Thermo Scientific icap RQ ICP-MS: Typical limits of detection
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1 TECHNICAL NOTE Thermo Scientific icap RQ ICP-MS: Typical limits of detection Author Tomoko Vincent Keywords BEC, interference removal, KED, LOD Introduction Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is known to be a powerful technique for the analysis of trace elements in many application areas such as environmental analysis, food safety testing and clinical analysis. The main reasons to choose ICP-MS are its low limits of detection combined with an extended linear dynamic range and the ability to analyze varying sample matrices without suffering from extensive matrix effects. The Thermo Scientific icap RQ ICP-MS has been designed to deliver these characteristics while also offering the greatest ease of use and the simplest method development. In order to cover a broad range of different applications, the icap RQ ICP-MS is equipped with proprietary skimmer cone insert technology that allows the operator to easily optimize the characteristics of the instrument. The insert portfolio comprises a standard High Matrix insert to cover most applications, a High Sensitivity insert for ultra-trace analyses, and a Robust insert where higher matrix tolerance is needed. Detection limits are a set of key performance indicators detailing an instrument s capabilities and are useful as an aid in determining that instrument s suitability to a chosen task. They demonstrate the lowest level of analyte distinguishable from the background noise under optimal conditions and are typically determined several times for statistical accuracy.
2 In order to accurately detect and quantify an element of interest, it has to be made sure that the measured isotope can be detected free from spectral interferences. The most commonly observed interferences are socalled polyatomic interferences, which are formed through recombination of ions after leaving the plasma, or in the interface. For effective interference removal in single quad ICP-MS instruments, collision/reaction cells (CRCs) are most commonly used. CRCs may be operated in different ways depending on the nature of the interference that has to be eliminated, however, the most comprehensive approach is the use of an inert gas, such as He, and the use of Kinetic Energy Discrimination (KED). In KED, unwanted polyatomic interferences are filtered out based on the difference in collision cross-section sizes of the analyte and polyatomic interferences. In addition, the proprietary design of the Thermo Scientific QCell CRC adds an automatically configured low mass cut-off to the interference removal toolbox, which filters out unwanted precursor ions. These ions are then unable to recombine later in the QCell CRC, backgrounds are reduced further than KED alone and detection limits are improved. Limits of Detection Detection limits themselves can be defined as either the Instrument Detection Limit (IDL) or the Method Detection Limit (MDL), and are accompanied by the Background Equivalent Concentration (BEC). The IDL defines the lowest concentration of an analyte that can be detected under ideal conditions by the instrument, and is normally measured on a single element basis using a clean sample, e.g using ultrapure 2% nitric acid matrix. The MDL, in comparison, determines the lowest level of analyte that can be detected in a sample matrix using the proposed method of analysis and takes into account sample preparation steps. This is usually determined on a multi-element basis by diluting standard solutions to concentration levels that can no longer be accurately read, or by adding a low concentration spike into a real sample. There are numerous procedures for determining and calculating the MDL, but most methods require numerous analytical runs, over several days, to ensure a realistic determination of instrument performance. Method Sample preparation Blank solutions and calibration standards at 1, 5 and 10 µg L -1 were prepared gravimetrically by adding the appropriate quantity of a multi-elemental stock solution (SPEX CertiPrep ) directly to a solution containing 2% m/m HNO 3 (65% HNO 3 Optima grade, Fisher Chemical) and 0.5% m/m HCl (32-35% HCl Optima grade, Fisher Chemical). All solutions were prepared in freshly rinsed vials. This acid matrix was selected to reflect a sample preparation procedure that is broadly appropriate to a wide variety of industries and applications. Instrument configuration An icap RQ ICP-MS was used for all tests. The instrument was equipped with a MicroMist borosilicate nebulizer (Glass Expansion, Australia), a Peltier-cooled, quartz spraychamber (operating at 3 C), a 2.5 mm ID quartz injector and a demountable quartz torch. High sensitivity, High matrix and Robust interface skimmer cone inserts were used in this study. Due to the relatively high concentration of HCl in the acid matrix used in this study (0.5% m/m), a high number of complex Cl-based polyatomic interferences were expected. Consequently, the system was optimized using KED interference correction for all the analytes in this study. The instrument configuration and operation parameters are shown in Table 1. Table 1. Instrument configuration and operating parameters. Parameter Value Spraychamber Quartz cyclonic, cooled at 3 C Nebulizer Injector Interface Plasma power MicroMist borosilicate pumped at 400 µl min mm Quartz injector Ni sample cone and insert type skimmer 1550 W Nebulizer gas 1.1 L min -1 CRC gas He 4.5 ml min -1 KED Lens setting 3 V Auto tune method 2
3 Results As described in the sample preparation section, each sample reagent solution contained a high amount of HCl (approximately 0.5 m/m %). Therefore a high amount of complex Cl based polyatomic interferences were created, leading to adverse effects on the detection of a variety of elements. The effect of applying kinetic energy discrimination for interference removal is demonstrated with the measurement of As. Figures 1a and 1b show comparisons between the calibration curve results with STD mode and He KED mode on 75 As. In STD mode, a high background of about 100 kcps is observed that compromises the attainable detection limit. When KED is applied, the background is reduced significantly. An examination of the two calibration curves produced confirms that He KED mode effectively eliminated interferences and dramatically improved the detection limit for As from µg L -1 to µg L -1 and the BEC from 3.7 µg L -1 to µg L -1. Figure 1b. Calibration curve of 75 As in He KED mode. The same scenario can be seen for 51 V and 52 Cr, whereby the comprehensive He KED performance generated excellent calibration curve results and both analytes achieved LODs of less than 3 ng L -1 (Figures 2 and 3). Figure 1a. Calibration curve of 75 As in STD mode. Figure 2. Calibration curve of 51 V in He KED mode. 3
4 The analysis has demonstrated that using a single He KED measurement mode enables the icap RQ ICP-MS to achieve simple, high-sensitivity, multi-element sample analysis. The typical performance of the icap RQ ICP-MS using STD and He KED mode are shown in Table 2, where detection limits were calculated using the raw intensity data from the standard and the blank, as per following equation: IDL = 3SD blk x STD conc STD x BLK x Where: IDL is the instrument detection limit SD blk is the standard deviation of the intensities of the multiple blank measurements Figure 3. Calibration curve of 52 Cr in He KED mode. Figure 4 shows the calibration curve for 7 Li with He KED mode, the high transmission flatapole design of the QCell CRC delivers good sensitivity even for low mass elements, such that low ng L -1 LODs can be achieved. STD x is the mean signal for the standard BLK x is the mean signal for the blank STD conc is the concentration of the standard Figure 4. Calibration curve of 7 Li in He KED mode. 4
5 Table 2. Typical LODs achieved with the icap RQ ICP-MS in STD and He KED mode, using the three available skimmer cone inserts. All results are reported in ng L -1. Measurement mode STD Insert Li Be B Na Mg Al Measurement mode He KED Insert Li Be B Na Mg Al K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Se Rb Sr Y Zr Nb Mo Ru Rh Pd Ag Cd In Sn Sb Te Cs Ba La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Hf Ta W Re Ir Pt Au Hg Tl Pb Bi Th U Rb Sr Y < Zr Nb Mo Ru Rh Pd Ag Cd In Sn Sb Te < Cs Ba La Ce Pr Nd < Sm Eu < Gd < Tb < Dy Ho < Er < Tm < Yb < Lu < Hf Ta W Re Ir Pt Au Hg Tl Pb Bi Th U
6 Conclusion The icap RQ ICP-MS system with its integrated Thermo Scientific Qtegra ISDS Software demonstrated excellent performance to provide a significant improvement to analytical laboratory capabilities through simplicity, productivity and robustness. The flexible configuration delivers a complete solution for a wide range of trace elemental analysis in both research and routine applications. Find out more at thermofisher.com/sq-icp-ms For Research Use Only. Not for use in diagnostic procedures Thermo Fisher Scientific Inc. All rights reserved. SPEX CertiPrep is a trademark of SPEX CERTIPREP, INC. All other trademarks are the property of Thermo Fisher Scientific. This information is presented as an example of the capabilities of Thermo Fisher Scientific products. It is not intended to encourage use of these products in any manner that might infringe the intellectual property rights of others. Specifications, terms and pricing are subject to change. Not all products are available in all countries. Please consult your local sales representative for details. TN43427-EN 0117
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