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DUAL VIEW ICP-OES
MINUS THE WAIT
Introducing the Agilent 5100 ICP-OES
Ross Ashdown
MP-AES & ICP-OES
Product Manager
October 15, 2014
3
Dual View Minus the wait
Agenda
Highest throughput with highest performance
• What is the 5100 ICP-OES?
• How does the 5100 work?
•
Key benefits
• Analytical performance and applications
Agilent 5100 Synchronous Vertical Dual View ICP-OES
4
Dual View Minus the wait
Agenda
Highest throughput with highest performance
• What is the 5100 ICP-OES?
• How does the 5100 work?
•
Key benefits
• Analytical performance and applications
Agilent 5100 Synchronous Vertical Dual View ICP-OES
5
Concept
Make ICP-OES easier to use, cheaper to run and maintain,
without compromising analytical speed or performance.
• New software and sample introduction components
• New high specification hardware platform
Agilent Confidential
October 15, 2014
6
What is the 5100 Synchronous Vertical Dual View
(SVDV) ICP-OES?
Vista Chip II CCD
High Speed Pump
Agilent Confidential
October 15, 2014
7
What is the 5100 Synchronous Vertical Dual View
(SVDV) ICP-OES?
DSC
Mode Selector
Agilent Confidential
October 15, 2014
8
What is the 5100 Synchronous Vertical Dual View
(SVDV) ICP-OES?
SSRF
Services
Vertical Torch
Agilent Confidential
October 15, 2014
9
Dual View Minus the wait
Agenda
Highest throughput with highest performance
• What is the 5100 ICP-OES?
• How does the 5100 work?
•
Key benefits
• Analytical performance and applications
Agilent 5100 Synchronous Vertical Dual View ICP-OES
10
How does the 5100 work?
Cool Cone Interface
Snout
Agilent Confidential
October 15, 2014
11
How does the 5100 SVDV with DSC technology work?
Patented DSC technology for ICP-OES provides DV without compromise.
• Single reading of the plasma for both radial and axial.
• Vertical torch gives high matrix capability
Dichroic
Spectral
Combiner
(DSC)
Mirror
To detector
Vertical
torch
Hole
5100 SVDV Mode Selector
DSC
5100 SVDV Pre-optics
October 15, 2014
12
Future Proof Your Lab
5100 SVDV ICP-OES is 4 instruments in 1
1. Synchronous VDV Mode
2. Radial Mode
3. Axial Mode
+
RAD
AX
4. Conventional Simultaneous Dual View Mode
October 15, 2014
13
Dual View Minus the wait
Agenda
Highest throughput with highest performance
• What is the 5100 ICP-OES?
• How does the 5100 work?
•
Key benefits
• Analytical performance and applications
Agilent 5100 Synchronous Vertical Dual View ICP-OES
14
Benefits of the 5100
Lowest cost
of ownership
• Fastest sample
throughput of difficult
samples
• Low gas consumption
October 15, 2014
15
Benefits of the 5100
Lowest cost
of ownership
• Fastest sample
throughput of difficult
samples
• Low gas consumption
Enhanced
Performance
• Analytical
performance
• System robustness
and reliability
October 15, 2014
16
Benefits of the 5100
Lowest cost
of ownership
• Fastest sample
throughput of difficult
samples
• Low gas consumption
Enhanced
Performance
• Analytical
performance
• System robustness
and reliability
Simple
Operation
• Software
• Hardware
October 15, 2014
17
1. Lowest cost of ownership
• High throughput facilitates low Ar consumption per sample
- (a) DSC. (b) VistaChip II. (c) 80 rpm pump. (d) SVS 2+
•
•
•
•
50% Lower power and 50% lower exhaust requirements.
27MHz Solid State RF
Robust vertical torch
Increased self maintainability
Vendor Vendor
SVDV
A
B
USEPA 200.7 (min)
Ar L/sample
Valve/No Valve
0.97
2.3
2.3
20
38
43
Valve
Valve
Valve
Ar/sample
50
45
40
35
30
25
20
15
10
5
0
5100 SVDV
Vendor A
Vendor B
October 15, 2014
18
2. Enhanced Performance
Long Term Stability
•
4Hr Long Term Stability with complex matrix
•
25% NaCl spiked with 250 ppb multi-element solution
•
<2.4% RSD
140%
250ppb As/Se/Pb/Cd solution in 25% NaCl
120%
% Readback
100%
80%
60%
40%
20%
0%
0:00:00
0:28:48
0:57:36
1:26:24
As 188.980
1:55:12
2:24:00
Time (h:mm:ss)
Cd 228.802
Pb 220.353
2:52:48
3:21:36
3:50:24
4:19:12
Se 196.026
October 15, 2014
19
3. Simple Operation
• Plug-and-play torch and SIS
• Enhanced user maintainability
- Pre optic window (axial and radial)
- Optics gas filter
October 15, 2014
20
3. Simple Operation
• ICP Expert software
- Intuitive workflow
- Trend monitoring of argon
backpressure to the nebulizer
and argon emission per
sample
• e-Familiarization DVD videos
- Software
- Hardware
- Routine Maintenance
October 15, 2014
21
Dual View Minus the wait
Agenda
Highest throughput with highest performance
• What is the 5100 ICP-OES?
• How does the 5100 work?
•
Key benefits
• Analytical performance and applications
Agilent 5100 Synchronous Vertical Dual View ICP-OES
22
Agilent 5100 ICP-OES
Animal Food Product Application
October 15, 2014
23
Analysis of Animal Food Products using the Agilent
5100 ICP-OES SVDV
• Elemental Analysis on animal food products – nutrient, micro
nutrient and toxic elements.
• Requirements of food and agriculture samples with ICP-OES
analysis:
•
High throughput capability
•
Large linear dynamic range
•
Instrument sensitivity
•
Easy to use
Experimental – Trace metals in meat sample
Instrumentation
Instrument:
Agilent 5100 ICP-OES SVDV
Sample Introduction System: Seaspray with Double Pass G/C
Sampling:
SPS3 Autosampler
Software:
ICP Expert V7
Agilent 5100 SVDV ICP-OES
SVDV sample
introduction
Agilent SPS3
ICP Expert V7
October 15, 2014
25
Sample Preparation
• NBS 1577 Bovine Liver SRM
• 0.5g/50ml 6ml HNO3 and 1ml H2O2 microwave digest.
• Final acid concentration 12% v/v
• Spike recovery also performed on elements that were <MDL
Ethos One
Microwave Digester
October 15, 2014
26
Instrument Operating Conditions
Instrument Parameter
Setting
Read Time
10s
Replicates
3
Sample uptake delay
20
Stabilization time
10 sec
Rinse time
30 sec
Fast Pump (80 rpm)
On
RF power
1.20 kW
Aux flow
1.0 L/min
Plasma Flow
12.0 L/min
Nebulizer flow
0.70 L/min
October 15, 2014
27
Calibration curve for Na 589 line with SVDV
Agilent 5100 ICP-OES wavelengths and calibration
parameters selected for analysis.
Element
Wavelength (nm)
Correlation Coefficient
Background Correction
K
766.491
0.99966
Linear
Na
589.592
0.99978
Linear
Fe
238.204
0.99999
Linear
Cu
327.395
1.00000
Linear
Zn
213.857
1.00000
Linear
Mn
257.610
0.99998
Linear
Se
196.026
1.00000
Linear
Pb
220.353
0.99999
Linear
Cd
228.802
1.00000
Linear
As
188.980
1.00000
Linear
Ca
396.847
0.99997
Linear
Co
238.892
0.99999
Linear
Mg
279.078
0.99968
Linear
Mo
202.032
1.00000
Linear
Ag
328.068
1.00000
Linear
TI
190.794
1.00000
Linear
October 15, 2014
29
Results for Standard Reference Material 1577
Element
MDL
(mg/kg)
Measured
Values
(mg/kg)
SD
Certified
Value
(mg/kg)
SD
%Recovery
K 766
7.80
9832
5.2
9700
0.06
101
Na 589
9.08
2410
2.9
2430
0.013
99
Fe 238
0.17
258
1.9
270
20
96
Cu 327
0.16
203
1.1
193
10
105
Zn 213
0.33
131
0.56
130
10
901
Mn 257
0.008
9.8
0.01
10.3
1.0
96
Cd 228
0.13
0.26
0.02
0.27
0.04
96
October 15, 2014
30
Results for Standard Reference Material 1577
The following values are not certified:
SD
Certified
Value
(mg/kg)
%Recovery
0.16
123
103
603
2.4
605
100
0.18
3.4
0.05
3.2
106
0.01
0.142
0.002
0.140
102
Element
MDL
(mg/kg)
Ca 396
6.0
Mg 279
0.83
Mo 202
Sr 407
Measured
Result
(mg/kg)
126
October 15, 2014
31
Results for Bovine Liver Matrix
Spiked with 100 ppb Standard
Element
MDL
(ppb)
Spike
Recovered
Values
(ppb)
SD
Spike Added
(ppb)
% Spike
Recovery
Pb 220
4.8
109
0.003
100
109
Se 196
8.5
103
0.001
100
103
Co 238
2.0
110
0.002
100
110
Ag 328
2.1
107
0.001
100
107
As 193
36
96
0.004
100
96
As 188
12
99
0.004
100
99
Tl 190
7.7
103
0.001
100
103
October 15, 2014
32
Results
• Synchronous analysis of low concentration micronutrient and
toxic elements were performed with higher concentration
nutrient elements.
• Excellent linearity was displayed for Na and K nutrient
elements when measuring synchronously with the
micronutrients and toxic elements.
• All recoveries were within 10% of certified concentration.
October 15, 2014
33
Agilent 5100 ICP-OES
Environmental Application
October 15, 2014
34
Analysis of Environmental Samples using the Agilent
5100 ICP-OES SVDV
• Elemental Analysis on water samples
Measurement challenge:
How to improve sample throughput when measuring water samples,
according to the US EPA 200.7 method: “Determination of Metals and
Trace Elements in Water, Solids and Biosolids by ICP-AES?
Solution
Using the Agilent 5100 Synchronous Vertical Dual View ICP-OES,
fitted with a Switching Valve System and an autosampler allowed the
analysis of a sample every 58 seconds, with excellent recoveries and
measurement stability and a 50% reduction in argon consumption.
October 15, 2014
35
Experimental
Instrumentation
Agilent 5100 Synchronous Vertical Dual View ICP-OES
Fitted with:
• Seaspray nebulizer
• Single-pass glass cyclonic spray
chamber
• White-white pump tubing
• Standard 1.8 mm injector torch
Agilent 5100 Synchronous Vertical Dual View ICP-OES
October 15, 2014
36
Experimental
Instrumentation
Accessories:
• SVS 2+ Switching Valve System reduces sample uptake, stabilization
times, and rinse delays.
• SPS 3 autosampler
October 15, 2014
37
Experimental
Operating parameters
Table 1. Agilent 5100 SVDV operating parameters
Parameter
Setting
Read time (s)
20
Replicates
2
Sample uptake delay (s)
0
Stabilization time (s)
10
Rinse time (s)
0
Pump Speed (rpm)
12
Fast pump (rpm)
off
RF power (kW)
1.50
Aux flow (L/min)
1.0
Plasma flow (L/min)
12.0
Nebulizer flow (L/min)
0.7
Viewing height (mm)
5
Background correction
Off‐Peak
October 15, 2014
38
Experimental
Operating parameters
Table 2. Agilent SVS 2+ Switching Valve System settings
Parameter
Setting
Sample loop size
(mL)
Loop uptake delay (s)
1.0
Uptake pump speed (rpm) - refill
355
Uptake pump speed (rpm) – move
355
Uptake pump speed (rpm) – inject
100
Time in sample (s)
6.6
Bubble inject time (s)
6.8
7.0
October 15, 2014
39
Experimental
Samples and sample preparation
•
Standards were prepared from single element standards and diluted
with 1% HNO3.
• 2 x trace metals in drinking water (TMDW) Certified Reference Materials
(CRM)* were analyzed:
• TMDW-A
• TMDW-B
Inter Element Corrections were used for interference correction
* Purchased from High Purity Standards, Charleston, South Carolina, USA.
October 15, 2014
40
Experimental
Method
•
•
Sample analysis was performed as per
US EPA method 200.7
Long term stability was also measured
according to US EPA method 200.7
October 15, 2014
41
Results and discussion
Linear Dynamic Range
•
•
•
The Vista Chip II CCD detector provides 8 orders of linear dynamic range
The synchronous measurement of axial and radial plasma views also aids
the upper concentration limit for each analyte.
Excellent upper concentration limit results were achieved for Na & K,
which the 5100 automatically measured in radial mode and for the
elements (particularly Mg, Ca, and Al) it automatically measured in axial
mode.
Table 3. Upper concentration limits for the 5100 SVDV ICP-OES. All measurements were determined in one analytical run.
Note: LDR for other elements listed in full application note.
Element
Al 308.215
Ca 315.887
K 766.491
Mg 279.079
Na 588.995
Linear Dynamic Range (ppm)
200
100
200
500
500
October 15, 2014
42
Results and discussion
Method Detection Limits
•
•
Excellent detection limits were obtained for the elements selected by the
instrument to be measured in the axial view e.g. As, Pb, and Se.
In the same measurement, detection limits for K and Na were equivalent
to those from a typical radial measurement.
Table 3. Method detection limits, acquired per EPA Method 200.7. All MDLs were determined in one analytical run.
Note: MDR for other elements listed in full application note.
Element
As 188.980
K 766.491
Na 588.995
Pb 220.353
Se 196.026
Method Detection Limit (ppb)
3.7
21.6
10.1
1.9
3.2
October 15, 2014
43
Results and discussion
Recoveries
•
•
The average of 7 analyses of 2 certified reference materials show
excellent recoveries for all elements
Demonstrates that the instrument can analyze trace elements in axial
view & measure Na and K at high levels in radial view – at the same time
Table 3. Recovery of elements in two CRMs. All analytes were determined in one analytical run.
Note: Data for other elements listed in full application note.
Element/
wavelength
(nm)
Al 308.215
Ca 315.887
Mg 279.079
K 766.491
Na 589.592
CRM-TMDW- A
Certified Measured
(μg/L)
(μg/L)
SD
125
31000
8000
2500
2300
15.7
423
54.8
19.6
24.9
131.0
31573
8175
2563
2412
Recovery
(%)
CRM-TMDW-B
Certified Measured
(μg/L)
(μg/L)
SD
Recovery
(%)
105
102
102
103
105
125
31000
8000
2500
22000
4.8
334
62.3
35.0
272
100
101
100
102
103
125.2
31411
8015
2561
22678
Axial
Radial
October 15, 2014
44
Results and discussion
Sample throughput
•
The Synchronous Vertical Dual View capability
of the 5100 measures both the axial and the
vertical view of the plasma at the same time
•
1 sample measurement = 58 seconds and
consumed < 21 L argon
•
This is 55% faster than conventional dual view ICPOES instruments, with approx 50% less argon
consumption per sample
October 15, 2014
45
Conclusion
Water samples were analyzed as per US EPA method 200.7, using the
Agilent 5100 SVDV ICP-OES with sample introduction accessories.
The study found that:
• The 5100 delivered accurate results in 58 seconds per sample.
• The 5100 consumed less than 21 L of argon per sample
• Excellent method detection limits in the μg/L (ppb) range were
obtained for all elements in a single run.
• Good recovery results for 26 elements in two CRMs were achieved
• Stability better than 1.3% for all elements during a 12 hour period
Comparing the results to those published by other ICP-OES
manufacturers allows us to calculate that the 5100:
• is up to 55% faster than dual view instruments
• consumes approx 50% less argon than dual view instruments
To find out more, visit agilent.com/chem
October 15, 2014
46
Agilent 5100 ICP-OES summary
Lowest cost of
ownership
Enhanced
Performance
Simple Operation
October 15, 2014
47
Questions
Visit us at www.agilent.com/chem/DualViewMinusTheWait
•
Technology Video
•
Application Notes
•
Technical Overviews
•
Agilent’s Atomic Spectroscopy Portfolio of Solutions
October 15, 2014
48