News from LabRulezICPMS Library - Week 49, 2025

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This week we bring you application notes by Agilent Technologies, LECO, Shimadzu and Waters Corporation!

1. Agilent Technologies: Determination of 21 Elements in Fertilizers using Autodilution with ICP-OES

Automated analysis of multinutrient fertilizers by Agilent 5800 VDV ICP-OES and ADS 2 autodilutor

• Application note
• Full PDF for download

Crop production relies heavily on fertilizers to achieve high yields, maintain soil fertility, and support sustainable agricultural practices. Fertilizers typically contain high concentrations of essential macronutrients like nitrogen (N), phosphorus (P), and potassium (K), plus lower levels of secondary and micronutrients. In addition to these beneficial elements, fertilizers may also contain contaminants such as heavy metals introduced during manufacturing or from raw materials. To ensure product efficacy, safety, and regulatory compliance, multiple nutrients and potential contaminants must be accurately measured. However, the number of analytes, concentration range, and sample-to-sample variability present significant analytical challenges for laboratories requiring robust, high-throughput, and accurate quantitative methods.

Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) is a powerful technique that is widely used for the simultaneous analysis of multiple elements in complex sample matrices like fertilizers.1,2 Traditional workflows, however, often require manual preparation of calibration standards and tailored sample dilutions, processes that are time-consuming, error-prone, and can introduce contamination. Modern automation technologies such as the Agilent Advanced Dilution System (ADS 2) simplify the analysis, freeing analysts to focus on more productive tasks.3,4 Also, by enabling automatic, reactive dilutions based on sample concentration, the ADS 2 avoids manual intervention, reduces consumable usage, and improves data quality. Some key features of the ADS 2 include: 

• Autocalibration: Automatic generation of calibration curves from one or more stock solutions. This feature significantly reduces time spent on standard preparation, minimizes waste of single-use consumables, and lowers the risk of human error, simplifying the workflow and improving data reliability. 
• Prescriptive dilutions: Automatic dilution of solutions or samples by a known (prescribed) dilution factor before analysis. This feature is useful in labs where routine dilutions occur, eliminating a time-consuming manual step from daily workflows. 
• Reactive dilutions: Automatic real-time dilution of overrange samples that exceed calibration limits. This feature eliminates the need for manual dilutions or rework after the analysis, allowing greater flexibility and efficiency within a single method. 
• Summary Row: A smart software feature that selects and displays the best measurement from multiple iterations, while retaining access to all underlying data. This feature streamlines data review and significantly reduces the time spent on manual processing and reporting. 

In this study, the Agilent 5800 Vertical Dual View (VDV) ICP-OES with ADS 2 autodilutor was used to determine 21 elements in multinutrient fertilizers. The elements included aluminum, arsenic, boron, calcium, cadmium, cobalt, chromium, copper, iron, potassium, magnesium, manganese, molybdenum, sodium, nickel, phosphorus, lead, sulfur, selenium, vanadium, and zinc.

Experimental 

Instrumentation 

The Agilent 5800 VDV ICP-OES was configured with the integrated Agilent Advanced Switching Valve (AVS 7), ADS 2 autodilutor, and Agilent SPS 4 autosampler (Figure 1). The AVS and ADS 2 operate seamlessly together to enhance sample throughput, reduce turnaround time, and lower cost-per-sample. The ADS 2 enabled automated, precise preparation of calibration standards and sample dilutions, minimizing analyst workload and consumables use. Importantly, its integration with the AVS 7 ensures that no additional time is added when dilution is not required, overcoming a common limitation of other dilution systems. The SPS 4 autosampler provided automated sample delivery to the instrument. The 5800 ICP-OES was equipped with a SeaSpray nebulizer, double-pass cyclonic spray chamber, and Agilent semi-demountable VDV torch with a 1.8 mm id injector. All components were controlled by the Agilent ICP Expert Pro software5 (the ADS 2 is compatible with ICP Expert software version 7.7 or later). Automated Fitted Background Correction (FBC) was selected for background correction of each analyte.6

Conclusion 

The Agilent 5800 VDV ICP-OES paired with the Agilent ADS 2 autodilutor enabled the fast, high-throughput, multi-elemental analysis of fertilizer samples. The accurate quantification of 21 major and trace elements in microwave-digested fertilizer samples was assisted by the following features of the ADS 2: 

• Autocalibration: Calibration standards from 0 to 10 mg/L were automatically prepared from a single stock solution, minimizing manual preparation and ensuring consistent, accurate calibration across the range. Additional higher concentration standards were used for selected elements. 
• Prescriptive dilutions: Automatic dilution of solutions were performed using a known (prescribed) dilution factor before analysis, removing time-consuming and error-prone manual dilutions of the SRM samples. 
• Reactive dilution: Overrange analyte concentrations in two fertilizer samples triggered dynamic, real-time dilution, eliminating the need for prescreening or manual intervention. This reactive dilution capability streamlined the workflow. 
• Summary Row: The software feature automatically selected and displayed the most reliable results from multiple measurements of each fertilizer sample, simplifying data review while maintaining full traceability.

The automated-ICP-OES method produced high-quality results, with MDLs below 1 mg/kg for most elements. Accuracy was excellent, with all recoveries for both NIST 695 fertilizer SRM and spiked fertilizer samples falling within 100 ± 10% of expected values. The method also demonstrated excellent stability and robustness over nine hours. Following a 10x automatic prescriptive dilution of each QC using the ADS 2, recoveries ranged from 95 to 105%, with %RSDs below 3.5% for all elements, demonstrating the reproducibility of the autodilutor. 

This study confirms the suitability of the 5800 VDV ICP-OES for quantifying major, minor, and trace nutrients, as well as contaminant elements, in three commercial fertilizers— supporting regulatory compliance and product quality assurance. Productivity of the method was further enhanced by the ADS 2, which minimized manual handling and reduced the risk of errors during standard and sample preparation.

2. LECO: Determination of Nitrogen in Fertilizer

• Application note
• Full PDF for download

Nitrogen is one of the most important elements for plant development and is the macronutrient that is most often found to be deficient in arable soils used for crop production. Nitrogen plays a key role in the formation of enzymes and proteins, which promotes lush vigorous growth and development in plants that often leads to an increase in the yield from the plant. Fertilizers are utilized to re-introduce nitrogen back into arable soils. Fertilizers can be grouped by their makeup and/or origins into categories including inorganic and/or synthetic (including nitrates, ammonium, and urea) and organic (including compost materials and manures). The accurate and precise determination of nitrogen in all fertilizer types is not only important in the process of blending and preparing the fertilizer material for use, but also will have significant impact on the commercial value and guarantee of the fertilizer. 

The LECO FP828 is a combustion nitrogen/protein determinator that utilizes a pure oxygen environment in a vertical quartz furnace. A thermoelectric cooler removes moisture from the combustion gases before they are collected in a ballast. The gases equilibrate and mix in the ballast before a representative aliquot (3 cm³ or 10 cm³ volume) of the combustion gas is extracted and introduced into a flowing stream of inert gas (helium or argon) for analysis. The aliquot gas is carried to a thermal conductivity (TC) cell for the detection of nitrogen (N₂).

Instrument Model and Configuration 

Thermal conductivity detectors work by detecting changes in the thermal conductivity of the analyte gas compared to a reference/carrier gas. The greater the difference between the thermal conductivity of the carrier gas and the analyte gas, the greater sensitivity of the detector. The FP828 supports either the use of helium or argon as the instrument's carrier gas. When used as a carrier gas, helium provides the highest sensitivity, and the best performance at the lower limit of the nitrogen range. Argon can also be used as a carrier gas. The thermal conductivity difference between argon and nitrogen is not as great as the thermal conductivity difference between helium and nitrogen, therefore the detector is inherently less sensitive when using argon as a carrier gas.

TYPICAL RESULTS 

Data was generated utilizing a linear, forced through origin calibration using ~0.05 g of NIST 913b Uric Acid (33% N). Alternatively, LECO 503-530 LCRM Urea may be used for calibration. The calibration was verified using LECO 502-896 (Lot 1002) EDTA (9.57% N).

3. Shimadzu: Cross-Sectional Analysis of Power Semiconductor and Silver Sintering Die Attach Material

• Application note
• Full PDF for download

User Benefits

• Useful in evaluation of the particle shape of silver sintering die attach materials.
• Useful in evaluation of the sintered condition, such as voids, and the diffusion of elements at the bonding interface in silver sintering.
• Useful in research on surface properties, such as the film thickness in metalizing treatment

Power semiconductors are used in a wide range of applications, from household electrical appliances and automotive devices to power transmission and distribution systems. Recently, SiC (silicon carbide) semiconductors, which allow high-temperature operation, have attracted attention as a substitute for conventional Si (silicon) semiconductors. With application of SiC, the operating temperature of power semiconductors is expected to increase to 200 ˚C or more in the future. However, in this case, the heat resistance of the die bond where semiconductor chips are bonded to a substrate becomes an issue, as high-temperature operation may cause deterioration or embrittlement of the joining material. 

Silver (Ag) sintering materials can withstand high temperatures exceeding 200 ˚C and have excellent thermal conductivity, enhancing heat dissipation and realizing improved temperature management of devices. Since embrittlement can be preventing by using Ag sintering materials, thereby improving the reliability of the bonds, Ag particles have attracted interest as a die bond material with excellent heat dissipation. 

This Application News article introduces an example of analysis of a power semiconductor using an EPMA electron probe microanalyzer (EPMA-8050G).

Power Semiconductors 

With conventional Si semiconductor, a large amount of energy may be lost during power conversion, but energy loss can be improved significantly by introducing a SiC widegap power semiconductor. SiC has a wide bandgap and is superior in terms of pressure resistance and heat resistance due to its excellent thermal conductivity, which allows efficient management of generated heat and stable operation even under hightemperature environments 1), 2) . 

In the vertical package structure of a power semiconductor device, wiring is formed on the SiC device surface, and the heat generated by the semiconductor (die) is dissipated downward. The back of the SiC chip analyzed here was metalized by ion plating. Titanium (Ti) plating, nickel (Ni) plating, and gold (Au) plating were carried out. The AMB (Active Metal Brazing) substrate consisted of a three-layer structure of a pure copper (Cu) substrate, a ceramic substrate, and a pure Cu substrate. High bond strength and thermal conductivity were secured in the SiC chip and the AMB substrate by sintering Ag particles. 

Conclusion

In response to high-temperature operation of power semiconductor devices, Ag particles have attracted considerable attention as a die bond material. Their high-temperature resistance and superior heat dissipation properties are expected to improve device reliability and are being utilized in research and development, such as evaluation of the bond interface.

4. Waters Corporation: Identify and Characterize Particles in the Visible Size Range with Aura

• Application note
• Full PDF for download

Characterizing large visible contaminants is essential for patient safety and mandated by both USP 788, 790, and 1046. Drug formulations for parenteral injection are required to meet certain standards for subvisible particles (>100 µm) and must be completely free of visible particles (>1 µm–100 µm).1 Therefore, subvisible and visible particle analysis is necessary throughout the drug development process to ensure that products do not produce unwanted adverse side-effects or reductions in efficacy.2 However, traditional detection methods for subvisible and visible particles like dynamic flow imaging (FI) and light obscuration (LO) are plagued by a number of limitations that hamper analysis, including:

• Particle fragmentation, also known as clipping, observed during particle detection with flow imaging techniques.3
• A low refractive index contrast encountered when measuring biologic particles in liquid media that makes it difficult to distinguish translucent particles from background.4
• A small depth of focus in a wide fluidic channel area that exacerbates particle fragmentation and dramatically reduces sampling efficiency. This makes accurate large particle detection nearly impossible.
• Clogging that occurs when visible particles flow through the fluidic chambers of flow-based systems like FI or LO.
• Visible particle inspection performed by manual operators that is highly error prone.5

Aura™ Systems are powered by backgrounded membrane imaging (BMI), a USP 788 Method 2 compliant digital imaging method that conducts both subvisible and visible particle analysis. Calibrated using a microscopy reference slide, Aura provides accurate and linear data for particles up to 5.6 mm in equivalent circular diameter on 96-well small volume plates and 14 mm on 24-well large volume plates, well into the visible range. 

In this application note, we demonstrate the capability of Aura instruments and Particle Vue Software to characterize visible particle aggregates stemming from various biologic drug formulation processes. A comparison of both visible and subvisible NIST ethylene tetrafluoro ethylene (ETFE), large adeno-associated virus (AAV) aggregates, large cellular aggregates from CAR-T cell therapies, and large fibrous contaminants in cell therapies are used as models to illustrate how Aura can analyze a range of samples while providing accurate size characterizations. In addition, side illumination membrane images (SIMI) and fluorescent membrane microscopy images (FMM) provide further information about the visible particle samples and their nature.

Conclusion 

Aura particle analysis systems and Particle Vue Software can analyze particles well into the visible size range, solving a long-standing analytical problem in biologic, cell, and gene therapy characterization. BMI enables accurate sizing and morphological determination of large aggregates and Aura’s FMM, present in both the Aura and Aura CL Systems, allows for specific particle identification to understand the nature and origin of the visible aggregates. Accurately size, characterize, and identify particles from small to large for all biological samples using Aura to ensure proper assessment of both visible and sub visible particles.