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Determination of Diethanolamine and Triethanolamine in Surface Finishing, Wastewater and Scrubber Solutions

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Determination of Diethanolamine and Triethanolamine in Surface Finishing, Wastewater and Scrubber Solutions Application Update 126 Update Application Determination of Diethanolamine and Triethanolamine in Surface Finishing, Wastewater and Scrubber Solutions Thermo Fisher Scientific Inc. Introduction Alkanolamines are important in the chemical and pharmaceutical industries for production of emulsifying agents and the manufacturing of laundry additives and dyes. The analysis of alkanolamines is also important in metal surface finishing and in wastewater effluents. They are commonly used in acid gas removal systems (scrubbers) in both oil refineries and natural gas plants. Hydrogen sulfide and carbon dioxide are two of the primary acid gases formed in a refinery. When the gases are dissolved in an aqueous medium, they dissociate to form weak acids. Amines, weak bases, combine chemically with the weak acids to form salts, thus removing the acid gases from the process stream. When the amine solution becomes overloaded with salts, the efficiency of the scrubbing process is adversely affected. Thus, continuous chromophores or fluorophores, derivatization of the monitoring of the amine solution can improve amine alkanolamines is required prior to detection. As a result, makeup, improve final product performance, and decrease the data collected by these alternate methods are prone system maintenance, Figure 1. Monitoring soil and water to numerous matrix interferences and shortened column samples in and around a refinery can identify sources of life. Ion chromatography (IC) works particularly well scrubber leaks before any serious losses or environmental for separations of alkanolamines. The sensitivity by contamination occurs, Figure 2. Alkanolamines are also conductivity detection, however, is poor because of the used in surface finishing as shown in Figure 3 to control low equivalent conductance of alkanolamines. the etching process of aluminum and aluminum alloys in the aerospace industry.1-4 Recommended Equipment Several alternatives are currently available for the Thermo Scientific Dionex Series 4500i* with a Pulsed determination of alkanolamines, including wet chemistry, Amperometric Detector (PAD II) or a Pulsed Electro- gas chromatography and traditional high performance chemical Detector (PED) liquid chromatography. However, these methods are time * Equivalent or improved results can be achieved using consuming, with sample preparation and analysis times as the Thermo Scientific Dionex ICS-5000+ system. long as two hours. Because these compound lack natural 2 ™ ™ ™ Column: Thermo Scientific Dionex OmniPac Column: Dionex OmniPacPAX-500 PAX-500 Analytical and Guard Guard and Separator Eluent 1: 300 mM sodium hydroxide Eluent: 150 mM NaOH - 5% ACN Eluent 2: 10% v/v acetonitrile/water Detector: PAD II, Gold working electrode Eluent Proportion: 50/50 mix Reference cell - eluent Flow: 1mL/min Range 30 KnA Detector: PED or PAD II, Gold working electrode Potential Time solvent compatible cell E1 = 0.08 V T1 = 540 mS Ag/AgCl reference electrode E2 = 1.00 V T2 = 420 mS Range 30K nAmperes E3 = 0.080 V T3 = 420 mS Potential Time Sample Loop: 50 µL E1 = 0.08 V T1 = 540 mS Sample Prep: 1/1000 in 150 mM NaOH E2 = 1.00 V T2 = 420 mS E3 = -0.08 V T3 = 420 mS Peaks ppm Sample Loop: 50 µL 1. Unknown – Sample Prep: Original sample diluted 1:100 5 2. Unknown – 3. Diethanolamine – 2 with 150 mM sodium hydroxide 4. Unknown – Peaks Level 5. Triethanolamine 54 ppm 1. DEA 10 ppm 2. TEA 10,000 ppm 2 3. Unknown – 4. Unknown – 4 1 3 3 1 4 0.00 5.00 10.00 5.00 Minutes 0 1 2 3 4 5 Minutes Figure 1. Diethanolamine determination in an oil refinery triethanolamine scrubber solution. Figure 3. TEA determination in an operational alkaline etch solution. Column: Dionex OmniPac PAX-500 Analytical and Guard Eluent: 150 mM NaOH - 2% ACN Flow: 1 mL/min Detector: PAD II, Gold working electrode Reference cell - eluent Range 30 K Detector: PAD II, Gold working electrode solvent compatible cell Reference cell - eluent Range 30 K Potential Time E1 = 0.08 V T1 = 540 mS E2 = 1.00 V T2 = 420 mS E3 = 0.80 V T3 = 420 mS Sample Loop: 50 µL Sample Prep: Filter and Direct Injection Peaks ppm 3 1. Unknown – 2. Unknown – 3. Diethanolamine 6.04 1 2 0 2 4 6 Minutes Figure 2. Oil refinery pond water for diethanolamine. Application Update 126 Update Application Preparation of Reagents and Standards Standards were prepared in 150 mM sodium hydroxide at the 0.1, 1, 10, 50, 75, and 100 ppm levels. Linearity Conditions over the range of 0.1 to 100 ppm using a 50 µL sample Column: Dionex OmniPac PAX-500 Analytical exhibited a coefficient of determination (r2) greater than and Guard 0.998 for each alkanolamines. Precision, expressed as percent relative standard deviation (%RSD) for 374 Eluent 1: 300 mM sodium hydroxide replicate analyses of the alkanolamines at the 70 ppm Eluent 2: 10% v/v acetonitrile/water level was better than 3% in an operational alkaline etch Eluent Proportion: 50% E1/50% E2 solution. The method detection limit by direct injection Flow Rate: 1 mL/min using a 50 µL loop has shown to be 10 parts-per-billion in an alkaline etch solution. Peak areas were used in Detector: PED or PAD II, Gold working electrode preference to peak height for quantification of the Solvent compatible cell alkanolamines. Ag/AgC1 Reference electrode Range 30K nA Precautions Potential Time The eluent used in this method contains sodium hydroxide E1 = 0.08 V T1 = 540 mS and acetonitrile. Acetonitrile in a high pH solution E2 = 1.00 V T2 = 420 mS decomposes to weak organic acids and other compounds. E3 = -0.08 V T3 = 420 mS These decomposition products, when present, interfere with Sample Loop: 50 µL the electrochemical detector’s response. The acetonitrile Sample Prep: Dilute in 150 mM sodium hydroxide decomposition reaction is not rapid, and small amounts of the breakdown components have no immediate effects It is recommended that all standards and samples be upon the analysis. To avoid this decomposition reaction, prepared and stored in 150 mM sodium hydroxide. on line low pressure mixing using the Thermo Scientific Alkanolamines are not stable at low pH and quickly Dionex Gradient Pump is recommended to blend separate degrade. Standards and samples prepared in deionized sodium hydroxide and acetonitrile solutions together. water also degrade but more slowly. References Results and Discussion 1. Johnson, D.C.; LaCourse, W.R., Anal. Chem. 1990, 62, Determination of total alkanolamines in this method is 589A–596A. accomplished using liquid chromatography on Dionex 2 Burwell, K.F.; Dubek, D.J.; Sigmund, P.W., Hydrocarbon OmniPac columns and Pulsed Amperometric Detection Processing, March 1982, 108–116. (PAD). The blended isocratic eluent is 150 mM sodium hydroxide solution containing 5% acetronitrile. The 3. Keaton, M.M.; Bourke, M.J., Hydrocarbon Processing, sodium hydroxide in the eluent maintains a high pH thus August 1983. suppressing ionization of the alkanolamines. Under these 4. Campbell, D.C.; Carson, S.; Heberling, S.; Bramer, conditions the alkanolamines are retained and separated D.V., Improved Separation and Detection of Alkanol- by a reverse phased mechanism on the Dionex OmniPac amines using Liquid Chromatography and PAX-500 analytical column. The acetonitrile present in Electrochemical Detection, Submitted to: Journal of the eluent controls the retention of the alkanolamines. Chromatography. Increasing the acetonitrile concentration reduces the retention times. www.thermoscientific.com/chromatography ©2014 Thermo Fisher Scientific Inc. All rights reserved. ISO is a trademark of the International Standards Organization. All other trademarks are the property of Thermo Fisher Scientific and its subsidiaries. This information is presented as an Thermo Fisher Scientific, example of the capabilities of Thermo Fisher Scientific products. It is not intended to encourage use of these products in any Sunnyvale, CA USA is manners that might infringe the intellectual property rights of others. Specifications, terms and pricing are subject to change. ISO 9001:2008 Certified. Not all products are available in all countries. Please consult your local sales representative for details. 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