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Ion Chromatography Applications in the Power Industry
Dionex Corporation Sunnyvale, CA
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Content
● Introduction ● Eluent Generation and Purification ● Suppression
● Applications ● On-line Sample Preparation ● Borated Waters ● Amines – Matrices and Analytes
● Conclusions
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Automation Challenges - IC for Trace Analytics
● Eluent Preparation ● Separation ● Calibration ● Sample Preparation ● Quantification
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Reagent-Free Ion Chromatography (RFIC) Eluent Generation and Purification
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Principles of RFIC - Eluent Generation
Vent
Pump
H2O
[KOH] α Current Flow Rate
H2
Degas Unit
Cation Exchange Connector
CR-ATC Anion Trap
KOH + H2
KOH Electrolytic Chamber
EluGen® KOH Cartridge Pt Anode [ + ]
K+
Pt Cathode (2H2O + 2e– 2OH– + H2)
OH–
KOH H2O
K-Reservoire
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RFIC-EG Chemistries
● RFIC – KOH ● RFIC – NaOH ● RFIC – LiOH ● RFIC – MSA ● RFIC – Carbonate ● RFIC – Carbonate / Bicarbonate
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Continuously Regenerated Trap Column (CR-TC)
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Continuously Regenerated Anion Trap Column (CR-ATC)
Purpose: Residual Carbonate Removal from Supply Water
H2CO3 CO32–+ 2H+
Cathode (–)
OH–
CO32–
Anode (+)
H2O
From Suppressor
Regen Effluent
From EG Cartridge
H2O + H2CO3
To Degas and Waste
To Degas and Inj. Valve
H2O 2H+ + ½O2 + 2e–
2H2O + 2e– 2OH– + H2
H2O H+ + OH–
Anion Exchange Resin
Anion Exchange Membrane
2 OH– KOH + K2CO3 K+ OH–
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Chemical Suppression
HF, HCl, H2SO4 in H2O
NaF, NaCl, Na2SO4 in NaOH
Sample: F-, Cl-, SO42-
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NaOH, H2
Waste/Vent Waste/Vent Anode
To Detector
H+ + O2 H2 + OH-
H2O H2O H+ , X- in H2O
H2O H2O
H2O, O2
Cation- Exchange
Membranes
OH-
Na+, X- in NaOH Eluent Cathode
H2O 2H+ + ½ O2 + 2e-
2H2O + 2e- 2OH- + H2
H+ Na+OH- X-
Chemistry and Ion Movement in an Anion Self Regenerating Suppressor (SRS®)
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Ultrapure Water (UPW) Analysis
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IC for Trace Ionic Impurities in UPW
Anions (e.g., F-, Cl-, SO42-) Suppressed conductivity
Cations (e.g., Li+, Na+, K+, Mg2+) Suppressed conductivity
Silica (as dissolved SiO2-) Post-column derivatization
with Vis detection
Transition metals (e.g., Cu2+, Ni2+, Zn2+, Mn2+)
Post-column derivatization with Vis detection
Boron (as B(OH)4-) Suppressed conductivity
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Large Volume Injections
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Column: IonPac® AS4A, 2 mm (microbore)
Inj. Volume: 20 µL Flow Rate: 0.5 mL/min
Eluent: 1.8 mmol/L Sodium carbonate 1.7 mmol/L Sodium bicarbonate
Peaks: 1. Fluoride 2 mg/L 2. Chloride 3 3. Bromide 10 4. Nitrate 10 5. Phosphate 15 6. Sulfate 15
18
0
µS
1 2
3 4
5 6
0 5 10 Minutes
18
0
µS 1 2 3 4
5 6
Column: IonPac AS4A, 4 mm (standard bore)
Inj. Volume: 20 µL Flow Rate: 2.0 mL/min
Increased Mass Sensitivity: 2 mm Technology
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Power Plant Polisher Effluent
Blank
0 5 Minutes
15 -0.1
0.7
µS
-0.1
0.7
µS
1 2
3 4 7 8
9 10 11
Column: IonPac® AS11, 2 mm Gradient: NaOH from 0.5 to 26 mmol/L Inj. volume: 750 µL Detection: Suppressed conductivity,
external water mode Peaks: Blank Polisher
Effluent (µg/L) (µg/L)
1. Fluoride <0.01 0.09 2. Acetate <0.01 0.05 3. Formate <0.01 0.46 4. Chloride <0.02 0.34 5. Nitrite <0.02 <0.02 6. Bromide <0.03 <0.03 7. Nitrate <0.02 0.40 8. Unidentified _ _ 9. Carbonate _ _ 10. Sulfate <0.02 0.10 11. Oxalate <0.02 0.07 12. Phosphate <0.1 <0.1
Direct Injection Analysis of Power Plant Condensate Polisher Effluent
10 20
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Column: IonPac® AG15-5 µm, 3 mm AS15-5 µm, 3 mm
Eluent: 7 to 40 mmol/L KOH (EG) Flow rate: 0.5 mL/min Detection: Suppressed conductivity Inj. volume: 1000 µL
Peaks: 1. Fluoride 0.16 µg/L 2. Acetate 1.2 3. Formate 3.9 4. Chloride 0.44 5. Nitrite 1.3 6. Carbonate – 7. Sulfate 3.6 8. Unknown – 9. Nitrate 0.15 10. Unknown – 11. Phosphate 0.86
0.15
0.75
10 20 30
µS
Minutes
12
3
4
5
6 7
8 9 10 11
Fossil Fuel Power Plant - Condensate Discharge Water
0
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Column: IonPac® CS12A (2 mm) Eluent: 11 mmol/L sulfuric acid Flow rate: 0.25 mL/min Inj. volume: 500 µL Peaks: 1. Lithium 0.25 µg/L
2. Sodium 1.0 3. Ammonium 1.2 4. Potassium 2.5 5. Magnesium 1.2 6. Calcium 2.5
2
µS
0
1 2
3
5 4
6
Minutes 0 2 4 6 8 10 12 14 16
Trace Cations by Direct Injection
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1
2
3
0 2.5 5 7.5 10 12.5 15 17.5 20 Minutes
-0.05
0.04
µS
Column: IonPac® CS12A, 2 mm Eluant: 10 mmol/L sulfuric acid Flow rate: 0.25 mL/min Inj. volume: 40 mL, concentrated Detection: Suppressed conductivity,
External water mode
Peaks: 1. Sodium < 10 ng/L 2. Ammonium < 10 3. Trimethylamine -
Cations in Ultrapure Water
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AutoPrep – Simplifying IC Trace Determinations
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System calibration ● A small loop of known volume is loaded with standard ● Multiple valve toggles (or flips) determine the “level” of the calibration ● Contents of small loop are pushed to a concentrator column ● Contents of concentrator eluted for analysis ● Chromeleon establishes a multi-point calibration
Sample analysis ● Sample is loaded onto a large volume loop (10 mL) ● The large loop contents are pushed onto the concentrator ● Contents of concentrator eluted for analysis
AutoPrep IC System
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Colu
mn
Supp
ress
or
DP1
DP2
AS-HV
Large Loop
Small Loop
Standard
ATC
Waste
Waste
AutoPrep IC System
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Colu
mn
Supp
ress
or
DP1
DP2
AS-HV
Large Loop
Small Loop
Standard
ATC
Waste
Waste
AutoPrep IC System
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Colu
mn
Supp
ress
or
DP1
DP2
AS-HV
Large Loop
Small Loop
Standard
ATC
Waste
Waste
AutoPrep IC System
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Colu
mn
Supp
ress
or
DP1
DP2
AS-HV
Large Loop
Small Loop
Standard
ATC
Waste
Waste
AutoPrep IC System
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Colu
mn
Supp
ress
or
DP1
DP2
AS-HV
Large Loop
Small Loop
Standard
ATC
Waste
Waste
AutoPrep IC System
![Page 26: Ion Chromatography Applications in the Power Industrytools.thermofisher.com/content/sfs/brochures/88273-PR-Principles... · Ion Chromatography Applications ... Exchange Connector](https://reader035.fdocuments.us/reader035/viewer/2022062504/5a9d9e0d7f8b9a42488b8c3e/html5/thumbnails/26.jpg)
Colu
mn
Supp
ress
or
DP1
DP2
AS-HV
Large Loop
Small Loop
Standard
ATC
Waste
Waste
AutoPrep IC System
![Page 27: Ion Chromatography Applications in the Power Industrytools.thermofisher.com/content/sfs/brochures/88273-PR-Principles... · Ion Chromatography Applications ... Exchange Connector](https://reader035.fdocuments.us/reader035/viewer/2022062504/5a9d9e0d7f8b9a42488b8c3e/html5/thumbnails/27.jpg)
Colu
mn
Supp
ress
or
DP1
DP2
AS-HV
Large Loop
Small Loop
Standard
ATC
Waste
Waste
AutoPrep IC System
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Colu
mn
Supp
ress
or
DP1
DP2
AS-HV
Large Loop
Small Loop
Standard
ATC
Waste
Waste
AutoPrep IC System
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Colu
mn
Supp
ress
or
DP1
DP2
AS-HV
Large Loop
Small Loop
Standard
ATC
Waste
Waste
AutoPrep IC System
![Page 30: Ion Chromatography Applications in the Power Industrytools.thermofisher.com/content/sfs/brochures/88273-PR-Principles... · Ion Chromatography Applications ... Exchange Connector](https://reader035.fdocuments.us/reader035/viewer/2022062504/5a9d9e0d7f8b9a42488b8c3e/html5/thumbnails/30.jpg)
Colu
mn
Large Loop
DP1
Small Loop
Standard
DP2
ATC
Waste
Waste AS-HV
Supp
ress
or
AutoPrep IC System
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AutoPrep IC System – Ultrapure Water Analysis
0 5 10 15 20 26 –0.20
0
1
µS
Minutes
F Cl NO2
24865
F 24
Cl 22
NO2 42
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AutoPrep IC System – Ultrapure Water Analysis
Li 12 Na 28
NH4 13
K 15 Mg 8 Ca 11
0 5 10 15 20 26 –0.100
–0
0.500
µS
Minutes
Li Na NH4 K Mg Ca
24869
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AutoPrep IC System – Chromeleon® Panel
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AutoPrep IC System
AutoPrep: A series of automated steps to prepare samples on-line.
● Simplifies trace analysis ● Contamination-free
● On-line and automated calibration ● On-line and automated sample preparation.
● Lower detection limits ● Less than 5 ng/L (ppt)
● Less manual errors ● Improved reliability
● Lower labor costs
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RFIC-ESP – Electrolytic Sample Preparation
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RFIC-ESP on the ICS-2100
2 1 10
9 8
6 5
4 3
7
Large Loop
Small Loop
Concentrator
Analytical Column
Guard Column
Standard Pump
W aste
1 2
3
4 5
6
AS-HV
Detector
Waste
W ater Purifier
CRD
Suppressor
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Cathode
Anode
Cation Exchange Membrane
Anion Exchange Membrane
Water
UPW Mixed Bed
RFIC-ESP: How Does the Water Purifier Work?
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Cathode Anode
Anion Cation
OH- H+
H+ OH- H2O
H2O H2O
RFIC-ESP Device – Electrolytic Water Purifier
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2 H2O + 2 e- 2 OH- + H2 H2O 2 H+ + ½ O2 + 2 e-
Cathode Anode
Anion Cation
OH- H+
H+ OH- H2O
H2O H2O
Na+ Cl- Cl- Na+
UPW
RFIC-ESP Device – Electrolytic Water Purifier
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ASRS
Eluent Generator
Concentrator Column
Guard Column Detector
Eluent Suppressed
Eluent
Pure Water
Electrolytic Water Purifier
Standard or Sample (10 µL)
Large volume Autosampler
3 10
5 8
New RFIC-ESP IC Technique
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Eluent Generator
Guard Column
Eluent Suppressed
Eluent
Pure Water
Standard
Electrolytic Water Purifier
ASRS Detector
New RFIC-ESP IC Technique
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Eluent Generator
Guard Column
Eluent Suppressed
Eluent
Pure Water
Standard
Repeat Load/Inject 5 times
Use same flushing volume
Electrolytic Water Purifier
ASRS Detector
New RFIC-ESP IC Technique
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RFIC-ESP - Untreated vs. Treated Water
0 22
0
1.25 Untreated Water RFIC-ESP Treated Water
Fluoride
Chloride
Nitrite Sulfate
Nitrate
Minutes
µS
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3 12 0.08
0.48
µS
Minutes
Fluoride Chloride
Nitrite
Carbonate
Bromide
Sulfate
Nitrate Phosphate
RFIC-ESP – Automated Calibration
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RFIC-ESP – Automated Calibration
Standard amounts
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● Only one pump needed ● Simplifies trace analysis ● Very low backgrounds ● Very low detection limits – less than 5 ppt ● Sample calibration and concentration is automated ● High degree of automation
● Fewer errors, improved reliability, lower labor costs
RFIC-ESP - Summary
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Anion Determination in Borated Water
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4
3
2
1
0 5 Minutes
15
Anions in Borated Water – PWR Primary Water Circuit
Column: IonPac® AG10, AS10 Eluent: 85 mmol/L NaOH Flow rate: 1 mL/min Detection: Suppressed conductivity, Injection: 12 mL Concentrator: AC10 Peaks: 1. Fluoride
2. Borate 3. Chloride 5 µg/L 4. Sulfate
10
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Combination of AutoPrep with On-line Matrix Elimination
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M+X–
M+ M+
H+X–
H2O Regenerant
Sample in
H2O + MOH
H+X–
To Concentrator Column
MOH
On-line Sample Preparation – CR-CTC II
Continuously Regenerated-Cation Tray Column (CR-CTC II) for on-line RFIC sample pretreatment – Removal of cations including Lithium Note: Power to the CR-CTC II should be turned on only when sample is flowing through the unit.
LiOH Li+
H+
OH- H2O
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RFIC-ESP™: CR-CTC II Sample Prep when Concentrating a Large Volume (40 mL) of Sample
Instrument: ICS-3000 and AS RFIC-ESP: CR-CTC II and AG4A concentrator Column: IonPac® AG4A (4 mm)/ AS4A (4 mm) RFIC-EG: KOH Gradient, 100 mM borate Flow Rate: 1.5 mL/min Inj. Vol.: 40 mL sample Detection: Suppressed conductivity Sample: Simulated reactor water,
3.5 ppm Lithium hydroxide
30
µS
Sample after CR-CTC II Sample w/o CR-CRC II
Fluoride
Chloride Sulfate
0
0 25 Minutes
CR-CTC II
3 2
1
10
8 7
4
9 5 6
Pump
AS
Guard
Suppressor
Column
Detector
Concentrator
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Determining Trace Anions in Borated Water
DI Water
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Minutes
Small Organic and Common Inorganic Anions
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Minutes
(A) Original
(B) Spiked
Trace Anions in Borated Water
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Ammonium and Hydrazine in PWR Secondary Water
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Column: IonPac® AG15, AS15, 2 mm Eluent: KOH-Gradient Eluent Source: EGC II KOH with CR-ATC Flow Rate: 0.40 mL/min Temperature: 30°C Sample. Volume: 2 mL Concentrator: AC10 Detection: ASRS® ULTRA II, 2 mm, recycle mode,
65 mA Carbonate Removal Device CRD-200
Sample: 10 ppm Ammonium
Peaks: 1. Fluoride 10 µg/L 2. Chloride 10 3. Carbonate – 3. Sulfate 10
Trace Anions in Ammoniated Water
0 5 10 15 20 25 30
0
6
Minutes
1
2 3 µS
4
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Hydrazinated Water – PWR Secondary Circuit
Column: IonPac® AG15, AS15, 2 mm Eluent: KOH-Gradient Eluent Source: EGC II KOH with CR-ATC Flow Rate: 0.40 mL/min Temperature: 30 °C Sample. Volume: 10 mL Matrix Elim. Vol.: 12 mL Concentrator: AC15 (2 mm) Detection: ASRS® ULTRA II, 2 mm,
recycle mode No CRD-200 used
Sample: Hydrazine (200 ppb) in UPW
Anions: s. Chromatogram Concentrations single digit ppb
µS
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Real World Sample – PWR Secondary Cooling Water
Column: IonPac® AG15, AS15, 2 mm Eluent: KOH-Gradient Eluent Source: EGC II KOH with CR-ATC Flow Rate: 0.40 mL/min Temperature: 30 °C Sample. Volume: 10 mL Matrix Elim. Vol.: 12 mL Concentrator: AC15 (2 mm) Detection: ASRS® ULTRA II, 2 mm,
recycle mode No CRD-200
Sample: Cooling water
Concentrations: single digit µg/L
µS
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Amines – Matrices and Analytes
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Column: IonPac® CS14, CG14 (2 mm) Eluent: 8 mmol/L MSA in 5 % CH3CN Flow rate: 0.25 mL/min Inj. volume: 1.0 mL concentrated on
IonPac CG14 (2 mm) Detection: Suppressed conductivity
Peaks: 1. Lithium 0.5 (µg/L) 2. Sodium 2.0 3. Ammonium 150 4. Potassium 2.0 5. Morpholine 2000 6. Magnesium 2.0 7. Calcium 10
0 8
0
8
µS
3
1 2
4
2 4 6 10 12 14 16
5
6 7
Trace Cations in Morpholine Treated Water
Minutes
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High-to-Low Ratio of Ammonium to Hydrazine
Column: IonPac® CS16 Eluant: 7 mmol/L MSA (EG), gradient to 52 mmol/L MSA from 20 to 25 min, step to 7 mmol/L
MSA at 30 min Flow rate: 1.2 mL/min Inj. volume: 25 µL Temperature: 40 °C Detection: Suppressed conductivity
AutoSuppression, Recycle Mode
Peaks: 1. Sodium 2 µg/L 2. Ammonium 20,000 3. Hydrazine 200
4. Potassium 2 5. Magnesium 2
6. Unknown – 7. Calcium 14 11 21 31
Minutes
0.23
0.53
µS
1 3
4 5 6 7
2
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Elution of Ethanolamine and Hydrazine
Suppressed Conductivity Detection
0.32
0.45
µS 1 2
3
4
0 5 10 15 20 25
Column: IonPac® CS16, 3 x 250 mm Eluent: EG40, 12 mM, MSA Temperature: 23 °C Flow Rate: 0.36 mL/min Inj. Volume: 25 µL
Peaks: 1. Sodium – µg/L 2. Ammonium – 3. Ethanolamine 50 4. Hydrazine 200
Minutes 0 5 10 15 20 25
26.0
38.3
nC
3
4
Electrochemical Detection
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Minutes
µS
0 10 5 15 20 25
0
1
3
4 5
5
2
6
7
Column: IonPac® CG15/CS15 Eluant: 5 mmol/L sulfuric acid / 9 % CH3CN Flow rate: 1.2 mL/min Temperature: 40°C Inj. volume: 25 µL Detection: Suppressed conductivity,
AutoSuppression, external water mode
Peaks: 1. Lithium 1 mg/L 2. Sodium 4
3. Ethanolamine 3 4. Ammonium 5
5. Magnesium 5 6. Calcium 10
7. Potassium 10
Isocratic Separation of Ethanolamine
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Column: IonPac® CS18, 2 mm Eluant: 0.5 mmol/L MSA (EG), gradient to 3 mmol/L
at 16 min, gradient to 25 mmol/L at 30 min Flow rate: 0.30 mL/min Temperature: 40°C Inj. volume: 5 µL Detection: Suppressed conductivity,
AutoSuppression, recycle mode
Peaks: 1. Lithium 0.05 mg/L 2. Sodium 0.20 3. Ammonium 0.25 4. Ethanolamine 2.0 5. Potassium 0.50 6. 2-(2-aminoethoxy)ethanol 3.0 7. 5-amino-1-pentanol 3.0 8. Morpholine 3.0 9. 3-methoxypropylamine 3.0
10. 2-diethylaminoethanol 3.0 11. 3-quinuclidinol 2.0 12. Magnesium 0.25 13. Calcium 0.50 14. Ethylenediamine 2.0 15. Cyclohexylamine 3.0
Power Plant Relevant Amines
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Thank You