News from LabRulezICPMS Library - Week 39, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in week 39, 2024? Check out new documents from the field of spectroscopy, especially ICP/MS techniques!

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This week we bring to you applications by Agilent Technologies, Shimadzu, Thermo Fisher Scientific, and Metrohm!

1. Thermo Fisher Scientific: Robust analysis of a variety of water and wastewater samples according to U.S. EPA Method 6020B (SW-846)

• Application

Goal

To evaluate and demonstrate performance of the Thermo Scientific™ iCAP™ RQplus ICP-MS for robust analysis of a variety of wastewater samples according to the compliance requirements of U.S. EPA Method 6020B.

Keywords: ICP-MS, EPA Method 6020B, iCAP RQplus, robustness, matrix tolerance, Argon Gas Dilution, quality control, regulatory compliance

Introduction

As a result of factors such as climate change, increasing population, and ongoing industrialization, various types of solid and liquid waste are being introduced or released into the environment, causing damage to the ecosystem. Though there are several preventive measures in place globally to control the entry of these waste materials into the environment and protect it from pollution, it is extremely difficult to reduce these anthropogenic contamination sources to zero.

The U.S. Environmental Protection Agency’s (EPA) Office of Solid Waste and Emergency Response (OSWER) and Office of Resource Conservation and Recovery (ORCR) regulate all waste under the Resource Conservation and Recovery Act (RCRA). The RCRA’s goals are to:

1. Protect the public from the hazards of waste disposal
2. Conserve energy and natural resources by recycling and recovery
3. Reduce or eliminate waste, and
4. Clean up waste that may have spilled, leaked, or was disposed of improperly.

The OSWER/ORCR publication SW-846, entitled “Test Methods for Evaluating Solid Waste, Physical/Chemical Methods”, is the EPA’s official compendium of analytical and sampling methods that have been evaluated and approved for use for analysis relating to the RCRA regulations. SW-846 functions primarily as a guidance document setting forth acceptable, although not required, methods for the regulated and regulatory communities to use in responding to RCRA-related sampling and analysis requirements. SW-846 is a multi-volume document that changes over time as new information and data are developed. It was first issued by the EPA in 1980 and is currently in its fifth edition.

As a part of a recent edition, this EPA method has been revised to EPA Method 6020B, which provides guidelines on target analytes, detection limits, sample collection, preparation and storage, and various quality control protocols to follow while performing such analyses.

This application note discusses a total workflow of the analytical method developed for analysis of water and wastewater samples using the iCAP RQplus ICP-MS, which offers a comprehensive solution for effective and trouble-free analysis of samples containing high dissolved solids, such as wastewaters and solid wastes. The Thermo Scientific™ Qtegra™ Intelligent Scientific Data Solution™ (ISDS) Software was used to control the iCAP RQplus ICP-MS instrument and to generate, process, and report analytical data, ensuring that the entire workflow meets the requirements described in EPA Method 6020B, including all the applicable QC checks. To verify the consistent performance of the instrument over time, a sequence of 200 samples was repeated over three consecutive days, so that 600 unknown samples were analyzed successfully.

Conclusion

The iCAP RQplus ICP-MS was extensively tested for compliance with EPA Method 6020B. The quality of the analytical data obtained over three consecutive days of measurements demonstrated that the built-in argon gas dilution system for controlled and automatic dilution of the sample aerosol is a powerful solution for laboratories analyzing demanding samples, such as soil digests or wastewater under high throughput conditions. The overall performance of the instrument suggests that reliable analysis of these type of samples can be performed without need of any maintenance and with no instrument downtime over three or more days of analytical work. Some of the important outcomes of this study are summarized below:

• All the requirements of EPA Method 6020B were met during the test period of three days, enabling the analysis of a total of 600 samples. 
• The instrument detection limits (IDLs) and lower limits of quantification (LLOQs) achieved met and exceeded the requirements given in the method, which suggests that the employed methodology, with its optimized argon gas sample dilution, is suitable for achieving the required robustness and instrument sensitivity for these types of samples.
• Analyzing standard solutions containing concentrations above the highest point of the calibration according to section 9.6 of EPA Method 6020B established the wider linear range for each analyte (specifically up to 1,000 mg·L-1 for major elements like Na, K, Ca, Mg, Al, and Fe). This offers great flexibility for analyzing samples without the need for further dilution and improves productivity of the analytical laboratory. The wide linear range established for each analyte, with the optimized instrument settings that include AGD, enable the analysis of various environmental samples with wide concentration ranges within the same run.
• Results observed during analysis of ICB and CCB blank quality control samples indicated that the proposed method ensures minimum carryover between samples, enabling trouble-free measurement of high numbers of samples across the full calibrated concentration range.
• The accuracy obtained for ICV and CCV standard solutions over three consecutive days ensures the reliability and consistency of instrument performance while analyzing challenging high TDS containing samples, such as wastewater and solid waste digests.
• The analytical data obtained during analysis of interference check solutions (ICSA and ICSAB) highlight the effectiveness of single KED mode using helium as the collision gas in removing potential polyatomic interferences on each analyte, ensuring interference-free analysis every time.
• The data obtained during analysis of matrix-spiked and duplicate measurements demonstrated that minimum or no matrix effect was encountered when analyzing complex matrices such as wastewater.
• The observed behavior of the internal standards on three consecutive days of analysis highlights the robustness and consistency of the instrument performance. The consistent internal standard readback within the range of 75–125% suggests that the developed methodology is a reliable solution for effective handling of high-TDS-containing samples with no impact from the matrix content.
• The Qtegra ISDS Software provides all the necessary tools including different QC functions, automatic calculations, and limit and flag functionality to ensure that the analysis is performed as per the compliance requirements of EPA Method 6020B.

2. Metrohm: Inline monitoring of cell cultures with Raman spectroscopy

• Application

Cell culture is a key part of the biopharmaceutical industry to monitor the health of cells. Tight control of this process is necessary to overcome unwanted side reactions or poor yields.

Glucose is essential for cell energy, but its conversion to energy through glycolysis produces lactate. Lactate accumulation induces acidity, causing cellular stress and reduced cell growth rates.

Manual laboratory methods can be quite cumbersome and can introduce bias depending on the analyst, resulting in inaccurate results and sample contamination. To address these issues, inline Raman spectroscopy is a very well-suited analysis technique for this industry as it does not require any reagents and the sample remains unaltered.

This Process Application Note presents a method to accurately monitor cell growth inside a bioreactor in «real-time» with the 2060 Raman Analyzer from Metrohm Process Analytics. In this case, an inline process analyzer is the preferred solution to guarantee high product quality and avoid contamination from measurement.

INTRODUCTION

Cell culture is an essential step in the production of a wide range of biopharmaceuticals, including complex therapeutic proteins, monoclonal antibodies, and vaccines [1]. This process involves growing cells in a controlled environment, typically in a bioreactor, to produce the desired product.

Glucose is an important component of cell culture, as it provides cells with the energy they need to grow, divide, and form the final product [2]. Figure 1 illustrates the fundamental process of converting glucose into energy within a cell.

The conversion of glucose to energy (i.e., glycolysis) results in the production of lactate, the ionized form of lactic acid. Accumulation of lactate in cell culture media can adversely impact cell growth and productivity. As lactate functions as an acid, its buildup in the culture medium can lower the pH, inducing cellular stress and diminishing growth rates [4].

To prevent lactate accumulation, manufacturers must monitor and adjust cell culture conditions to maintain lactate levels within an acceptable range. This may involve continuously measuring the glucose concentration in the culture medium, ensuring precise adjustments to prevent over- or underdosing. Typically, analysts perform such measurements manually (offline). However, contamination is common in this setup, and the data fails to reflect the true state of the cell culture process. 

A safer, more efficient, and faster way to monitor multiple parameters simultaneously in bioreactors is via inline analysis with reagent-free Raman spectroscopy (Figure 2). This is a nondestructive and non-contact technique – thus it is ideal for inline analysis directly at the bioreactor (Figure 2, left side).

The 2060 Raman Analyzer by Metrohm Process Analytics enables the comparison of «real-time» spectral data from the process to a reference method (e.g., titration, ion chromatography, HPLC) to create a simple, yet indispensable calibration model for monitoring glucose and lactate in the cell culture bioreactor.

«Real-time» analysis of the state of the culture keeps the glycolysis reaction within control. Additionally, inline analysis can provide information about the current state of different processes (e.g., substrate consumption and kinetics).

CONCLUSION

Raman spectroscopy is used for many different applications and industries where high-quality data is essential. The 2060 Raman Analyzer is a high-performance Raman system designed for operations like cell culture monitoring, which require non-contact analysis. Together with Metrohm’s Vision and IMPACT software, the 2060 Raman Analyzer can be used to acquire near real-time results, supporting time-critical processes such as pharmaceutical development.

3. Agilent Technologies: High-Throughput Analysis of Additive- Elements and Wear Metals in Lubricants by ICP-OES

• Application

Fast analysis times using the Agilent 5900 ICP-OES with AVS and oil autosampler referencing ASTM D5185-18

Introduction

Tribology is an interdisciplinary area of science that studies how different surfaces interact together. Better understanding of friction, wear, and lubrication has many practical applications within engineering, manufacturing, transport, energy, and sport.¹

Oils and lubricating fluids are vital for the ongoing performance of machinery and equipment as they minimize wear on components and extend the life of parts. Since oils deteriorate during use and over time, it is important to monitor their composition to prevent equipment failures and optimize maintenance schedules and costs. Due to its exceptional robustness and stability, ICP-OES is often used for the multi-element analysis of wear metals and additive-elements in oils and lubricants in various industries.²

Tracking the elemental profile of wear metals is an important safety control procedure for predictive/preventive maintenance purposes. If certain metals, such as the ones listed in Table 1, are identified in the oil or are seen to be changing in concentration over time, action can be taken before the equipment is damaged by further wear.

Oil additives such as antioxidants, corrosion inhibitors, demulsifying, antifoam agents, detergents, metal deactivators, and tackiness agents are used to improve existing properties or provide desirable properties. Some other chemicals, such as pour point suppressors and VI improvers, are used to suppress undesirable properties. Monitoring the inorganic components of these types of chemicals can be a useful way to check for the presence of additives in oil and their level of depletion over time.

Zinc (Zn) typically indicates the presence of zincdialkyl-dithiophosphate (ZDDP), an antiwear additive. Molybdenum dithiocarbamate (Mo DTC) is another common additive that is used to reduce friction. Extreme pressure (EP) additives typically include phosphorus (P) and sulfur (S). Detergents include calcium (Ca) and magnesium (Mg), and sometimes barium (Ba). Detergents work by suspending particulates in oil so they can be removed by a filter. Antifoam agents typically include silicon (Si).

Wear metals and additive elements are included in the list of 22 elements specified in ASTM D5185-18 Standard Test Method for Multielement Determination of Used and Unused Lubricating Oils and Base Oils. ASTM D5185-18 is widely used in the industry for the elemental analysis of used and unused oils by ICP-OES.³

The goal of this application was to develop a simple, fast, ASTM 5185-18-compatible method for the analysis of both wear metals and additives. To achieve these objectives, an Agilent 5900 Synchronous Vertical Dual View (SVDV) ICP-OES was used for the analysis of 140 used engine oils and lubricating fluids referencing ASTM D5185-18.

To meet the sample-to-sample throughput goal of under 30 s, including rinsing, the integrated Agilent Advanced Valve System (AVS 6) of the 5900 and external Cetac Oils 7400 Homogenizing Autosampler were used. The AVS 6/7 is standard on the 5900 ICP-OES.⁴

The 5900 uses smart software tools within the Agilent ICP Expert Pro software to help the analyst develop methods that produce accurate data. The following smart tools were used in this study:

• IntelliQuant Screening: the fast acquisition mode allows analysts to perform a full semiquantitative spectrum scan of up to 78 elements in just a few seconds.⁵ IntelliQuant Screening automatically identifies the best element wavelength for each type of sample matrix that is analyzed, indicates the level of dilution to use, and suggests the concentration range of calibration standards.
• Fitted Background Correction (FBC): the software routine automatically corrects simple and complex background structures without requiring time-consuming investigation of the sample matrix.⁶

The ICP-OES method followed criteria set out in ASTM D5185-18, which included analyzing a NIST oil standard reference material (SRM) to assess its accuracy.

Conclusion

The study has outlined a fast, simple, and robust method for analyzing new and used oils according to ASTM 5185–18 using the Agilent 5900 SVDV ICP-OES and Cetac 7400 Oil autosampler. Wear metals, additives, and contaminants were measured in a wide range of 140 real-world railroad samples.

The oil autosampler improved the consistency of mixing samples using a stirring paddle for each sample and an automated drip tray helped to minimize cross contamination between samples. The integrated AVS 6 valve system of the 5900 enabled automated sample introduction, reducing the sample analysis time to 29 s including rinse. To maintain a high level of productivity, interactive, real-time control of instrument parameters was used to monitor the analysis during each run, including monitoring of the RF generator and internal standard responses.

The IntelliQuant Screening program is an invaluable tool for the analysis of wear metals and additives in engine oils and fluids. Full-wavelength scans of samples were acquired for each sample within 12 s sample-to-sample. The data was used to determine the calibration range, sample dilution factors, and to identify or confirm the best wavelengths to use for some elements in the quantitative method. Analysts can also display the semiquantitative data in different ways, helping with trend analyses of metals in oils and lubricating fluids.

The quantitative method met the requirements of ASTM 5185 standard method. Excellent recoveries were obtained for the wear metals in the NIST lubricating oil SRM, and repeated analysis of the SRM nine times throughout the run showed a good level of precision. The control charts for Ca and Mo obtained by plotting the results for every third sample in a block of 60 engine oil samples showed that the elements remained within the three sigma control limits.

The speed, robustness, and simple operation of the 5900 make it highly suited to the routine analysis of unused and used oils and lubricants. Analysts can conduct trend analysis of key elements in used oils based on either semiquantitative or quantitative measurements of samples over time. The availability of flexible and clear presentation tools for trend data enables engineers to make well-informed decisions regarding maintenance actions or adjustments to operating conditions.

4. Shimadzu: Determination of Arsenic Species in Apple Juice by LC-ICP-MS Analysis

• Application

User Benefits

• Arsenic species can be analyzed using an LC-ICP-MS system.
• Enables the safety level of arsenic in food to be evaluated.
• Using a method package for analyzing arsenic species eliminates the need to register analytical conditions, etc.

Introduction

The natural environment contains many kinds of substances. These include hazardous substances such as arsenic. However, arsenic exists in a variety of forms, and the toxicity differs depending on the form. Generally, arsenite is more toxic than arsenate, and organic arsenic is less toxic than inorganic arsenic. It is difficult to completely avoid arsenic in the natural environment since it is also contained in drinking water and agricultural/livestock products. The foods we eat also might contain various types of arsenic. U.S. Food and Drug Administration (FDA) sets action levels when a level of a contaminant is unavoidable, to inform industry on the level of contamination above which the FDA may regard certain foods as adulterated. 1) For these reasons, various surveys and studies on arsenic in food products are being conducted around the world.

One method for analyzing trace quantities of arsenic with high sensitivity is ICP-MS. However, although ICP-MS can measure the total concentration of arsenic, it cannot discriminate between different forms of the element. While determining the total concentration of arsenic is important, it is also important to determine the concentrations of specific forms.

The arsenic species can be separated using a liquid chromatograph (LC). By connecting the LC unit to an ICP-MS on-line, the arsenic species can be analyzed with high sensitivity. This article describes an example of analyzing the arsenic species contained in apple juice using an LC-ICP-MS.

Conclusion

This study confirmed that the LC-ICP-MS system can be used to analyze arsenic species in apple juice spiked with arsenic and pretreated simply by dilution.

And this result is below the action level of 10 μg/kg for inorganic arsenic set by The Food and Drug Administration’s (FDA) and this apple juice is generally considered safe.²⁾