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Volume 30 Issue 6
Dec.  2019
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Wei Zhao, Keqing Zong, Yongsheng Liu, Zhaochu Hu, Haihong Chen, Ming Li. An Effective Oxide Interference Correction on Sc and REE for Routine Analyses of Geological Samples by Inductively Coupled Plasma-Mass Spectrometry. Journal of Earth Science, 2019, 30(6): 1302-1310. doi: 10.1007/s12583-019-0898-5
Citation: Wei Zhao, Keqing Zong, Yongsheng Liu, Zhaochu Hu, Haihong Chen, Ming Li. An Effective Oxide Interference Correction on Sc and REE for Routine Analyses of Geological Samples by Inductively Coupled Plasma-Mass Spectrometry. Journal of Earth Science, 2019, 30(6): 1302-1310. doi: 10.1007/s12583-019-0898-5

An Effective Oxide Interference Correction on Sc and REE for Routine Analyses of Geological Samples by Inductively Coupled Plasma-Mass Spectrometry

doi: 10.1007/s12583-019-0898-5
Funds:

the National Natural Science Foundation of China 41530211

the MOST Special Fund from the State Key Laboratory of Geological Processes and Mineral Resources, China University of Geosciences, Wuhan MSFGPMR01

the National Natural Science Foundation of China 41473031

More Information
  • Oxide interference correction plays a vital role in the accurate determination of trace element compositions of geological samples by inductively coupled plasma-mass spectrometry (ICP-MS). In this study,we found that the oxide production is mainly controlled by the gas flow of the ICP-MS and a constant oxide correction factor (OCF) can be measured during a routine analysis. Thus,we can obtain the oxide production by just investigating the gas flow for a fixed ICP-MS system with monitoring of OCF. Si,Ba and LREE oxide interferences on the Sc,Eu and Gd of four geological standard samples GSP-2,JP-1,GBW03112 and GBW03113 were corrected by such method and the results were in good agreement with the recommended values. Therefore,the present study provides a simple and fast correction method for the oxide interferences of the geological samples during the routine analyses. Furthermore,a Microsoft Excel spreadsheet template integrating the correction equations was devel-oped in an in-house software (ICPMSDataCal) for effective calibration.
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An Effective Oxide Interference Correction on Sc and REE for Routine Analyses of Geological Samples by Inductively Coupled Plasma-Mass Spectrometry

doi: 10.1007/s12583-019-0898-5
Funds:

the National Natural Science Foundation of China 41530211

the MOST Special Fund from the State Key Laboratory of Geological Processes and Mineral Resources, China University of Geosciences, Wuhan MSFGPMR01

the National Natural Science Foundation of China 41473031

    Corresponding author: Keqing Zong

Abstract: Oxide interference correction plays a vital role in the accurate determination of trace element compositions of geological samples by inductively coupled plasma-mass spectrometry (ICP-MS). In this study,we found that the oxide production is mainly controlled by the gas flow of the ICP-MS and a constant oxide correction factor (OCF) can be measured during a routine analysis. Thus,we can obtain the oxide production by just investigating the gas flow for a fixed ICP-MS system with monitoring of OCF. Si,Ba and LREE oxide interferences on the Sc,Eu and Gd of four geological standard samples GSP-2,JP-1,GBW03112 and GBW03113 were corrected by such method and the results were in good agreement with the recommended values. Therefore,the present study provides a simple and fast correction method for the oxide interferences of the geological samples during the routine analyses. Furthermore,a Microsoft Excel spreadsheet template integrating the correction equations was devel-oped in an in-house software (ICPMSDataCal) for effective calibration.

Wei Zhao, Keqing Zong, Yongsheng Liu, Zhaochu Hu, Haihong Chen, Ming Li. An Effective Oxide Interference Correction on Sc and REE for Routine Analyses of Geological Samples by Inductively Coupled Plasma-Mass Spectrometry. Journal of Earth Science, 2019, 30(6): 1302-1310. doi: 10.1007/s12583-019-0898-5
Citation: Wei Zhao, Keqing Zong, Yongsheng Liu, Zhaochu Hu, Haihong Chen, Ming Li. An Effective Oxide Interference Correction on Sc and REE for Routine Analyses of Geological Samples by Inductively Coupled Plasma-Mass Spectrometry. Journal of Earth Science, 2019, 30(6): 1302-1310. doi: 10.1007/s12583-019-0898-5
  • An Agilent 7500a ICP-MS was used for measurements. Samples were introduced by a Meinhard PFA nebulizer with a Scott double pass water cooled spray chamber, quartz glass torch, and nickel sampler and skimmer cones. The sampling depth was fixed at 6 mm during the whole data acquisition process. The plasma gas flow rate and the auxiliary gas flow rate were fixed at 15 and 1 L min-1, respectively. The instrument was optimized based on the maximum sensitivity of 7Li, 89Y and 205Tl ions signals. The oxide and double-charged ion production were maintained at lower than 1% and 2%, respectively. The detailed operating conditions and acquisition parameters of the ICP-MS are summarized in Table 1.

    Instrument Agilent 7500a
    Plasma power 1 380 W
    Torch Quartz glass torch
    Sampling depth 6 mm
    Plasma gas flow 15 L min-1
    Auxiliary gas flow 1 L min-1
    Sample gas flow 1.1 L min-1
    Carrier gas flow 0.54 L min-1
    Makeup gas flow 0.56 L min-1
    Nebulizer Meinhard type
    Spray chamber Double scott, cooled at 2 ℃
    Sample uptake rate 0.3 mL min-1
    Interface Ni sampler and skimmer cones
    Extraction lens voltage Optimized for maximum sensitivity (7Li, 89Y, 205Tl)
    Oxide yield (156 : 140) < 1%
    Double-charged (140 : 70) < 2%
    Points per peak 3
    No. of replicates 3
    Internal standard 115In

    Table 1.  Instrumental operating conditions

    To establish the relationship between the oxide production and the instrument parameters, mono-elemental solutions were made and analyzed, including 5 μg mL-1 (Si) and 500 ng mL-1 (Ba and REEs from La to Dy) diluted from the NACIS solutions at 1 000 μg mL-1 with HNO3 (2% v/v) by two steps. The concentrations were selected in such a way that the signals of M+ and MO+ could be high enough than the backgrounds for precise determination. The analyzable isotopes and potential oxide interferences are listed in Table 2. Due to the low isotopic abundances of 17O (0.04%) and 18O (0.2%), oxide species from these isotopes are negligible. Because of low production of hydroxide, only oxide interference is considered in our scheme.The sample gas flow rate varied from 0.9 to 1.25 L min-1, covering the possible routine variation range of sample gas flow rates. Meanwhile the relationships between the oxide production, and RF power (1 000 to 1 500 W) and sample uptake rate (0.16–1.29 mL min-1) were investigated as well.

    Element Mass Interfering species
    Si 29
    Sc 45 29Si16O
    Ba 135
    137
    La 139
    Ce 140
    Pr 141
    Nd 146
    Sm 147
    Eu 153 137Ba16O
    Gd 158 142Ce16O 142Nd16O
    Tb 159 143Nd16O
    Dy 163 147Sm16O
    Ho 165 149Sm16O
    Er 166 150Sm16O 150Nd16O
    Tm 169 153Eu16O
    Yb 172 156Gd16O 156Dy16O
    Lu 175 159Tb16O

    Table 2.  The potential oxide interference on Sc and REE

    Four rock reference materials including GSP-2, JP-1, GBW03112 and GBW03113 were analyzed in this study. About 50 mg sample powders were digested in a teflon bombs with HF+HNO3 mixture. The details about the sample preparing procedure are the same as Liu et al. (2008a).

  • Our equation is established based on the general template presented by Aries et al. (2000) for calculating signal intensity of each element M

    where "m" is the signal intensity measured at mass m, M+ is the own signal intensity of m, M-16O+ is the contribution of an interfering element to "m", whose mass is "m-16".

    For any elements M and N, OCF (oxide correction factor) is defined as the ratio of MO+/M and NO+/N. Under given plasma condition, the oxide production and OCFs obtained by measuring the standard solutions should be theoretically the same as the sample solutions.

    Then in the sample solutions, any oxide contribution (MO+) can then be calculated by the following Eq. (3)

    Shibata et al. (1993) demonstrated that the oxide production in ICP mainly depends on the plasma temperature (T) and oxygen partial pressure (PO)

    where K(MO+) is the dissociation/formation constant, m (g mol-1) is the weight of each species, Z is the partition function, D0 (eV) is the dissociation energy of MO+ bond, k is the Boltzmann constant and h is the Planck constant.

    When rearranging Eq. (4), OCF could be obtained as Eq. (5), which indicates that OCF is only related to the plasma temperature.

  • The stability of oxide production was measured by monitoring mono-solutions of Ba and Ce. As shown in Fig. 1a, ratios of BaO+/Ba+ and CeO+/Ce+ vary in a very small range within 10% and 5%, respectively, which could be caused by the gradually blocking of cone orifice (Vaughan and Horlick, 1990a). The calculated OCF values vary within 5%, which can be considered as a constant during routine analysis.

    Figure 1.  Oxide production of barium, cerium and OCF versus (a) time, (b) RF power, (c) sample gas flow rate, and (d) sample uptake rate (mL min-1). RF power, sample gas flow rate and sample uptake rate were set at 1 380 W, 1.1 L min-1 and 0.33 mL min-1, respectively in Fig. 1a. For Figs. 1b, 1c and 1d, the condition of plasma was single changed. The solid curves show the variation of oxide production and OCF with the changed plasma parameters (two steps fitting).

    The temperature of plasma could be easily influenced by RF power, sample gas flow rate and sample uptake speed, accordingly the oxide production and OCF are dependent (Longerich, 1989). As shown in Fig. 1b, CeO+/Ce+ decreased from 196% to 0.7%, and BaO+/Ba+ from 1.12% to 0.04% when RF power was changed from 1 000 to 1 500 W. During the same time the sample gas flow rate increased from 0.9 to 1.2 L min-1, CeO+/Ce+ varied from 0.3% to 3.3%, and abrupt changed to 400% as the aerosol speed increased to 1.25 L min-1 (Fig. 1c). BaO+/Ba+ shows similar trend, which varied from 0.016% to 3% with the sample gas flow rate from 0.9 to 1.25 L min-1 (Fig. 1c). The sample uptake rate could be adjusted by the pump speed, which changed from 0.16 to 1.29 mL min-1, CeO+/Ce+ rises from 0.33% to 1% (Fig. 1d).

    For a long period of routine analysis, the RF power and sample uptake rate are fixed at 1 380 W and 0.33 mL min-1, respectively, considering the greater sensitivity and lower oxide production and double-charged ions. However, the sample gas flow rate is adjusted for better sensitivity before every experiment, which mainly varied from 1.0 to 1.15 L min-1. It means that the OCF would be changed daily. However, a relationship between the OCF and sample gas flow rate should exist, the variation trend is clearly described in Fig. 2, and the selected flow rate was from 0.9 to 1.2 L min-1 that including the routine experimental range. The formulas could be obtained by three steps fitting for calculating any OCF under given gas flow rate.

    Figure 2.  The plot of cerium normalized OCF value versus sample gas flow rate. The soild curves were obtained by three steps fitting.

    Here Ce was used as the normalizing element, as any elements satisfied that: (1) shows similar behavior as other elements in oxide formation; (2) no or least isobaric interference is observed in itself; (3) high enough of concentration as well as oxide production for accurate determination to calculate oxide production ratios, could be used for normalizing.

    A Microsoft Excel spreadsheet template that combines those correction equations was developed in an in-house software (ICPMSDataCal) (Liu et al., 2010, 2008b) to deduct the interference intensities, which facilitates the data management. When analyzing the solution data with ICPMSDataCal, the oxide interference correction is optional. Accordingly, if an element needs to be corrected, the current total gas flow and CeO/Ce are needed to input the ICPMSDataCal. Therefore, when the data is exported, the software can deduct oxide interference automatically (Fig. 3). The corrected data in this paper are all calculated by ICPMSDataCal.

    Figure 3.  The operation procedure of ICPMSDataCal for correcting oxide interference.

  • Scandium has similar chemical properties to the REEs and they are always analyzed together in most geochemical researches. Sc is monoisotopic (mass 45) and isobaric with 29Si16O and 28Si16O1H. Furthermore, Si is a major element in rocks with high concentration. Although most of silicon could be evaporated with fluorine as SiF4 during the rock digestion procedure, a little silicon residue still can affect accurate determination of Sc.

    In this study, GSP-2 was analyzed and summarized in Table 3. 29Si16O and 28Si16O1H contributed 130% of the signal on mass 45 for the uncorrected data, while the corrected content of Sc agreed well with the recommend value (Table 3).

    Sample GSP-2 (μg g-1)
    Analysis ICP-MS HR-ICP-MS
    Reference This study Pretorius et al. (2006) GEOREM
    Uncorrected Corrected
    Element n=3 RSD% n=3 RSD%
    Sc 14.6 1.5 6.3 0.5 6.2 6.3
    La 184 0.3 184 0.3 197 180
    Ce 418 0.7 418 0.7 498 410
    Pr 53 0.5 53 0.5 60 51
    Nd 204 0.3 204 0.3 224 200
    Sm 27 1.2 27 1.2 27 27
    Eu 2.4 0.5 2.3 0.5 2.4 2.3
    Gd 13.3 0.3 12.2 0.3 12.2 12
    Tb 1.41 0.4 1.33 0.5 1.4 1.31
    Dy 6.2 0.7 6.2 0.7 6 6.1
    Ho 1 1.1 1 1.1 0.99 1
    Er 2.5 0.6 2.4 0.6 2.5 2.2
    Tm 0.31 3.1 0.31 3.1 0.31 0.29
    Yb 1.7 1.0 1.7 1.0 1.77 1.6
    Lu 0.25 1.6 0.25 1.6 0.25 0.23

    Table 3.  Summary of analytical results (μg g-1) of trace elements for GSP-2 compared with the published values

  • The interference degree of BaO+ on Eu+ is determined by the Ba/Eu ratio in samples and the oxide production ratio of ICP-MS. Aries et al. (2000) considered that the influence of oxide interference could be ignored when the oxide interference contribution is less than 5%. Excessive correction leads to more uncertainty in the results. According to our laboratory conditions, as the interference contribution is 5%, the Ba/Eu ratio is 500. Figure 4 displays the Eu content versus Ba/Eu ratio of some geological standards, which could clearly recognize samples that need correction.

    Figure 4.  The plot of Eu content versus Ba/Eu ratio of some typical geological standards (reference values from GEOREM, http://georem.mpch-mainz.gwdg.de).

    JP-1, GBW03112 and GBW03113 are characterized by high Ba/Eu ratios of 4 700, 6 700 and 4 800, respectively, and each sample was analyzed three times during one-month period. Averages (uncorrected and corrected data) and reference values are presented in Table 4. Chondrite-normalized REE patterns for them are shown in Fig. 5.

    Element JP-1 (ng g-1) GBW03112 (μg g-1) GBW03113 (μg g-1)
    This study References This study References This study References
    Uncorrected Corrected Dulski (2001) Qi et al. (2005) Makishima and Nakamura (2006) Uncorrected Corrected Wang (2012) Uncorrected Corrected Wang (2012)
    La 30 30 34 30.8 26.8 2.23 2.23 2.9 4.11 4.11 4.48
    Ce 59.1 59.1 63 53.6 59.7 4.33 4.33 4.77 7.04 7.04 6.29
    Pr 7.5 7.5 8.9 7.65 7.4 0.49 0.49 0.58 0.87 0.87 0.78
    Nd 32.8 32.8 33 29.7 31.8 1.75 1.75 1.88 3.32 3.32 2.91
    Sm 9 9 9 7.69 8.4 0.33 0.33 0.35 0.56 0.56 0.52
    Eu 3.2 2.2 2.1 1.09 2.4 0.067 0.05 0.05 0.16 0.1 0.11
    Gd 8.8 8.8 9 6.44 9.7 0.22 0.22 0.27 0.4 0.4 0.45
    Tb 2 2 1.6 1.74 1.9 0.029 0.03 0.04 0.06 0.06 0.07
    Dy 13.6 13.6 13.2 13 14.6 0.16 0.16 0.2 0.35 0.35 0.39
    Ho 3.3 3.3 3 3.12 3.6 0.03 0.03 0.03 0.07 0.07 0.08
    Er 12.7 12.7 11.2 11.1 12.3 0.088 0.09 0.1 0.19 0.19 0.22
    Tm 2.9 2.9 2.3 2.12 2.4 0.015 0.01 0.02 0.03 0.03 0.03
    Yb 22.8 22.8 20.9 18.8 20.9 0.093 0.09 0.11 0.21 0.21 0.22
    Lu 4.5 4.5 4 3.38 4.2 0.017 0.02 0.02 0.03 0.03 0.03

    Table 4.  Summary of analytical results of trace elements for JP-1, GBW03112 and GBW03113 compared with the published values

    Figure 5.  Chondrite-normalized REE patterns for (a) JP-1, (b) GBW03112 and (c) GBW03113. Data were normalized by the CI-chondrite average values from Sun and McDonough (1989).

    JP-1 has ultra-low REE content (average < 50 ng g-1), uncorrected Eu data showed an obviously positively anomaly (Fig. 5a). The corrected data in this study agree well with the recommend data obtained by conventional QP-ICP-MS (Dulski, 2001), pre-concentration technique (Qi et al., 2005) and isotope dilution-internal standardization method (Makishima and Nakamura, 2006). Membrane-desolvation could effectively remove the solvent loading to plasma to reduce the oxide interference in ICP. The corrected data of GBW03112 and GBW03113 in this study are almost consistent with the referred values obtained by membrane-desolvation (Wang, 2012) (Figs. 5b, 5c). The slightly variable HREE in the two samples are possibly caused by REE heterogeneities in 50 mg weight (Nakamura and Chang, 2007).

  • Generally, interference in ICP-MS is ubiquitous, and the degree of interference depends on the ratio of interference element and analyte element. Figure 6 shows Pr/Gd ratio to Gd and Nd/Tb to Tb. With the analyzed element changing, the interference faced changes, e.g., when 157Gd used to quantify Gd, 141PrO is needed to consider, while the time 158Gd is tested, oxide interference from Ce and Nd must be taken into account. In case of oxide interference contribution above 5%, the correction is worth considering, then Pr/Gd ratio above 2.5 and Nd/Tb ratio higher than 140 that reach the correction level according to the instrument conditions in this study.

    Figure 6.  The Pr/Gd ratio versus Gd (a) and Nd/Tb ratio versus Tb (b) diagrams of some geological standards (reference values from GEOREM, http://georem.mpch-mainz.gwdg.de).

    As displayed in Table 3, Gd of GSP-2 decline from 13.3 ppm to 12.2 ppm after oxide interference correction, and the corrected value is consistent with the recommended value.

  • In this paper, an effective correction scheme has been described for accurate determination of trace elements by deducting the oxide interference, which is based on calculating oxide production ratios from mono-solutions under a series of sample gas flow rates. This correction method could easily count the involved oxide contribution from the calibration equations, even if the plasma condition (associated with the sample gas flow rate) is altered, and can be applied to diverse types of samples. A Microsoft Excel spreadsheet template is developed in an in-house software (ICPMSDataCal) that is able to deduct the interference intensities rapidly and conveniently.

  • This research was supported by the National Natural Science Foundation of China (Nos. 41473031, 41530211), the MOST Special Fund from the State Key Laboratory of Geological Processes and Mineral Resources, China University of Geosciences, Wuhan (No. MSFGPMR01). We are grateful to the editors for editorial handling and three anonymous reviewers for their critical and constructive comments that have greatly improved the quality of this paper. The final publication is available at Springer via https://doi.org/10.1007/s12583-019-0898-5.

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