High Pressure Ion Chromatography

Report
Advances in Trace Element Analysis
2013 ACS Spring Meeting Workshop
Art Fitchett and Fergus Keenan
The world leader in serving science
1
Agenda
• Ion Chromatography (IC)
• High Pressure Ion Chromatography (HPIC)
• Inductively Coupled Plasma (ICP)
• ICP-OES
• ICP-MS
• IC-ICP-MS
• Speciation
2
Why High Pressure Ion Chromatography
• Remember UHPLC?
• As the particle size decreases from 8µm to 4µm, 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.
3
HPIC Theory
Influence of the Particle Diameter on Pressure and Efficiency
1200
Theoretical Plate Height [µm]
100
1000
Column pressure [bar]
10 µm particles
5 µm particles
3 µm particles
2 µm particles
Optimal flow rate
for maximum
separation
efficiency /
resolution
800
600
400
200
0
0
0
2
4
6
Linear Velocity u [mm/s]
8
10
0
2
4
6
8
Linear Velocity u [mm/s]
Faster Flows for Faster Separations generate Higher Pressure
Smaller Particles for Higher Efficiency generate Higher Pressure
4
10
HPIC System Specifications
Format
Capillary
Microbore
Standard Bore
Flow Rate Range
0.001-0.100 mL/min in 0.001
µL/min increments
Typical range: 5-20 µL/min
0.001-10 mL/min in 0.001
µL/min increments
Typical range: 0.2-0.5 mL/min
0.001-10 mL/min in 0.001
µL/min increments
Typical range: 1-2 mL/min
Max. Pressure
5
5000 psi (eluent generation)
5000 psi (eluent generation)
5000 psi (eluent generation)
6000 psi (pump pressure range) 6000 psi (pump pressure range) 6000 psi (pump pressure range)
Column i.d.s Supported
0.2-0.6 mm
1-3 mm
3-7 mm
Yearly Eluent Usage
(continuous operation)
5.25 L (10 µL/min)
131L (0.25 mL/min)
525 L (1 mL/min)
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
6
New High Efficiency Dionex IonPac 4µm IC Columns in
Analytical and Capillary Formats
4 µm
Ion-exchange columns with 4 µm particle-size
Benefits
• Smaller particles provide better performance
• Faster run times with higher flow rates using
150 mm columns
• Better resolution with standard flow rates using
250 mm columns
SEM Image of 4 µm
Supermacroporous Bead
Applications
• Anions in environmental
waters
• Organic acids in foods
and beverages
• Amines in chemical
process solutions
10
5.5
5
µS
10
µS
Minutes
40
High Resolution using the
Dionex IonPac AS11-HC-4µm
µS
0
0
Minutes
40
High Resolution using the
Dionex IonPac CS19-4µm
-0.5
0
Minutes
Fast Run using the
Dionex IonPac AS18-4µm
Improved Resolution Provides Faster Runs and Better Results
7
3
Improved Separations using 4 µm Particle Size
Capillary Columns
25
Thermo Scientific™ Dionex™ IonPac™ AG11-HC-4µm/AS11-HC-4µm
3600 psi
21 22
20
13
µS
6
8
12 14
9
2
17
16
19
11
4 5 7 10
1 3
24 26
27 29
23
25
15
18
28
0
Dionex IonPac AG11-HC/AS11-HC
2200 psi
µS
-15
0
6
12
18
Minutes
8
Eluent Source: Thermo Scientific 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,
15–30 mM from 14 to 23 min,
30–60 mM from 23 to 31 min
Flow Rate:
15 µL/min
Inj. Volume:
0.40 µL
Temperature: 30 °C
Detection:
Suppressed conductivity,
Thermo Scientific™ Dionex™ ACES™ 300
Anion Capillary Electrolytic Suppressor,
recycle mode
24
30
Peaks:
1. Quinate
2. Fluoride
3. Lactate
4. Acetate
5. Propionate
6. Formate
7. Butyrate
8. Methylsulfonate
9. Pyruvate
10. Valerate
11. Monochloroacetate
12. Bromate
13. Chloride
36 14. Nitrite
15. Trifluoroacetate
mg/L
5.0
1.5
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
2.5
5.0
5.0
16. Bromide
17. Nitrate
18. Carbonate
19. Malonate
20. Maleate
21. Sulfate
22. Oxalate
23. Tungstate
24. Phosphate
25. Phthalate
26. Citrate
27. Chromate
28. cis-Aconitate
29. trans-Aconitate
mg/L
5.0
5.0
--7.5
7.5
7.5
7.5
10.0
10.0
10.0
10.0
10.0
--10.0
Faster Run Times without Sacrificing Resolution
Inorganic anions separation using a 4 µm capillary column
20
1
2
34
Column:
56
Eluent Source:
Eluent:
Col. Temp.:
Inj. Volume:
Detection:
7 30 µL/min, 2820 psi
25 µL/min, 2430 psi
20 µL/min, 2030 psi
µS
Peaks:
15 µL/min, 1570 psi
10 µL/min, 1140 psi
-15
0
9
Dionex IonPac AS18-4µm,
0.4 × 150 mm
Dionex EGC-KOH (Capillary)
30 mM KOH
30 °C
0.4 µL
Suppressed Conductivity,
Dionex ACES 300
5
Minutes
10
1. Fluoride
2. Chloride
3. Nitrite
4. Sulfate
5. Bromide
6. Nitrate
7. Phosphate
0.2
1
1
1
1
1
2
mg/L
Fast Run on the Dionex IonPac AS18-4µm Column
2
5.5
3
4
1
Dionex IonPac AS18-4µm, 0.4 × 250
Peaks:
1.
2.
3.
4.
5.
6.
7.
5 6
µS
7
-0.5
0
10
Column:
mm
Eluent Source:
Eluent:
Flow Rate:
Inj. Volume:
Col. Temp.:
IC Cube Temp.:
Detection:
1
2
3
Minutes
4
5
Dionex EGC-KOH Cartridge (Capillary)
35 mM KOH
30 µL/min
0.4 µL
30 °C
15 C
Suppressed conductivity,
Dionex ACES 300,
recycle mode
Fluoride
Chloride
Nitrite
Sulfate
Bromide
Nitrate
Phosphate
0.2 mg/L (ppm)
0.5
1.0
1.0
1.0
1.0
2.0
Faster Run Times without Sacrificing Resolution
Inorganic anions separation using a 4 µm Microbore column
3
70
6 8
2 4
1
Column:
Instrument:
7
5
9
0.50 mL/min, 4200 psi
Eluent Source:
Eluent:
Flow Rate:
Inj. Volume:
Column Temp.:
Detection:
0.45 mL/min,3800 psi
µS
Peaks:
0.40 mL/min, 3300 psi
0.25 mL/min, 2200 psi
-20
0
1
2
3
4
5
Minutes
11
6
7
8
9
Dionex IonPac AS18-4µm, 2 150 mm
Thermo Scientific™ Dionex™ ICS-5000+
HPIC™ System
Dionex EGC 500 KOH
23 mM Potassium hydroxide
0.25, 0.40, 0.45, and 0.50 mL/min
5 µL
30 °C
Thermo Scientific™ Dionex™ ASRS™ 300
Anion Self-Regenerating Suppressor™,
2 mm, recycle
1. Fluoride
2. Chlorite
3. Chloride
4. Nitrite
5. Carbonate
6. Bromide
7. Sulfate
8. Nitrate
9. Chlorate
0.5
5.0
3.0
5.0
20.0
10.0
10.0
10.0
10.0
mg/L
Isocratic Separation of Common Anions Using the
Dionex IonPac AS18-4µm Column (4 ×150 mm) at Various Flow Rates
Inorganic anions separation using a 4 µm Standard bore
7
3
column4
1.0 mL/min
6
8
Column:
Dionex IonPac AG18-4µm/AS18-4um
6
2574 psi
2
µS
9
1
5
0
0
2
4 Minutes 6
6
8
10
7
3
µS
4
1.25 mL/min
3332 psi
8
6
2
9
1
5
Peaks:
0
0
2
4 Minutes
6
6
8
10
7
3
µS
1.5 mL/min
3891 psi
8
6
4
2
9
5
1
0
0
12
2
(4 × 150 mm)
Eluent:
23 mM KOH
Eluent Source: Dionex EGC III KOH Cartridge
Flow Rate:
See chromatograms
Inj. Volume:
10 µL
Temperature: 30 °C
Detection:
Suppressed conductivity,
Dionex ASRS 300, AutoSuppression,
recycle mode
4
Minutes
6
8
10
1. Fluoride
2. Chlorite
3. Chloride
4. Nitrite
5. Carbonate
6. Bromide
7. Sulfate
8. Nitrate
9. Chlorate
0.5
5
3
5
20
10
10
10
10
mg/L
Fast Analysis of Drinking Water Using High-Pressure IC
Column:
Instrument:
Eluent Source:
Eluent:
Flow Rate:
Inj. Volume:
Column Temp.:
Detection:
1.8
2
Sample:
Sample Prep.:
5
µS
Peaks:
4
1
3
6
7
0.8
0
1
3
2
Minutes
13
4
5
Dionex IonPac AS18-4µm, 2  150 mm
Dionex ICS-5000+ HPIC system
Dionex EGC 500 KOH
23 mM Potassium hydroxide
0.50 mL/min
5 µL
30 °C
Dionex ASRS 300, 2 mm, 15 mA,
recycle
Municipal City A
5-fold dilution with deionized water
1. Fluoride
2. Chloride
3. Nitrite
4. Carbonate
5. Sulfate
6. Nitrate
7. Chlorate
0.4
2.3
< 0.1
--3.5
< 0.1
< 0.1
mg/L
High Resolution Cation Analysis on IonPac CS16
at Different Flow Rates
Column:
7
Eluant:
Flow rate:
30 µL/min 3600 psi
20 µL/min 2400 psi
4
C
10 µL/min 1200 psi
5
µS
Inj. volume:
Temperature:
Detection:
6
IonPac CS16,
2 x 250 mm x 0.5 mm ID
30 mmol/L MSA (EG)
A: 10 µL/min
B: 20 µL/min
C: 30 µL/min
0.4 µL
40 °C
Suppressed conductivity
CCES 300,
AutoSuppression,
Recycle mode
B
Peaks:
A
1
2
3
-1
0
14
20
Minutes
40
1. Lithium
2. Sodium
3. Ammonium
4. Potassium
5. Magnesium
6. Calcium
0.5 mg/L
2.0
2.5
5.0
2.5
5.0
Capabilities of HPIC in Capillary Format
Increased Capabilities:
• Faster separations with higher flow rates (left)
• Higher resolution with longer columns (right)
Thermo Scientific™ Dionex™
IonSwift™ MAX-100: 11 minutes
4.5
10000:1 Na : Ammonia
5
15,16
24 µL/min – 3900 psi
17
3
µS
67
1
2
45
19
11
12
8
1
13 14
9
10
Single Dionex
IonPac CS16
B
-0.5
0
15
5
Minutes
10
15
-2
2
Two Dionex IonPac
CS16 in series
µS
18
0
1
Minutes
2
16
Using HPIC to Identify Spoilage in Beverages
7
6
Column:
Dionex IonPac AS11-HC-4µm
Capillary (0.4  250 mm)
Eluent Source: Dionex EGC-KOH (Capillary)
Gradient:
Potassium hydroxide,
1 mM from 0 to 8 min, 1-30 mM from
8-28 min, 30-60 mM from 28-38 min,
60 mM from 38-42 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
15 µL/min, 3600 psi
15
9
3
µS
4
10
6
1
2
16
13
8
11
12
Peaks:
14
5
17 19
18
0
0
10
20
Minutes
16
30
42
1. Quinate
2. Fluoride
3. Lactate 
4. Acetate 
5. Formate
6. Unknown
7. Chloride
8. Unknown
9. Malate-Succinate
10. Carbonate
11. Maleate
12. Sulfate
13. Oxalate
14. Unknown* 
15. Phosphate
16. Citrate
17. cis-Aconitate
18. trans-Aconitate
19. Unknown
The Dionex ICS-5000+ HPIC
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
17
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
Thermo Scientific™ Dionex™
IC Cube™ Cartridge
HPIC - High Resolution, Fast Analyses
18
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
19
Advances in Trace Element Analysis
Fergus Keenan
Field Marketing Manager
The world leader in serving science
20
Agenda
• Advances in ICP-OES technology
• High speed analysis
• Advances in ICP-MS
• Intelligent Auto-dilution
• QCell technology
• Trace element speciation by IC-ICP_MS
21
iCAP 7600 ICP-OES
• Powerful analytical detection &
resolution
• Choice of plasma orientation to enable
enhanced application suitability
• Intelligent software for powerful autooptimization of the sample intro system
• Advanced data acquisition including
‘Sprint’ modes for ultimate productivity &
versatility
• Comprehensive accessory compatibility
for liquid & solid sampling
Who’s it for
• Labs requiring the extreme productivity
• Labs who perform highly variable &
demanding research-based applications
• Labs who require solid sampling
capability
22
Open Access Sample Introduction Compartment
• Large fully opening outer door
• Improved user access
• Clear view of plasma source
• Simplifies optimization
• Easy access to sample introduction
• Simple change of components
• Peri-pump
• 12 roller for smooth flow, micro tension control
• Better stability allows shorter dwell times
• Sprint Valve System
• Highest Sample Throughput of any ICP
• Drain Sensor
• Monitors drain, detects leaks or blockages
• Accessories
• Easy connection of Argon Humidifier, Hydride Generation and Laser Ablation
accessories
23
“Better user access, compatible with all accessories”
Sprint valve system – How does it work?
24
Sprint valve system – How does it work?
25
Why segmented stream?
Uptake / Washout Profile with Contiguous Flow
Raised baseline
Long transients
Uptake / Washout Profile with Segmented Stream
Discrete washout steps
True baseline
Sharp transients
26
Case-study – Wear Oil Analysis
Typical Oil Method
Sprint Valve
Oil Method
(already speed-optimized)
Analysis Step
1.Autosampler Movement
2. Sample Uptake
5 sec.
15 sec.
3. Stabilization
20 sec.
4. Measurement
10 sec.
5. Rinse
30 sec.
Total Time
27
Time
Required
80 sec.
Analysis Step
Time
Required
1. Autosampler
Movement, Sample
Uptake, Stabilization,
and Rinse
17 sec.
2. Measurement
10 sec.
Total Time
27 sec.
Intelligently Monitored Wash
10000000
• Software automatically
detects washout to baseline
for selected analytes
1000000
100000
10000
• Non-productive time reduced;
analysis time optimized
1000
100
10
• Washout completed sooner
• Maybe no wash is needed?
28
1
0
20
40
60
80
100
120
140
160
180
200
CASE STUDY: Ultra-Fast Agricultural Soil Analysis
• The soil samples were dried and ground 5 g of sample
• 20 ml of the 1M ammonium acetate solution was added.
• Samples shaken vigorously for at least 5 minutes and left to react
overnight.
• Samples were then shaken again and filtered before being made up to
250 ml with de-ionized water.
• Sample extracts were analysed directly using the Sprint acquisition mode
which further enhances the speed of the instrument.
• A locally sourced soil sample was extracted 5 times & each extract was
analysed 10 times
• The total time required for these 50 repeats was 11 minutes and 35
seconds or 13.9 seconds per sample.
29
Ultra-Fast Agricultural Soil Analysis
30
Ultra-Fast Agricultural Soil Analysis
31
Ultra-Fast Agricultural Soil Analysis
32
Advances in Interference Removal in ICP-MS
The world leader in serving science
33
iCAP Q - Dramatically Different ICP-MS
34
iCAP Q - Dramatically Different ICP-MS
• Easy to use and learn
• Reliability
• New interface cone design giving less memory effects and less drift
• Lower service costs and new longer life detector supplied as standard
• Productivity
• Single mode analysis capability for high throughput and quick flush times with the QCell
• Cost of ownership
• Lower gas consumption per analysis reduces running cost
• Longer life components (cones, detector) reduces lifetime cost
• Service contracts reduced by 30% over XSERIES2
• Performance
• Best Signal /Noise of any Quadrupole ICP-MS on the Market
• Best interference removal with unique QCell technology
• New Leading Edge Design
• Smallest bench space requirements by unique ion optics design
• QCell Flatapole technology for the best in interference removal
• The only quadrupole MS to offer singe mode analysis
35
Spectral Interferences
Caused by molecular species
formed in plasma overlapping with
analyte isotope
ArAr, ArO, ArN,
ArC, ArH, ArCa,
ArNa, ArK, ArMg,
ArCl, ClO, NO,
CO, CaO, NaO,
etc
Products
36
Ar, Air
(O, N, C)
H2O,
Ca, Na,
K, Mg,
Cl, etc
Reaction
Reactants
Collision/Reaction Cell Technology
Collision/Reaction Cell Technology
•
•
•
•
A multipole enclosed in a cylinder
Controlled flow of gas into the cell
Interaction of ions with the gas
If reactive gas used, reactions occur
• All cells are reaction cells
M+ only out
M+ and
XnYn’+
37
The Basis of KED Operation
38
51V+
51[ClO]+
~140 pm
~250 pm
Collisional Energy Loss and Filtering: KED
Energy Barrier
Cell
Post-Cell
Pre-Cell
Small
collision
crosssection M+
Larger
collision
crosssection
MO+
X
Increasing exit energy
Bolder shades indicate higher
energy for M+ and MO+ ions
Key:
He atom
M+ ion
MO+ ion
39
Improving Collision Cell Design
•QCell with low mass cut-off
•Flatapole technology for improved
transmission
•Non-consumable, zero-maintenance
•50% smaller volume for faster mode
switching, <10s
•Single mode interference removal with He
•Can also use reactive mode with O2, H2 or
NH3 mixes
40
QCell – Low Mass Cut-Off KED mode
QCell Mass Cut-Off
Region (here all
masses below 39)
2
Measuring 56Fe
3
41
1
QCell: Effect of Low Mass Cut-Off on in-cell Interference Formation
42
QCell Comparative Performance– He KED mode, No spike
• 5%HNO3, 5%HCl, 1%IPA, 1%H2SO4
43
QCell Comparative Performance– He KED mode, 10ppb Spike
• 5%HNO3, 5%HCl, 1%IPA, 1%H2SO4
+ 10ppb Spike of Li, Be, B, Na, Mg, Al, K, Ca, Sc, Ti, V, Cr,
Mn, Fe, Ni, Co, Ni, Cu, Zn, Ga, Ge, As, Se
Note Co
sensitivity
41,000cps/ppb
44
QCell Comparative Performance– He KED mode, No spike
• 5%HNO3, 5%HCl, 1%IPA, 1%H2SO4, 200ppm Na, 200ppm Ca, 500ppm P
45
QCell Comparative Performance– He KED mode, 10ppb Spike
• 5%HNO3, 5%HCl, 1%IPA, 1%H2SO4, 200ppm Na, 200ppm Ca, 500ppm P
+ 10ppb Spike of Li, Be, B, Na, Mg, Al, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Ni, Co, Ni, Cu,
Zn, Ga, Ge, As, Se
46
Analysis of Selenium
78Se
Sensitivity 8441 cps/ppb
IDL 5ppt
7%H2/He KED
47
Analysis of Vanadium without reactive gases
Sensitivity 2,100 cps/ppb
BEC 24ppt
0.5% HCl, He KED mode
48
Collisional Focusing for High Sensitivity Uranium Measurement
Sensitivity 1223 cps/ppt
IDL 16ppq
Collisional focusing with 7.8mL/min He
49
IC-ICP-MS for Elemental Speciation
The world leader in serving science
50
How can we Perform Speciation Analysis?
Separation
Thermo Scientific Dionex ICS-5000 IC
51
Detection
Thermo Scientific iCAP Q ICP-MS
Why use ICP-MS for Speciation Analysis?
• It can detect most of the periodic
table with sub ppt detection limits
• It has >9 orders of magnitude
linear dynamic range
• The (atmospheric, ground
potential) ICP ion source is easily
connected to a wide range of
coupled accessories:
• Ion Chromatography (IC); Gas
Chromatography (GC); High
performance liquid chromatography
(HPLC)…
• ICP-MS is the ideal elemental
detector for speciation analysis!
52
What are the Advantages of Ion Chromatography?
• Metal-free systems
• Powerful separation
chemistries
• Reagent-Free Ion
Chromatography (RFIC)
• Extensive IC product line for
full flexibility
53
A Complete, Integrated IC-ICP-MS System
• Very simple hardware
connection:
• Simple interchange between
standard ICP-MS analysis
and IC-ICP-MS
• No need to turn off plasma
Inert tubing
0.125 mm i.d.
• A single software interface for
both the IC and ICP-MS:
• Thermo Scientific Chromeleon
interface built into workflow
• Fully integrated analysis
• No trigger cable required
• One sample list
54
Data
System
Speciation of As in Apple Juice
• Differentiation between (toxic) inorganic As(III) & As(V)
species and (non-toxic) organic species (MMA etc)
• Requirements:
• Single run anionic and cationic technique since both positive and
negative charged species can be present in a sample
• Good chromatographic resolution to separate out species
• Sharp peaks for improved sensitivities
55
iCAP Qc with Dionex ICS-5000
• 0.45 ppb of each As standard
• 6 species
• ~8000 cps / ppb
• ~15 minute analysis
• Anion Exchange:
• Dionex AS7 (2x250mm)
• Gradient elution with 20-200 mM
ammonium carbonate
• Flow rate: 0.3 mL/min
• Injection volume: 20 µL
56
As Species Detection Limits by IC-ICP-MS
Compound
57
Detection limit pg g-1
AsB
2.3
DMA
3.8
As3+
4.6
AsC
4.4
MMA
11.4
As5+
1.2
As Species in Apple Juice
58
As Speciation in Apple Juice
• iCAP Qc with Dionex ICS-5000:
• Anion exchange chromatography
AsB
DMA
As(III)
AsC
MMA
As(V)
Sum of Species
Total As
0.002
0.004
0.005
0.004
0.011
0.001
-
0.005
Juice 3
ND
ND
0.5 ± 0.01
ND
ND
0.7 ± 0.01
1.2
1.7 ± 0.05
Juice 4
ND
0.4 ± 0.05 0.3 ± 0.01
ND
0.1 ± 0.05 0.7 ± 0.01
1.5
1.8 ± 0.05
MDL
• iCAP Qc benefits:
• Low method detection limits: 0.001 and 0.01 ng/g per species, 0.005
ng/g total As vs current EPA MCL (maximum contaminant level) is 10
ng/g in drinking water
59
IC-ICP-MS analysis of As in Organic Brown Rice Syrup
• Media reports and scientific publications
on the determination of arsenic (As) in
foodstuffs have sparked renewed
interest from consumer groups and
politicians leading to responses from
national regulatory bodies.
• Following the publication of a report on
high As levels in organic brown rise
syrup the United State Food and Drug
Administration (FDA) stated that it was
carrying out a study on As in rice and
rice products that is due to report later
in 2012.
60
Analysis of As in rice syrup
• Three different OBRS samples were sourced and prepared for
analysis.
• A closed microwave digestion method was used.
• Preparation of the OBRS samples for As speciation analysis was
achieved by taking 1.5 g of OBRS, adding 15 mL of 0.28 M HNO3 and
refluxing for 90 minutes.
61
Speciation of As in OBRS
• IC-ICP-MS speciation analysis showed that the predominant As
species in the OBRS samples tested was the toxic inorganic As(III) with
over 80% of the total arsenic concentration
• (equivalent to 86 – 109 ng /g As (III)).
62
iCAP Q - Dramatically Different ICP-MS
63
Summary
• iCAP 7600 is the fastest ICP-OES system available
• With the iCAP Q ICP-MS is completely automated from
standard prep to sample dilution and automated
interference free analysis
• The patented QCell combines low mass filtering with
Collision Reaction Cell Technology for best-in-class
interference removal
• Ion Chromatography is for elemental speciation studies due
to it inert metal free pathway and comprehensive method
set for metal ion and organo-metallic separations
64

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