The advent of Reagent-Free™ Ion Chromatography (RFIC™) has fundamentally changed the practice of ion chromatography in laboratories worldwide.    RFIC systems make it possible to perform a wide range of ion chromatographic separations using only deionized water as the carrier.  RFIC systems combine three core technologies: electrolytic eluent generation that generates acid, base, or salt eluents for IC separations, self-regenerating electrolytic suppression that produces the regenerant ions necessary for eluent suppression, and continuously regenerated trap column (CR-TC) that removes trace-level contaminants.  For many applications, RFIC systems provide high performance with increased sensitivity and the flexibility to perform isocratic and gradient separations using alkali hydroxides (e.g., KOH), methanesulfonic acid (MSA), or carbonate/bicarbonate eluents.  The RFIC systems offer IC users the benefits of simplicity and ease of use, and improved reproducibility.  In addition to saving time, labor, and operating costs, RFIC systems eliminate errors associated with manual eluent preparation. This effectively improves IC method performance and reproducibility.  In this presentation, we will review the operation principles and development history of key electrolytic devices used in the RFIC systems.  We will also discuss the current state-of-the art of RFIC systems and their used in conventional-scale and capillary-scale IC separations of target analytes in various sample matrices.

This presentation will detail the latest capability in high-performance suppressed ion chromatography coupled with mass spectrometry detection, specifically triple-quadrupole mass spectrometry for quantitative applications. Working with colleagues across fields of environmental sciences and climate change, natural product development and the aquacultural sciences, our IC-MS system has delivered outstanding sensitivity and analytical performance in applications where selective trace and ultra-trace analysis of small inorganic and organic ions are required. The presentation will include three specific projects, the analysis of aerosols for bushfire biomarkers, the analysis of aquacultural saline waters for oxyhalides species, and the analysis of xylooligosaccharides from lignocellulosic biomass. Challenges, solutions and quantitative outcomes will be presented. 

Glycans play a critical role in all biology, existing either as free sugars or attached to macromolecules pre- or post-translationally. Glycans can dramatically alter the function of macromolecules, and therefore, understanding a molecular system necessitates the identification and characterization of all the sugars in the system’s glycome. Few tools are currently available to analyze the glycome without derivatization, and fewer still are available for the unbiased characterization of the total glycome without dividing it into targeted subsets. In this talk, we described the implementation of a novel column, the Thermo Scientific™ CarboPac™ PA300-4µm column, in an HPAE-PAD-MS platform for the detection and structural characterization of oligosaccharides from biological and food samples. The detailed instrument setup coupled with the CarboPac PA300-4µm affords an unbiased window into the total glycome, allowing for the characterization of both neutral and charged species alike.

Haloacetic acids (HAAs) are among the disinfection byproducts produced during chlorination of water. EPA method 552.3 using GC-ECD requires extraction and derivatization that can take up to 4 hours. Ion chromatography-mass spectrometry (IC-MS/MS), per EPA Method 557 provides results that can be analyzed in 35 min. This presentation shows (IC-MS/MS) system to system variability with results from a repeatability study of multiple systems using HAA9, Bromate, and Dalapon. 

The sample-to-results workflow uses a modified QuPPe extraction with cartridge solid-phase extraction clean-up. Analysis of wheat, leek and baby food samples, with and without the use of labelled internal standards to determine calibration approaches producing results fully compliant with the EU SANTE guidelines for validation and ongoing quality control. The workflow is available as an “off-the-shelf kit,” which includes all instruments, software, necessary consumables, suitability check standard solutions, and a detailed deployment guide for fast implementation and enablement of ongoing optimum performance. You will discover the advantages of IC over other separation techniques, gain a better appreciation of the overall productivity benefits provided by the Thermo Scientific™ Anionic Pesticide Explorer workflow and the level of compliance, productivity and robustness possible by using the workflow in routine analysis.
 

The quantification of hydrogen peroxide can be challenging. Its small molecular structure and high oxidization strength make it very reactive. Many methods involved derivatization with some form of a chemical reaction. However, they are not always very reliable or reproducible. This talk will cover how to assay hydrogen peroxide directly, using High-Performance Anion Exchange chromatography with pulse amperometry detection (HPAE-PAD). There is no derivatization required. This method can be used for low-level analysis such as cleaning swabs and assaying the purity of hydrogen peroxide in the Semicon industry.

This presentation will cover the methods used for analyzing sugars in food in a busy contract testing laboratory  to meet nutritional information requirements and why ion chromatography is the technique of choice to cover this vital analysis.

This session will focus on troubleshooting in ion chromatography. A strategic framework for successful troubleshooting in ion chromatography will be discussed. The presentation will cover column, suppressor and detector related troubleshooting. Example chromatographic data and written descriptions will be provided to illustrate issues observed in ion chromatography. Attendees will have a chance to vote on the most likely explanation for each performance issue prior to a reveal of the root cause. 

This talk will cover anion exchange, cation-exchange and carbohydrate separation stationary phases. For each class of stationary phases, the earliest implementation will be discussed along with relevant technical developments over succeeding years. In addition, recent new product introductions and possible future directions for new products will also be discussed. 

An insight into what is key to everyday assays when switching to ion chromatography-mass spectrometry. This talk will look at how simple it is to combine ion chromatography with mass spectrometry with Thermo Fisher Scientific hardware and software, and sharing data to show how you can elevate your workflows for key application areas such as anions, polar pesticides and haloacetic acids.

Maintaining ultra clean water in boiler cooling systems is vital for power plants to avoid the risk of corrosion.  As consultants to the power industry, we regularly supply methodology to analyse trace anions and cations for plant upkeep.  This presentation will demonstrate the importance of trace analysis to the power industry and the method improvements that were made when we upgraded our IC system to the Thermo Scientific™ Dionex™ Integrion™.

This talk will explore how HPAEC-PAD can be utilised for in depth characterisation of carbohydrate active enzymes and polysaccharide utilisation systems from members of the human gut microbiota.

"Pesticides" is a term that covers over 1000 compounds. Lucky, a great majority of them can be extracted with one of the generic extraction protocols (QuEChERS, SweEt, miniLuke) and subsequently analysed by LC-MS/MS or GC-MS/MS. Nevertheless, some compounds require a special approach, highly polar and ionic pesticides (e.g. glyphosate and its metabolites) are amongst them. Derivatisation overcomes the problem with poor retention in reversed-phase chromatography, however this approach is laborious, and it cannot be applied to all ionic compounds. Ion chromatography is an interesting solution for the problems with chromatographic analysis of polar pesticides. This technique provides reasonable retention times for a broad spectrum of polar analytes. Although the mobile phase contains potassium hydroxide, the suppressor makes the effluent fully compatible with the electrospray ionisation and mass spectrometry. The presentation will give a short overview of the applications and benefits of high-performance ion chromatography coupled to high-resolution mass spectrometry. Both qualitative and quantitative aspects of the pesticide residue analysis will be discussed. Amongst the matrices, there will be fruit and vegetables, acorns, honey, and pollen.

The presentation will show how combustion-IC can be utilized to increase quality, efficiency and automation of the measurement of the individual halogens and sulphur in primary and secondary energy sources, industrial raw materials, intermediates, final products as well as residues and waste water. There will be examples from different industries to spotlight the opportunities while informing on technical requirements for a robust routine.

In Europe, haloacetic acids are recently regulated in drinking water due to their health effects. These compounds are the second most prevalent class of disinfection by-products in drinking water after THMs and the first one in swimming pools. In the literature, the analytical techniques of liquid or gas chromatography, coupled with single or triple quadrupole detectors are often preceded by time-consuming and costly preparation steps. LERES has developed a method for the analysis of regulated and non-regulated HAAs with an IC-MS. The method is simple, without sample preparation, very sensitive and solvent free. In the first half of 2020, the method was used for an analysis campaign in drinking water and swimming pools in Brittany. The analytical method and some results of this campaign are presented.

The rise in the need for greener energy has led to more R&D into long lfe batteries, typically using Lithium ion technology.  This presentation will look at the uses of IC with mass spectrometry and speciation with IC-ICP-MS as a valuable tool in researching raw materials  and in QA testing  to identify trace contaminants in lithium ion batteries. 

Since July 2018 several drugs have been recalled due to contamination with N-nitrosodimethylamine (NDMA), a probable human carcinogen. Dimethylamine (DMA) and nitrite are precursors in the formation of NDMA. Ion chromatography (IC) methods were developed for the determination of these two precursors in drug substances and drug products. . The methods for DMA should be applicable to other amines to assess the likelihood of the formation of other nitrosamines in pharmaceutical products. 

The world has created many great works of art and monumental buildings. The challenge is to maintain them for future generations. The advancement of analytical sciences over the past half century has delivered many analytical tools that have helped guide art and architecture preservation and restoration. As these practices have become more sophisticated, ion chromatography (IC) is one of the tools those charged with preservation and restoration are using. This presentation will review how IC is being used by these analysts, what they have learned, and what their applications can teach us about the practice of IC.

Perchlorate is a known groundwater and drinking water contaminant with natural and manufacturing sources. A trace level ion chromatography tandem mass spectrometry (IC-MS/MS) method has been used to analyze samples from two High Arctic ice caps, where contaminants are exclusively received from atmospheric sources. Depth samples collected from Devon and Agassiz Ice Caps (Nunavut, Canada) demonstrated the seasonal and longer term anthropogenic influence on the atmospheric perchlorate formation. A recently developed method for the analysis of Cr(VI) with a direct isotope dilution (DID) quantification approach demonstrated the capability of the IC-MS/MS instrumentation, complementing the traditional ion chromatography separation with inductively coupled plasma mass spectrometry (ICP-MS) approach presented in method EPA 6800. The technique allowed to compensate for any loss of Cr(VI) occurring between collection and analysis time that can affect sample integrity and introduce possible biases in measured concentrations. The DID method achieved trace level analysis with an MDL of 2 ng/L.

Sour natural gas contains unacceptably high concentrations of corrosive gases that must be neutralized into sweet natural gas product. The refineries neutralize the sour gas using concentrated alkanolamines, which are then regenerated during a recycling process. This presentation discusses an ion chromatography application to determine the concentration and therefore the effectiveness of the alkanolamines and the concentrations of accumulating corrosive cationic contaminants. The application using a novel stationary phase to elute the alkanolamines in an elution window between the monovalent cations and the divalent cations with a 0.4 µL injection to minimize dilution and column overload. The method development, method qualification, and sample results are presented.   

Recent developments in the analysis of anionic polar pesticides have led to an increase in testing and regulation in surface and drinking water as well as food and beverages samples. However, developments in the analysis of cationic polar pesticides have lagged their anionic counterparts, primarily because of the analytical challenges. Advances using the Quick Polar Pesticides (QuPPe) method combined with IC-MS/MS have successfully demonstrated the applicability for the analysis of anionic polar pesticides, particularly glyphosate. However, for cationic polar pesticides, previous work has demonstrated an inability to resolve the Diquat / Paraquat peak pair. This combined with their similar m/z ratios makes it difficult to use IC-MS/MS methods for this application. Cationic polar pesticides such as chlormequat, diquat, mepiquat and paraquat may occur as residues in food, but may not be included in pesticide monitoring programs due to the difficulty in the determination of these target analytes using generic multi-residue methods. To address this analytical challenge, we have recently developed the Thermo Scientific™ Dionex™ IonPac™ CS21-Fast-4µm column to provide satisfactory separation of the four key quaternary polar pesticides: chlormequat, diquat, mepiquat and paraquat. This work demonstrates a new IC-MS/MS method to identify and quantify low concentrations of quaternary amine cationic polar pesticides in foods and beverages using a Thermo Scientific™ Dionex™ ICS-6000 Ion Chromatography System and IonPac CS21-Fast-4µm column coupled with a Thermo Scientific™ TSQ Altis™ triple quadrupole electrospray mass spectrometer. In this paper, we will discuss the IC-MS/MS method and demonstrate its applicability for determination of chlormequat, diquat, mepiquat and paraquat in the extracts of food and beverage samples prepared using the QuPPe sample preparation technique.

A recently developed method for the analysis of Cr(VI) with a direct isotope dilution (DID) quantification approach demonstrated the capability of the IC-MS/MS instrumentation, complementing the traditional ion chromatography separation with inductively coupled plasma mass spectrometry (ICP-MS) approach presented in method EPA 6800. The technique allowed to compensate for any loss of Cr(VI) occurring between collection and analysis time that can affect sample integrity and introduce possible biases in measured concentrations. The DID method achieved trace level analysis with an MDL of 2 ng/L. 

Since the 1980s the electronics industry has utilized ion chromatography (IC) analysis to understand the relationship of ions, and some organics, to product reliability.  From component and board fabrication, to electronic assemblies and their end-use environment, IC analysis has been the de facto method for evaluating ionic cleanliness of electronic hardware.  Typical ions accounted for have included chloride, bromide, nitrate, sulfate, weak-organic acid (WOA), sodium and ammonium. Environmental and other concerns have driven the industry to adopt myriad flux formulations, which has created a need to further differentiate weak-organic acids beyond what a typical IC system can provide.  

By utilizing an Ion Chromatography – Mass Spectroscopy (IC–MS) system optimized for organic separation, we can use the same column technology for the typical suite of anion/organic species, then run the sample through a quadrupole mass spectrometer which provides the molecular weight assessment of residues for over two dozen channels. This capability is critical to our failure analysis work at Foresite, as it allows for identification of specific organic acids and flux activators. This information can aid in identifying specific residue sources (e.g. board fabrication, SMT paste flux, waver solder liquid flux, hand solder flux or a completely different flux pen, or bottle or paste flux). 

Artificial sweeteners are used as sugar substitutes in food and beverage products. The popularity of artificial sweeteners is increasing as more consumers are concerned about obesity and dental decay caused by consuming natural sugars. Artificial sweeteners are broadly classified into two categories: nutritive and non-nutritive sweeteners. Recently, naturally occurring rare sugars have emerged as an alternative category of sweeteners. Allulose is one such low-calorie sweetener that occurs in small amounts in wheat and dried fruits, such as raisins and dried figs. Allulose’s chemical structure is similar to fructose, but it is not metabolized in the same way and contributes less calories. For labelling purposes, it is important to determine the amount of sweetener used in low-calorie foods and beverages. High-performance anion-exchange chromatography with pulsed amperometric detection (HPAE-PAD) is a well-established technique for carbohydrate determinations. In this work, we developed and validated an HPAE-PAD method to determine sucrose and three sugar substitutes (erythritol, allulose, and sucralose) in low calorie/ zero sugar/ sugar-free foods and beverages. These sugar substitutes are often used in combination in food and beverages to create the same level of sweetness as natural sugars and minimize less desired flavors of the sugar substitutes. The separation of these sweeteners was achieved on a Thermo Scientific™ Dionex™ CarboPac PA20 column. This column facilitates determination of the sugar substitutes in sugar-free samples with minimum sample preparation and an overall injection to injection time of 25 min. In this work, we analyzed five commercial sugar-free products: two sugar-free protein bars, a keto cookie baking mix, a sugar-free vitamin water, and a zero-sugar sports drink for their erythritol, allulose, and sucralose contents. The method showed good precision and accuracy with a recovery range of 83-116% for the samples tested.

Significant effort continues in delineating the extent of Per- and Polyfluoroalkyl Substance (PFAS) environmental impacts worldwide and recent advances in remedial approaches hold promise. However, the extent of remedial effort required for many of these sites remains unknown due to the presence of unknown or uncharacterized PFAS, which are not included as part of the suite of PFASs routinely monitored. However, these may transform to the monitored compounds or otherwise contribute to the risk burden of a site. The challenge in accounting for this pool of uncharacterized PFAS (the Dark Matter) can be significant as its nature and quantity is generally unknown. The issue may become more critical as jurisdictions consider moving to a ‘P-Sufficient’ or class-based approach to PFAS regulation.i 

Bureau Veritas Laboratories is actively developing technologies to determine the magnitude of total PFAS in environmental matrices such as soil, water and biota, as well as aqueous film forming foam (AFFF) and other industrial and consumer products. In this presentation the available technologies for providing data on total PFAS will be reviewed, and a detailed explanation of Total Organofluorine by Combustion Ion Chromatography and its practical application will be discussed. We will describe achievements to date in developing practical methods for a range of matrices as well as lessons learned and anticipated next steps. The role that this new analysis option is likely to take in the investigation of PFAS sources and remediation will be described. 

Since the 1980s the electronics industry has utilized ion chromatography (IC) analysis to understand the relationship of ions, and some organics, to product reliability.  From component and board fabrication, to electronic assemblies and their end-use environment, IC analysis has been the de facto method for evaluating ionic cleanliness of electronic hardware.  Typical ions accounted for have included chloride, bromide, nitrate, sulfate, weak-organic acid (WOA), sodium and ammonium. Environmental and other concerns have driven the industry to adopt myriad flux formulations, which has created a need to further differentiate weak-organic acids beyond what a typical IC system can provide.  

By utilizing an Ion Chromatography – Mass Spectroscopy (IC–MS) system optimized for organic separation, we can use the same column technology for the typical suite of anion/organic species, then run the sample through a quadrupole mass spectrometer which provides the molecular weight assessment of residues for over two dozen channels. This capability is critical to our failure analysis work at Foresite, as it allows for identification of specific organic acids and flux activators. This information can aid in identifying specific residue sources (e.g. board fabrication, SMT paste flux, waver solder liquid flux, hand solder flux or a completely different flux pen, or bottle or paste flux). 

Modern laboratories performing applied analytical testing fulfill a wide range of tasks using different types of analytical instrumentation. In the inorganic laboratory, ion chromatography (IC) is used for the determination of common anions, analysis of disinfection byproducts or carbohydrate screening. At the same time, screening for heavy metals is accomplished using techniques such as inductively coupled plasma mass spectrometry (ICP-MS). Whereas IC is a powerful separation technique for ionic or polarizable species, ICP-MS is a powerful element selective detector. Both techniques can provide valuable information to estimate the level of contaminants in a sample, but at the same time, both techniques face limitations, that may yield only part of the story based on the analytical information that each deliver. For example, using ICP-MS, all information related to the chemical species in which an element is present is lost during the ionization process, and in many cases that makes it impossible to make judgments regarding toxic risk based solely on the concentration for a given analyte alone. With common detection systems used in conjunction with IC, such as conductivity detection, detection power may be a limiting factor, or a complex setup might be required in order to selectively convert an analyte into a photoactive compound for colorimetric detection. In these cases, it is beneficial to combine the best of both worlds – the separation power of IC and the detection sensitivity of ICP-MS, to obtain an even more powerful hyphenated system. The related activity “to identify and measure the quantities of one or more individual chemical species in a sample” is often referred to as speciation analysis. This presentation will highlight that it has never been easier to utilize hyphenated techniques in routine analysis, especially when analyzing food and beverages, where speciation can play a vital role to understand the risk associated with the presence of contaminants such as arsenic, iodine or mercury. Dedicated solutions for integrated hardware control and simple method development are key for solutions for routine application. However, modern technology to remove or eliminate spectral interferences is equally important and will also be highlighted.

Ever since the introduction of ion chromatography (IC) in 1975, suppressor devices are used in combination with conductivity detection to chemically reduce the background conductance of the electrolyte used as the eluent, while at the same time enhancing analyte conductivity and thus increasing sensitivity. Although this sensitivity increase is the primary advantage of the suppression technique in comparison with nonsuppressed conductivity detection, selectivity is also increased, because chemical modification of eluent and analytes turns the conductivity detector from a bulk-property detector into a solute-specific one. The use of high-capacity ion exchangers requiring a much higher electrolytic strength in the mobile phase as well as the hyphenation of IC with mass spectrometry are not feasible without the use of suppressor systems. 

The type of suppressor devices has changed significantly over the past four decades, starting with periodically regenerated suppressor columns in the original embodiment of IC all the way to continuously regenerated, membrane-based devices that are predominantly used today. Thermo Fisher Scientific currently offers a whole portfolio of chemically and electrolytically operated suppressor devices that are specifically designed for various applications. The scope of this workshop is to give some guidelines for selecting the right suppressor for a given application together with recommendations for their proper use.