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FIELD APPLICATION REPORT

ICP-OPTICAL EMISSION

Iron Ore Sample Analysis in the

Presence of High Dissolved Solids
Using the Optima ICP

Authors:
Cynthia P. Bosnak

Perkin Elmer Life and

Analytical Sciences
710 Bridgeport Avenue
Shelton, CT 06484

In tr od uct io n

A steel company must monitor iron ore samples from a mining operation continuously, 24 hours a day, 7 days a week. Prior
to analysis by inductively coupled plasma (ICP), the iron ore samples are solubilized using a fusion process. This procedure
produces solutions that have high levels of dissolved solids. Additionally, to guarantee product quality, very tight quality
control limits, as low as ±2% for some analytes, are required.

This workload requires that the ICP system used must run continuously while meeting these strict QC requirements. Also,
there must be very little downtime required for performing instrument maintenance. The Optima™ 4300 DV ICP system is
capable of meeting these rigorous requirements.

Figure 1. Optima 4300 DV ICP system.

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Ex pe riment al

Instrument
The Optima 4300 DV ICP system (Figure 1) equipped with an AS-93plus autosampler (Figure 2), which includes an
integrated rinse pump, was used for this analysis. The demountable torch cassette included a baffled, cyclonic spray chamber
with a low-flow GemCone™ nebulizer, a 2.0 mm quartz injector, and a single-slot, quartz torch (Figures 3-4).

Figure 2. AS-93plus autosampler. Figure 3. Demountable torch cassette.

Figure 4. Sample introduction system. Figure 5. GemCone nebulizer.

The GemCone nebulizer (Figure 5) has a large sample orifice that resists clogging. It is made from a corrosion resistant
PEEK material to tolerate high acid concentrations.

The adverse effects from high dissolved solids can be very pronounced when analyzing these samples by inductively coupled
plasma. Some mechanisms used to minimize these effects are:

• Shear gas
• Manual integration mode
• 2mm quartz injector
• Dilute aqua regia rinse solution
• High plasma gas flow
• Torch position set to -3mm

Figure 6. Effect of shear gas.

To eliminate the adverse effects of the cooler tail plume of the plasma, the Optima ICP systems use a shear gas (Figure 6).
This minimizes the possibility of corrosion or sample deposition on the optical system components. The shear gas also limits
the “self-absorption” zone to provide longer linear dynamic ranges and minimizes matrix effects for axial viewing.

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The use of manual integration mode provides the simultaneous integration of the analytes and internal standard in a very
short analysis time. Please note: Manual integration should be used with caution. The integration time should typically be
at least 100 msec to prevent data acquisition errors.

The use of a 2.0 mm quartz injector provides less heat transfer from the plasma to reduce the amount of solids buildup in the
injector tip.

A 5% v/v aqua regia (HNO3/HCl) solution containing 0.01% Triton X-100 is used to rinse between each sample. This helps
to decrease the solids buildup in the injector and torch.

A higher plasma gas flow of 20 L/min narrows the shape of the plasma and lessens the solids buildup on the torch (Figures 7-
8). This permits a longer time between cleanings of the torch and gives a longer torch lifetime.

Figure 7. Plasma gas flow 15 L/minute. Figure 8. Plasma gas flow of 20 L/minute.

The torch position greatly influences the amount of solids that build up on the injector and torch. It is important to use a
position of -3 mm to produce a gap between the plasma and the injector tip. This ensures less heat transfer and reduces the
amount of solids buildup. By using the demountable torch cassette, it is easy to reproducibly set the torch to the same
position each time (Figures 9-11).

Figure 9. Torch position setting. Figure 10. Plasma at 0 mm torch position. Figure 11. Plasma at -3 mm torch position.

Sample Preparation
The iron ore sample (0.4 g) is placed in a platinum crucible and 0.5 g NaNO3, 3 g LiBO2, and 4 mL saturated KI solution is
added. The sample is then fluxed using a Claisse Fluxer and a fusion pellet is formed. The sample is transferred to 100 mL
of 10% HNO3, stirred for 5 minutes, and then placed into a cool water bath which brings it to room temperature in about 5
minutes. Yttrium internal standard is added and the sample is diluted up to 200 mL final volume with deionized water. This
solution is directly analyzed on the Optima 4300 DV ICP system.

Standards
Certified iron ore reference standards are used for calibration and are prepared in the same manner as the samples.

Result s

Quality Control
Quality control reference materials are prepared in the same manner as the samples and standards. These solutions are
analyzed every ten samples. The QC tolerance within the run is ±2% for some analytes. Table 1 lists the recoveries of some
key analytes while Table 2 details the instrument conditions and method parameters.

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T ab l e 1 . A n a l yt e R eco ve r i es T ab l e 2 . M et h od P ar a met ers
Conc. QC
Elements/Wavelengths Function
Ana ly te ( wt %) L i m it s
Si 251.611 nm Analyte
SiO2 4.01 3.93-4.09 Al 308.215 nm Analyte
Al2O3 0.07 0.04-0.10 Ca 317.933 nm Analyte
Mg 285.213 nm Analyte
CaO 3.78 3.70-3.86 Mn 257.610 nm Analyte
MgO 1.19 1.11-1.29 Y 371.029 nm Internal Standard
Mn 0.09 0.04-0.14 Manual Integration
0.1 second Integration time
2.0 seconds Read time
Plasma Parameters
Plasma gas 20 L/min
Auxiliary gas 0.5 L/min
Nebulizer gas 0.7 L/min
Power 1450 Watts
Viewing distance 15 mm
Plasma View Radial
Sample flow rate 2.00 mL/min
Sample flush time 15 seconds
Sample flush rate 2.5 mL/min
Sampler wash parameters 15 seconds, after every sample

Peak Processing
Peak Algorithm Peak Area, 3 points/peak
Spectral Correction 2-Point Background Correction
Internal Standard Yttrium, Assigned to All Analytes
Calibration Equation Linear, Calculated Intercept
Standard/Sample Units Wt%

Co nc lus ion

The Optima 4300 DV ICP system is capable of performing very high precision analyses even in the presence of high
dissolved solids during a long analysis. The effects of high dissolved solids are overcome by using a combination of shear
gas, manual integration mode, a 2.0 mm quartz injector, high plasma gas flow, a torch position of -3 mm and a dilute aqua
regia rinse solution. This provides a very rugged system to meet the highly stringent QC requirements that are necessary for
this type of analysis.

Perkin Elmer Life and

Analytical Sciences
710 Bridgeport Avenue
Shelton, CT 06484-4794 USA
Phone: (800) 762-4000 or
(+1) 203-925-4602
www.perkinelmer.com

For a complete listing of our global offices, visit www.perkinelmer.com/lasoffices

©2004 PerkinElmer, Inc. All rights reserved. The PerkinElmer logo and design are registered trademarks of PerkinElmer, Inc. Optima and GemCone are trademarks of
PerkinElmer, Inc. or its subsidiaries, in the United States and other countries. All other trademarks not owned by PerkinElmer, Inc. or its subsidiaries that are depicted herein are
the property of their respective owners. PerkinElmer reserves the right to change this document at any time without notice and disclaims liability for editorial, pictorial or
typographical errors.

The data presented in this Field Application Report are not guaranteed. Actual performance and results are dependent upon the exact methodology used and laboratory conditions.
This data should only be used to demonstrate the applicability of an instrument for a particular analysis and is not intended to serve as a guarantee of performance.

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