News from LabRulezICPMS Library - Week 51, 2025

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

1. Agilent Technologies: Measurement of Bidirectional Transmittance Distribution Function

Using the Agilent Cary 7000 universal measurement spectrophotometer

• Application note
• Full PDF for download

The bidirectional transmittance distribution function (BTDF) is a fundamental concept in optical metrology, describing how light is transmitted through a material in various directions. Understanding BTDF is essential for characterizing the optical properties of materials. 

To address BTDF, it is important to first understand the bidirectional scattering distribution function (BSDF). BSDF encompasses both the bidirectional reflectance distribution function (BRDF) and BTDF. While BRDF measures how light is reflected off a surface, BTDF focuses on the transmission of light through a material. Together, these functions provide a comprehensive picture of how light interacts with materials, enabling precise characterization of their optical behavior.^1,3 

BTDF measurements are used in diverse fields to understand how light is transmitted through materials. In computer graphics, BTDF data enables realistic rendering of materials, enhancing visual simulations and animations with lifelike quality.⁴ Remote sensing relies on BTDF to calibrate satellite sensors, improving the accuracy of earth observation data necessary for monitoring environmental changes and weather patterns.⁵ Optical device design benefits from BTDF measurements by optimizing the performance of lenses, diffusers, and light-emitting devices, ensuring efficient light transmission.⁴ In materials science, BTDF characterizes the optical properties of new materials, aiding in the development of advanced composites and coatings.⁶ The food industry uses BTDF to assess the quality and consistency of products through their optical characteristics, which is vital for quality control.⁶ The solar industry uses BTDF to enhance the efficiency of solar panels and photovoltaic devices by understanding light transmission properties.⁶ Additionally, the aerospace sector uses BTDF to evaluate the optical properties of materials used in satellites and other space applications, ensuring reliable performance under various conditions.⁴ 

The focus of this work is to demonstrate that BTDF measurements in the visible and near-infrared (NIR) spectral range can be easily performed using the Agilent Cary 7000 universal measurement spectrophotometer (UMS), Figure 1. Alternatively, the Agilent Cary 5000 and 6000i instruments equipped with the universal measurement accessory (UMA) may also be used for BTDF measurements. These instruments offer automated control over detector position, sample rotation, and polarization, making BTDF measurements straightforward and reliable.

Setup for the Cary 7000 UMS 

The Cary 7000 UMS was used for measurements of directional and bidirectional transmittance with in-plane geometries ranging from −85° to 85° viewing angles. The instrument is easily configured using Agilent Cary WinUV software, as shown in Figures 4 and 5, and method parameters are summarized in Table 1. The source system included a quartz tungsten-halogen lamp and a deuterium arc lamp for UV illumination, coupled with a Littrow out-of-plane DMC. The DMC output slit provided a 4 nm bandwidth for the illuminating beam. The optics directed the beam onto a chopper, forming a double-beam photometric configuration. The reference beam monitored the illumination source for any drift in intensity, while the sample beam was shaped by vertical and horizontal slits to control convergence, resulting in an approximately 5.0 × 4.5 mm beam spot on the sample. 

The detection system included a set of turntables regulated by an optical encoder wheel with an angular resolution of 0.02°. The sample holder and detector turntables set the incident and viewing zenith angles within ± 85°. If BRDF were to be performed, excluded angles would be between ± 10° due to shadowing by the detector. The detector setup featured a calibrated aperture with an 18.00 mm diameter and a sample-to-detector-aperture distance of 129 mm, resulting in a solid angle of 0.0153 sr. The scattered light was collected by an off‑axis mirror onto a dual-band Si/InGaAs photodetector for the visible and NIR wavelength range.

Results and discussion

BTDF measurement by the Cary 7000 UMS 

The Cary 7000 UMS was used to measure the spectral BTDF of two samples: fused synthetic silica (HOD‑500) and porous polytetrafluoroethylene (PTFE). Measurements were conducted across the wavelength range of 450 to 1,650 nm in 50 nm intervals, and viewing zenith angles from –35° to 35° in 5° steps. Figures 6 and 7 illustrate the BTDF results for both samples. Figure 6A shows the BTDF of the HOD‑500 sample, while Figure 6B presents the BTDF of the PTFE sample. Both samples exhibited near-Lambertian characteristics and a smooth increase in BTDF as a function of wavelength.

Conclusion 

The Cary 7000 universal measurement spectrophotometer (UMS) is an effective and user-friendly instrument for assessing the bidirectional transmittance distribution function (BTDF) across visible and near-infrared wavelengths. Its automated features, including detector positioning, sample rotation, and polarization control, streamline the measurement process, ensuring simplicity and reliability. The Cary 7000 UMS consistently delivers precise results with acceptable levels of uncertainty, making it ideal for routine BTDF assessments. Its intuitive interface and seamless integration with Cary WinUV software make it versatile for various optical metrology applications, offering a practical solution for both researchers and industry professionals.

2. Metrohm: Online zinc/nickel plating bath analysis with X-ray fluorescence

• Application note
• Full PDF for download

Electroplating is a technique that uses electrical current to apply a thin coating of one material, such as nickel or zinc, onto the surface of another material, such as copper. Zinc and zinc-based alloys, such as zinc-nickel (Zn/Ni), are commonly used to protect steel from corrosion. Zn-Ni alloys are especially popular, as they offer a corrosion resistance that is greater than that of pure zinc [2,3]. 

Both alkaline and acidic Zn/Ni baths are commonly used for electroplating (Figure 1). Each bath type offers unique advantages depending on the application [4]. Alkaline Zn/Ni baths are known for producing highly uniform coatings with good throwing power, making them ideal for complexshaped components. On the other hand, acidic Zn/Ni baths offer higher deposition rates and can deliver smooth, bright finishes that are often preferred for aesthetic applications [4].

Electroplating baths are sensitive to various processrelated fluctuations that significantly impact metal deposition and influence the final coating thickness and quality. These variations can arise due to changes in temperature, plating tank metal concentration levels, or contamination. Analyzing the bath solution frequently is crucial to maintain stable plating conditions and minimize material waste. Continuous monitoring of the plating solutions helps ensure that the concentration of metals remains within the optimal range. 

The metal content in electroplating baths is often measured manually in on-site laboratories. Classical wet chemistry techniques, AAS, and ICP-OES are commonly used for this purpose. While these methods are effective, they can be time consuming, require skilled personnel, and may not provide realtime data. This potentially leads to delayed corrections and material inefficiencies. Modern process analytical technologies (PAT) are increasingly being adopted in electroplating operations to automate and optimize the monitoring of plating baths. These systems continuously analyze critical bath parameters such as metal concentration, pH, temperature, and conductivity in real time. All these factors directly influence the quality and uniformity of the deposited metal coating.

The 2060 XRF Process Analyzer from Metrohm Process Analytics (Figure 2) offers an effective solution to continuously monitor electroplating baths. By providing real-time measurements of metal concentrations such as Zn and Ni, this process analyzer helps maintain the ideal bath composition required for consistent and high-quality coatings.

Conclusion

The 2060 XRF Process Analyzer is a reliable solution for the metal finishing industry, offering real-time monitoring of zinc and nickel concentrations in electroplating baths. Its ability to continuously measure these key bath parameters ensures consistent coating quality, reduces material waste, and improves process efficiency.

3. Shimadzu: Determination of Elemental Impurities in Petroleum Distillates Using ICP-MS ~ASTM D8110-17~

• Application note
• Full PDF for download

User Benefits

•  Enables the analysis of elemental impurities in various kinds of petroleum distillates (light and middle distillates) with the sample preparation method that involves only dilution with organic solvents.
• Metal elements in petroleum distillates (light and middle distillates) can be accurately analyzed over a long period of time.
• Solvent-resistant peristaltic pump tubing enables the addition of internal standard elements in-line, even for organic solvent analysis, thereby eliminating the need for manual addition.

The concentration of metal elements in petroleum products needs to be controlled due to concerns that they can act as catalyst poisons and affect product quality. Additionally, it is important to measure the concentration of heavy metals to reduce environmental impact during emissions. Traditionally, analytical methods using ICP Optical Emission Spectrometry (ICPOES), such as ASTM D7111-161), have been employed to determine metal elements in petroleum products. However, in recent years, there has been a demand for more sensitive analytical methods using ICP mass spectrometry (ICP-MS), such as ASTM D8110-172), to detecttrace amounts of metal elements. 

ASTM D8110-17 is the test method for the analysis of elements in petroleum distillates (light and middle distillates) using ICP-MS. Since this method involves diluting the sample with organic solvents, it is necessary to introduce organic solvent samples into the ICP-MS. 

In this Application News, various light and middle distillates were diluted with organic solvents in accordance with ASTM D8110-17 and trace elements were analyzed using the ICPMS-2050 (Fig. 1). The validity of the analytical results was confirmed through spike recovery tests and the analysis of reference material for residual fuel oil. Additionally, the stability of the analysis over long periods of time was evaluated.

Removal of Interference and Detection Limit 

To analyze metal elements with high sensitivity in organic solvents, it is important to eliminate interference caused by carbon from the organic solvent. For example, there are carbonderived polyatomic ion interferences such as 12C12C+ for 24Mg, 12C16O+ for 28Si, and 40Ar12C+ for 52Cr. By using collision mode with helium gas or reaction mode with hydrogen gas, these interferences can be eliminated, enabling sensitive analysis. As an example, Fig. 2 shows the calibration curve for Mg under each condition. In the No Gas mode, the influence of 12C12C+ results in a high background equivalent concentration (BEC), making it challenging to analyze trace amounts of 24Mg. However, in collision mode, the interference from 12C12C+ was reduced, and BEC of 80 ng/g was obtained. Furthermore, in reaction mode, the interference from 12C12C+ was significantly reduced, and BEC of 0.8 ng/g was obtained, which enables trace amounts of 24Mg analysis. Detection limits are shown in Table 4. The detection limit was calculated as the concentration that gives a signal equivalent to three times the standard deviation (σ) of the calibration blank sample (STD0).

Long Term Stability 

To evaluate the long-term stability of organic solvent analysis using the ICPMS-2050, light and middle distillates were analyzed over approximately 6 hours. To confirm the variability of the quantitative results, Check Standards were analyzed before sample analysis, every 10 samples, and at the end of the analysis. The results are shown in Fig. 3. All quantitative results of the Check Standard fell within the range of 90 to 110 % based on the prepared concentrations, which meets the validation requirements of ASTM D8110-17 (red dashed line). Additionally, the change in the intensity of the internal standard elements over approximately 6 hours are shown in Fig. 4. The change in intensity of the internal standard elements were within 90 to 120 %, which also falls within the validation requirements of 50 to 150 % asspecified in ASTM D8110-17 (red dashed line). These results indicate that the ICPMS-2050 has sufficient long term stability for the analysis of organic solvent samples.

Conclusion 

In this Application News, the analysis of metal elements in light and middle distillates was performed using the ICPMS-2050 and the organic solvent introduction system. Good results were obtained from spiking recovery tests and the analysis of reference material for residual fuel oil, demonstrating that trace metal elements in light and middle distillates can be accurately quantified with a simple sample preparation method that involves only dilution with organic solvents. Furthermore, the recoveries of the Check Standards and the change in intensity of the internal standard elements also satisfied the validation requirements of ASTM D8110-17, confirming stable analysis over long periods of time. Since it is possible to analyze without the complex procedures required for acid decomposition, the risk of volatilization or contamination of the target elements during the sample preparation process is reduced. Additionally, the use of solventresistant peristaltic pump tubing enables the in-line addition of internal standard elements, further reducing the time required for sample preparation.