Aplikace

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.

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.

Benzbromaron is one of the main uricosuric drugs currently used. In addition to sophisticated and expensive LC-MS and GC-MS methods, benzbromaron can be effectively determined by titration with sodium hydroxide solution using a straightforward, fully automated sample preparation method. A high-frequency homogenizer comminutes one or three tablets within 90 or 120 s respectively. The overall analysis time is 8 minutes. Ten-fold determinations with one and three tablets resulted in a benzbromaron content of 99.2 and 98.7 mg per tablet respectively. Increasing the number of tablets from one to three lowers the RSD from 1.36 to 0.88%. These results show an excellent agreement with the benzbromaron content indicated by the manufacturer (approx. 100 mg/tablet).Besides the presented Titrando/homogenizer combination, the other two members of the 815 Robotic Soliprep Sample Processor family offer comprehensive sample preparation possibilities within the fields of IC, HPLC, ICP or voltammetry.

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.

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.

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).

The analysis described in this poster dicusses thermometric titration as a promising method for the straightforward sodium determination in foodstuffs. Thermometric sodium titration was tested for its applicability to various food matrices such as soups, gravy and several salty snacks. Enthalpy change can be monitored as a change in temperature of the solution using a sensitive digital thermometer. The sodium determination described here relies on the exothermic precipitation of elpasolite (NaK2AlF6). The titrant is a standard aluminum solution which contains an excess of potassium ions. The titration is performed directly on a suspension of the food sample and is completed in under two minutes. The method is robust, can be fully automated and due to the highly reproducible high-frequency homogenization, copes with a variety of challenging food matrices (ketchup, instant soups, pretzels, etc.). In addition to this application note, you can find more information on thermometric sodium determination in foods in our application video available on YouTube: https://youtu.be/lnCp9jBxoEs

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.

The poster describes the development of an automated Karl Fischer method for determining the water content in different edible oils.

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.

Non-enzymatic ethanol sensor based on a nanostructured disposable screen-printed electrode.

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.

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.

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.

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.

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.

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%.

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.

A complete tap water analysis includes the determination of the pH value, the alkalinity and the total water hardness. Both the pH measurement and the pH titration by means of a standard pH electrode suffer from several drawbacks. First, the response time of several minutes is too long and, above all, the stirring rate significantly influences the measured pH value. Unlike these standard pH electrodes, the Aquatrode Plus with its special glass membrane guarantees rapid, correct and very precise pH measurements and pH titrations in solutions that have a low ionic strength or are weakly buffered. Total water hardness is ideally determined by a calcium ion-selective electrode (Ca ISE). In a complexometric titration, calcium and magnesium can be simultaneously determined up to a calcium/magnesium ratio of 10:1. Detection limits for both ions are in the range of 0.01 mmol/L.

Compared to the classical Epton titration, potentiometrically indicated two-phase titrations using organic-solvent-resistant Surfactrodes can be easily automated and require no toxic and environmentally hazardous chloroform. Even challenging matrices such as fats and oils in bath oils and hair conditioners or strong oxidizing agents in washing powder and industrial cleaners do not interfere with the titration of the ionic surfactants. Results obtained show excellent agreement to those of the Epton titration. Irrespective of the matrix, relative standard deviations of threefold determinations are all below 2.1%. While the Surfactrode Resistant is mainly used for oil-containing formulations, the Surfactrode Refill is ideal for washing powders and soaps. Both electrodes excel by their ruggedness and allow the rapid and precise determination of anionic and cationic surfactants.

This poster presents a highly reproducible procedure for the determination of the sodium contribution of acid-extractable organic species in Bayer process liquor. The precision of the method is estimated to be 0.2% RSD.

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.

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.

Hydroxyl is an important functional group and knowledge of its content is required in many intermediate and end-use products such as polyols, resins, lacquer raw materials and fats (petroleum industry). The test method to be described determines primary and secondary hydroxyl groups. The hydroxyl number is defined as the mg of KOH equivalent to the hydroxyl content of 1 g of sample.The most frequently described method for determining the hydroxyl number is the conversion with acetic anhydride in pyridine with subsequent titration of the acetic acid released: H3C-CO-O-CO-CH3 + R-OH -> R-O-CO-CH3 + CH3COOH. However, this method suffers from the following drawbacks: - The sample must be boiled under reflux for 1 h (long reaction time and laborious, expensive sample handling) - The method cannot be automated - Small hydroxyl numbers cannot be determined exactly - Pyridine has to be used, which is both toxic and foul-smellingBoth standards, ASTM E1899-08 and DIN 53240-2, offer alternative methods that do not require manual sample preparation and therefore can be fully automated: The method suggested in ASTM E1899-08 is based on the reaction of the hydroxyl groups attached to primary and secondary carbon atoms with excess toluene-4-sulfonyl-isocyanate (TSI) to form an acidic carbamate. The latter can then be titrated in a non-aqueous medium with the strong base tetrabutyl- ammonium hydroxide (TBAOH). The method suggested in DIN 53240-2 is based on the catalyzed acetylation of the hydroxyl group. After hydrolysis of the intermediate, the remaining acetic acid is titrated in a non-aqueous medium with alcoholic KOH solution. The present work demonstrates and discusses an easy way to determine the hydroxyl number according to ASTM E1899-08 or DIN 53240-2 with a fully automated titrimetric system for a great variety of industrial oil samples.

The 800 Dosino controlled by tiamo™ or Touch Control can be used universally for dosing and liquid handling tasks in both the analytical laboratory or directly in the synthesis laboratory. This poster looks at three typical liquid handling applications, the synthesis of metal-organic compounds, the preparation of standards, and the determination of pharmaceutical ingredients.

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.

The presence of excessive water in plastics adversely affects the performance of polymeric goods which is why water determination is of crucial importance. This article describes the accurate and straightforward determination of the water content using the Karl Fischer Oven Method in ten different plastic types that are not amenable to direct Karl Fischer titration. The experiments revealed that besides the determination of the oven temperature, sample preparation is one of the most important steps of the analysis, especially in case of hygroscopic plastic samples.

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.

The thermometric titration method presented here permits a simple and direct determination of the total acid number (TAN) in petroleum products. It is an invaluable alternative to current manual and potentiometric methods. Thermometric titration uses a maintenance-free temperature sensor that does not require rehydration and is free of fouling and matrix effects. The procedure requires minimal sample preparation. Results agree closely with those from the potentiometric titrimetric procedure according to ASTM D664, but the thermometric titration method is far superior in terms of reproducibility and speed of analysis, with determinations being complete in approximately one minute.

The poster describes how different suppressors (MSM and MCS) work and mentions possible applications.

The poster describes the water determination in pharmaceuticals using the Karl Fischer oven technique.

By combining the information from electrochemical and spectroscopic techniques, UV/VIS spectroelectrochemistry (UV/VIS-SEC) allows a comprehensive analysis of electron-transfer processes and complex redox reactions. The anodic oxidation of a N-aryl-D2-pyrazoline derivative was investigated by combining cyclic voltammetry and UV/VIS spectroscopy. In-situ measured UV/VIS absorbance depicted the absorption changes that accompanied the anodic oxidation and could therewith prove the stability of the electrogenerated radical cation. UV/VIS-SEC provides a powerful tool for the in situ study of shorter-lived species, reaction mechanims, and kinetics in a wide variety of electrochemical active organic, inorganic, and biological molecules.

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.

Because of its toxicity, the World Health Organization recommends a maximum arsenic content in drinking water of 10 μg/L. Anodic stripping voltammetry with the scTRACE Gold offers a straightforward, highly affordable alternative to spectroscopic determination.

The poster shows the use of Vis-NIR spectroscopy for the simultaneous quantification of cobalt content, solids content, relative density and viscosity in paint driers as an outstanding alternative to conventional wet chemical laboratory methods. The advantages of the expanded wavelength range over the visible range become clear in this application: the visible range (400 – 780 nm) correlates directly with the cobalt content; the NIR range (780 – 2500 nm) is used for determining the chemical and physical parameters.

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.

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.

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.

Commercially available fuels are complex mixtures of hundreds of different hydrocarbons. For the calibration of the test engines or advanced experimental and computational research they are modeled by means of multicomponent surrogate mixtures that adequately represent the desired physical and chemical characteristics. By definition, every octane and cetane number corresponds to a specific mixing ratio of primary reference fuels (PRFs). Based on this information, the tiamoTM controlled automatic dosing device prepares the surrogate mixtures. The setup drastically minimizes time-consuming and error-prone manual preparation steps and the contact with hazardous solvents. Additionally, precise and accurate results are displayed on customizable reports that fully comply with all current GLP and GMP requirements.

The water content of tablets determines the release of their active ingredients as well as their chemical, physical, microbial and shelf-life properties. Accordingly, the water content is of crucial importance and has to be accurately determined. This paper describes the straightforward determination of the water content using automated volumetric Karl Fischer titration (KFT). Tedious sample preparation steps are eliminated by using a high-frequency homogenizer that additionally serves as a stirrer. Prior to titration, the homogenizer comminutes the tablets directly in the KF solution. As the comminution process takes place directly in the hermetically sealed titration vessels, interference from atmospheric humidity does not occur. Even after 24 h in the vessels, the moisture content of four different tablet type samples was within 93…108% of the initially determined values. With a coefficient of determination of 0.99993 the KF method is highly linear for water amounts between 4 and 215 mg. For all investigated tablet types, KFT provides results that lie within the range expected by the manufacturer.

For a variety of reasons, the water content of chocolate is of crucial importance and has to be accurately determined. This poster compares an automated version of the Karl Fischer titration (KFT) using the sequential addition of various solvents with the widespread manual titration at elevated temperatures using a chloroform/methanol mixture. The water contents determined by the two procedures show excellent agreement. However, manual titration requires laborintensive sample preparation, the side reactions are difficult to quantify and hazardous halogenated solvents have to be used. In contrast, automated KFT is straightforward, uses non-hazardous solvents, allows to quantify the side reactions and is easily applicable to water determinations in sugar- and fat-containing matrices.

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.

Sodium fluoride is used as a preservative in biological samples for alcohol analysis. All submitted blood samples, including those taken from vehicle drivers suspected of driving under the influence of liquor, have to be tested for adequate preservation prior to alcohol determination by gas chromatography. This is critical to ensure adequate sample preservation. Inadequate sample preservation may allow glycolysis and/or microorganism growth to produce ethanol.In the past this has been done by direct potentiometric measurement using a fluoride-selective electrode (F ISE), an ion meter and certified NaF standards. The sodium fluoride level was determined manually by dipping the electrode directly into the blood sample. Results were recorded manually. This poster describes two independent automated methods of analysis that allow the minimization of this tedious and time-consuming procedure.In the first one, the fluoride content in a blood aliquot is measured by direct potentiometric measurement after the addition of TISAB and deionized water. The second method employs the titration of the sample aliquot with La(NO3)3 after adding a buffer solution.

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.

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.

Lead is known to be highly toxic, and lead salts are easily resorbed by humans. Cases of chronic lead poisoning caused by lead metal used in the water piping system are well known. Therefore, the control of drinking water for lead content is of utmost importance. The Lead and Copper Rule (LCR) published by the USEPA (United States Environmental Protection Agency) states an action limit of 15 μg/L lead for drinking water. Using a portable voltammetric instrument, lead can be determined in these concentrations directly at the point of sampling.

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.

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.

This article describes rapid and sensitive bromate determination in drinking and table water by means of anion chromatography with post-column derivatization and subsequent spectrophotometric detection.

The rapid growth of the Earth's population has led to massive increases in the consumption of energy and resources and in the production of consumer products and chemicals. It is estimated that 17 million chemical compounds are currently on the market, of which 100,000 are produced on a large industrial scale. Many of these enter the environment. This leads to a demand for sensitive analytical procedures and high-performance analytical instruments.pH value, conductivity and oxygen requirement are important characteristics in water and soil analysis. The first two of these can be determined rapidly; for the third, the titration that is used is also the one used in numerous single determinations. This article describes several important standard-compliant determinations in water and soil analysis.