Determination of Calcium and Magnesium in Brine

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1 Application Note Determination of Calcium and Magnesium in Brine INTRODUCTION To prevent membrane poisoning, new membrane technology in chlor-alkali cells requires feed brine that is relatively free of alkaline earth metals. Membrane manufacturers recommend that saturated brines be purified to a total hardness below µg/l (ppb) to extend membrane life and ensure electrical current efficiency in the cell. Industrial laboratories have been concerned with the determination of calcium and magnesium in brine for a number of years. For example, investigators at Vulcan Chemical developed an IC method for the determination of alkaline earth metals in high-purity brine in the 98s. The method in this Application Note can be considered an extension of previous work at Vulcan Chemical. This Application Note describes a method for determining low µg/l amounts of calcium and magnesium in a % sodium chloride brine by ion chromatography. A column, which selectively retains calcium and magnesium and has a low affinity for sodium, is used to concentrate calcium and magnesium from the brine. The concentrated calcium and magnesium are separated on an IonPac CSA cation-exchange column and detected by suppressed conductivity detection. EQUIPMENT Dionex DX- Ion Chromatography system consisting of: GP Gradient CD Conductivity Detector LC Chromatography Enclosure equipped with a rear-loading Rheodyne injection valve Rinsing, (P/N ) LC Chromatography Organizer equipped with a rear-loading Rheodyne injection valve -L Plastic bottle (for mm hydrochloric acid rinsing solution) PeakNet Chromatography Workstation REAGENTS AND STANDARDS Deionized water (DI H O), Type I reagent grade, 8 MΩ-cm resistance or better > 99% Methanesulfonic acid (Fluka or equivalent) Hydrochloric acid, ultrapure reagent (J.T. Baker ULTREX II,.9% or equivalent) Sodium hydroxide, % (w/w) aqueous solution (Fisher Scientific or equivalent) Brine (% sodium chloride solution, kindly provided by Dr. David Hildebrand, Vulcan Chemical, Wichita, Kansas, USA) CONDITIONS Trap (for contaminants in the rinse solution): - (P/N 9) : Analytical s: Eluent: Eluent Flow Rate: Rinsing Reagent: CC- (P/N 97) IonPac CSA Analytical, x mm (P/N 7) IonPac CGA Guard, x mm (P/N 7) A: mm Methanesulfonic acid ml/min mm Hydrochloric acid Application Note

2 Rinsing Flow Rate: ml/min Rinse Time: min Total Run Time: min Volume: µl Detection: Suppressed conductivity, CSRS -II ( mm), AutoSuppression recycle mode System Backpressure: psi (.9. MPa) Background:. µs Time Functions Program Time A(%) Valve Valve Remarks (min) Initial load inject. load load Fill sample loop. inject load to. load inject Begin sampling. load inject Finish sampling Valve is used for loading the concentrator column (). Valve is used for eluting and separating compounds of interest on the CSA analytical column. Begin sampling refers to data collection (the column is switched in-line with the CGA and CSA columns.) PREPARATION OF SOLUTIONS AND REAGENTS Standard Solutions Stock magnesium standard solution ( mg/l) (VWR Scientific) Stock calcium standard solution ( mg/l) (VWR Scientific) Calibration Standard Solutions Appropriate calibration standards are prepared from mg/l standards specified above. Select a range similar to the expected analyte concentrations in the samples. All standards should be prepared in brine. Eluent Solutions Stock eluent solution: M Methanesulfonic acid Weigh 9. g of deionized water (Type I reagent grade, 8 MΩ-cm resistance or better) into an eluent bottle. Degas for approximately minutes. Tare the bottle and carefully add. ml of > 99% methanesulfonic acid directly to the bottle. Working eluent solution: mm Methanesulfonic acid Weigh 98. g of deionized water (Type I reagent grade, 8 MΩ-cm resistance or better) into an eluent bottle. Degas for approximately minutes. Add ml of M methanesulfonic acid to the bottle. Stock rinsing solution: M Hydrochloric acid Weigh 99.7 g of deionized water (Type I reagent grade, 8 MΩ-cm resistance or better) into an eluent bottle. Degas for approximately minutes. Tare the bottle and carefully add 9. ml of ultrapure reagent grade hydrochloric acid directly to the bottle. Working rinse solution: mm Hydrochloric acid Weigh 999. g of deionized water (Type I reagent grade, 8 MΩ-cm resistance or better) into an eluent bottle. Degas for approximately minutes. Add ml of M hydrochloric acid directly to the bottle. Stock sample ph adjustment solution: mm Sodium hydroxide Weigh 9. g of deionized water (Type I reagent grade, 8 MΩ-cm resistance or better) into an eluent bottle. Degas for approximately minutes. Tare the bottle and carefully add. g of % sodium hydroxide directly to the bottle. Standards and Preparation Add. ml of mm sodium hydroxide solution to 9.8 ml of sample (brine). The final concentration of sodium hydroxide is mm. SYSTEM OPERATION System configuration and operation parameters for this application are outlined in previously published documents., The sensitive analysis of calcium and magnesium in brine is accomplished in four steps:. Fill the sample loop. the concentrator column. Eliminate the sodium matrix. Separate calcium and magnesium Determination of Calcium and Magnesium in Brine

3 Figure shows how the system performs these tasks. In Figure A, the system is in the standby mode, ready for sample analysis. In Figure B, Valve is switched to the LOAD position and the sample is loaded into the µl sample loop on Valve. Handling The black rubber plunger in disposable plastic syringes can be a source of contamination. To minimize the introduction of contamination, pull rather than push the sample into the loop, as shown in Figure B. Be sure to pull slowly so that bubbles are not introduced. The loop should be overfilled by at least times its capacity (> µl) to ensure reproducible results. It is important to have the column in line between the pump and Rheodyne Valve ( Figure A) to remove the significant amount of calcium and magnesium present in the mm hydrochloric acid solution. The contamination level of calcium and magnesium in the mm hydrochloric acid solution depends on the reagent purity and grade of DI water. A water blank should be run before analyzing mm ft of. in. Inject s Figure A Initial conditions mm Time: min. ft of. in. s Figure B ing the sample loop Application Note

4 samples. If there has been a significant increase in magnesium and calcium, the capacity of the is exhausted. To clean the, flush with approximately ml of. M hydrochloric acid. Matrix Elimination After the sample loop is filled, mm hydrochloric acid from the transfers the sample out of the loop and onto the column in the opposite direction of the eluent (Figure C). Calcium and magnesium are retained on the concentrator column. The sodium matrix is removed from the column with mm hydrochloric acid from the flowing at ml/min for minutes ( head pressure should be at least psi). Finally, activating Valve to the INJECT position switches the column in-line with the eluent stream and the analytical columns (Figure D). Calcium and magnesium are then eluted from the column in the reverse mm Time: min. Inject ft of. in. s 7 Figure C ing the concentrator column and eliminating the matrix mm Time: min. ft of. in. Inject s 8 Figure D Chromatography of retained Calcium and Magnesium Determination of Calcium and Magnesium in Brine

5 direction of the concentration step and separated on the CGA and CSA columns. Special care should be taken to minimize contamination. The deionized water used for preparing the rinse solution, eluent, and sodium hydroxide solution should be free of measurable levels of ionic impurities, organics, microorganisms, and particulate matter larger than. µm in diameter. Peak Area y = 8.7x + r =.9999 Mg concentration (µg/l) RESULTS AND DISCUSSION For the best performance at low µg/l levels, it is critical that baseline noise be kept to a minimum. An equilibrated system will demonstrate a conductivity background between. µs. Peak-to-peak noise is typically ns and system backpressure is psi (.9. MPa). A system blank is determined by using deionized water as the sample. This blank establishes the baseline and confirms the lack of contamination in the system. A small amount of sodium contamination in the system does not interfere with calcium and magnesium detection. In these experiments, purified brine from a major chlor-alkali producer was used. Brine prepared with commercially available sodium chloride (VWR, reagent grade) contained over µg/l of calcium and magnesium. All standards must be prepared in brine. In the method described here, trace levels of magnesium and calcium in brine are concentrated on a column, which is more selective for divalent than monovalent cations. For optimum calcium and magnesium recovery, the sample ph must be adjusted to.. At high ph values, the selectivity for divalent over monovalent cations is increased. At lower ph values, calcium and magnesium recoveries are poor and are not linear within the concentration range used for this analysis. Calcium and magnesium recoveries were not increased with sample ph values higher than.. Figures and show that the detection of calcium and magnesium is linear in the low µg/l range. Even at ph., the column binds some sodium. To remove sodium, the is rinsed with mm hydrochloric acid. Higher concentrations of hydrochloric acid cause a reduction in calcium and magnesium recovery, while lower hydrochloric acid concentrations increase the rinse time required for rugged chromatography. Despite washing the column for minutes to eliminate the matrix, detectable levels of sodium elute from the to the CSA column (see Figure ). However, this level of sodium does not interfere with the detection of low concentrations of calcium and magnesium (see Figure ). Shorter wash times (less than Figure Peak Area Figure µs Figure Magnesium calibration in brine y = 8.x + 7. r =.9999 Ca concentration (µg/l) Calcium calibration in brine : CC- Analytical s: IonPac CSA Analytical, x mm IonPac CGA Guard, x mm Eluent: A: mm Methanesulfonic acid Eluent Flow Rate: ml/min Rinsing Reagent: mm Hydrochloric acid Rinsing Flow Rate: ml/min Rinse Time: min Total Run Time: min Volume: µl Detection: Suppressed conductivity, CSRS-II ( mm), AutoSuppression recycle water mode Peaks:. Lithium. Sodium. Potassium 8 Minutes 9 Brine blank Application Note

6 minutes) were investigated and did not adequately eliminate the sodium interference. The injection volume was optimized at µl. A larger injection volume may exceed the column capacity and cause irreproducible results. The data in Table show that µg/l of calcium and magnesium can be easily quantified in brine. SUMMARY The method outlined in this Application Note accurately quantifies low µg/l amounts of calcium and magnesium in brine by using an on-line matrix elimination technique.. : CC- Analytical s: IonPac CSA Analytical, x mm IonPac CGA Guard, x mm Eluent: A: mm Methanesulfonic acid Eluent Flow Rate: ml/min Rinsing Reagent: mm Hydrochloric acid Rinsing Flow Rate: ml/min Rinse Time: min Total Run Time: min Volume: µl Detection: Suppressed conductivity, CSRS-II ( mm), AutoSuppression recycle water mode Peaks:. Lithium. Sodium. Potassium. Magnesium. Calcium REFERENCES. Personal communication, Dr. David Hildebrand, Vulcan Chemical, Wichita, Kansas, USA.. Dionex Corporation, Determination of Trace Anions in Isopropyl Alcohol, Application Note 8.. Kaiser, E.; Wojtusik, M. J. J. Chromatogr. A. 99, 7, 8. LIST OF SUPPLIERS J.T. Baker Incorporated, Red School Lane, Phillipsburg, New Jersey, 88, USA. Tel.: VWR Scientific, P.O. Box 79, San Francisco, California, 9, USA. Tel.: Fluka Chemika-BioChemika, Fluka Chemie AG, Industriestrasse, CH-97, Buchs, Switzerland. Tel.: 8 7. µs Figure 8 Minutes ppb of Calcium and Magnesium in brine Table Area counts and RSD of ppb calcium and magnesium in brine Injection # ppb Magnesium ppb Calcium (area count) (area count) Average 87 9 RSD.8. is a trademark and CSRS, IonPac, and AutoSuppression are registered trademarks of Dionex Corporation. Ultrex is a registered trademark of J.T. Baker. Printed on recycled and recyclable paper with soy-based inks. Dionex Corporation Dionex Corporation Dionex U.S. Regional Offices Dionex International Subsidiaries 8 Titan Way Salt Lake City Technical Center Sunnyvale, CA (8) 77-8 Austria () Belgium () 8 Canada (9) 8-9 France 9 8 Germany -99- P.O. Box West South, Suite A Westmont, IL () 789- Italy () Japan () 88- The Netherlands () Switzerland () 99 United Kingdom (7) 97 Determination of Calcium and Magnesium in Brine Sunnyvale, CA Salt Lake City, UT Houston, TX (8) 87- * Designed, developed, and manufactured under an NSAI registered ISO 9 Quality System Atlanta, GA (77) -8 (8) 77-7 (8) Marlton, NJ (9) 9- LPN 99 M / Dionex Corporation

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