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IC – What’s in your Sample? Salt Lake City, UT Spring 2012
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Overview Fruit and Specialty Juices Coffee Carbonated Beverages Vitamin and Sports Beverages
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1° Amines R-NH 2 2° Amines R’ R-N-H 4° Amines R 4 N + Functional Groups Detected with Suppressed Conductivity 3° Amines R’ R-N-R” Suppressed Conductivity Detection Inorganic Anions e.g., F _, CI _, NO 2 _, NO 3 _, SO 4 2 _, PO 4 3 _, I _, Br _, CIO 3 _, SCN _, S 2 O 3 2 _ Inorganic Cations Alkali Metals: Li +, Na +, K +, Rb +, Cs +, Alkaline Earths: Mg 2+, Ca 2+ Sr 2+, Ba 2+, Ammonia: NH 4 + Phosphates O R-O-P-OH OH Sulfates R-O-S-OH O O Sulfonates R-S-OH O O Phosphonates R-P-OH O OH Carboxylics R-C-OH O
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Typical Workflow: Traditional IC (IonPac AS19 Gradient Analysis) Results Start-up: Equilibration: Total Time = 1 Hour Run 3 Standards: Total Time = 1 h 30 min Total Analysis Time: Total Time = 6 hours Run 5 Samples: Total Time = 2 h 30 min Eluent Preparation Total Time = 1 Hour
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Typical Workflow: Capillary IC Always On – Always Ready (IonPac AS19 Gradient Analysis) “IC on Demand” Results Run Check Standard: Total Time = 30 min Run 5 Samples: Total Time = 2 h 30 min Total Analysis Time: Total Time = 3 hours
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CAPILLARY IC: FRUIT AND SPECIALTY JUICES
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µS Analysis of Apple Juice by High Pressure Capillary IC 0102030 –20 0 60 1 2 3 4 6 7 8 9 10 11 B A Column:Thermo Scientific Dionex IonSwift ™ MAX100G, MAX100, 0.25 mm Eluent Source: Thermo Scientific Dionex EGC-KOH Eluent A:0.1–1 mM KOH for 7 min, 2–25 mM KOH in 13 min, 25–65 mM KOH in 10 min Eluent B:0.1–1 mM KOH for 4.5 min, 2–25 mM KOH in 5.4 min, 25–65 mM KOH in 10 min Flow Rate A:12 µL/min Flow Rate B:18 µL/min Suppressor:Suppressed conductivity, Thermo Scientific Dionex Anion Capillary Electrolytic Suppressor (ACES ™ -300) Inj. Volume:0.4 µL Sample:Apple Juice (1:40 Dilution) Temperature:30 °C Peaks:1. Quinate 2. Glycolate 3. Lactate 4. Pyruvate 5. Galacturonate 6. Malate 7. Sulfate Minutes 27222 8. Oxalate 9. Phosphate 10. Citrate 11. Isocitrate 12. cis-Aconitate 13. trans-Aconitate 32 2 1 4 5 6 5 7 8 9 12 13 10 12 13 11 B 3900 psi 2000 psi
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Fast High-Pressure Separations of Organic Acids in A Diluted Orange Juice Sample 8 Thermo Scientific Column: Thermo Scientific Dionex IonSwift MAX-100 guard, MAX-100, 0.25 mm Thermo Scientific Eluent Source: Thermo Scientific Dionex EGC-KOH capillary cartridge Gradient: A: 0.1 mM KOH from -10 to 0.1 min, 0.1–2 mM from 0.1 to 5 min, 2–25 mM from 5 to 20 min, 25–65 mM from 20 to 30 min, 65 mM from 30 to 45.1 min B: Same gradient adjusted for flow rate Column Temp.:30 °C Inj. Volume: 0.4 µL Thermo Scientific Dionex Detection:Suppressed conductivity, Thermo Scientific Dionex ACES™, recycle Sample Prep.:1:40 dilution, filter, 0.45 µm Peaks: 1.Quinate 2.0 mg/L8. Maleate 0.1 mg/L 2.Lactate 3.29. Sulfate2.0 3.Formate 0.7 10. Oxalate4.6 4.Chloride 1.0 11. Phosphate7.5 5.Nitrate -- 12. Citrate125 6.Glutarate -- 7.Malate25 AA BB Minutes 0 30 -5 10 µS 20 1 5 8 11 12 10 9 7 6 4 3 2 12 7 11 10 9 A: 12 µL/min 2100 psi B: 24 µL/min 4200 psi
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Column: CarboPac ® PA 20 (0.4 × 150 mm) Temperature: 30 ºC Eluent: 50 mM Potassium hydroxide (EG) Flow Rate: 10 µL/min Inj. Volume: 0.40 µL Detection: PAD, 4–potential carbohydrate, Au Ref. Electrode: PdH Gasket Thickness: 25 µm Samples: Juice samples (1–5000 dilution) Standard (20 µM) Peaks: 1. Glucose 2. Fructose 3. Sucrose 20 120 nC Minutes 05 10 3 2 1 1 1 2 2 3 3 Cranberry–Raspberry Juice Orange Juice Standard Analysis of Carbohydrates in Juices by Capillary HPAE-PAD 2785 9
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CAPILLARY IC: COFFEE
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Separation of Anions in a Brewed Caffeinated Coffee Sample by Capillary IC 1 10 Column:Thermo Scientific Dionex IonSwift MAX100 guard, MAX100 0.25 x 250 mm Eluent Source:EGC-KOH capillary Gradient: 0.1 mM KOH from -10 to 4 min, 0.1–2 mM from 4 to 6 min, 2–15 mM from 6 to 12 min, 15–35 mM from 12 to 16 min, 65 mM from 17-30 min Column Temp.:30 °C Flow Rate:12 µL/min Inj. Volume: 0.4 µL Detection:Suppressed conductivity, Anion Capillary Electrolytic Suppressor, (ACES™), recycle Sample Prep.:1:50 dilution Peaks:1.Quinate10. Malate 2.Lactate11. Itaconate 3. Acetate 12.Sulfate 4.Propionate 13.Fumarate 5.Formate 14.Oxalate 6.Chloride15. Phosphate 7. Bromide16. Citrate 8.Nitrate17.Isocitrate 9.Glutarate 4 8 7 12 2 3 6 9 13,14 11 16 5 15 17 Minutes 30 10 20 0 -0.1 µS 3.5
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Separation of Anions in a Brewed Decaffeinated Coffee Sample by Capillary IC 1 10 4 8 7 12 Minutes 2 3 6 9 14 13 11 16 30 10 20 0 -0.1 µS 3.5 5 15 17 Column:Thermo Scientific Dionex IonSwift MAX100 guard, MAX100, 0.25 x 250 mm Eluent Source:EGC-KOH capillary Gradient: 0.1 mM KOH from -10 to 4 min, 0.1–2 mM from 4 to 6 min, 2–15 mM from 6 to 12 min, 15–35 mM from 12 to 16 min, 65 mM from 17- 30min Column Temp.:30 °C Flow Rate:12 µL/min Inj. Volume: 0.4 µL Detection:Suppressed conductivity, Anion Capillary Electrolytic Suppressor, (ACES™), recycle Sample Prep.:1:50 dilution Peaks:1.Quinate10. Malate 2.Lactate11. Itaconate 3. Acetate 12.Sulfate 4.Propionate 13.Fumarate 5.Formate 14.Oxalate 6.Chloride15. Phosphate 7. Bromide16. Citrate 8.Nitrate17.Isocitrate 9.Glutarate
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Separation of Coffee Sugars Column: CarboPac PA 20 (0.40 x 150 mm) Temp.: 30 C Eluent (EG): 3 mM KOH (0–45 min), 100 mM KOH (45–50 min), 3 mM KOH (50–70 min) Flow Rate: 9 µL/min Inj. Volume :0.40 µL Detection:PAD, Au, Carbohydrate 4-Potential Waveform Ref. Electrode: PdH Samples:Standard (10 µM) / Coffee (1:1000 dilution) Peaks: 1. Mannitol2. Galactosamine 3. Arabinose4. Galactose 5. Glucose6. Sucrose 7. Xylose8. Mannose 9. Fructose10. Ribose *. Unknown
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CAPILLARY IC: CARBONATED BEVERAGES
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Fast High-Pressure Separations of Anions in a Diet Cola Beverage by Capillary IC 15 Column:Thermo Scientific Dionex IonSwift ™ MAX-200G, MAX-200, 0.25 mm 250 mm Eluent Source: Thermo Scientific Dionex EGC-KOH cartridge Gradient: KOH gradient from 2 mM to 50 mM Inj. Volume:0.4 µL Column Temp.:30 °C Detection:Suppressed Conductivity, Thermo Scientific Dionex ACES ™ -300, Anion Capillary Electrolytic Suppressor total Peaks:1. Chloride 26.0 mg/L 2. Nitrate 7.3 3. Sulfate 50.3 4. Phosphate226.1 5. Citrate48.1 20 µS Minutes 10 µL/min 1900 psi 0 10 -5 C A B 20 µL/min 3700 psi 25 µL/min 4500 psi 1 2 3 4 55 5 4 3 5 2 1
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Fruit-Flavored Carbonated Beverage by High Pressure Capillary IC Column:Thermo Scientific Dionex IonSwift ™ MAX100G, MAX100, 0.25 mm Eluent Source: Thermo Scientific Dionex EGC-KOH Gradient: A: 0.1 mM KOH from -10 to 0.1 min, 0.1–2 mM KOH from 0.1 to 2 min, 2–15 mM KOH from 2 to 8 min 15–35 mM KOH from 8 to 12 min B:0.1 mM KOH from -5 to 0.1 min, 0.1–2 mM KOH from 0.1 to 1 min, 2–15 mM KOH from 1 to 4 min 15–35 mM KOH from 4 to 6 min Flow Rate:A: 12 B: 24 µL/min Inj. Volume:0.4 µL Column Temp.:30 °C Detection:Suppressed Conductivity, Thermo Scientific Dionex Anion Capillary Electrolytic Suppressor (ACES ™ -300) Peaks:1. Quinate 2. Chloride 3. Benzoate 4. Malate 5. Carbonate 6. Phosphate 7. Citrate 8. Isocitrate 1 2 3 7 6 4 5 1 2 3 µS 10 -2 Minutes 2030 100 6 7 4 8 A B 8 24 µL/min, 4200 psi 12 µL/min, 2000 psi
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Fast Separation of 10-Fold Diluted Fruit Fiz Sports Beverage on ICS-4000 00 µS -0.1 2 Column: Thermo Scientific Dionex IonPac AG18-Fast, AS18-Fast, 2 mm Eluent Source:Thermo Scientific Dionex EGC-EG Eluent:23 mM Potassium Hydroxide Flow Rate: 0.55 mL/min Inj. Volume:5 µL Column Temp.:30 °C Detection: Thermo Scientific Dionex ASRS 300, 2 mm, 32 mA, recycle Sample Prep.: 10-fold dilution, filtered, 0.45 µm, Thermo Scientific Dionex OnGuard ® RP Peaks:1. Acetate-- mg/L 2. Formate-- 3. Unknown-- 4. Chlorite ?-- 5. Chloride0.4 6. Nitrite-- 7. Carbonate-- 8. Bromide3.0 9. Malate-- 10.Nitrate0.1 10.Nitrate0.1 9 8 17 10 2 6 5 3 4 1 2 3 450 Minutes
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CAPILLARY IC: VITAMIN AND SPORTS BEVERAGES
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Anions in a Sports Beverage by High Pressure Capillary Column:Thermo Scientific Dionex IonSwift ™ MAX100G, MAX100, 0.25 mm Eluent Source: Thermo Scientific Dionex EGC-KOH Gradient: A: 0.1 mM KOH (0.1 min), 0.1–2 mM (0.1 to 2 min), 2–15 mM (2 to 8 min), 15–35 mM (8 to 12 min), 35 mM (12 to 20 min) B: adjusted for flow rate Inj. Volume:0.4 µL Column Temp.:30 °C Detection:Suppressed Conductivity, Thermo Scientific Dionex ACES ™ -300, Anion Capillary Electrolytic Suppressor Sample: Low carbohydrate sports beverage Sample Prep.:Filtered, Thermo Scientific Dionex OnGuard ™ RP, 1:10 dilution Peak:1. Acetate -- mg/L 2. Chloride 41.3 3. Carbonate-- 4. Sulfate 0.1 5. Phosphate34.5 6. Citrate 331 Minutes µS 118 2 2030 100 -5 5 3 6 1 1 2 3 5 6 4 4 B A 24 µL/min, 4200 psi 12 µL/min, 2000 psi
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Fast Separation of a 1:10 Diluted Gatorade G2 Reduced Carbohydrate Sports Beverage 1 2 3 45 Minutes 0 µS 10 Column: Thermo Scientific Dionex IonPac AG18-Fast, AS18-Fast, 2 mm Eluent Source:Thermo Scientific Dionex EGC-EG Eluent:23 mM Potassium Hydroxide Flow Rate: 0.55 mL/min Inj. Volume:5 µL Column Temp.:30 °C Detection: Thermo Scientific Dionex ASRS 300, 2 mm, 32 mA, recycle Sample Prep.: 10-fold dilution, filtered, 0.45 µm, Thermo Scientific Dionex OnGuard RP Peaks:1. Fluoride-- mg/L 2. Formate-- 3. Chloride41 4. Carbonate-- 5. Sulfate -- 6. Nitrate-- 5 4 1 3 6 2
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Fast Separation of 1:10 Diluted, Gatorade G2 Sports Beverage on ICS-4000 Column: Thermo Scientific Dionex IonPac AG22-Fast, AS22-Fast, 2 mm Eluent:4.5 mM Sodium Carbonate 1.4 mM Sodium Bicarbonate Flow Rate: 0.30 mL/min Inj. Volume:2.5 µL Column Temp.:30 °C Detection:Thermo Scientific Dionex ASRS 300, 2 mm, 7 mA, recycle Sample Prep.:10-fold dilution, filtered, 0.45 µm, Thermo Scientific Dionex OnGuard RP Peaks:1. Acetate-- mg/L 2. Unknown-- 3. Chloride39 4. Carbonate-- 5. Sulfate-- 6. Nitrate-- 0510 15 20 40 4 1 5 6 2 3 µS Minutes
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Fast Separation of 1:10 Diluted, Glacial Vitamin Beverage on Integrated IC System 5 010 20 30 Minutes µS 1 2 5 3 4 6 Column: Thermo Scientific Dionex IonPac AG22-Fast, AS22-Fast, 2 mm Eluent:4.5 mM Sodium Carbonate 1.4 mM Sodium Bicarbonate Flow Rate: 0.30 mL/min Inj. Volume:2.5 µL Column Temp.:30 °C Detection:Thermo Scientific Dionex ASRS 300, 2 mm, 7 mA, recycle Sample Prep.:10-fold dilution, filtered, 0.45 µm, Thermo Scientific Dionex OnGuard RP Peaks:1. Fluoride1.6 mg/L 2. Acetate-- 3. Chloride4.4 4. Nitrate2.6 5-7. Unknown -- 8. Citrate -- 7 8
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IC can be used in a broad variety of raw ingredient and finished product testing. Capillary IC is “Always Ready” allowing you to start running samples whenever on demand, and continue to run them without compromise. Demonstrated capabilities with Functional Waters, Juices, Dissolved Tablets, and other beverages Summary Capillary IC is a quantum leap ahead!
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Thank you!
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