News from LabRulezICPMS Library - Week 52, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 22nd December 2025? Check out new documents from the field of spectroscopy/spectrometry and related techniques!

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This week we bring you application notes by Agilent Technologies, Metrohm and Shimadzu!

1. Agilent Technologies: Trace Elemental Analysis of Precursor Materials Using ICP-MS/MS

Robust detection of Pt, Ag, Cd, and Ti in high-metal matrices using the Agilent 8900 ICP-QQQ and reactive cell gases 

• Application note
• Full PDF for download

Precursor materials are fundamental to the fabrication of integrated circuits (ICs). In atomic layer deposition (ALD), they enable the controlled growth of ultrathin films on semiconductor substrates—an essential capability for scaling advanced device architectures. Because even trace metal impurities in precursors can degrade film performance and device yield, both suppliers and manufacturers routinely analyze these materials. Due to its sensitivity and multi-elemental capabilities, inductively coupled plasma mass spectrometry (ICP-MS) is the industry standard for assessing elemental impurities in semiconductor materials.¹ However, the high concentration of the metallic (high-matrix) content of precursors and the prevalence of polyatomic and doubly charged ion (M++) spectral overlaps arising from the matrix on key analytes present challenges for accurate analysis by single-quadrupole ICP-MS. At one time, high-resolution (HR)-ICP-MS (m/Δm up to 10000) was the best choice for solving these kinds of analytical problems. But some interferences require a resolution that exceeds the capability of current HR-ICP-MS instruments. In these cases, the samples are sometimes diluted to reduce the concentration of matrix elements, but dilution cannot totally solve the interference and may negatively affect detection limits. 

Triple quadrupole ICP-MS (ICP-QQQ or ICP-MS/MS) combined with collision/reaction (CRC) gases overcomes these limitations by selectively removing or avoiding interferences without compromising sensitivity. Agilent ICP-QQQ systems use two quadrupoles (Q1 and Q2) as unit mass filters, enabling MS/MS operation and the controlled use of reactive cell gases. Q1 controls which ions enter the CRC and Q2 controls which ions reach the detector.^2–4 

In this study, we evaluated the performance of the Agilent 8900 ICP-QQQ to determine key analytes in three simulated precursor materials. Each sample contained a highconcentration matrix of hafnium (Hf), zirconium (Zr), or molybdenum (Mo), which cause interferences on platinum (Pt), silver (Ag), and cadmium (Cd) and titanium (Ti), respectively. To demonstrate the 8900 ICP-QQQ system’s ability to remove spectral interferences without sacrificing sensitivity, we quantified the four analytes in the three matrices using optimized instrument operating conditions.

Experimental

Instrumentation 

An Agilent 8900 Semiconductor configuration ICP-QQQ (#200) fitted with the optional m-lens was used for all measurements. The 8900 #200 includes an inert (HF-resistant) sample introduction system comprising a 200 μL/min MicroFlow PFA nebulizer, a PFA spray chamber, endcap, and connector tube, and a demountable torch with a 2.5 mm internal diameter (id) sapphire injector. The cones comprised a Pt-tipped sampling cone and Pt-tipped, Ni-based skimmer cone for m-lens. The samples were self-aspirated using an Agilent SPS 4 autosampler. Hot plasma conditions (1% CeO+ /Ce+ ) were used during the analysis of the high-matrix samples. 

The 8900 ICP-QQQ was operated in MS/MS mode for all measurements. Ammonia (NH3 ) —plus a flow of helium (He) as a buffer gas—and oxygen (O2 ) were used as reactive cell gases to resolve the matrix-based interferences. Various CRC tuning modes and Q1–Q2 mass setting combinations were tested to obtain the best conditions for each analyte. The optimized operating conditions for the analysis are detailed in Table 1.

Conclusion 

The Agilent 8900 Semiconductor configuration ICP-QQQ was evaluated for its ability to eliminate spectral interferences on four analytes—Pt, Ag, Cd, and Ti—in simulated semiconductor precursor materials using MS/MS and reactive cell gases. To accommodate challenging samples comprising Hf (500 ppm), Zr (500 ppm), and Mo (360 ppm) under hot plasma conditions (1% CeO+ /Ce+ ), the 8900 was equipped with the optional m-lens. 

Ammonia was applied in both on-mass and mass-shift modes to quantify Pt, Ag, and Cd at single-digit or sub-ppt levels. Oxygen on-mass mode effectively removed Mo-based doubly charged ion interferences on Ti, enabling accurate detection at single-digit ppt concentrations. Repeated analysis of the MoCl5 samples spiked at 50 ppt with %RSDs below 10% demonstrated the instrument’s robustness and consistent performance for ultratrace quantification in complex matrices. 

The 8900 ICP-QQQ delivered low background, high sensitivity, and reliable interference control, making it suitable for method development and trace-level screening of semiconductor materials.

2. Metrohm: Fat content analysis in olive pomace with NIR spectroscopy

• Application note
• Full PDF for download

Olive pomace is the main residue of the olive oil extraction process. It is a thick sludge – the remaining pulpy material after most of the oil is removed from the olive paste. To extract the remaining oil it contains, the olive pomace is treated with solvents. After refining and mixing this with edible virgin olive oil for flavor, aroma, and color, olive pomace oil is obtained. Olive pomace oil is used in cooking for its milder flavor and stability at high temperatures [1], as well as being nutritionally relevant due to its high oleic acid content (C18:1) [2]. Olive pomace fat analysis is necessary to check the efficiency of the oil removal process. The official method to determine this requires a time-consuming drying step followed by solvent extraction. Near-infrared spectroscopy (NIRS) is a fast, chemical-free method for olive pomace testing without any sample preparation.

EXPERIMENTAL EQUIPMENT

140 samples of olive pomace were measured on a Metrohm NIR Analyzer. All measurements were performed in reflection mode (1000–2250 nm) using the large cup accessory. The samples were measured in rotation to collect spectral data from several areas. Spectral averaging of signals from several spots helped to reduce sample inhomogeneity. Metrohm software was used for all data acquisition and prediction model development.

RESULTS

The obtained NIR spectra of olive pomace samples (Figure 1) were used to create a prediction model for quantification of fat content. The quality of the prediction model was evaluated using a correlation diagram (Figure 2) which displays a high correlation between the NIR prediction and the reference values measured with Soxhlet extraction. The respective figures of merit (FOM) display the expected precision of a prediction during routine analysis.

CONCLUSION 

This Application Note shows the feasibility of using NIR spectroscopy for olive pomace fat analysis. By using NIRS, chemical-free analysis can be conducted within seconds—a quick, easy, cost-effective alternative to determine the efficiency of the olive pomace oil removal process.

3. Shimadzu: Analysis of Pharmaceutical Raw Materials Compliant with ICH Q3D Guideline Using ICP-MS with Collision Mode

• Application note
• Full PDF for download

User Benefits

• The 24 elements identified in the ICH Q3D guideline can be measured with high sensitivity.
• Pharmaceutical raw materials that are dissolved in ethanol can be easily analyzed using the Shimadzu ICP-MS organic solvent system.

The presence of impurities in pharmaceutical ingredients is a concern within the medical pharmaceutical industry. Therefore, the International Council on Harmonisation of Technical Requirementsfor Registration for Pharmaceuticalsfor Human Use requires the management of metallic impurities in pharmaceuticals through guidelines using ICP-MS (ICH Q3D) ^{1), 2)} . This standard specifies the Permitted Daily Exposure (PDE) for 24 elements of toxicological concern in oral preparations, injectables, and inhalants. 

In the case of oral preparations, only the seven elements of Classes 1 and 2A are considered, except in instances where elements are intentionally added, such as when used as catalysts during synthesis. However, the sources of elemental impurities are diverse and include not only components such as active pharmaceutical ingredients and excipients but also manufacturing equipment and utensils. 

ICP-MS has the advantage of being able to analyze various trace elements simultaneously. It is often used for the analysis of elemental impuritiesin pharmaceuticals. The analyte for ICP-MS is usually a liquid sample, so solid samples require pretreatment. 

In this Application News, we measured three types of pharmaceutical raw materials and analyzed the impurities using the Shimadzu ICP-MS organic solvent system. Furthermore, the accuracy, precision, detection limits and specificity of 24 target elements are presented according to USP^{3), 4)} and EP, assuming measurements below the Control Threshold of 30 % of the PDE.

Instrument Configurations and Analysis Conditions 

Table 2 shows the instrument configuration for ICP-MS (ICPMS-2040). The organic solvent system was used to introduce the ethanol. By using the platinum sampling cone, damage from long-term exposure to organic solvents during analysis can be reduced. To reduce the labor required for sample preparation, the internal standards were added using the Online Internal Standard Kit. The analysis conditions are shown in Table 3.

Accuracy and Precision Validation Results 

Measurements were carried out for n = 3 spiked samples with the target concentration of 50 % and 150 %, and n = 6 spiked samples with the target concentration and the blank (unspiked) sample. Spike recovery was calculated by averaging the quantitative values of all samples. Tables 6 to 8 show the measurement results. 

Accuracy: Spike recovery of the samples at each of the target concentrations of 50 %, 100 %, and 150 % was in the range of 94 % to 111 %, thereby satisfying the acceptance criterion. Precision (Repeatability): RSD of the spiked samples with the target concentration ranged from 0.27 % to 3.79 %, satisfying the acceptance criterion. 

Limit of quantitation: As accuracy for 50 % of the target concentration satisfied the acceptance criterion, the limit of quantitation could be confirmed. 

Specificity 

ICP-MS analysis often requires evaluation for potential interference by isotypes, polyatomic ions originating from Ar, oxides of coexistent elements and chloride ions. Here, the Cd was assessed. MoO, originating from the Class 3 element Mo, causes interference with Cd. A 1350 μg/L Mo solution (concentration equivalent to 1.5J) was analyzed, and the amount of interference with Cd was measured. Here, in addition to using collision gas, interelement correction was also performed. Table 5 shows the results. 

When the collision gas was used without interelement correction, interference by MoO was reduced but not eliminated. However, the quantitative value was below the lower limit of detection when the collision gas was used in combination with interelement correction. This result confirmed that the use of interelement correction, together with a collision gas, enables the appropriate correction of interference that could not be eliminated by the collision gas alone.

Conclusion 

In this Application News, we measured three types of pharmaceutical raw materials and analyzed 24 elements indicated in the ICH Q3D guideline using the Shimadzu ICP-MS organic solvent system. In accordance with the pharmacopeias (USP, EP), the accuracy, precision, quantification limit, and specificity were confirmed. The results of the validation demonstrated that the performance meets the acceptance criteria with a sufficient margin. Based on the above, it was determined that the Shimadzu ICPMS-2040 is an effective analytical method for the 24-element analysis of pharmaceutical raw materials that can be dissolved in ethanol.