8 Dionex IonPac Conductivity ESI MS/MS tracking of close-eluting analytes. Stuber and Reemtsma AS24 Column cell 6 discuss the challenges of quantification using LC-ESI-MS Eluent: KOH, 0.3 mL/min Waste Solvent addition 100% CH CN, 0.3 mL/min in the presence of significant matrix effects, and provide 3 25676 some guidance for using internal standards. Most of the Figure 2. Thermo Scientific Dionex ICS-3000 chromatography system currently published work describing various analytical schematic, showing matrix diversion and mass spectrometric detection. approaches for determination of HAAs, however, does not adequately address the challenges of very high-ionic Recommended Equipment strength matrices, or the need for internal standards to Dionex ICS-3000 Chromatography System obtain accurate and precise quantification. • DP Dual Pump module (or SP and an AXP) Figure 1 shows the chromatogram of the nine standards, – DP1 Analytical Pump the two matrix diversion windows, and the general form – DP2 Pump is used to deliver post-suppressor of the KOH gradient. The three periods noted in the figure acetonitrile correspond to three periods for data collection in the Analyst method program. Figure 2 shows the general • DC Dual-Zone Chromatography module instrumentation schematic. • CD Conductivity Detector • AS Autosampler with sample tray cooling Column: Dionex IonPac AS24 250 × 2mm i.d., • EG Eluent Generator AG24 50 × 2 mm KOH Gradient: 7 mM for 0–18 min then 18 mM for 18–36.5 min, • Mixing tee (Upchurch, part number U-466) then 60 mM for 36.6–52 min Eluent Flow Rate: 0.30 mL/min Mass Spectrometer Postcolumn Solvent: 100% acetonitrile at 0.3 mL/min • Triple Quadrupole Mass Spectrometer with electrospray Suppressor: Thermo Scientific Dionex ASRS™ 300 interface capable of negative ion detection, or ™ Anion Self-Regulating Suppressor , equivalent 2 mm, external water mode Matrix Diversion: 17–22 and 33–41 • Nitrogen and Zero Air supplies as specified by MS Sample Volume: 100 µL Loop; 0.8 µL injection valve dead volume manufacturer Column Compartment Period 3 Temperature: 15 ºC • 25-pin relay cable connecting mass spectrometer to DP pump module; pins 19 (red) and 7 (black) in the DP Period 2 Re-equilibration connector Period 1 KOH gradient Software Link™ 3 1. MCAA • Thermo Scientific Dionex DCMS 2.0 software 7500 2. MBAA – or higher Cl– Br 3. DCAA 6500 – NO3 4. BCAA Standards 2– 5500 CO3 5. DBAA – • Deionized water: 18 MΩ or better Intensity, cps SO 2 4500 4 6. TCAA 7. BDCAA • Acetonitrile (HPLC grade) 3500 5 6 8. CDBAA 4 • Analyte standard mix (1000 µg/mL) of the nine native 7 9. TBAA 2500 HAAs; monochloroacetic acid (MCAA), monobromo- 2 8 1500 Br– 9 acetic acid (MBAA), dichloroacetic acid (DCAA), 1 500 trichloroacetic acid (TCAA), dibromoacetic acid (DBAA), chlorobromoacetic acid (CBAA), chlorodibro- 0 51015202530354045505560 moacetic acid (CDBAA), dichlorobromoacetic acid Minutes 25675 (DCBAA), and tribromoacetic acid (TBAA) purchased Figure 1. Chromatogram produced by chromatography conditons and mass from Restek (P/N31896). spectrometer conditions provided in Table 1. The shaded areas show the time windows for matrix diversion to waste and the matrix ions that elute in those windows. The time windows for data collection in Periods 1, 2, and 3 are indicated. • Internal standards from us are: monochloroacetic Conditions 3 acid-2-13C (1000 µg/mL, P/N 069406), monobromo- acetic acid-1-13C (1000 µg/mL, P/N 069407), Chromatography Conditions dichloroacetic acid-2-13C (1000 µg/mL, P/N 069408), Column: Dionex IonPac AS24 250 × 2mm i.d., and trichloroacetic acid-2-13C (1000 µg/mL, Dionex IonPac AG24 50 × 2mm P/N 069409). KOH Gradient: Time KOH (mM) Standards are dissolved in methyl tert-butyl ether (MtBE). –7.0 7 A working standard mixture of the four internal stan- 0.0 7 dards was prepared in deionized water. All standard 18.0 7 solutions were kept refrigerated at 4 °C when not in use. 36.5 18 Standards in the 2–5 µg/L range are stable for 14 days when stored at 4 °C with PTFE/silicone septa. Because the 36.6 60 standards are purchased in MtBE, which has limited 52.0 60 solubility in water (~ 5%), not more than ~ 0.5% of Eluent Flow Rate: 0.30 mL/min MtBE is added when making the mixtures, relative to the Postcolumn Solvent: 100% acetonitrile at 0.3 mL/min total water volume. Suppressor: Dionex ASRS 300 Anion Sample Preparation Self-Regulating Suppressor, Samples were collected in amber glass bottles with 2 mm, external water mode PTFE-lined screw caps. Crystalline or granular ammo- Anion Trap: Thermo Scientific Dionex CR-ATC nium chloride is added to the sample containers to Continuously Regenerated Anion Trap, 2 mm produce a final concentration of 100 mg/L of ammonium Matrix Diversion: 17–22 and 33–41 chloride. The preservation requirements are exactly the same as those described in EPA Method 552.3. Sample Volume: 100 µL sample loop Column Compartment Temperature: 15 ºC Autosampler Temperature: 8 °C Detector Compartment Temperature: 30 °C Mass Spectrometric Conditions: Tables 1–5 Table 1. API2000 conditions. Source- Declustering Focusing Collision Entrance Collsion Cell Collision Cell Dwell Analyte KOH Gradient Transition Dependent Potential Potential Energy Potential Entrance Exit Potential Time Parameters (V) (v) (eV) (V) Potential (V) (V) (mSec) MCAA 92.9/34.9 Curtain 20 –20 –300 –12 –10 –12 –6 600 each MCAA-21-13C 93/34.9 CAD 2 7 mM Ionspray –4500 MBAA 0–18 min 137/78.8 Temp 475 °C MBAA-1-13C 138/78.8 –11 –350 –12 –7 –10 –14 600 each GS1/GS2 90/90 Dalapon 141/97 –13 –350 –11 –8 –13 –6 500 Curtain 25 DCAA 127/82.9 CAD 4 18 mM –11 –320 –12 –6.5 –12 –6 500 each DCAA-2-13C 128/84 Ionspray –4500 18–36.5 min. BCAA 170.8/78.8 Temp 475 °C –16 –300 –28 -6 –14 –8 500 GS1/GS2 90/90 DBAA 214.7/170.7 –11 –350 –12 –4.5 –15 –10 500 TCAA 161/116.9 –6 –290 –7 –7 –13.7 –13.7 400 each TCAA-2-13C 162/118 Curtain 25 CAD 4 BDCAA 60 mM 207/81 or Ionspray –4500 –12 –300 –6 –4 –15 –14 400 36.6–52 min 79/79 Temp 475 °C CDBAA 207/78.8 GS1/GS2 90/90 –11 –300 –20 –4 –15 –6 400 TBAA 250.75/78.8 15 –350 –28 –5 –12 –12 400 4 Table 2.
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