Capillary Ion Chromatography and High-Pressure Ion Chromatography: Applications and Solutions

Transcription

1 Capillary Ion Chromatography and High-Pressure Ion Chromatography: Applications and Solutions Peter Bodsky Field Marketing Manager, North America 1 The world leader in serving science

2 Outline Capillary Ion Chromatography (IC) High Pressure IC and Why A Look Back: Review of Suppression, Reagent-Free Ion Chromatography (RFIC ) Advantages of HPIC Systems and Columns 4 µm Particle Column Technology Applications Data HPIC Instrumentation Accelerated Solvent Extraction, Solid-Phase Extraction, and Sample Preparation 2

3 The Dimension of Scale Parameter Analytical IC Capillary IC Column Diameter 4 mm 0.4 mm Flow Rate 1.0 ml/min 10 µl/min Injection Volume 25 µl 0.4 µl Eluent Consumption 43.2 L/month L/month EGC Lifetime (@75 mmol/l) 28 days 18 months EG Current (50 mm KOH) 80.4 ma ma K + Consumption/Year 26.3 Moles (50 mm KOH) Moles (50 mm KOH) H 2 O Consumption/Year L 5.25 L 3

4 The Dimension of Scale The Concentration Factor Overlay of chromatograms with 4 mm, 2 mm, and 0.4 mm columns all with equal injection volume (0.4 µl) Conductivity [µs] Capillary IC with 0.4 µl injection volume Lithium Sodium Microbore IC with 0.4 µl injection volume Ammonium Sodium Potassium Lithium Ammonium Potassium Magnesium Magnesium Calcium Calcium 16 Standardbore IC with 0.4 µl injection volume Sodium Potassium Lithium Ammonium Magnesium Calcium Retention time [min] 4

5 Capillary IC Dimension of Scale Overlay of chromatograms from 4 mm, 2 mm and 0.4 mm all with same injection volume Capillary IC with 0.4 µl Injection Volume Lithium Sodium Ammonia Potassium Magnesium Calcium Conductivity [µs] Microbore IC with 0.4 µl Injection Volume Lithium Sodium Ammonia Potassium Magnesium Calcium 16.0 Standard bore IC with 0.4 µl Injection Volume Lithium Sodium Ammonia Potassium Magnesium Calcium Retention Time [min] 5

6 Concentration Sensitivity Comparison Capillary IC vs. Standard-bore IC Conductivity [µs] Capillary 1 IC: 0.4 mm Thermo Scientific Dionex IonPac CS12A Column with 0.4 µl Injection 10 µl/min Lithium Sodium Ammonium Potassium Standard-bore IC: 4 mm Dionex IonPac CS12A Column with 40 µl Injection 1.0 ml/min Lithium Sodium Ammonium Potassium Magnesium Magnesium Calcium Calcium The amounts of the analytes injected on the 4 mm column are 100 times of those injected onto the 0.4 mm column The concentrations of separated analytes going through the conductivity detector are the same in both systems A capillary IC system using the 0.4 mm columns provides the same concentration sensitivity as standard-bore IC system using the 4 mm columns Retention Time [min] 6

7 Capillary Technology: The Dionex IC Cube Cartridge CRD 200 Guard and Separation Column 3.5 Side View of Cap Suppressor Suppressor Injection Valve 6.5 Thermo Scientific Dionex IC Cube Cartridge EG Degas 7

8 Fewer Connections Dual Analytical 60 Fluidic Connections Dual Capillary 26 Fluidic Connections Change an IC Cube with all consumables 6 connections! 8

9 Typical Workflow: Traditional IC Dionex IonPac AS19 Column Gradient Analysis Start-up: Equilibration: Total Time = 1 Hour Run 3 Standards: Total Time = 1 h 30 min Eluent Preparation Total Time = 1 Hour Results Total Analysis Time: Total Time = 6 hours Run 5 Samples: Total Time = 2 h 30 min 9

10 Typical Workflow: Capillary Ion Chromatography Always On Always Ready Dionex IonPac AS19 Gradient Analysis Run Check Standard: Total Time = 30 min Run 5 Samples: Total Time = 2 h 30 min Results Total Analysis Time: Total Time = 3 hours Capillary IC Redefines Ion Chromatography: IC on Demand 10

11 Capillary IC Value: Best Results 4.00 Sulfate Nitrite Fluoride Conductivity [µs] 2.00 Chlorate Chloride Chlorite Bromide Nitrate Dionex IonPac AS19 Isocratic (10 ml/min) 0.4 mm 250 mm Fluoride 6.0 Chlorite Retention Time [min] Chloride Nitrite Chlorate 14.0 Bromide Nitrate 18.0 Sulfate Retention Time (% RSD) Peak Area (% RSD) Overlay of 50 Consecutive Analysis

12 Separation of 22 Anions µs 16.0 Overlay of 30 consecutive runs % RSD retention times: 0.09% for arsenate to 0.18% for fluoride Fluoride Acetate Formate Bromate Chlorite Chloride Nitrite Chlorate Bromide Nitrate Sulfate Malonate Selenate Oxalate Iodide Thiosulfate Chromate Phosphate Fumarate Arsenate Thiocyanate Column: Dionex IonPac AS19 (250 mm 0.4 mm ID) Eluent: KOH (EG) Gradient: 10 mmol/l (0 to 10 min), mmol/l (10 to 42 min), mmol/l (42 to 45 min) Flow rate: 10 µl/min Temperature: 30 C Detection: Suppressed conductivity Suppressor: Thermo Scientific Dionex ACES 300 Anion Capillary Electrolytic Suppressor Perchlorate Minutes 50 12

13 Capillary IC Values: Small Sample Sizes Limited Volumes Precious/Valuable samples (Metabolomics) Corrosion detection Safety Toxic/Dangerous samples Reduced Waste Cost Less overall waste to dispose of. i.e. Radioactive waste Conductivity [µs] Potassium Sodium Lithium Ammonia Magnesium Calcium 0.4 µl Injection volume: Blue Capillary IC Black Standard bore IC Retention Time [min] 13

14 Inorganic Anions at Trace Concentrations Column: Dionex IonPac AS19 column ( mm) Eluent Source: Thermo Scientific Dionex EGC-KOH Eluent Generator Cartridge (Capillary) Eluent: Flow Rate: 20 mm KOH 10 µl/min Temperature: 30 C Suppressor: Detection: Injection Volume: 10 µl Electrolytic capillary anion suppressor used in conjunction with a capillary CRD Suppressed conductivity µs Standards in deionized water Deionized water Minutes 20.0 Peak Concentration (ppb) 1. Fluoride Chloride Nitrite Bromide Nitrate Carbonate 7. Sulfate

15 Anions Large Loop Direct Injection of 10 µl 0.4 µs Minutes B A Column: Dionex IonPac AG19, AS19, mm Eluent Source: Dionex EGC-KOH capillary Eluent: 14 mm KOH for 7 min, mm (7 25 min), 14 mm ( min) Flow Rate: ml/min Col. Temp.: 30 C Inj. Volume: 10 µl Detection: Suppressed conductivity, Dionex ACES 300, Thermo Scientific Dionex CRD 200 Carbonate Removal Device Samples: A: Blank B: Diluted anion standard A B Peaks: 1. Fluoride µg/l 2. Acetate Formate Chloride Nitrite Bromide Nitrate Carbonate Sulfate Phosphate

16 HPIC (High-Pressure Ion Chromatography) 16

17 Why HPIC Remember UHPLC? As the particle size decreases from 8 µm to 4 µm, column efficiency doubles This drop in particle size increases the column pressure by 4x Like HPLC, IC is moving toward smaller particle column technology HPIC Instrumentation can now handle the pressure of these smaller particle columns, even at higher flow rates 17

18 HPIC Theory 100 Influence of the particle diameter on pressure and efficiency 1200 Theoretical Plate Height [µm] 10 µm particles 5 µm particles 3 µm particles 2 µm particles Optimal flow rate for maximum separation efficiency / resolution Column pressure [bar] Linear Velocity u [mm/s] Linear Velocity u [mm/s] Faster flows for faster separations generate higher pressure Smaller particles for higher efficiency generate higher pressure 18

19 HPIC System Advantage HPIC systems + 4 µm particle-size columns deliver significant performance advantages Smaller resin particle columns Produce more efficient peaks Impact chromatographic speed and resolution Easier integration more accurate and reliable results Increase sample throughput without compromising data quality Improved quality of analytical results 19

20 Dionex ICS HPIC System Expanding chromatographic control of IC a look back Packed bed suppression reduced background due to mobile phase for improved signal Electrolytic suppression greater flexibility with respect to mobile phase selection/strength, no chemical regeneration RFIC electrolytic eluent generation makes gradient separations as easy as isocratic just add water Capillary IC 18 months continuous operation, infrequent calibration. IC on Demand. HPIC smaller particle columns for improved efficiency, resolution, and chromatographic flexibility 20

21 Improved Separations: 4 µm Capillary Columns 25 µs 0 µs Dionex IonPac AG11-HC 4 µm/as11-hc 4 µm 3600 psi Dionex IonPac AG11-HC/AS11-HC 2200 psi Minutes Eluent Source: Dionex EGC-KOH Eluent Generator Cartridge (Capillary) Gradient: Potassium hydroxide: 1 mm from 0 to 5 min, 1 15 mm from 5 to 14 min, mm from 14 to 23 min, mm from 23 to 31 min Flow Rate: 15 µl/min Inj. Volume: 0.40 µl Temperature: 30 C Detection: Suppressed conductivity, Dionex ACES 300 Anion Capillary Electrolytic Suppressor, recycle mode Peaks: mg/l mg/l 1. Quinate Bromide Fluoride Nitrate Lactate Carbonate Acetate Malonate Propionate Maleate Formate Sulfate Butyrate Oxalate Methylsulfonate Tungstate Pyruvate Phosphate Valerate Phthalate Monochloro Citrate 10.0 acetate 27. Chromate Bromate cis-aconitate Chloride trans-aconitate Nitrite Trifluoroacetate

22 High-Efficiency Dionex IonPac 4 µm HPIC Columns Improved resolution, faster runs, and better results Ion-exchange columns with 4 µm particle size Benefits Smaller particles provide better performance Fast run times with higher flow rates using 150 mm columns High resolution with standard flow rates using 250 mm columns Applications Anions in environmental waters Organic acids in foods and beverages Amines in chemical process solutions 5.5 µs -0.5 Fast Run on Dionex IonPac AS18 4µm 10 µs SEM Image of 4 µm Supermacroporous Bead Minutes 3 0 Minutes 40 0 Minutes 40 High Resolution using the Dionex IonPac AS11-HC 4µm 5 µs High Resolution using the Dionex IonPac CS19 4µm Ion Chromatography Reagent-Free IC Capillary IC Chromatography Data System Software 22

23 Faster Run Times Without Sacrificing Resolution Inorganic anions separation using a 4 µm capillary column 20 µs µl/min, 2820 psi 25 µl/min, 2430 psi 20 µl/min, 2030 psi Column: Dionex IonPac AS18 4µm, mm Eluent Source: Dionex EGC-KOH (Capillary) Eluent: 30 mm KOH Col. Temp.: 30 C Inj. Volume: 0.4 µl Detection: Suppressed Conductivity, Dionex ACES 300 Peaks: 1. Fluoride 0.2 mg/l 2. Chloride 1 15 µl/min, 1570 psi 3. Nitrite 1 4. Sulfate 1 5. Bromide 1 10 µl/min, 1140 psi 6. Nitrate 1 7. Phosphate Minutes 10 23

24 High Resolution Cation Analysis Using a Dionex IonPac CS16 column at different flow rates 7 30 µl/min 3600 psi 20 µl/min 2400 psi 4 10 µl/min 1200 psi µs C 5 6 B A Minutes Column: Dionex IonPac CS16, mm 0.5 mm ID Eluant: 30 mmol/l MSA (EG) Flow rate: A: 10 µl/min B: 20 µl/min C: 30 µl/min Inj. volume: 0.4 µl Temperature: 40 C Detection: Suppressed conductivity Thermo Scientific Dionex CCES 300 Cation Capillary Electrolyte Suppressor, AutoSuppression, Recycle mode Peaks: 1. Lithium 0.5 mg/l 2. Sodium Ammonium Potassium Magnesium Calcium

25 Fast Determinations of Cations in Municipal Wastewater 14 µs B µl/min 3720 psi 4 5 A µl/min 1250 psi Minutes Column: Dionex IonPac CG16/CS16 columns, 0.5 mm i.d. Eluent Source: Dionex EGC-MSA Cartridge (Capillary) Eluent: 30 mm MSA Flow Rate: A: ml/min, B: ml/min Inj. Volume: 0.4 µl Column Temp.: 40 C Detection: Suppressed Conductivity, Dionex CCES 300, recycle mode Sample: Wastewater diluted 50-fold, filtered, 0.2 µm Peaks: 1. Sodium mg/l 2. Ammonium Potassium Magnesium Calcium

26 Fast Determinations of Inorganic Anions in Municipal Wastewater 1.7 µs D C Column: Dionex IonPac AG18 4µm/ AS18 4µm, 0.4 mm i.d. Eluent Source: Dionex EGC-KOH Cartridge (Capillary) Eluent: 23 mm KOH Flow Rate: ml/min Inj. Volume: 0.4 µl Column Temp.: 30 C Detection: Suppressed conductivity, Dionex ACES 300, recycle mode Sample Prep: Diluted 1000-fold, filtered, 0.2 µm Samples: A: Influent B: Primary effluent C: Trickling effluent D: Final effluent B 0 0 A 1 2 Minutes 3 4 Peaks (Total): A B C D 1. Chloride mg/l 2. Nitrite Carbonate Sulfate Nitrate

27 Common Anions in Treated Wastewater 60 µs Column: Dionex IonPac AG19/AS19 columns, 0.4 mm i.d. Eluent Source: Dionex EGC-KOH cartridge (Capillary) Gradient: 10 to 25 mm KOH (0 10 min) 25 to 70 mm KOH (10 20 min) 10 mm KOH (20 25 min) Flow Rate: ml/min Inj. Volume: 0.4 µl Column Temp.: 30 C Detection: Suppressed conductivity, Dionex ACES 300, recycle mode Sample: Treated wastewater, filtered, 0.2 µm Minutes Peaks: 0.4 mm i.d. 4 mm i.d.* 1. Fluoride 1.76 mg/l Chloride Bromide Nitrate Sulfate Phosphate *Data from 4 mm i.d. column using appropriate run conditions (Thermo Scientific Dionex ICS-1100) 27

28 Using HPIC to Identify Spoilage in Beverages 6 µs µl/min, 3600 psi Minutes Column: Dionex IonPac AS11-HC 4 µm Capillary ( mm) Eluent Source: Dionex EGC-KOH (Capillary) Gradient: Potassium hydroxide, 1 mm from 0 to 8 min, 1 30 mm from 8-28 min, mm from min, 60 mm from min Flow Rate: 15 µl/min Inj. Volume: 0.4 µl Column Temp.: 30 C Detection: Suppressed conductivity Dionex ACES 300, recycle mode Sample Prep.: 1:40 dilution with deionized water Peaks: 1. Quinate 11. Maleate 2. Fluoride 12. Sulfate 3. Lactate 13. Oxalate 4. Acetate 14. Unknown* 5. Formate 15. Phosphate 6. Unknown 16. Citrate 7. Chloride 17. cis-aconitate 8. Unknown 18. trans-aconitate 9. Malate-Succinate 19. Unknown 10. Carbonate 28

29 Fast Analysis of Drinking Water Using High-Pressure IC 1.8 µs 2 5 Column: Dionex IonPac AS18 4µm, mm Instrument: Dionex ICS HPIC system Eluent Source: Dionex EGC 500 KOH Eluent: 23 mm Potassium hydroxide Flow Rate: 0.50 ml/min Inj. Volume: 5 µl Column Temp.: 30 C Detection: Thermo Scientific Dionex ASRS 300 Anion Self-Regenerating Suppressor 2 mm, 15 ma, recycle Sample: Municipal City A Sample Prep.: 5-fold dilution with deionized water Peaks: 1. Fluoride 0.4 mg/l 2. Chloride Nitrite < Carbonate Sulfate Nitrate < Chlorate < Minutes 29

30 High-Pressure Capabilities of IC Expanded Performance Up to 5000 psi, in continuous operation, and with RFIC-EG Faster separations with higher flow rates (left) Higher resolution with longer columns (right) 4.5 Thermo Scientific Dionex IonSwift MAX-100: 11 minutes 24 µl/min 3900 psi 15, :1 Na : Ammonia µs µs 2 CS B 5 Minutes CS Minutes 16 30

31 High-Pressure Ion Chromatography HPIC systems provide better performance HPIC systems allow for continuous operation up to 5000 psi HPIC systems: High-pressure ion chromatography in an all PEEK plastic IC High-pressure Reagent-Free (RFIC) ready Smaller 4 µm particle-size ion-exchange columns in a variety formats 31

32 Two-Dimensional Ion Chromatography 2D-IC IC x IC 32

33 Sensitivity Improvement Increased with Capillary IC 1st Dimension Large Loop injection Large Loop EG Pump Partially resolve analyte from matrix Load Inject Valve 1 4-mm Column Suppressor CRD Cell 1 Intermediate Step Transfer cut volume Trap and focus ions of interest 2nd Dimension Separate on smaller ID column Different Selectivity Signal Enhancement Cell 2 CRD Suppressor 0.4-mm Column 2-mm Column 4-mm Column Concentrator Transfer to 2-D Load Concentrator Pump EG Valve 2 33

34 Sensitivity Improvement RFIC using hydroxide eluents suppressed to water, lower background RFIC in 2-D IC 4/2 mm results in 4x sensitivity enhancement 2-D IC in 4/0.4 mm format improves sensitivity 100x Dimension Sensitivity Flow rate (ml/min) First (4mm) 1 1 Second (2mm) Second (0.4mm)

35 2D-IC Determination of Bromate in Drinking Water 0.60 µs µs First Dimension IonPac AS19 Concentrator Second Dimension IonPac 24 BrO Minutes Used for high matrix samples More robust than post-column methods EPA Method 317 uses a toxic, unstable reagent EPA Method 326 is complicated, less robust RFIC - Just add water Full Thermo Scientific Dionex Chromeleon Chromatography Data System software control EPA-approved methods EPA Method Bromate EPA Method Perchlorate EPA Haloacetic Acids (pending) Proven and validated for low ppb detection 35

36 Trace Analysis of HAAs Using a 2-D IC 3 First Dimension Second Dimension Recovery >90% for 9 HAAs First Dimension Column: Dionex IonPac AS24, 4 mm Flow rate: 1.0 ml/min Suppressor: Dionex ASRS 300, 4 mm Column temp.: 15 C Inj. volume: 1000 µl Second Dimension Column: IonPac AS26, 2 mm Flow rate: 0.25 ml/min Suppressor: ASRS 300, 2 mm Column temp.: 15 C Concentrator: Thermo Scientific Dionex IonPac UTAC-LP2 Ultra Trace Anion Concentrator Column Peaks Concentration (µg/l) 1. MCAA MBAA DCAA BCAA DBAA TCAA BDCAA CDBAA TBAA 100 High ionic strength water (specified in EPA methods): chloride, bicarbonate, sulfate 100 mg/l each; nitrate; orthophosphate 10 mg/l each 36

37 Trace Analysis of Perchlorate with IC IC 2.5 µs Perchlorate A. First-Dimension Conditions Column: Dionex IonPac AG16, AS16, 4 mm Flow rate: 1.0 ml/min Eluent: 65 mmol/l KOH (EG) B. Second-Dimension Conditions Column: Dionex IonPac AS20, 0.4 mm Flow rate: 10 µl/min Eluent: 35 mmol/l KOH (EG) Brand A bottled water (263 ng/l perchlorate) Brand B Bottled water (38.5 ng/l perchlorate) 30 ng/l perchlorate in DI water DI water Minutes 45 37

38 38 AutoDilution

39 Challenge of Wastewater/Drinking Water Analysis High concentrations of dissolved salts: Exceed column capacity Poor chromatography Peak suppression Inaccurate reporting Exceed linear calibration range Analyte-specific Inaccurate results 12,000 µs Minutes µs Minutes Undiluted Diluted Decrease column lifetime 39

40 Obtaining Accurate Data Manual analysis Post-run Determine concentration from chromatogram peak area Exceed limit dilute re-run sample Pre-run Manual conductivity measurement Exceed limit dilute run sample Tedious Dilutions prone to errors 40

41 Increasing Accuracy with Automation Automated analysis AutoDilution Post-run analysis using ion chromatograph software to determine if too much sample was loaded In-line Conductivity Conductivity measured prior to loading sample onto column Exceeding upper limit triggers loading of less sample Less sample injected Smaller sample loop Partial loop Automated sample dilution Loading of much lower sample amounts 41

42 Automated Analysis: AutoDilution Wastewater Thermo Scientific Dionex AS-AP Autosampler Thermo Scientific Dionex ICS-2100 RFIC System Centrifugation IC System Filtration Chromatogram Chromeleon CDS Software Automated Sample Dilution Yes No Does peak area or height exceed cutoff? AutoDilution Report 42

43 Automated Analysis: In-line Conductivity and Dilution Thermo Scientific Dionex Sample Conductivity and ph Accessory Wastewater Thermo Scientific Dionex AS-AP Autosampler Dionex ICS-2100 RFIC System Centrifugation Filtration Does conductivity exceed cutoff? Yes Automated Sample Dilution No IC System Chromatogram Report Chromeleon CDS Software 43

44 Automatically Diluted Fracking Flowback Wastewater 2,400 µs µs Minutes Anions Column: Dionex IonPac AG18/AS18 columns, 4 mm i.d. Eluent Source: Dionex EGC III KOH cartridge Eluent: 39 mm KOH Flow Rate: 1 ml/min Inj. Volume: 25 µl Col. Temp.: 30 C Detection: Suppressed conductivity, Dionex ASRS 300 Anion Self- Regenerating Suppressor, recycle mode Sample: 100-fold diluted fracking flowback, filtered, 0.2 µm Peaks: Measured Undiluted 1. Acetate < 0.05 mg/l < 5 2. Formate < 0.05 < 5 3. Chloride , Sulfate Bromide Minutes 44

45 Automatically Diluted Fracking Flowback Wastewater 80 2 Cations µs µs Minutes Minutes Column: Dionex IonPac CG16/CS16 columns, 0.4 mm i.d. Eluent Source: Dionex EGC-MSA (capillary) cartridge Eluent: 30 mm MSA Flow Rate: 0.01 ml/min Inj. Volume: 0.4 µl Col. Temp.: 40 C Detection: Suppressed conductivity, Dionex CCES 300 Cation Self- Regenerating Suppressor, recycle mode Sample: 1000-fold diluted fracking flowback, filtered, 0.2 µm Peaks: Measured Undiluted 1. Lithium < 0.05 mg/l < 5 2. Sodium , Ammonium Potassium Magnesium 1.1 1, Calcium ,000 45

46 Method Determination of Hexavalent Chromium in Drinking Water by Ion Chromatography with Post-Column Derivatization and UV-Visible Spectroscopic Detection Replaces EPA Method

47 Health Effects of Chromium Chromium-3 A nutritionally essential element often added to dietary vitamin supplements Chromium-6 (Chromate) Strong oxidizer Genotoxic carcinogen (California Public Health Goal = 0.02 μg/l Cr+6 ) 47

48 System Configuration for Hexavalent Chromium Eluent Autosampler High-Pressure Nonmetallic Pump 1000 µl Sample Loop Thermo Scientific Dionex IonPac NG1 Post column Reagent Diphenylcarbazide U.S. EPA Method Thermo Scientific Dionex IonPac AS7 2mm Mixing Tee Knitted Reaction Coil (750 µl) UV-Vis Detector Waste

49 Chromate Detection Blank and low-level chromate Comparison of chromate in high ionic-strength water (HIW) and Sunnyvale tap water 2.5 mau Column: Dionex IonPac AS7 (2 50 mm), AS7 ( mm) Eluent: 250 mm (NH 4 ) 2 SO 4, 100 mm NH 4 OH Flow: 0.36 ml/min Inj. Vol: 1000 µl Postcolumn Reagent: 2 mm diphenylcarbazide 10% methanol 1N sulfuric acid Reaction Coil: 125 µl Flow Cell: Standard (PEEK), 11 µl A. DI water blank B µg/l Cr(VI) in DI water Column: Dionex IonPac AS7 (2 50 mm), AS7 ( mm) Eluent: 250 mm (NH 4 ) 2 SO 4, 100 mm NH 4 OH Flow: 0.36 ml/min Inj. Vol: 1000 µl Postcolumn Reagent: 2 mm diphenylcarbazide 10% methanol 1N sulfuric acid Reaction Coil: 125 µl Flow Cell: Standard (PEEK), 11 µl A. 0.1 µg/l Cr(VI) in DI water B. 0.1 µg/l Cr(VI) in HIW C. 0.1 µg/l Cr(VI) spiked in Sunnyvale, CA tap water B A Minutes 49

50 Chromate in Tap Water 16.2 mau Column: Dionex IonPac AS7 (2 50 mm), AS7 (2 250 mm) Eluent: 250 mm (NH 4 ) 2 SO 4, 100 mm NH 4 OH Flow: 0.36 ml/min Inj. Vol: 1000 µl Postcolumn Reagent: 2 mm diphenylcarbazide 10% methanol 1N sulfuric acid Reaction Coil: 125 ml Flow Cell: Standard (PEEK), 11 µl A. Sunnyvale, CA tap water µg/l B. San Jose, CA tap water 1.29 µg/l B A Minutes Signal Offset 10% Sunnyvale, CA µg/l San Jose, CA 1.3 µg/l 50

51 Column Dimension Comparison Method Detection Limit (MDL) for Chromate Based on a 1000 µl Injection Column Format Chromate Concn. (µg/l) Std. Dev. (µg/l) RSD (%) MDL* (µg/l) 4 mm mm * MDL = (Standard Deviation) (t s, 99 ), where t s, 99 = 3.14 for n = 7. MDL = 1 ppt (with 2 mm column format) LOQ = 3 ppt 51

52 Dionex ICS-4000 Capillary HPIC System Dedicated Capillary HPIC New level of resolution and speed Delivering best in class sensitivity Simplifies workflows Increases analytical efficiency and productivity Small footprint Electrochemical, conductivity, or charge detection HPIC - High Resolution, Fast Analyses IC Cube Cartridge 52

53 The Dionex ICS HPIC System High Pressure Ion Chromatography High pressure capable with both capillary and standard flow rates Continuous operation up to 5000 psi when configured as a Reagent-Free (RFIC) system Increased productivity with fast run times Improved separations and higher resolution with 4 µm particle columns HPIC - High Resolution, Fast Analyses 53

54 The Dionex Ion Chromatography Product Line RFIC HPIC Dionex ICS-900 Dionex ICS-1100 Dionex ICS-1600 Dionex ICS-2100 Dionex ICS-4000 Dionex ICS

55 High-Pressure Ion Chromatography HPIC systems provide better performance HPIC systems allow for continuous operation up to 5000 psi HPIC systems High-pressure ion chromatography in an all PEEK plastic IC High-pressure Reagent-Free ready Smaller 4 µm particle-size ion-exchange columns in a variety formats 55

56 Thank you! 56