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ICP-OES methods
E-book
How to optimize your
ICP-OES methods
E-book
With the increasing sophistication of instrument software, it can be difficult to keep up with all
the powerful functionality that’s built in–functionality that could be making your life easier.
Here are the top 9 functions you should know about.
Moreover, find in this ebook how the ICP Expert Software features an array of flexible
performance and productivity enhancements that add more power to your ICP-OES analyses.
Now you can get the right results every time and :
Discover how with the 9 Tips to optimize your ICP-OES methods and a selection of
ICP Expert technical notes.
How to optimize your
ICP-OES methods
9 tips to make you more efficient
(and get the right results)
9 tips to make you more efficient
(and get the right results)
Setting the rinse time in a method can be tricky. If the sample rinse time
in your method is too short, you risk introducing carryover. Residual
Use dynamic rinse
liquid from the previous sample will impact the accuracy and precision
1 times to slash
sample-to-sample
of the next sample. Conversely, if the sample rinse time is too long,
then you are wasting time and rinse solution.
run time
Use a dynamic rinse control function that automatically adjusts the rinse time
to suit the concentration of each sample. Typically, these functions monitor
the signal to detect when all the sample has been rinsed out. When it reaches
a user-defined threshold, the instrument moves to the next sample.
Labs often run only a limited number of methods on each ICP-OES. You
3 valve to run more allows sample to be loaded while the rinse solution is pumped into the sample
samples with higher introduction system. Using a switching valve eliminates delays between rinsing
accuracy and sample measurement, saving time and gas and improving precision, and
stability. There are even models with extra ports to enable online addition of
internal standards. A fully integrated switching valve is the best choice as it
can then be controlled within the instrument method.
9 tips to make you more efficient
(and get the right results)
If you have multiple analysts using the same ICP-OES, consistent torch
alignment may be a problem. The process of removing a torch and getting
If you are receiving samples from new customers, or new sources, they
may contain unexpected interferences, which can cause major headaches.
5 Identify unexpected
interferences before
Identifying and correcting for interferences is critical for ensuring accuracy—
but it often requires the skills of an experienced spectroscopist. Look for
they impact results
functionality in your instrument software that manages interferences by
dynamically adjusting background correction points. Typically, this is based on
a spectrum of the sample, which highlights any potential interferences.
Figuring out what went wrong when you get an inaccurate analytical result
can be challenging. Fortunately, there are software functions available that
Troubleshoot
6
take a snapshot of each sample scan during the analysis. You can quickly
erroneous results
review a sample scan to see what might have caused the error—the problem
without re-analysis
might be interference from another element or elements at unexpectedly
high concentrations. Sometimes, you can reprocess the data from that sample
scan to deliver a correct result, without rerunning the sample.
9 tips to make you more efficient
(and get the right results)
7 wavelength to lifesaver when you have high-matrix samples with substantial interferences,
confirm sample as it gives you confidence that you can use data from another wavelength
results if things don’t work out with the primary one. Collecting data from multiple
wavelengths per element is also useful for routine samples. You can use the
data from each line to compare the reported concentration of the element. If
the concentrations match up, you’re assured that the result is correct.
Occasionally a run has been going for some time when you notice a decrease
in sensitivity. Many instruments have built-in diagnostic tests to help identify
8 Use the instrument
test tools what might be going wrong. Simply stop the run, run the tests, and use the
results to guide you in troubleshooting the problem.
Hitting the top of your calibration range can force you to dilute and rerun samples.
There’s functionality available that allows you to monitor two or more
wavelengths of different sensitivities for each element. If you suffer an
Technical Overview
Introduction
The Agilent 5110 ICP-OES provides fast sample analysis, using less gas,
without compromising on performance for tough samples. It has been
designed for ease-of-use, with this philosophy driving the design of both the
hardware and the ICP Expert software that controls the instrument.
The ICP Expert software features a clear, logical The Agilent SPS 4 Autosampler is fully controlled
workflow that simplifies analyses, even for experienced through ICP Expert software. The user can select
users. To set up and perform an analysis, you simply the sample rack type, rinse pump control speed and
follow the sequence of pages in the displayed order. control the probe through the autosampler window or
The current page is highlighted to provide full visibility autosampler tab in ICP Expert. Control of the IsoMist
of your progress in the workflow (Figure 4). programmable temperature controlled spray chamber is
also fully integrated into the ICP Expert Software.
Video help
Figure 6. The parameter calculator and setup conditions for the AVS 6/7
Switching Valve makes instrument setup and method development easy.
Intelligent Rinse
The Intelligent Rinse software function is available
in the ICP Expert Software Pro pack. It monitors the
intensities of nominated element wavelengths during
the rinse period, automatically ending the rinse when
these intensities reach a threshold. The threshold is
Figure 5. On demand help videos for sample introduction system components based on which rinse setting you select: Thorough,
and routine maintenance tasks.
Moderate, or Quick. This allows the rinse period to
vary, depending on the time taken to wash out each
individual sample. This improves sample throughput
whilst preserving the accuracy of results.
3
Integrated control of ESI prepFAST™ IntelliQuant Calibration Kit. For full flexibility, a custom
IntelliQuant calibration can be measured and stored for
The 5100/5110 ICP-OES can be coupled with the ESI particular sample matrices, such as organic solvents.
prepFAST autodilution system. This will enable the Any updated or new IntelliQuant calibration is measured
following labour saving functions: in the standard quantitative analytical sequence,
meaning no separate analyses or additional worksheets
• Multipoint calibration from a single stock are required.
standard—no need to manually make up standards,
saving time and avoiding mistakes The IntelliQuant interface features a periodic table heat
map that shows which elements have been found in a
• Automatic overange dilution—when a sample is sample and their approximate concentration (Figure 7).
detected as being outside the calibration range, a
dilution will automatically be performed
Agilent’s IntelliQuant is a feature in the ICP Expert Figure 7. IntelliQuant generates a heat map to visually present the relative
concentrations of elements present in a sample.
software that identifies and calculates an approximate
concentration (semi-quantifies) of up to 70 elements
in a sample. This enables users to quickly check the A full wavelength spectrum (Figure 8) is also displayed
approximate concentration of many elements in their after the scan, providing more information about the
sample, without any changes to the method or preparing elements present and any potential interferences. You
additional multi-element standards. IntelliQuant can zoom in on the spectrum for further detail. Changes
measurements can be performed with every analysis. can be made to the IntelliQuant setup with results
For stored calibrations, simply activate IntelliQuant and reprocessed in real-time, saving valuable time during
select the stored IQ calibration file before running an method development or analysis.
analysis.
4
Figure 8. The IntelliQuant interface displays the full wavelength scan of the sample (top) and a detailed spectrum view of any selected wavelength range from
the full scan, which includes labeled element peaks (bottom)
Correction options to suit any situation FACT provides real-time spectral correction by
using an advanced spectral modelling technique
The Agilent ICP Expert software provides many choices to mathematically deconvolute (i.e. separate) the
of correction options for both background or spectral analyte signal from the raw spectrum. Models
interferences: are built by measuring the expected components
separately and the response for each. This typically
• Fitted background correction: utilizes a includes measuring a blank solution, a pure
sophisticated mathematical algorithm to model analyte solution and pure interferent solutions.
the background signal under the analyte peak and Figure 9 displays a FACT model being applied to
is applied simultaneously upon measurement of Cd 214.439, with Fe interferent, with FACT being
the analyte peak, providing fast, easy and accurate able to mathematically separate the two peaks to
background correction. ‘Fitted’ not only provides accurately measure the analyte signal.
accurate correction of both simple and complex For overlapping interferences that cannot be
background structures, it also requires no method resolved using Fitted background correction or
development. FACT, Inter-element correction (IEC) is available.
Figure 10. Background correction options are flexible and easily edited post-
analysis, recalculated in real-time.
Figure 13. View the interactive Instrument Status page to check the current
status of the instrument and identify causes of problems
References
completion of the test cycle, a report in PDF format can Published October 1, 2017
Publication number: 5991-7720EN
be exported.
Rapid sample screening and simplified
method development with IntelliQuant
Technical Overview
Introduction
In addition to routine quantitative elemental analyses using ICP-OES,
analytical laboratories often want to quickly identify other elements in their
samples. For example:
• Food testing labs analyzing a routine set of elements want to be aware
of the presence of additional elements that may be of concern from a
quality control perspective
For full flexibility a custom IntelliQuant calibration can A full wavelength spectrum (Figure 2) is also displayed
be measured and stored. This calibration can be fully after the scan, providing more information about the
customized to contain any set of elements over the elements present and any potential intereferences. You
desired calibration range. can zoom in on the spectrum for further detail.
2
Figure 2. The IntelliQuant interface displays the full wavelength scan of the sample (top) and a detailed spectrum view of any selected wavelength range from
the full scan, which includes labeled element peaks (bottom).
3
Example analysis Table 1. IntelliQuant semi-quantitative recoveries for elements in two food
CRMs.
Five pre-digested Certified Reference Materials (CRMs), Orchard Leaves Powdered Milk Solution
representing a range of sample types were analyzed (CRM-OL) (CRM-MP)
using IntelliQuant on an Agilent 5110 SVDV ICP-OES. Element & CRM IntelliQuant CRM IntelliQuant
wavelength Value Value Value Value
Results were obtained using an updated IntelliQuant (nm) (µg/mL) (µg/mL) (µg/mL) (µg/mL)
calibration, with the IntelliQuant Calibration Kit multi- Aluminum
element standards being measured on the instrument 237.312 3 3 0.02 –
during a standard analytical run. All measurements were Arsenic
188.98 0.1 0.07 0.002 –
taken in the Synchronous Vertical Dual View (SVDV) Barium
mode of the instrument. 614.171 0.5 0.5 – –
Cadmium
214.439 0.001 – – –
Semi-quantitative recoveries for all elements in the food
Calcium
CRMs are shown in Table 1. Results for environmental 318.127 200 204 130 136
CRMS are shown in Table 2. IntelliQuant’s retrospective Chromium
wavelength selection capabilities were utilized to avoid 205.56 0.03 0.03 0.0003 –
spectral interferences and achieve optimum semi- Cobalt
230.786 0.002 – 0.0004 –
quantitative accuracy. Copper
213.598 0.1 0.09 0.007 –
By changing the wavelengths used to estimate Iron
the concentrate of those elements that were being 273.358 3 3 0.02 –
Lead
impacted by interference, it was possible to achieve 217.000 0.5 0.5 0.002 –
recoveries for almost all measured elements in the five Magnesium
CRMs within ± 20% of the certified value. The accuracy 277.983 60 57 12 12
of these results demonstrate IntelliQuant’s potential as Manganese
293.931 1 1 0.003 –
an extremely useful rapid screening tool. Nickel
231.604 0.01 – – –
References Phosphorus
177.434 20 20 100 99
Potassium
CCD and CID solid-state detectors, Agilent publication 766.491 150 140 170 153
5991-4854EN, (2014). Selenium
196.026 0.0008 – 0.001 –
Silicon
243.515 5 7 – ––
Sodium
589.592 1 1 50 44
Vanadium
311.837 0.005 – – –
Zinc
334.502 25 30 0.5 0.6
4
Table 2. IntelliQuant semi-quantitative recoveries for elements in three environmental CRMs.
5
www.agilent.com/chem
Agilent shall not be liable for errors contained herein or for
incidental or consequential damages in connection with
the furnishing, performance or use of this material.
Benefits of Agilent's Intelligent Rinse Intelligent Rinse* maximises throughput by optimising the rinse
–– Shorter rinse durations between time between samples
samples When setting up an ICP-OES method, you are normally forced to specify a
–– Increased sample throughput rinse time that will suit your highest concentration samples. This rinse time is
–– Simplified method setup–no need then used for all samples, even those with much lower concentrations of the
to accurately predict required rinse analytes.
durations
Rinse times depend on several factors, such as the type and length of the
sample introduction tubing, the specific sample introduction components
used and the nature of the samples and elements being analysed. As
shown in the figure, samples with low concentrations of an element take a
shorter time to wash out than higher concentrations—with over two minutes
difference between the highest and lowest concentrations shown. If your
samples have a large variation in concentrations, using the same rinse time
for each can add considerable time to the analytical run.
Agilent's Intelligent Rinse software function monitors the intensities of
nominated element wavelengths during the rinse period, automatically
Agilent's Intelligent Rinse function adjusts rinse ending the rinse when these intensities reach a user-specified threshold. This
time, based on the time taken to wash out each
element in your sample. In this example, Intelligent allows the rinse period to vary, depending on the time taken to wash out each
Rinse saved over two minutes of unnecessary individual sample. This increases sample throughput whilst preserving the
rinse time when measuring samples at the low end
of the calibration compared with those at higher
accuracy of results.
concentrations.
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