Ion chromatography applications

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.

This White Paper discusses USP <1225> and how ion chromatography determines active ingredients in pharma products (assays) as well as identifies impurities and degradation components.

N-Methylpyrrolidone (NMP) is crucial for lithium-ion battery production. Metrohm’s intelligent Preconcentration Technique with Matrix Elimination enables µg/L-level anion analysis in NMP.

The Metrosep A Supp 21 column and 948 Continuous IC Module, CEP enable efficient, automated single-run analysis of major anions and disinfection byproducts in water.

The assay of calcium acetate, often used as a phosphate binder for dialysis patients, can be performed with ion chromatography (IC) as per USP <621> and <1225>.

Potassium citrate and citric acid oral solutions act as systemic alkalizers. Potassium assays, validated per USP <621> and <1225>, use IC with L76 cation-exchange columns.

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

Microbore ion chromatography offers better sensitivity, shorter retention times, and consumes less eluent, increasing sample throughput and reducing running costs.

Tris(hydroxymethyl)aminomethane (TRIS) is often used in life science applications and its purity must be monitored. This analysis is possible with ion chromatography.

The USP and FDA started to modernize several monographs and General Chapters. In many cases, IC-focused methods have replaced older, wet chemistry procedures. Learn more about the USP modernization initiative and the advantages of ion chromatography in this white paper.

Nitrosamine formation can be avoided by controlling the nitrite concentration in pharmaceutical products and processes. To monitor nitrosamine formation, sensitive analytical methods such as ion chromatography for the determination of nitrite in pharmaceutical products and substances are essential.

Nitrosamine presence in medicines, even at trace level poses high safety risks to patients (carcinogenic). Nitrosamine formation can be avoided by controlling and monitoring the nitrite concentration in pharmaceutical products and substances. This Application Note describes the analysis of nitrite in duloxetine hydrochloride with ion chromatography (IC).

This White Paper will walk you through the selection process of ion chromatography as the best analytical tool in the product development of a cell-based gene therapy.

Compounded injections of sodium bicarbonate are sterile solutions for correcting metabolic acidosis and other conditions requiring systemic alkalinization. Compounded injections of sodium phosphates serve as a phosphate source to either prevent or correct hypophosphatemia in patients with restricted oral intake. Ion chromatography (IC) with suppressed conductivity detection is the standardized way to accurately quantify sodium in these solutions.

This White Paper compares automated Inline Ultrafiltration and Inline Dialysis to the traditional Carrez clarification procedure for the analysis of milk samples by ion chromatography (IC). A continuous test series over approximately six months proved Inline Dialysis to be a reliable and valuable alternative to treat dairy products prior to IC analysis.

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

Iodine is an essential mineral for human health, where it is necessary for e.g., the production of thyroid hormones. The presented method describes the determination of free iodide in milk samples using Metrohm Low Volume Inline Dialysis for automated sample preparation prior to injection into an ion chromatograph (IC) and subsequent amperometric detection in direct current (DC) mode.

Anticavity pharmaceuticals like sodium fluoride and acidulated phosphate topical solution products require strict quality control. This Application Note outlines the fluoride IC assay as described in the USP Monograph Sodium Fluoride and Acidulated Phosphate Topical Solution.

In severe cases of cyanide poisoning, sodium nitrite is used along with sodium thiosulfate for treatment. This Application Note describes the nitrite ion chromatography assay with the Metrosep A Supp 4 column and suppressed conductivity detection. This column equivalency study was in cooperation with the USP according to the USP General Chapter <621>.

Lithium-ion batteries (LIBs) are the most common rechargeable options available today. Production of LIBs needs to follow stringent quality standards.

As an alternative to titration, ion chromatography (IC) with suppressed conductivity detection has been approved by USP as validated method to quantify chloride content in NaCl tablets for solution or oral use.

An ion chromatography (IC) assay with suppressed conductivity detection is the standardized way to accurately quantify phosphate in phosphates compounded injections.

Ion chromatography (IC) provides an automated, fast, and sensitive solution to accurately quantify cationic and anionic components including acetate simultaneously. This comprehensive approach makes IC an economic alternative to traditional techniques for the quality control of pharmaceutical solutions like haemodialysis concentrates. Ease-of use, accuracy, and the high-throughput of IC increase productivity and comply with the demands of modern routine and research labs.

Monitor adsorbable organic halogens (AOX) in water using combustion ion chromatography (CIC) for precise analysis of AOCl, AOBr, AOI, and total AOX.

Combustion ion chromatography (CIC) measures AOX (adsorbable organically bound halogens, i.e., AOCl, AOBr, AOI) and AOF as well as CIC AOX(Cl) according to DIN 38409-59 and ISO 18127.

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.

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.

Ion chromatography with PCR and UV/VIS detection provides a highly specific and sensitive method for bromate analysis, meeting EPA Method 317 and ISO 11206 requirements.

White paper on monitoring corrosion and the benefits of online or inline chemical analysis over manual sampling and offline laboratory methods for corrosion monitoring. Online and inline process application solutions for corrosion prevention with related application notes for further information are presented.

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

Efficiently analyze food products with ion chromatography (IC). Discover its robust applications in quality control for beverages, food additives, and dairy.

Determination of fluoride, hypophosphite, chlorite, bromate, chloride, nitrite, bromide, chlorate, nitrate, phosphite, phosphate, sulfate, and iodide using anion chromatography with conductivity detection after chemical suppression.

Determination of hydroxylamine, ethanolamine, triethanolamine, and hydrazine using cation chromatography with direct conductivity detection.

Gentamicin is an aminoglycoside antibiotic and is composed of a number of related gentamicins. It is applied for several types of infections. For the determination of the major components, USP asks for chromatographic separation with pulsed amperometric detection using a gold working electrode. A post-column addition of NaOH is performed prior to the detection.

Fast IC means a high sample throughput. This is attained with short columns, relatively high flows and strong eluents. Sulfite can be determined in beer alongside sulfate and other anions with the Metrosep A Supp 10 - 50/4.0.

The determination of disinfection byproducts is essential for drinking water manufacturers. This Application Note shows the determination of chlorite and bromate in addition to the standard anions. In order to reduce eluent consumption, separation takes place on a Metrosep A Supp 5 - 250/2.0 Microbore column, followed by conductivity detection after sequential suppression.

Water chemistry of the water-steam cycle is crucial for maintaining plant reliability and for ensuring optimal plant operational conditions. Impurities such as corrosion products in ionic, colloidal, or oxide forms are ubiquitous in feedwater, condensate, and reactor coolant. This application shows the determination of sub-ppb levels of Cu, Ni, Zn and standard cations (e.g., Na+, NH4+, Mg2+, Ca2+) in the water-steam cycle of a BWR.

Determination of lead, zinc, indium, cadmium, cobalt, ammonium, potassium, manganese, magnesium, and calcium using cation chromatography with direct conductivity detection.

Worldwide, milk and dairy products are vital sources for human nutrition. A major component and energy source in dairy products is lactose. To efficiently metabolize lactose, the enzyme lactase is indispensable. However, globally nearly 70% of the population is lactose intolerant and they have difficulties to digest lactose. Lactose malabsorption leads to numerous gastrointestinal and extra-intestinal symptoms and other complaints with varying extents. Therefore, consumers rely on accurate food labels and for manufacturers appropriate sensitive analytical techniques are a must to comply with these demands. Ion chromatography with pulsed amperometric detection (IC-PAD) enables the determination of very low lactose contents. Validation according to AOAC requirements shows the high sensitivity and reliability of this method as a routine analysis.

Haloacetic acids (HAAs) are commonly produced as disinfection byproducts (DBPs) from water treatment processes. Some HAAs are regulated by the authorities and have been classified as potentially carcinogenic. They have traditionally been analyzed by gas chromatography (GC), a technique that requires time-consuming sample extraction and derivatization, leading to higher costs per analysis. Ion chromatography hyphenated to mass spectrometry (e.g., single or triple quadrupole MS systems) is a powerful tool that can handle many challenging analytical tasks such as measuring μg/L levels of HAAs in potable water samples. This White Paper explains the benefits of using this hyphenated technique for the accurate measurement of HAAs in potable water.

Haemophilus influenzae type B (Hib) is a major cause of bacterial meningitis in children in many countries. The capsular polysaccharide (PS) of Hib plays an important role in the virulence of the organism. The polysaccharide capsule hides cell surface components from elements of the mammalian immune system, such as antibodies and complement proteins that otherwise would activate mechanisms to kill the pathogen. Vaccines require rigorous characterization and assays to ensure final product quality and consistency. For glycoconjugate vaccines, it is important to measure both free and total PS to ensure the quality. A large amount of unconjugated PS may suppress immunity to the antigen. Additionally, the presence of free PS is a key indicator of process consistency. Current methods to determine PS content in vaccines such as Hib are imprecise and unreliable, especially if the vaccine contains a sugar stabilizer (e.g. lactose). Ion chromatography with pulsed amperometric detection (IC-PAD, or HPAEC-PAD) offers a simpler procedure and better sensitivity than other assays to quantify PS (here, polyribosylribitol phosphate [PRP]) in Hib vaccine.

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.

Sulfites are well-known additives in foods and beverages used to extend shelf life and preserve colors. Such properties have led to the broad usage of sulfites in a range of foodstuffs like fruits, cereals, vegetables, seafood, juices, alcoholic and non-alcoholic (soft) beverages, and in some meat products. The term «sulfites» describes a group of molecules that include sulfur dioxide (SO2) and chemically related molecules like sodium sulfite (Na2SO3), sodium bisulfite (NaHSO3), or sodium metabisulfite (Na2S2O5). Sulfite intake has been correlated with several adverse reactions, and therefore sulfites are included in the FAO/WHO Codex Alimentarius list. Labelling sulfite content in foods and beverages is necessary when the total concentration exceeds 10 mg/kg. Metrohm ion chromatography allows the reliable measurement of sulfite in different matrices using either conductivity or amperometric detection. The inclusion of automated sample preparation and cleaning steps with Metrohm instrumentation saves additional analyst time and helps increase sample throughput.

Speciation analysis is an important tool in analytical chemistry giving information about the quantitative distribution of different oxidation states of one and the same metal ion. The speciation of iron(II) and iron(III) (Fe 2+/Fe 3+) is achieved by ion chromatographic separation of their anionic dipicolinic acid complexes. Afterwards, post-column reaction with 4-(2-)pyridylazo-resorcinol (PAR) allows VIS detection at 510 nm.

Crude oil typically contains no organic halides. These are introduced at production sites, in pipelines, or in storage tanks. These components produce HF, HCl, and other acids in reforming and hydro-treating processes, leading to corrosion and catalyst poisoning. Speciation of the halides is an important parameter to measure in order to trace the contamination source. The current specifications expect to find less than 2 mg/kg organic chlorine in crude oil. Sulfur in crude oil could be quantified on the fly. Due to the specific request in this application, only the halogens are determined.

The Eco IC is an entry-level instrument that is particularly suitable for routine operations and water analysis. It is equipped with a conductivity detector and can be used both with and without chemical suppression. This Application Note describes the determination of anion content with the Metrosep A Supp 17 - 250/4.0 column. This column model is particularly suitable for water analysis at room temperature.

Ion chromatography trace analysis of anions in seawater is difficult, due to the high chloride concentrations. In contrast to chloride, nitrite, bromide and nitrate absorb UV radiation in the low wavelength range, thus enabling a UV detection of these three anions. This Application Note describes the separation on a column of the Metrosep Carb 2 - 100/4.0 type with a sodium chloride eluent. This minimizes the influence of the surplus chloride and enables low detection limits.

Free white paper gives comprehensive overview of how to reliably assess the quality of infant formula with ion chromatography.

Determination of trace levels of cations and amines in hydrogen peroxide is important in quality determination of high-grade semiconductor chemicals. In particular, some manufactures look for 1 ppb trimethylamine or less in hydrogen peroxide samples. Ion chromatography after MiPCT-ME* with conductivity detection after sequential cation suppression is applied.

Learn about PFAS, their impact on water quality, EU Directive 2020/2184, and the benefits of AOF measurement using combustion ion chromatography (CIC).

Nitrite and nitrate salts are used as preservatives for meat and meat products. Nitrate salts (labeled E 251 or E 252) have a low toxicity but long-term exposure is of concern, as the lower gut reduces them to nitrite, a precursor of nitrosamines (classified as carcinogenic). Nitrite itself is classified as probably carcinogenic to humans. The European Food Safety Authority (EFSA) lists the MPL (maximum permitted levels) after the manufacturing process for nitrite (labeled E 249 or E 250) as between 50–180 mg/kg, and for nitrate between 150–300 mg/kg, depending on the product. The European Commission (Regulation (EC) No 1333/2008) limits nitrate and nitrite salts in processed meat to less than 150 mg/kg. Ion chromatography with UV detection offers a robust and universal method for quality control of nitrite and nitrate in different meat matrices. Additional sample preparation techniques like Inline Ultrafiltration help to save time and costs as well as overcome analysis issues with difficult sample matrices.

Calcium carbonate has a wide applicability in the pharmaceutical industry as an excipient and also as an active ingredient, and in the food industry as a major dietary supplement. The U.S. Pharmacopoeia (USP) monographs for calcium and magnesium carbonates tablets as well as calcium carbonate and magnesia chewable tablets currently describe manual titration as the assay procedure for calcium and magnesium. The USP has embarked on a global initiative to modernize many of the existing monographs across all compendia. In response to this initiative, two alternative analytical methods were developed to determine the analytes calcium and magnesium. This Application Note presents ion chromatography (IC) procedures using conductivity detection that provide better accuracy and specificity and are suitable for the intended purpose. These validated IC methods (according to USP General Chapter <1225>) offer a significant improvement to the existing assays because they can simultaneously determine both analytes calcium and magnesium, saving both time and effort.

Lithium is a soft alkali metal that is typically obtained from salt lake brines. Lithium is used for many applications, but especially for production of lithium-ion batteries in electric cars, mobile phones, and more. This Process Application Note presents a method to monitor lithium as well as other cations in brines by online process ion chromatography (IC), a multiparameter analytical technique that can measure ionic analytes in a wide range of concentrations.

The short Metrosep C Supp 2 - 100/4.0 allows applying a higher eluent flow. Together with a more concentrated eluent (7.0 instead of 5.0 mmol/L nitric acid) the run time of the four cations, sodium, potassium, magnesium, and calcium can be reduced to 5 minutes. Conductivity detection after sequential suppression is applied.

Cation analysis by IC in wastewater is a proven method. Limiting factor is often the Na/NH4 separation. High sodium concentrations may make ammonium determination impossible due to peak overlapping. The use of sequential suppression and a Dose-in gradient improve the Na/NH4 separation and enables determination of low ammonium concentrations.

Acidic solutions used as scrubber solutions for ammonium typically have a pH of 2 or lower. This pH value is too low for silica based IC columns typically applied in direct conductivity detection of cations. The Metrosep C Supp 2 - 250/4.0 is polymer based and allows injecting low pH samples. An acidified drinking water sample spiked with ammonium is analyzed. The results indicate that such acidic solutions can be analyzed with conductivity detection after sequential cation suppression.

The Metrosep C Supp 2 column family is polystyrene/divinylbenzene based and therefore sequential cation suppression may be applied. This AN shows the separation and detection of different amines on the 150 mm version of the column with subsequent conductivity detection after sequential cation suppression.

Succinylcholine is a short-term paralyzing agent used e.g., for tracheal intubation. Choline is a building block of the drug and needs to be determined as an impurity. USP applies cation chromatography with conductivity detection after suppression. Eluent composition and column type do not exactly comply with the USP method. However, the results fulfill the respective requirements. The choline concentration of the sample is out of USP specifications.

Biogenic amines are released during the winemaking process. In wine, they are present as odorless salts. However, in the mouth their flavor is partially liberated, influencing the appearance for the wine taste. Besides this, biogenic amines have been related to lack of hygiene or poor manufacturing practices. The biogenic amines are determined applying suppressed cation chromatography.

Trace cation analysis in high purity water (sub-μg/L range) requires cation chromatography after sequential suppression and intelligent Preconcentration Technique (MiPCT). Trace cations in deionized water (DI) are determined and the method detection limit (MDL according to US EPA) as well as the limit of detection (LOD = 3 x S/N) is calculated. MDL and LOD are very similar in the lowest ng/L range for this setup with 6 mL preconcentration volume.

Hydrogen peroxide is available in different purity grades depending on its use. High purity H2O2 (electronic grade) requires very low contamination levels, e.g., less than 1 μg/L of trimethylamine (TMA). This application describes the determination of trimethylamine in a high-purity H2O2 solution (30%). Analysis is performed using Inline Preconcentration with Matrix Elimination (MiPCT-ME) applying conductivity detection after sequential cation suppression.

Lithium hexafluorophosphate (LiPF6) is used as an electrolyte in rechargeable batteries. Its high solubility in non-polar solvents and its non-coordinating character in particular make lithium hexafluorophosphate the ideal salt for use in lithium-ion cells. This Application describes the determination of cation traces in LiPF6 with conductivity detection following sequential suppression.

Boiler feed water is a working medium in thermal power plant. To keep corrosion low, the pH value should be in the slightly alkali range, which is why amines are added to the feed water. This addition must be monitored regularly. Also important is the monitoring of the sodium concentration, because an increase of this indicates that cooling water is seeping into the condenser. Ion chromatography with conductivity detection following sequential suppression is the optimum system for monitoring, particularly in combination with intelligent Sample Preconcentration and Matrix Elimination.

Sequential suppression in cation chromatography significantly improves detection limits. The determination of the blank value of the sample vial being used is thus essential for being able to achieve such low detection limits. The leaching tests of various sample vials proceed with the intelligent Preconcentration Technique with Matrix Elimination on the Metrosep C Supp 1 - 250/4.0 column with conductivity detection following sequential suppression. The 50 mL Corning® Cell Culture Flasks from Sigma-Aldrich (CLS430168) exhibit the lowest blank values.

Meropenem is a beta-lactam antibiotic that is classed among the carbapenems; it suppresses murein biosynthesis and thus the buildup of the bacterial cell wall. Dimethylamine is an important precursor in meropenem synthesis and must therefore be monitored as an impurity. Detection is performed on the Metrosep C Supp 1 - 250/4 column with subsequent conductivity detection after sequential suppression.

With the advent of electric automobiles, the demand for lithium batteries and with it the demand for lithium material will increase sharply. Brine lakes and hard silicate minerals are numbered among the most important sources of lithium. This Application Note addresses cation determination in seepage water from lithium minerals. Alkali and earth alkali metals are separated in the lithium digestions on the Metrosep C Supp 1 - 250/4.0 column, with subsequent conductivity detection after sequential suppression.

This Application Note shows the selectivity of the Metrosep C Supp 1 - 250/4.0 column for alkyl and ethanol amines in addition to standard cations under isocratic conditions. Quantification takes place using conductivity detection following sequential suppression.

Atorvastatin is a medication that is used for reducing cholesterol levels. A sensitive and reliable method for TBA detection is required, given that trace amounts of tetrabutylammonium (TBA) are to be found in the presence of atorvastatin and its derivatives. One such method is ion chromatographic separation on the Metrosep C Supp 1 - 250/4.0 with subsequent conductivity detection and sequential suppression.

Choline is important for the biosynthesis of numerous molecules, e.g., the neurotransmitter acetylcholine, and exists as an intermediate product in the human metabolism. Concentration determination takes place after microwave digestion. Separation is performed on the Metrosep C Supp 1 - 250/4.0 column following sequential suppression. Separation from the standard cations is outstanding.

The concentrations of toxic, biogenic amines in foods, particularly in fish and wine, are an important quality characteristic. The present Application Note shows the separation of putrescine, cadaverine and histamine in addition to the standard cations. Separation takes place on a Metrosep C Supp 1 - 250/4.0 with Dose-in Gradient; quantification via conductivity detection following sequential suppression.

Ammonium determination after sequential suppression frequently exhibits non-linear calibration curves. The reason for this is the ammonium hydroxide that arises and that is present in a form characterized by low dissociation. The sequential cation suppression forms the more highly dissociated ammonium hydrogen carbonate. Ammonium and the other standard cations exhibit linear calibration curves (R > 0.9997).

Cation chromatography with sequential suppression enables the determination of cations in their hydrogen carbonate form. The eluent – usually nitric acid – is converted into carbonic acid. Following its decomposition into carbon dioxide and water, the former is continuously removed by the CO2 suppressor. The reduction of baseline noise thus achieved permits the lowering of the detection limits and improves reproducibility, even at very low cation concentrations. This Note shows the reproducibilities determined for cation concentrations of 10 µg/L.

This Application Note presents ion chromatography with pulsed amperometric detection as fast and reliable method to determine low level lactose in complex matrices such as infant formula.

In gold mining, there is a tendency to switch from cyanide leaching to the much less toxic thiosulfate leaching process. Thiosulfate leaching is a sensitive process that requires more optimization of the components of the leach reaction to maximize gold recovery and reagent loss. Sulfite, thiosulfate, thiocyanate, and tetrathionate are separated on a Metrosep A Supp 5 - 250/4.0 column. Perchlorate is choosen as an eluent as most of the metal perchlorates are soluble in water. This avoids metal precipitation in the IC System.

The determination of iodate and iodide in used electroplating baths is a demanding task due to the high concentration of other ions. Iodate is used as a stabilizer for the bath and needs to be checked for proper electroplating. The use of a sodium chloride eluent, the Metrosep A Supp 5 - 250/4.0 column and direct UV/VIS detection permits the analysis of these samples without matrix interferences.

Seawater analysis with conductivity detection is difficult due to the high excess of chloride. Especially analyzing for nitrite and bromide, UV/VIS detection is preferred as chloride is not interfering with nitrite at 218 nm. This AN shows the determination of all three UV-absorbing anions in an artificial seawater.

Determination of nitrite and nitrate in a cooling lubricant using anion chromatography with conductivity detection (see AN S-274) and subsequent UV detection after sequential suppression and Metrohm Inline Dialysis.

The determination of PBBE (tetrabromobisphenol A - TBBPA, octabromodiphenyl ether - OCTA and decabromodiphenyl ether - DECA) in a polymer sample was carried out with the Nucleosil EC - 250 mm column; for this purpose a methanol and phosphate buffer was used as an eluent and subjected to UV detection in accordance with the IEC 62321 method for RoHS testing.

Determination of sulfide and thiosulfate in a process water using anion chromatography with UV/VIS detection after chemical suppression and conductivity detection.

Determination of nitrite, bromide, nitrate, and iodide in 10 g/L sodium chloride using anion chromatography with UV detection.

Determination of bromide in calcium chloride using anion chromatography with UV/VIS detection.

Water of the primary cycle of pressurized water reactors (PWR) contains boron for neutron absorption. The high borate content interferes with the direct analysis of trace anions. Inline Neutralization combined with variable preconcentration and Inline Matrix Elimination (MiPCT-ME) allows to remove boron as boric acid before injection.

The Metrohm IC Driver for OpenLab CDS opens ion chromatography to the world of HPLC, running under OpenLab CDS. In this application, a soft drink is analyzed for sugars and sugar alcohol content applying pulsed amperometric detection.

This Application Note shows the determination of glucose and galactose in a 2% solution of lactose. The separation is achieved on a Hamilton RCX-30 - 250/4.6 applying pulsed amperometric detection (PAD) at a gold electrode. Instrument control, data acquisition, and data handling is done by Empower 3.0 using the Metrohm IC Driver 2.0 for Empower.

This Application Note describes the separation of inositol, mannitol, glucose, xylose, fructose, lactose, sucrose and cellobiose on a column of the Metrosep Carb 2 - 150/4.0 type with subsequent pulsed amperometric detection (PAD).

Polydextrose is a low-calorie, synthetic polymer made of glucose. It is a recognized additive for foodstuffs. Hot water is used to extract the polydextrose from the foodstuff, after which it is centrifuged. Subsequent fermentation removes maltooligomers and fructans. Afterwards, the polydextrose is quantified using anion-exchange chromatography with pulsed amperometric detection.

The determination of sugar and sugar alcohols is very important for food analysis. The Dose-in Gradient system extends the gradient capability of the standard IC system. The isocratic system is expanded to form a binary gradient system with just one 800 Dosino and one T-piece.

Determination of sucrose, glucose, and sucralose in a low-calorie sweetener using ion-exclusion chromatography with pulsed amperometric detection after post-column addition of sodium hydroxide.

Evidence of maleic acid in Asian foodstuffs led to the recall of many starchy foods because long-term consumption of maleic acid can cause kidney problems. Cyclic kojic acid is however approved in Asia, both as a bleaching additive in foodstuffs and as a preservative in cosmetics. This Note describes their simultaneous determination in a single analysis.

Determination of sorbate and benzoate in a functional drink using ion-exclusion chromatography with suppressed conductivity detection.

Determination of glycolic acid, formic acid, acetic acid and carbonic acid in a scrubber solution using ion-exclusion chromatography with conductivity detection after chemical suppression.

Determination of organic acids and phosphate using ion-exclusion chromatography with direct conductivity detection.

Determination of chloride and sulfate in effluent after Metrohm Inline Dialysis using anion chromatography with direct conductivity detection.

Determination of acetate, chloride, citrate, and sulfate in a concentrate of an infusion solution using anion chromatography with direct conductivity detection. Non-suppressed IC is used to avoid interferences by the amino acids.

Determination of nitrate, sulfate, and thiocyanate in additives for building materials using anion chromatography with direct conductometric detection.

Determination of chloride, nitrate, and sulphate in sugar-containing solutions without matrix elimination using anion chromatography with direct conductometric detection.

Determination of silica (as silicate) in pure water with preconcentration using anion chromatography with direct conductivity detection (without any post-column reaction).

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

Sulfamic acid is a reasonably strong acid, used in descaling agents and for cleaning of dairy and brewing equipment. Here, a chemical solution is analyzed for sulfamate, chloride, nitrite, nitrate, and sulfate. As the solution can also contain hydramine, sufficient separation from the ions of interest is required.

OpenLab CDS is the newest generation of the Agilent chromatography data systems platform. The Metrohm IC Driver 1.0 for OpenLab CDS enables introducing Metrohm IC instruments to this platform for full control and data acquisition. This application shows the analysis of iodide by amperometric detection, enabling detection at trace levels. The eluent is produced automatically by the 941 Eluent Production Module. In this way, amperometric detection can be executed with the same functionality and performance as with MagIC Net.

Sodium fluoride gel for pharmaceutical use needs to comply with USP requirements. The actual monograph (USP 42) uses two different methods for the identification and the assay. Ion chromatography allows the analysis of these two parameters in one single determination. In the course of the USP monograph modernization, this ion chromatographic approach makes this type of analysis even easier.

The STREAM (suppressor treatment reusing eluent after measurement) is applied since quite some time. The suppressor rinsing with suppressed eluent is advantageous over ultrapure water rinsing: a smaller water dip, faster MSM equilibration, and the avoidance of an additional water supply are just a few. Injecting samples containing iron in the matrix under sulfuric acid regeneration yields reduced peak areas and broader peaks for phosphate. Switching to a regenerant based on sulfuric and oxalic acid allows full regeneration of the MSM. The overlay above shows three subsequently taken chromatograms after more than 300 injections of 10 mg/L iron(II) onto one single MSM chamber. No difference in peak shape or peak area is observed.

Soluble tungsten and molybdenum are available in soil mainly as their oxosalts, tungstate and molybdate. Tungstate is rather a hazardous compound, which may interfere with plant growth. Molybdate, on the other hand, is a required micronutrient, required e.g. for nitrate fixation in legumes. Both can easily be determined after alkaline digestion with ion chromatography followed by conductivity detection after chemical suppression.

Pyrophosphate is used as a stabilizer in aqueous hydrogen peroxide solution. “Reagent grade” solutions may contain pyrophosphate in the higher mg/L range, while “electronic grade” hydrogen peroxide should be free of this stabilizer. Here the determination of pyrophosphate in a high purity H2O2 solution (30%) is performed applying Inline Preconcentration with Matrix Elimination (MiPCT-ME) and a Dose-in Gradient.

Electronic-grade nitric acid may not contain more than the slightest traces of anion contaminations (in the mg/L range). The ion chromatography determination of these kinds of anion traces requires not only a high-capacity column but also an eluent that allows the nitrate to be eluted by the column, although only after all of the other ions of interest have been eluted. This separation is achieved on a column of the Metrosep A Supp 16 - 250/4.0 type with the aid of a strong carbonate/hydrogen carbonate eluent.

Chrome plating is an important electroplating technique that covers metal or plastic surfaces with a thin layer of chromium for both protection and decoration purposes. The sulfate and sulfuric acid concentrations in the baths are important parameters in the coating process and require continuous monitoring. The anions in the chrome baths are separated on the Metrosep A Supp 5 - 250/4.0 column and are determined using conductivity detection in accordance with sequential suppression.

Fast IC means a high sample throughput. This is attained with short columns, relatively high flows and strong eluents. Applied to drinking water analysis this means: determining chloride, nitrate and sulfate within 3 minutes.

Metrohm Inline Preconcentration Technique with Matrix Elimination (MiPCT-ME) is a powerful tool that combines preconcentration, matrix elimination, and multilevel calibration. The latter only requires a single multi-ion standard solution. The 800 Dosino takes over all liquid handling tasks. The shown system setup allows sample analysis from 0.1 µg/L up to 1.0 mg/L.

Eluent preparation on demand (EPOD) is the convenient and flexible way of automatic eluent preparation. The 849 Level Control together with an 800 Dosino equipped with a 50 mL dosing unit are used to dilute an eluent concentrate to the final eluent concentration. The use of eluent concentrates is suitable for any type of eluent. This facilitates unattended operation of the system over several weeks (see AN C-134 for cation eluent preparation).

Determination of acetate, chloride, nitrite, bromide, nitrate, phosphate, sulfate, oxalate, fumarate, and molybdate using anion chromatography with conductivity detection after chemical suppression.

Determination of fluoride, chloride, nitrate, phosphate, and sulfate on a short column or the ions mentioned plus bromate and nitrite on a long column in water samples applying intelligent column-switching using anion chromatography with conductivity detection after sequential suppression.

Long-term determination of standard anions with automatic inline eluent preparation applying Dosino and Level Control technology using anion chromatography with conductivity detection after sequential suppression.

Determination of chloride, sulfite, sulfate, and thiosulfate in a process water using anion chromatography with conductivity detection after chemical suppression and subsequent UV/VIS detection.

Determination of chromate in cement using anion chromatography with conductivity detection after chemical suppression.

Determination of chloride and sulfate in an electrolyte used in sensors for transcutaneous CO2 measurement using anion chromatography with conductivity detection after chemical suppression.

Determination of sulfate in gentamicin sulfate using anion chromatography with conductivity detection after chemical suppression.

Qualitative determination of chloride, phosphate, and sulfate as well as chlorite, nitrite, chlorate, bromide, and chromate in urine using anion chromatography with conductivity detection after chemical suppression.

Determination of nitrate and phosphate in a liquid fertilizer using anion chromatography with conductivity detection after chemical suppression.

Determination of fluoride, chloride, nitrite, selenite, phosphate, nitrate, sulfate, and selenate using anion chromatography with conductivity detection after chemical suppression.

Determination of chloride, nitrite, and sulfate in a used zinc bath using anion chromatography with conductivity detection after chemical suppression.

Determination of acetate, chloride, nitrate, phosphate, and sulfate in mayonnaise using anion chromatography with conductivity detection after chemical suppression and advanced dialysis for inline sample preparation.

Determination of arsenite, arsenate, selenite, selenate, chloride, and sulfate using anion chromatography with a combination of suppressed and non-suppressed conductivity detection.

Determination of bromoacetate, methanesulfonate, chloride, phosphate, and sulfate in an acidic cleaning solution using anion chromatography with conductivity detection and chemical suppression.

Determination of α-glycerophosphate and β-glycerophosphate in amino acids using anion chromatography with conductivity detection after chemical suppression.

Determination of fluoride, chloride, nitrite, bromide, nitrate, phosphate, sulfite, and sulfate in river water using anion chromatography with conductivity detection after chemical suppression.

Determination of chloride, bromide, nitrate, phosphate, and sulfate in 20% NaOH after inline neutralization by cation exchange on the 793 IC Sample Prep Module using anion chromatography with conductivity detection after chemical suppression.

Determination of formate, acetate, chloride, benzoate, and oxalate in phenolic extracts using anion chromatography with conductivity detection after chemical suppression.

Determination of chloride, nitrite, bromide, nitrate, phosphate, and sulfate in Schoeniger absorption solution using anion chromatography with conductivity detection after chemical suppression.

Determination of chloride and sulfate in potassium tetraborate (KB4O7 * 4 H2O) using anion chromatography with conductivity detection after chemical suppression.

Determination of gluconate, fluoride, formate, chloride, nitrate, and salicylate using anion chromatography with conductivity detection after chemical suppression.

Determination of fluoride, chloride, nitrate, and sulfate in corrosion powder using anion chromatography with conductivity detection after chemical suppression.

Determination of iodide and thiosulfate in photographic process wastewater using anion chromatography with amperometric detection at the carbon paste electrode after chemical suppression.

Determination of fluoride, chloride, bromide, and sulfate in bath salts (sea salt) using anion chromatography with conductivity detection after chemical suppression.

Determination of fluoride, chloride, phosphate, and sulfate in boric acid using anion chromatography with conductivity detection after chemical suppression.

Determination of sulfate in diesel engine coolant using anion chromatography with conductivity detection after chemical suppression and dialysis for sample preparation.

Determination of chloride, nitrate, and sulfate in ultrapure water after sample preconcentration using anion chromatography with conductivity detection after chemical suppression.

Determination of chloride, sulfite, and sulfate in a surfactant solution using anion chromatography with conductivity detection after chemical suppression.

The exploration and processing of lithium ores is gaining importance with the growing demand for lithium hydroxide. Lithium hydroxide is a key component in the manufacturing of rechargeable batteries for use in various applications including electric vehicles, home storage systems, power tools and consumer electronics. To ensure the efficiency for advanced processing of high purity lithium hydroxide, a fast and reliable quantitative detection technique is required. This application has been developed to monitor the lithium, sodium, and calcium content in the lithium processing samples and mineral concentrates.

As an alternative to flame photometry, ion chromatography with non-suppressed conductivity detection has been approved by the USP as a validated method to quantify potassium content in potassium bicarbonate and potassium chloride effervescent tablets for oral solution. The Metrosep C 6 - 150/4.0 column (L76) provides the required separation of potassium and magnesium. The present IC method has been validated according to USP General Chapter <621>.

Within the scope of the USP monograph modernization, potassium is determined in potassium bitartrate applying cation chromatography with direct conductivity detection. The USP41 monograph for “Potassium bitartrate” does not yet mention an assay for potassium. The separation is performed on a Metrosep C 6 - 150/4.0 column (L76). The assay of potassium is performed with two commercially available products according to USP definitions. All acceptance criteria are fulfilled.

Abrasive machining of e.g., metal parts requires a cooling lubricant. Their purpose besides cooling and lubrication is to inhibit corrosion. Amines are added to the emulsion to keep the pH high. In the actual application, DCHA and MDCHA have to be analyzed besides other amine components and inorganic cations. To avoid oil contamination on the IC system, Inline Dialysis is applied. The detection is performed by direct conductivity detection.

Cation content in snow is greatly dependent on sampling site. Roadside samples are likely to exhibit a high sodium content caused by the use of road salt. This application shows the analysis of a snow sample from a roadside. Separation is performed on a microbore Metrosep C 6 - 250/2.0 column with direct conductivity detection. The 250 mm column was selected due to the large difference in concentrations between sodium and ammonia. This condition enables a baseline separation of the two cations.

Tobacco additives may contain cations like ammonium (see AN-C-168) as well as other cations as counter ions of organic acids. These additives include components to retain moisture and flavor of the tobacco. Ammonium is added to increase the appeal of smoking, and is therefore considered to increase the addictive potential. The determination of cations in tobacco additives is performed by ion chromatographic separation followed by non-suppressed conductivity detection.

1,3,5-trioxane is a heterocyclic compound formed by trimerization of formaldehyde. Trioxane is used for the production of polyformaldehyde plastics such as poly(oxymethylene) (POM) and solid fuels. Aqueous 1,3,5-trioxane solutions frequently contain trace triethylamine that requires quantification. This is performed on the Metrosep C 3 - 250/4.0 column with subsequent direct conductivity detection.

Biogenic amines and trimethylamine N-oxide (TMAO) are indicators for the quality of grape fermentation. The consumption of amine-rich wines often leads to headaches, which is why the amine concentrations in wine must be monitored. This Application Note describes the determination of trimethylamine N-oxide, putrescine, cadaverine and histamine, in addition to various standard cations, with the aid of the Metrosep C 6 - 100/4.0 column and subsequent direct conductivity detection.

Polyols are important raw materials in polyurethane production. Contamination in the raw materials have a great influence on reactions and impair the quality of the end product. Alkali metals are particularly strong catalysts for linear or branched reactions. A rapid and precise method for their simultaneous determination is ion chromatography following Inline Matrix Elimination.

Fast IC means short run times and a high sample throughput on columns with a relatively high flow rate and the standard eluent. Mono-, di- and trimethylamine are separated with the Metrosep C 4 - 150/2.0 within four minutes.

Cleanliness is indispensable in electronics production. Ionic contaminations in particular lead to a drastic worsening of the quality of the printed circuit boards. The present Application Note describes the determination of cations on printed circuit board surfaces. The intelligent Partial Loop Injection Technique (MiPT) used for this purpose permits the determination of cations and anions in the same sample. The determination of the anions is described in AN-S-317.

The determination of low ammonium concentrations besides excess sodium is demanding due to the small retention time difference of these two cations. This Application Note shows direct conductivity detection as an ideal means to detect ammonium in a wastewater sample containing 400 mg/L sodium. AN-S-313 shows the analysis of nitrite traces.

The determination of cations in tap water is a simple IC application. Here it is used to present Metrohm's intelligent Pick-up Technique (MiPuT). MiPuT enables the injection of volumes of minimum size from very small sample quantities. In the present case, two volumes of 10 µL from a sample 100 µL in size are used for anion and cation analysis, respectively. The calibration takes place through the injection of various volumes of a single standard solution. AN-S-302 describes the corresponding anion determination.

Partial loop injection is a well known way of sample introduction to HPLC. In ion chromatography, it is not yet used to a large extent. Liquid handling with Metrohm's Dosino technology now enables to use partial loop injection on a highly reproducible and accurate level. It includes multi-level calibration out of one standard solution. This Application Note shows its use for parallel anion and cation determination in tap water applying one single Sample Processor. The anion results are shown in Application Note S–287.

Determination of lithium, sodium, ammonium, potassium, manganese, calcium, magnesium, strontium, and barium using cation chromatography with direct conductivity detection.

Determination of monomethylamine (MMA), dimethyl-amine (DMA), and trimethylamine (TMA) in the presence of lithium, sodium, ammonium, potassium, cesium, calcium, and magnesium using cation chromatography with direct conductivity detection.

Determination of strontium and barium in monoethylene glycol using cation chromatography with direct conductivity detection.

Calibration of lithium, sodium, ammonium, zinc, potassium, magnesium, and calcium using the partial loop technique and cation chromatography with direct conductivity detection. This technique allows a calibration range of 1:100 (e.g. 1 μg/L to 100 μg/L corresponding to 2 μL to 200 μL injected volume) out of 1 calibration solution. Applying the full range of partial loop injection to the samples one calibration covers a sample concentration range of 1 to 10'000 e.g. 2 μL of a 10 mg/L solution corresponds to the highest calibration level (100 μg/L) while 200 μL of a 1 μg/L solution corresponds to the lowest calibration level.

Determination of lysine as well as sodium, ammonium, potassium, and calcium in bulk lysine using cation chromatography with direct conductivity detection.

Determination of trans-4-methylcyclohexylamine in a pharmaceutical product using cation chromatography with direct conductivity detection.

Determination of copper, zinc, iron(II), and manganese in red wine using cation chromatography with UV/VIS detection after post-column reaction with PAR.

Determination of potassium, magnesium, and calcium in biodiesel using cation chromatography with direct conductivity detection applying automated extraction and subsequent Metrohm Inline Dialysis.

Determination of traces of lithium, sodium, ammonium, potassium, calcium, and magnesium in ethanol using cation chromatography with direct conductivity detection after Metrohm Inline Matrix Elimination.

Determination of dimethylamine (DMA), trimethylaminoxide (TMAO), trimethylamine (TMA), putrescine, cadaverine, and histamine in a fish sample using cation chromatography with direct conductivity detection.

Determination of betaine in the presence of standard cations in an Echinacea product using cation chromatography with direct conductivity detection.

Determination of trimethylamine in hydrogen peroxide (31 %) using cation chromatography with direct conductivity detection after inline matrix elimination, inline preconcentration, and inline calibration.

Determination of sodium, potassium, calcium, magnesium, putrescine, cadaverine, and histamine in a wine sample using cation chromatography with direct conductivity detection.

Determination of sodium, potassium, calcium, and magnesium in the water soluble fraction of a washing powder using cation chromatography with direct conductivity detection.

Determination of zinc, sodium, ammonium, and manganese in the presence of magnesium and calcium in an extract of a zinc compound using cation chromatography with direct conductivity detection.

Determination of calcium and magnesium in rock extracts using cation chromatography with direct conductivity detection.

Determination of calcium and magnesium in high-purity sodium chloride using cation chromatography with direct conductivity detection.

Determination of sodium, potassium, calcium, and magnesium in a drip feeding formula using cation chromatography with direct conductivity detection and dialysis as sample preparation.

Cellulose ester foils are produced using chlorinated solvents. The residual amount of the solvent used in production evaporates within a few days in ambient conditions. The residual solvent is determined by combustion IC, through the conversion of organically bound chlorine to chloride by pyrohydrolysis. The final product needs to be free of all chlorinated solvents. Therefore, critical contents of such compounds can be detected in quality control analysis. Application of MiPT in this study has enabled an automated and precise calibration out of a single standard.

Iron ore is an important resource for steel production. Its natural content of halogens is a quality characteristic due to the corrosiveness of the respective halogenides. Combustion IC applying the sacrificial vial technology is used for the analysis of fluorine and chlorine in ore. WO3 usually is added to improve the release of SO2 and therefore sulfur recovery. In this application, it also significantly improves the recovery of fluoride.

Coal contains a certain amount of fluorine, chlorine, and sulfur compounds. During combustion of the coal, these components release corrosive acids (e.g., fluorine compounds form hydrofluoric acid). Thermal power plants therefore request low-fluorine coal to avoid massive hydrofluoric acid production. In this application note, fluorine content in coal is determined by ion chromatography after pyrohydrolysis.

The burning of coal contaminates the atmosphere with halogens. Fluorine and chlorine are natural components of coal, whereas the bromide that is found therein is often adulterated as calcium bromide in order to reduce mercury emissions. This Application Note shows the results of combustion digestion with Combustion IC for three coal samples, each with a different bromide content.Keyword: pyrohydrolysis

Clay is used for the manufacture of roofing tiles. Quality controls during this process require the determination of halogen and sulfur content. This is ideally accomplished using Metrohm Combustion IC. With this method, the sulfur is determined as sulfate and the halogens as halogenides. Because clay often contains high contents of alkali and earth alkali metal ions that attack the pyrolysis tube, tungsten oxide is added prior to combustion.Keyword: pyrohydrolysis

Polyisobutene (PIB) is an important raw material for a large range of products. Quality control requires the determination of the fluorine content. This task is easily done by Metrohm Combustion IC applying flame sensor technology and Inline Matrix Elimination.Keyword: pyrohydrolysis

Latex gloves are used in clean room environments in order to prevent contaminations. The use of gloves that release corrosive halogenides or sulfate is forbidden in nuclear power plants. The total content of halogen and sulfur is determined by means of Combustion Ion Chromatography. An eluate test is carried out to check the elutable percentage of halogens and sulfate from gloves. Sample preparation is comprised of preconcentration and matrix elimination (MiPCT-ME), as described in AN-S-304.Keyword: pyrohydrolysis

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.

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.

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.

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.

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.

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 presents the ion chromatographic determination of organic degradation products such as glycolate, formate and acetate besides the standard anions fluoride, chloride, nitrate and sulfate.

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 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.

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.

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.

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.

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.

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.

High-Performance Liquid Chromatography (HPLC) and Ion Chromatography (IC) are commonly used in the pharma, food, and environmental sectors to analyze samples for specific components and to verify compliance with norms and standards. However, users of HPLC may run into the limitations of this technique, e.g., when analyzing standard anions or certain pharmaceutical impurities. This white paper outlines how such challenges can be overcome with IC.

For the first time, glyphosate determination and that of its primary metabolite AMPA in drinking water using IC with pulsed amperometric detection (flexIPAD) in the low µg/L range are shown. Compared to HPLC analysis with a mass-selective detector, it is a very cost-effective method for determining the glyphosate and AMPA content in water and foodstuffs. With a detection limit at approx. 1 µg/L, compliance with limit values for glyphosate can be monitored in the USA, Canada, and Australia, among others.

The content of organic chloride in crude oil is determined according to ASTM D8150 in the naphtha fraction after distillation. The naphtha fraction is washed with caustic and water, respectively, to remove hydrogen sulfide and inorganic halides. Here, the determination of organic chloride after inline combustion is presented. Although the sulfur content was of no interest in this application, the same setup allows sulfur quantification.

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

Monitoring the range of organic acids in wine is crucial to improve flavor and quality, and to fulfill universal standardized criteria such as the International Code of Oenological Practices. Analytically, organic acids can be properly determined with ion chromatography (IC) and suppressed conductivity detection. As a multicomponent method, inorganic acids can also be resolved which are also valuable tracers for wine quality and taste. This Application Note presents two IC methods for wine quality analysis: a fast isocratic screening method of major organic acids and anions including sulfite, and a complex monitoring method with a binary gradient to separate 15 organic acids. Inline Ultrafiltration was used for economical sample treatment.

This Application Note presents an update to the standard AOAC method for total GOS determination in foodstuffs.

Application: Free and total carbohydrate determination in instant coffee with IC-PAD according to AOAC 996.04 and ISO 11292.

This Application Note presents ion chromatography as a precise method to analyze anions in beer as well as cations with non-suppressed conductivity. Automation with Inline Ultrafiltration is also discussed.

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