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Perchlorate contamination in drinking water may have different sources. Besides natural deposits, anthropogenic sources like fertilizers and rocket fuel residue add to hazardous water contamination. Perchlorate interferes with iodine uptake into the thyroid gland. Newborns and children are particularly vulnerable, affected as thyroid hormones are essential for growth. Besides ion chromatography (IC) followed conductivity detection, IC hyphenated with an MS detector can be used to measure perchlorate down to sub-µg/L levels. In this application IC is hyphenated with a triple-quadrupole MS (IC-MS/MS) for perchlorate determination in order to meet the requirements of EPA 332.0. This IC-MS/MS setup avoids the possible interference of sulfate.

Ion chromatography mass spectrometry (IC-MS) is a powerful tool that can handle many challenging analytical tasks which cannot be performed adequately by IC alone. IC-MS is a robust, sensitive, and selective technique used for the determination of polar contaminants like inorganic anions, organic acids, haloacetic acids, oxyhalides, or alkali and alkaline earth metals. After separation of the sample components via IC, mass selective detection guarantees peak identity with low detection limits. The inclusion of automated Metrohm Inline Sample Preparation (MISP) allows not only water samples, but also chemicals, organic solvents, or post-explosion residues to be readily analyzed without need for extensive manual laboratory work. This White Paper explains the benefits of IC-MS over IC in certain cases, the hyphenation of IC and different MS systems, as well as related norms and standards.

The combination of ion chromatography and inductively coupled plasma mass spectrometry (IC-ICP/MS) is ideally suited for the detection of species of arsenic and mercury in their various oxidation levels and forms of chemical bonding. However, some species – as in the case of mercury – are reciprocally converted into one another during sample preparation, thus making a determination of the initial concentrations of the heavy metal species impossible. This article shows how these interconversions can be calculated with isotope dilution analysis and IC-ICP/MS in accordance with EPA method 6800.

This white paper presents IC-MS as powerful analysis technique. This multiparameter method determines various analytes such as inorganic cations and amines in one run.

On the basis of the experiments that have been performed, it is possible to determine the effectiveness of the ozonization of iodized X-ray contrast media using IC-ICP-MS via the amount of iodate formed. Whereas a 120-minute ozonization guarantees a practically quantitative decomposition of amidotrizoic acid to iodate, approximately 16% of the Iomeprol is still present under the same ozonization conditions. Given that only 14% is present in iodate form in the absence of iodide anions and given that additional, not yet identified peaks occur in the ion chromatogram, the presence of additional decomposition products containing iodine must be assumed. Nonetheless, it is not possible to detect the intact iodized X-ray contrast media with the selected ion chromatographic conditions. Furthermore, the possibility exists of identifying the peak of the unknown decomposition product of the Iomeprol using IC-ESI-TOF-MS.

Urea is not a typical analyte for ion chromatography. In combination with MS, however, IC is the method of choice for the trace analysis of urea in ultrapure water. This Application Note shows the determination of urea concentrations in the ppb range using the Metrosep C 6 - 250/4.0 column.

Ion chromatography tackles difficult separation problems of various ionic species and typically works with conductivity detection. Mass detection as a secondary independent detector significantly lowers the detection limits and confirms the identity of analytes even when coeluting. This poster describes how the combination of IC-MS and automated sample preparation techniques cope with the analysis of anions and oxoanions in challenging matrices such as soil or explosion residues.

Speciation analysis of iron is important, given that its oxidation level has a great influence on environmental response, not only with respect to its absorption by organisms but also to the transport and the storage of the element. Iron(II) and Iron(III) are separated on the Metrosep A Supp 10 S-Guard/4.0 column. IC-ICP/MS with isotope dilution is used for quantification.

This poster demonstrates the feasibility of coupling a Metrohm IC system to a PerkinElmer NexION ICP-MS, operated under Empower 3 Software.Using a Metrosep Carb 2 column, the chromatographic separation of both species was achieved with a high resolution. Low background and high sensitivity allow determination in the low ng/L range.Optimal separation and full complexation of Cr(III) is already possible with EDTA concentrations from 40 μmol/L in low matrix solutions and may need to be increased depending on the sample matrix.Handling of the system was easy and user friendly. It was shown that speciation of Cr(III) and Cr(VI) can be carried out on this system utilizing a professional data system for acquisition, processing, and reporting.

The new DIN draft standard 38407-53 outlines TFA analysis in water using direct injection LC-MS/MS, enabling quantification from 0.1–3.0 μg/L as shown in this Application Note.

Differentiation between Cr(III) and Cr(VI) is possible following ISO 24384 guidelines by combining ion chromatography with inductively coupled plasma mass spectrometry.

Determination of diethylamine and trimethylamine using cation chromatography with MS detection.

Determination of acetic, propionic, butyric, valeric, and caproic acid in produced water using anion chromatography with conductivity and MS detection after post-column addition of ammonia for MS detection and inline sample preparation by dialysis.

Hexavalent chromium, also referred to as chromate or Cr(VI), is considered toxic and potentially carcinogenic, which is why its concentrations in drinking water should be kept as low as possible. Determination of Cr(VI) is performed by combining ion chromatography with ICP/MS. Separation takes place on the Metrosep A Supp 1 Guard/4.6.

Determination of chlorite, chlorate, and perchlorate in explosion residue using anion chromatography with conductivity and MS detection in tandem.

Chromate (Cr(VI)) is considered toxic and potentially carcinogenic, which is why its concentrations in children's toys should be kept as low as possible. The EU directive 2009/48/EC defines limit values for the migration of chromate from children's toys. The hydrochloric-acid-containing migration solution is diluted with a buffer. 2000 μL of this solution are injected automatically using intelligent preconcentration technology and matrix elimination. Detection takes place via ICP/MS.

The maximum contaminant concentrations (Maximal Contaminant Level, MCL) of inorganic arsenic and selenium species in drinking water should not exceed 10 and 50 µg/L, respectively. Given that each of the two elements occurs in two oxidation levels – trivalent and pentavalent – a separation step is necessary prior to ICP/MS detection. This Application Note shows the simultaneous determination of the two arsenic (arsenite and arsenate) and selenium species (selenite and selenate). Separation takes place on the Metrosep Dual 3 - 100/4.0 column.

Determination of phosphate in produced water containing up to 100 g/L chloride as well as crude oil using anion chromatography with conductivity and MS detection after inline dialysis.

This article describes the investigation using ion chromatography and subsequent inductively coupled plasma mass spectronomy (ICP/MS) to determine the extent to which the iron(III) flocculation carried out in the context of wastewater treatment releases toxic gadolinium(III) ions as the result of recomplexing.

As a rule, soil contains small percentages of chromium that originate chiefly from rock weathering processes, although anthropogenic sources also exist. The speciation analysis of trivalent – Cr(III) – and hexavalent chromium – Cr(VI) – is important, because the former is a trace element and the latter is highly toxic. The two chromium species are separated as Cr(III)-EDTA-complex and chromate on the Metrosep A Supp 4 - 250/4.0 column. Mass spectrometric isotope dilution analysis (SIDMS) is used for quantification.

Determination of bromide and bromate in drinking water using anion chromatography with MS detection.

LC-MS/MS quantification methods are commonly used to determine trace levels of organic compounds. However, highly polar reversed phases (RPs) lack sufficient retention for very polar compounds, or they fail for charged organics. Separation using ion chromatography (IC) and subsequent MS/MS detection is an innovative alternative approach that combines the fast elution and flexibility of the IC system with the excellent resolution and high sensitivity of the MS/MS detector. This poster presents a fast, robust and reliable IC-MS/MS method for the detection of HAAs and other ionic analytes using the high-end MS/MS system QTRAP 6500+ from SCIEX coupled to a the 940 Professional IC Vario One SeS/PP/HPG instrument. This analytical setup is able to identify and quantify the presence of HAAs at trace levels with LLODs between 0.02 μg/mL and 0.2 μg/L on a single HAA. This capability easily fulfills the sensitivity requirements specified in EU Drinking Water Directive, which specifies a maximum residue level (MRL) of 60 mg/mL for the sum of monochloroacetic acid, dichloroacetic acid, trichloroacetic acid, monobromoacetic acid and dibromoacetic acid present in the representative sample.

The coupling of highly efficient ion chromatography (IC) to multi-dimensional detectors such as a mass spectrometer (MS) or an inductively coupled plasma mass spectrometer (ICP/MS) significantly increases sensitivity while simultaneously reducing possible matrix interference to the absolute minimum. By means of IC/MS several oxyhalides such as bromate and perchlorate can be detected in the sub-ppb range. Additionally, organic acids can be precisely quantified through mass-based determination even in the presence of high salt matrices. By means of IC-ICP/MS different valence states of the potentially hazardous chromium, arsenic and selenium in the form of inorganic and organic species can be sensitively and unambiguously identified in one single run.

Chlorinating drinking water can form carcinogenic byproducts. EPA Method 557 enables µg/L-level quantification of haloacetic acids using Metrohm IC-MS/MS technology.

During drinking water disinfection with chlorine, chloramine, or ozone, potentially toxic halogenated byproducts can be formed. The disinfectants can react with naturally occurring bromide and/or organic matter in the source water and form one of the most common and highly toxic disinfection byproducts (DBPs): haloacetic acids (HAAs). To protect human health, maximum tolerable levels of HAA in drinking waters are regulated (EPA 816-F-09-004). The EPA Method 557 specifies the analysis of HAAs beside bromate and dalapon by ion chromatography coupled to tandem mass spectroscopy (IC-MS/MS) with LODs varying from 0.02–0.11 µg/L. However, even with single MS, a high sensitivity is achieved to determine the current MCLs within an adequate accuracy. This Application Note describes the analysis of bromate, chlorite, monochloroacetic acid (MCAA), monobromoacetic acid (MBAA), bromochloroacetic acid (BCAA), bromodichloroacetic acid (BDCAA), dibromoacetic acid (DBAA), dichloroacetic acid (DCAA), tribromoacetic acid (TBAA), chlorodibromoacetic acid (CDBAA), and trichloroacetic acid (TCAA) with IC/MS. The Metrohm Driver 2.1 for EmpowerTM offers the analysis as a single software solution with EmpowerTM.

This White Paper focuses on selected IC-MS applications for the straightforward identification and quantification of organic acids and inorganic anions in different matrices.

The analytical challenge treated by the present work consists in detecting sub-ppm quantities of bromide, sulfate, aliphatic monocarboxylic acids and several alkaline earth metals in the presence of very high concentrations of sodium and chloride. Bromide, sulfate, acetate and butyrate can be reliably determined by suppressed conductivity detection. Due to matrix effects, propionate can only be detected qualitatively. This drawback can be overcome by coupling the ion chromatograph (IC) to a mass spectrometric (MS) detector. This results in reduced matrix interferences and significantly enhanced sensitivities. The cations magnesium, barium and strontium are determined by non-suppressed conductivity detection.

AOF (adsorbable organic fluorine) is used to screen for per- and polyfluorinated alkyl substances in aqueous matrices via pyrohydrolytic combustion and ion chromatography.

Drinking water which has been disinfected via the ozonation process can contain undesirable levels of bromate, a carcinogen, via oxidation of bromide in the raw water. Already several agencies including the World Health Organization have recommended concentration limits for bromate set in place to limit its risks to our health. Ion chromatography is mentioned in several analytical standards for the determination of disinfection byproducts (DBP) including bromate, such as EPA 300.1, 317.0, 321.8, 326.0, ASTM D6581, ISO 11206, and ISO 15061. Monitoring trace levels of bromate online means higher throughput and less time spent performing manual laboratory tests, and ensures quality drinking water is produced.

Forensic institutes examine terrorist attacks and warfare agents via trace detection analysis of the used explosives and their residuals. Of particular importance is the acquisition of «chemical fingerprints» for criminal investigation departments and governmental security agencies. Institutes for public health and environmental protection analyze such compounds that can contaminate the underlying soil and infiltrate ground water.Forensic investigation with ion chromatography (IC) using suppressed conductivity detection allows a sensitive and robust determination of anionic contaminants such as chlorate, thiosulfate, thiocyanate, and perchlorate next to the common inorganic anions over a broad concentration range.

This application focuses on the simultaneous analysis of cations and suppressed anions with a dual channel Metrohm IC operated by OpenLab CDS.

This Process Application Note describes a method to determine the strontium and barium concentration in brine as early detectors ofmembrane fouling via online process ion chromatography. Using this multiparameter analytical technique can help reduce the risk of premature membrane fouling and avoid unexpected maintenance and high utility costs with 24/7 automated analysis.

Organic halides must be monitored in the environment. Combustion ion chromatography (CIC) is used for accurate halogen analysis in solids following EN 17813:2023.