Application Finder
- 8.000.6005Hyphenated techniques as modern detection systems in ion chromatography
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.
- 8.000.6007Determination of sulfate in denatured ethyl alcohol according to ASTM D7319
In this poster a convenient direct injection suppressed ion chromatographic method for determining chloride and sulfate in denatured ethanol samples according to ASTM D7319 is presented.
- 8.000.6009Determination of lanthanides by ion chromatography using non-suppressed conductivity and UV/VIS detection
The simultaneous ion chromatographic determination of trace-levels of lanthanides (or lanthanoides) was achieved by using either direct non-suppressed conductivity detection or UV/VIS detection after post-column reaction (PCR) with arsenazo III at 655 nm. Conductivity detection under isocratic conditions resulted in an overall analysis time of approx. 70 minutes. In contrast, the determination of the lanthanides via gradient elution and subsequent spectrophotometric detection of the arsenazo III-lanthanide(III) complexes was performed within 22 minutes. Besides the outstanding analysis time, UV/VIS detection excelled by its enhanced selectivity and sensitivity and did not suffer from interferences by ubiquitous non-lanthanide impurities such as iron(III) or other transition metals. For both conductivity and spectrophotometric detection, the inclusion of sample preconcentration steps lowered the limit of detection (LOD) to the sub-ppb range.
- 8.000.6010Inline sample preparation – An effective tool for ion analysis in pharmaceutical products
By means of azide analysis in Irbesartan a simple, fast, precise and accurate ion chromatographic method for the determination of traces of inorganic contaminants in pharmaceuticals is described. Traces of toxic azides in pharmaceutical products can accurately be determined in the sub-ppb range after Metrohm Inline Matrix Elimination using isocratic ion chromatography (IC) with suppressed conductivity detection. While the azide anions are retained on the preconcentration column, the interfering pharmaceutical matrix is washed away by a transfer solution, ideally consisting of 70% methanol and 30% ultrapure water. The analytical setup provides a well-resolved azide peak and thus alleviates the common drawback of excipient interferences, especially from the nitrate anion. Calibration with azide standards is linear over the range of 5…80 ppb, providing a coefficient of determination of 0.9995. The limit of detection (LOD) and the limit of quantification (LOQ) of azide in Irbesartan are 5 and 30 µg/L respectively; the relative standard deviations (RSD) for the peak area, peak height and retention time being smaller than 3.9%. Robustness testing involved variation of column oven temperature and composition of the transfer solution and, in terms of peak area, provided RSDs smaller than 2.8% and 3.1% respectively.
- 8.000.6011Ion chromatographic determination of anions, cations and organic acids in biofuels
Quality and process control of biofuels require straightforward, fast and accurate analysis methods. Ion chromatography (IC) is at the leading edge of this effort. Traces of anions in a gasoline/ethanol blend can accurately be determined in the sub-ppb range after Metrohm Inline Matrix Elimination using anion chromatography with conductivity detection after sequential suppression. While the analyte anions are retained on the preconcentration column, the interfering organic gasoline/bioethanol matrix is washed away.Detrimental alkali metals and water-extractable alkaline earth metals in biodiesel are determined in the sub-ppm range using cation chromatography with direct conductivity detection applying automated extraction with nitric acid and subsequent Metrohm Inline Dialysis. Unlike high-molecular substances, ions in the high-ionic strength matrix diffuse through a membrane into the low-ionic water acceptor solution. In biogas reactor samples, low-molecular-weight organic acids stem from the biodegradation of organic matter. Their profile allows important conclusions concerning conversion in the anaerobic digestion reaction. Volatile fatty acids and lactate can be accurately determined by using ion-exclusion chromatography with suppressed conductivity detection after inline dialysis or filtration.
- 8.000.6012Automated logical dilution for ion chromatographic determinations
The combination of 850 Professional IC, 858 Professional Sample Processor, Dosino and MagIC NetTM software offers a variety of sophisticated ion chromatographic sample preparation techniques. One of these is the automated inline dilution of samples.After the first sample injection, MagIC NetTM verifies if the area of the sample peak lies within the calibration range. If the measured peak area is outside these limits, the software calculates the appropriate dilution factor, dilutes and automatically re-injects the sample. For all investigated ions (Li+, Na+, K+, Ca2+, Mg2+, F-, Cl- , NO2-, Br-, NO3-, SO42- ), automated logical dilution yielded coefficients of determination (R2) better than 0.9999. Direct-injection recoveries for cations and anions were within 98.6…99.5% and 93.4…100.4% respectively. In contrast, after logical dilution, recoveries for cations and anions were within 100.1…102.9% and 98.2…102.6% respectively. The relative standard deviations for all determinations involving diluted sample solutions were smaller than 0.91%.
- 8.000.6013Analysis of produced water contaminants by ion chromatography
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.
- 8.000.6014Determination of anions and cations in aerosols by ion chromatography
The study of adverse effects of air pollution requires semi-continuous, rapid and accurate measurements of inorganic species in aerosols and their gas phase components in ambient air. The most promising instruments, often referred to as steam collecting devices, are the Particle-Into-Liquid-Sampler (PILS) coupled to wet-chemical analyzers such as a cation and/or anion chromatograph (IC) and the Monitoring instrument for AeRosols and GAses (MARGA) with two integrated ICs. Both instruments comprise gas denuders, a condensation particle growth sampler as well as pump and control devices. While PILS uses two consecutive fixed denuders and a downstream growth chamber, the MARGA system is composed of a Wet Rotating Denuder (WRD) and a Steam-Jet Aerosol Collector (SJAC). Although the aerosol samplers of PILS and MARGA use different assemblies, both apply the technique of growing aerosol particles into droplets in a supersaturated water vapor environment. Previously mixed with carrier water, the collected droplets are continuously fed into sample loops or preconcentration columns for on-line IC analysis. While PILS has been designed to sample aerosols only, MARGA additionally determines water-soluble gases. Compared to the classical denuders, which remove gases from the air sample upstream of the growth chamber, MARGA collects the gaseous species in a WRD for on-line analysis. In contrast to the gases, aerosols have low diffusion speeds and thus neither dissolve in the PILS denuders nor in the WRD. Proper selection of the ion chromatographic conditions of PILS-IC allows a precise determination, within 4 to 5 minutes, of seven major inorganic species (Na+, K+, Ca2+, Mg2+, Cl-, NO3- and SO4 2-) in fine aerosol particles. With longer analysis times (10-15 minutes) even airborne low-molecular-weight organic acids, such as acetate, formate and oxalate can be analyzed. MARGA additionally facilitates the simultaneous determination of HCl, HNO3, HNO2, SO2 and NH3.PILS and MARGA provide semi-continuous, long-term stand-alone measurements (1 week) and can measure particulate pollutants in the ng/m3 range.
- 8.000.6015Effect of eluent composition and column temperature on IC column retention times
This work was carried out with a Metrosep C 2 - 150 separation column, the following eluent parameters being investigated: nitric, tartaric, citric and oxalic acid concentration and concentration of the complexing anion of dipicolinic acid (DPA). The aim was to determine the effect of these parameters plus that of the column temperature on the retention times of alkali metals, alkaline earth metals, ammonium and amines using ion exchange chromatography with non-suppressed conductivity detection. Due to similar affinities for the ion exchange column, transition metals are difficult to separate with the classical nitric, tartaric, citric and oxalic acid eluents. Partial complexation with the dipicolinate ligand significantly shortens the retention times and improves the separation efficiency. However, too strong complexation results in a rapid passage through the column and thus in a complete loss of separation. Apart from a change in the elution order of magnesium and calcium at high DPA concentrations, other non-amine cations are only slightly affected by the eluent composition. Irrespective of the tartaric acid and nitric acid concentration in the eluent, an increase in column temperature shortens the retention times and slightly improves the peak symmetries of organic amine cations, particularly in the case of the trimethylamine cation. In contrast, an increase in column temperature in the presence of DPA concentrations exceeding 0.02 mmol/L increases the retention time of the transition metals. Depending on the separation problem, variation of the pH value, the use of a complexing agent and/or an increase in column temperature are powerful tools for broadening the scope of cation chromatography.
- 8.000.6016Advantages of multidimensional ion chromatography for trace analysis
The analytical challenge treated in the present work consists in detecting trace concentrations (ppb) of bromide in the presence of a strong chloride matrix. This problem was overcome by separating the bromide ions from the main fraction of the early eluting chloride matrix (several g/L) by applying two sequential chromatographic separations on the same column. After the first separation, the main fraction of the interfering chloride matrix is flushed to waste, while the later eluting anions are diverted to an anion-retaining preconcentration column. After elution in counter flow, the bromide ions are efficiently separated from the marginal chloride residues. The four-point calibration curves for bromide and sulfate are linear in the range of 10…100 µg/L and 200…800 µg/L and yield correlation coefficients of 0.99988 and 0.99953 respectively. For the method shown here, a second injection valve and a preconcentration column are the only additional devices needed to master this demanding separation problem.
- 8.000.6017Determination of sulfide in mining leachates
Metal precipitation and cyanide recovery in the SART process (sulfidization, acidification, recycling, thickening) depend to a great extent on the sulfide concentration. Among the flow injection analysis methods coupled to wet-chemical analyzers, the combination of a gas diffusion cell with an ion chromatograph (IC) plus subsequent direct spectrophotometric detection has proven to be one of the most convenient methods of sulfide analysis.This paper deals with the determination of sulfide anions via the coupling of a gas diffusion cell to an IC with subsequent spectrophotometric detection.
- 8.000.6033Analysis of energetic materials in various water and soil samples using HPLC and LC-MS
In modern days, a new breed of energetic (explosive) materials is emerging. Traditional aromatic nitrates are still in use, but there is dire need of analytical techniques for energetic materials in the chemical class of peroxides, azo etc. This presentation will demonstrate the use of a modern HPLC system with traditional detector (DAD) and also coupled with mass spectrometry for the analysis of abovementioned various classes of energetic materials.
- 8.000.6035New column generation with built-in intelligence
Metrohm's iColumns are the first IC columns that are equipped with a data chip that stores freely definable data, fixed column data as well as data entered by the MagIC NetTM software. Any relevant information such as column type, standard parameters, maximum pressure, etc. can be called up at any time. Analysis data continuously entered by the MagIC NetTM software guarantees a complete column and GLP-compliant surveillance irrespective of the IC system in which the column is operated. The MagIC NetTM software surveys the critical column data and indicates any infringement of limits.
- 8.000.6037Fully automated inline eluent preparation on demand
By using the 800 Dosino and the 849 Level Control as the only additional devices, Metrohm`s intelligent ion chromatography (IC) systems - the 850 Professional IC and the Compact IC family - can be easily extended to perform any unattended inline eluent preparation. Fully controlled by MagIC NetTM, the 849 Level Control monitors the eluent level while the Dosino performs all dosing and liquid handling tasks. Consecutive injections of a 250-µg/L standard over approximately 20 days revealed an excellent retention-time stability. After more than 800 consecutive injections, relative standard deviations for anions (F-, Cl-, NO2-, Br-, NO3-, PO43-, SO42-) and cations (Li+ , Na+, NH4+, K+, Ca2+, Mg2+) were smaller than 0.55 and 0.41%, respectively. In the case of a 24-hour sequence, retention-time precision for anions and cations was better than 0.09 and 0.08%, respectively. The presented inline eluent preparation system increases the retention-time reproducibility and allows the determination of anions and cations over a one-month period without manual eluent preparation.
- 8.000.6039Mercury and arsenic speciation analysis by IC-ICP/MS
By means of IC-ICP/MS, different valence states of arsenic and mercury in the form of inorganic and organic species can be sensitively and unambiguously identified in one single run. Determination of common arsenic species in biological matrices is straightforward and can be performed down to the sub-ppb level.Species transformations of mercury that occur during several sample preparation techniques, however, require the use of specific isotope dilution mass spectrometry (SIDMS). This work illustrates the decisive advantage that Environmental Protection Agency (EPA) Method 6800 (SIDMS) offers for studying the transformations of mercury species during sample preparation of fish tissue samples. Because of the unique features and benefits of EPA Method 6800, it is expected that utilization of SIDMS will increase and that this valuable tool for optimizing and validating trace-metals-speciated sample preparation will gain much wider acceptance by analytical chemists.
- 8.000.6040Improved cation separation thanks to a new column material
Comparative measurements show that the new Metrosep C 4 cation column has even better separation characteristics than the previous Metrosep C 2 and Metrosep Cation 1-2 column types. The Metrosep C 4 column has a clearly improved peak shape which leads to a better separation of the individual peaks. Using Metrosep C 4 the number of theoretical plates per meter was noticeably higher than that obtained on the Metrosep C 2 or C 1-2 column. Additionally for standard cations transition metals and amines, the Metrosep C 4 column shows better results with respect to peak shape, peak height, resolution and asymmetry factor. The clearly improved resolution of the C 4 column with its narrow and high peaks achieves baseline separation for six standard and six transition metal cations. Analysis times and peak areas obtained with the C 4 column are in the same range as those obtained with its predecessors.As a result of the latest production methods and materials, the promising Metrosep C 4 column excels by an outstanding separation performance for complex mixtures comprising standard cations, transition metal cations and amines.
- 8.000.6041Simultaneous determination of fluoride species plus acid anions in etching baths by ion chromatography with dual detection
This poster presents a straightforward ion chromatographic determination of HF, HNO3, short-chain organic acids and H2SiF6 in etching bath samples. Standard ions such as fluoride, nitrate, acetate and sulfate are determined via suppressed conductivity detection while dissolved silicate is spectrophotometrically detected in the same run after downstream post-column reaction (PCR) as molybdosilicic acid. Analytical results of several commercial HF-HNO3-H2SiF6 mixtures obtained by ion chromatography (IC) and titration showed good agreement, which confirms the applicability of the presented «dual» detection IC method for controlling the composition of acidic texturing baths.
- 8.000.6042Straightforward multipoint calibration using a single standard
The combination of 850 Professional IC, 858 Professional Sample Processor, Dosino and MagIC NetTM software offers a variety of automated ion chromatographic sample preparation and calibration techniques available as an anion, cation or dual channel system. Calibration is straightforward and requires only one multi-ion standard.Inline calibration allows the calibration of any standard concentration in the ppt range by using one single stable standard solution at the ppb level. By using a preconcentration column and switching the valves one, two or more times different calibration concentrations at the ultra-trace level can be created with unprecedented reproducibility. The inline preconcentration technique uses a pre-concentration column and is ideally suited for trace analysis in complex matrices, especially when combined with matrix elimination. Besides facilitating the preparation of g/L to ng/L calibration graphs Metrohm`s intelligent techniques are capable of logical decision making. While Metrohm`s intelligent Partial Loop technique (MiPT) allows samples with a wide concentration range to be injected without previous manual dilution, the intelligent inline dilution technique, after the first sample injection, compares peak areas, calculates, if necessary, the dilution factor, dilutes and automatically re-injects the sample. The presented inline techniques allow the rationalization of the time-consuming, error-prone and cost-intensive manual preparation of standard solutions. They guarantee that the determined sample concentrations always lie within the calibration range. Higher sample throughputs as well as lower analysis costs and improved data reliability are achieved.
- 8.000.6043Automated dialysis as a sample preparation tool in ion chromatography
The analytical challenge treated in the present work consists in the determination of chloride, phosphate and sulfate in the presence of difficult sample matrices that interact with the stationary column phase or even render it unusable. Metrohm`s patented stopped-flow dialysis coupled to the new 881 Compact IC pro ion chromatograph overcomes these drawbacks. Two standard solutions covering the concentration ranges 1.0…3.6 mg/L and 10…36 mg/L as well as two samples, an ultra-high temperature (UHT) processed milk and a baby milk powder, were characterized in terms of analyte concentration, relative standard deviation, calibration quality, carryover and recovery rates. While the five-point calibration curves yielded correlation coefficients (R) better than 0.9999, carryover (between two subsequent injections of a concentrated sample and a blank) was less than 0.49%. Recoveries for the low (10…36 mg/L) and high standard concentrations (1.0…3.6 mg/L) were within 91…99% and 94…100%, respectively. Automated compact stopped-flow dialysis is a leading-edge sample preparation technique that ensures optimum separation performance by effectively protecting the column from detrimental matrix compounds.
- 8.000.6044Fully automated sample preparation for liquid chromatographic content determinations
Inline coupling of the 815 Robotic Soliprep with an ion chromatograph (IC) allows the straightforward determination of anions and cations in tablets. After automatic solvent addition and subsequent comminution, the homogenized tablet samples (Singulair and Bezafibrat) are filtered and subsequently transferred to the injector. The completely automated sample preparation saves both time and money, guarantees traceability of each sample preparation step and yields correct and precise results. In the range of 0.2…50 mg/L, six-point calibration curves for anions and cations yield correlation coefficients better than 0.99990 and 0.99991, respectively. While relative standard deviations (RSDs) for sub-ppm levels of nitrate, sulfate, calcium and magnesium in Singulair and Bezafibrat are smaller than 3.64%, RSD of ppm levels of chloride is better than 0.83%. The application of further inline sample preparation steps such as pulverizing, extracting, filtering or diluting facilitates numerous custom-tailored setups for ion determinations in exacting matrices such as animal feed, sediments or food.
- 8.000.6045Trace-level aliphatic amines in cationic pharmaceutical ingredients
The analytical challenge treated by the present work consists in detecting sub-ppb concentrations of low-molecular-weight amines in the presence of strongly retained cationic drugs by using ion chromatography (IC) with upstream inline coupled-column matrix elimination (CCME). In contrast to direct-injection IC, where the late elution of strongly retained drugs requires eluents with added acetonitrile, the CCME technique uses two preconcentration columns in series. In an «inverse matrix elimination step, cationic drug and target amines are trapped on a high-capacity and a very-high-capacity preconcentration column, respectively. During amine determination, a rinsing solution flushes the drug to waste. This significantly shortens the analysis time and improves sensitivity as well as selectivity. Besides the determination of monomethylamine in Nebivolol hydrochloride discussed here, the CCME technique is a promising tool for detecting further low-molecular-weight amines in a wide range of drugs.
- 8.000.6052Quality assurance of biofuels
This poster provides an overview of ion chromatographic methods combined with inline sample preparation for the determination of anions and water-extractable cations in biofuels. In addition, the determination of the oxidation stability is described.
- 8.000.6053Trace-level determination of perfluorinated compounds in water by suppressed ion chromatography with inline matrix elimination
This poster describes a simple and sensitive method for the determination of perfluorooctanoate (PFOA) and perfluorooctane sulfonate (PFOS) in water samples by suppressed conductivity detection. Separation was achieved by isocratic elution on a reversed-phase column thermostated at 35 °C using an aqueous mobile phase containing boric acid and acetonitrile. The PFOA and PFOS content in the water matrix was quantified by direct injection applying a 1000 μL loop. For the concentration range of 2 to 50 μg/mL and 10 to 250 μg/mL, the linear calibration curve for PFOA and PFOS yielded correlation coefficients (R) of 0.99990 and 0.9991, respectively. The relative standard deviations were smaller than 5.8%.The presence of high concentrations of mono and divalent anions such as chloride and sulfate has no significant influence on the determination of the perfluorinated alkyl substances (PFAS). In contrast, the presence of divalent cations, such as calcium and magnesium, which are normally present in water matrices, impairs PFOS recovery. This drawback was overcome by applying Metrohm`s Inline Cation Removal. While the interfering divalent cations are exchanged for non-interfering sodium cations, PFOA and PFOS are directly transferred to the sample loop. After inline cation removal, PFAS recovery in water samples containing 350 mg/mL of Ca2+ and Mg2+ improved from 90…115% to 93…107%.While PFAS determination of low salt-containing water samples is best performed by straightforward direct-injection IC, water rich in alkaline-earth metals are best analyzed using Metrohm`s Inline Cation Removal.
- 8.000.6055Liquid handling applied to automated sample preparation in liquid chromatography
In routine chemical analysis, the predominant challenge involves a higher sample throughput, improved reproducibility, liquid handling flexibility and reduced personnel costs. In response to these requirements, the 872 Extension Module Liquid Handling in combination with the MagIC NetTM software and the well-proven Dosino technology expands the possibilities of inline sample preparation and opens up new fields of application. Among others, the module can be used, together with an optional mixing vessel, for pH adjustments, pre-column derivatizations, or the mixing of solutions.As a representative of an inline sample preparation technique, this poster describes the performance of precise dilutions. By using only one single stable standard solution, multi-point calibration curves can be automatically recorded by diluting a concentrated standard in an external vessel.
- 8.000.6057Simultaneous determination of gamma-hydroxybutyric acid (GHB) and gamma-butyrolactone (GBL) in beverages
Psychoactive gamma-hydroxybutyrate (GHB) and its prodrug gamma-butyrolactone (GBL) are substances that are increasingly abused as date-rape and recreational (party) drugs. Since the non-controlled GBL converts into the illicit GHB both in-vivo and in-vitro, their legal distinction is of crucial importance.For the forensic determination of illegally added GHB and GBL in commonly consumed beverages, this work presents a simple and sensitive method that employs direct-injection ion chromatography combined with spectrophotometric detection. The method allows to trace GHB-GLB interconversion, whether in vivo or in vitro lactone cleavage or intramolecular GHB esterification, and thus complies with pertinent requirements of law enforcement agencies.
- 8.000.6058Analysis of airborne particulate matter by PILS-IC
This study compares air sampling data obtained by a filter-based method including off-line manual filter extraction followed by ion chromatographic analysis with those gained by an automated Particle-Into-Liquid-Sampler coupled to an ion chromatograph (PILS-IC).PILS-IC is a straightforward instrument for aerosol sampling that provides near real-time measurements for long-term unattended operation and is thus an indispensable tool to monitor rapid changes in aerosol particle ionic composition.
- 8.000.6059Determination of hazardous substances in electrical and electronic equipment
The Restriction of Hazardous Substances (RoHS) Directive 2002/95/EC stipulates maximum limits for the hazardous metals cadmium, lead and mercury as well as the hexavalent chromium and the brominated flame retardants in electrical and electronic products. To ensure compliance, reliable analysis methods are required.This poster deals with the wet-chemical determination of trace concentrations of the six RoHS-restricted substances in a wide variety of materials including metals, electrotechnical components, plastics and wires. After sample preparation according to IEC 62321, the metals lead, cadmium and mercury are best determined by anodic stripping voltammetry (ASV) and the flame retardants PBB and PBDE are quantified by direct-injection ion chromatography (IC) using spectrophotometric detection. Chromium(VI) can be determined either by adsorptive stripping voltammetry (AdSV) or IC. Both methods are very sensitive and meet prescribed RoHS limits.
- 8.000.6063Post-column chemistry for improved optical absorption detection
UV/VIS detection is one of the most sensitive detection techniques in trace-level chromatography. Sometimes, however, spectrophotometric detection lacks sensitivity, selectivity or reproducibility and chemical derivatizations are required. By using Metrohm`s rugged and versatile flow-through reactor, single- or multi-step derivatizations can be done fully automatically, in either pre- or post-column mode at any temperature between 25…120 °C. The variable reactor geometry allows to adjust the reactor residence time of the reactants according to derivatization kinetics. The flexibility of the reactor is demonstrated by optimizing four widespread post-column techniques: the relatively slow ninhydrin reaction with amino acids and the fast derivatizations of silicate, bromate and chromate(VI).
- 8.000.6064Microbore columns: a contribution to green chemistry
Available sample size, mass sensitivity, efficiency and the detector type are important criteria in the selection of separation column dimensions. Compared to conventional 4 mm i.d. columns, microbore columns excel, above all, by their low eluent consumption. Once an eluent is prepared, it can be used for a long time. Additionally, the lower flow rates of microbore columns facilitate the hyphenation to mass spectrometers due to the improved ionization efficiency in the ion source.With the same injected sample amount, a halved column diameter involves a lower eluent flow and results in an approximate four-fold sensitivity increase. In a converse conclusion, this means that with less sample amount, microbore columns achieve the same chromatographic sensitivity and resolution than normal bore columns. This makes them ideally suited for samples of limited availability.
- 8.000.6065Automated ion chromatographic determinations over six orders of magnitude
Metrohm`s intelligent Preconcentration Technique with Matrix Elimination (MiPCT-ME) excels in its capacity to perform automatic ion chromatographic determinations over 6 orders of magnitude. Crucial requirements for this are the system`s intelligence and the exact measurement of the sample volume. While the intelligence allows to compare results and take decisions, the dosing device takes over the high-precision liquid handling of even single-digit microliter volumes to the preconcentration column. By using only one analytical setup and without additional rinsing, samples containing both ultratraces and high concentrations can be analyzed.As the other Metrohm Inline Techniques, the MiPCT-ME technique presented reduces the workload, ensures complete traceability, is free of carryover effects and significantly improves accuracy and reproducibility of the results.
- 8.000.6071Trace-level determination of anions in the primary circuit of a PWR-type nuclear power plant using ion chromatography after inline sample preparation
The poster presents the ion chromatographic determination of organic degradation products such as glycolate, formate and acetate besides the standard anions fluoride, chloride, nitrate and sulfate.
- 8.000.6072Trace-level determination of cations in the secondary circuit of a PWR-type nuclear power plant using ion chromatography after inline sample preparation
The presented IC system with inline sample preparation allows the determination of traces of lithium and sodium (ppt) in the presence of ppm quantities of ammonium and ethanolamine.
- 8.000.6073Determination of anions in concentrated nitric acid by ion chromatography: the influence of temperature on column selectivity
Determination of chloride and sulfate in the presence of high nitrate concentrations. Optimization of the chromatographic separation by variation of the temperature and eluent composition.
- 8.000.6074Influence of pH, temperature, and molybdate concentration on the performance of the triiodide method for the trace-level determination of bromate (EPA 326)
This poster discusses results showing the influence of pH, temperature of the post-column reactor, eluent composition, and iodide concentration on the sensitivity of the triiodide method.
- 8.000.6075Determination of pyrophosphate, trimetaphosphate, tripolyphosphate, and standard ions in detergents or fertilizers using IC with a high-capacity suppressor
Three different suppressor systems are compared in terms of sensitivity. Additionally, binary gradient elution was applied to analyze phosphates in the presence of mono- and divalent ions.
- 8.000.6076Sequential suppression for conductivity detection in ion chromatography
The poster describes how different suppressors (MSM and MCS) work and mentions possible applications.
- 8.000.6085Monitoring of iodine- and gadolinium-containing contrast media in water treatment plants
The combination of ion chromatography (IC) and inductively coupled plasma mass spectrometry (ICP/MS) provides a rapid, reliable, and sensitive speciation analysis of wastewater-relevant free and complexed gadolinium compounds. IC-ICP/MS proceeds without costly sample preparation and provides important information on the supply, degradation, and fate of the contrast agents in the (waste)water. The method is also highly suitable for determining compounds containing gadolinium in biological matrixes such as urine or blood.Additionally, IC-ICP/MS is a powerful tool for monitoring inorganic and iodine-containing ionic oxidation byproducts that form during ozonation of iodinated X-contrast media.
- 8.000.6086Semi-continuous determination of anions, cations, and heavy metals in aerosols using PILS-IC-VA
This poster presents an approach that couples a Particle-Into-Liquid-Sampler (PILS) to a dual-channel ion chromatograph (IC) for measurement of aerosol anions and cations and a voltammetric measuring stand (VA) to determine the heavy metals. Feasibility of the PILS-IC-VA online system was demonstrated by collecting aerosol samples in Herisau Switzerland, at defined time intervals; air pollution events were simulated by burning lead- and cadmium-coated sparklers.
- 8.000.6087Determination of hexavalent chromium in drinking water according to a U.S. EPA Method
This poster looks at the possibility to modify the existing EPA Method to meet California's rigorous public health goal (PHG) of 0.02 µg/L. After optimizing instrument settings and method parameters, a method detection limit (MDL) of 0.01 µg/L is obtained.
- 8.000.6091Ion chromatographic determination of halogens and sulfur in solids using combustion as inline sample preparation
The Combustion IC system presented allows the automated determination of organic halogen and sulfur compounds in all flammable samples. Both combustion digestion, which is automatically controlled with a flame sensor, and the professional Liquid Handling guarantee highest precision and trueness. This poster describes the determination of the halogen and sulfur content in a certified polymer standard, a coal reference material as well as in latex and vinyl gloves.
- 8.000.6101Analysis of Anions and Oxoanions using Ion Chromatography Mass Spectrometry (IC-MS)
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.
- 8.000.6102Ion chromatography – the all-rounder for pharmaceutical analysis
Pharmaceutical analysis guarantees drug safety by providing information on the identity, content, quality, purity, and stability of pharmaceutical products using analytical chemistry. Ion chromatography (IC) offers a broad range of pharmacopeia-compliant applications for quality control, monitoring, and improving drug manufacturing.As a very accurate and versatile technique, IC meets the requirements of many pharmaceutical applications. IC is a USP-accepted standard method for the determination of active pharmaceutical ingredients (APIs), excipients, impurities,pharmaceutical solutions as well as pharmaceutical starting materials, finished pharmaceutical products (FPPs) and even body fluids.This poster describes some typical examples.
- 8.000.6103Speciation of Cr(III) and Cr(VI) by IC-ICP-MS and Empower 3
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.
- 8.000.6105Selective and Sensitive determination of Zinc in Various OTC formulations as per USP <591>
This poster presented jointly with USP at AAPS meeting shows the new USP method for zinc as per <591> using Ion Chromatography which is highly selective and sensitive. Selectivity is achieved by separation and further improved with PCR reaction. Sensitivity and wide linear quantification limit make the new USP method ideal for QA/QC. Automated PCR delivery makes the overall method performance easy to validate.
- 8.000.6106Potassium Assay in OTC Drug Products by Ion Chromatography
This poster presented jointly with USP at AAPS meeting shows, that we successfully developed and validated a single IC procedure for potassium assay and identification in potassium bicarbonate and potassium chloride for effervescent oral suspension. The optimized chromatographic conditions could be used for other cationic impurities, such as magnesium, calcium, sodium, and ammonium in potassium bicarbonate and potassium chloride for effervescent oral suspension. Single chromatographic method for assay and identification simplifies the overall QA/QC workflow.
- 8.000.6107USP Modernization Initiative: Ionic Impurities in Drug Substances by Ion Chromatography
This poster presented jointly with USP at AAPS meeting shows, that we successfully validated an IC method to determine chloride and sulfate in drug substances, potassium bicarbonate and potassium carbonate. The proposed IC method overcomes limitations of the turbidimetry/visual comparison methods.
- 8.000.6109USP Modernization Initiative: Iodide Assay by Ion Chromatography
Potassium iodide (KI) is used to treat overactive thyroid and to protect the thyroid gland from the effects of radiation from inhaled or swallowed radioactive iodine. Currently, in the USP Potassium Iodide Monograph, iodide identification is performed by wet chemistry and assay by manual titration, which has a history of reduced precision and accuracy. As part of USP’s global monograph modernization initiative, an alternative selective and sensitive method was developed and validated – ion chromatography (IC). The proposed IC method can also be used for the identification test as an alternative to wet chemistry.
- 8.000.6110Fluoride in OTC Products by Ion Chromatography
Fluoride is commonly used in dental products to help prevent tooth decay. When fluoride is present in high concentrations, these products are regulated by 21 CFR 355. Three fluoride compounds used in over the counter (OTC) anti‐cavity dental products are sodium fluoride, stannous fluoride and sodium monofluorophosphate (MFP). The assay of fluoride in these active ingredients and finished formulations are determined by manual titration, or by ion‐selective electrodes. As a part of USP’s global monograph modernization initiative, an alternative selective and sensitive method has been developed and validated – ion chromatography (IC). The proposed IC method can also be used for the identification test as an alternative to the wet chemistry method.
- 8.000.6112Technical Poster: Haloacetic acids in water
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.
- AB-128Electrochemical detection in HPLC
In our Instructions for Use for the 656 Electrochemical Detector the user will find all the basic information about how it works and how to use it as well as how to handle the electrodes. They also contain information about the demands placed on the separating system together with the causes of and remedies for detection problems.Application Bulletin no. 128 is intended to provide an overview of the most important substance classes and mention some compounds that can easily be determined oxidatively, i.e., with detection limits in the pg range; it also mentions possible working conditions for separation and electrochemical detection and illustrates them with examples.