アプリケーション検索（技術資料）

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.

Comparative measurements show that the new Metrosep C 4 cation column has even better separation characteristics than the previous Metrosep C 2 and Metrosep Cation 1-2 column types. The Metrosep C 4 column has a clearly improved peak shape which leads to a better separation of the individual peaks. Using Metrosep C 4 the number of theoretical plates per meter was noticeably higher than that obtained on the Metrosep C 2 or C 1-2 column. Additionally for standard cations transition metals and amines, the Metrosep C 4 column shows better results with respect to peak shape, peak height, resolution and asymmetry factor. The clearly improved resolution of the C 4 column with its narrow and high peaks achieves baseline separation for six standard and six transition metal cations. Analysis times and peak areas obtained with the C 4 column are in the same range as those obtained with its predecessors.As a result of the latest production methods and materials, the promising Metrosep C 4 column excels by an outstanding separation performance for complex mixtures comprising standard cations, transition metal cations and amines.

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.

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.

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.

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.

Metrohm`s intelligent Preconcentration Technique with Matrix Elimination (MiPCT-ME) excels in its capacity to perform automatic ion chromatographic determinations over 6 orders of magnitude. Crucial requirements for this are the system`s intelligence and the exact measurement of the sample volume. While the intelligence allows to compare results and take decisions, the dosing device takes over the high-precision liquid handling of even single-digit microliter volumes to the preconcentration column. By using only one analytical setup and without additional rinsing, samples containing both ultratraces and high concentrations can be analyzed.As the other Metrohm Inline Techniques, the MiPCT-ME technique presented reduces the workload, ensures complete traceability, is free of carryover effects and significantly improves accuracy and reproducibility of the results.

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

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 Bulletin is a supplement to Application Bulletin no. 36 (Half-wave potentials of inorganic substances) in the sense that the half-wave potentials of 100 different organic substances are listed. At the same time the supporting electrolytes used and the limits of determination are given.The various substances are listed in alphabetical order. The most important polarographically active functional groups are taken into consideration. This means that substances for related structures can also be determined polarographically in the same or similar supporting electrolytes, although they may not appear in the list.Unless otherwise stated, the half-wave potentials refer to a temperature of 20 °C, and the potentials are given in volts, measured with a sat. KCI-Ag/AgCl electrode assembly.The determination limits give the smallest concentrations which can be measured without risking serious errors in the results. In all cases, the limit of detection lies below the limit of determination.

This document explains how to measure Na ion concentration in diverse matrices with a sodium ion-selective electrode (Na-ISE) using direct measurement and standard addition.

This bulletin contains two parts. The first part gives a short theoretical overview while more details are offered in the Metrohm Monograph Conductometry. The second, practice-oriented part deals with the following subjects:Conductivity measurements in general; Determination of the cell constant; Determination of the temperature coefficient; Conductivity measurement in water samples; TDS – Total Dissolved Solids; Conductometric titrations;

Mixtures of aluminum and magnesium ions can be analyzed automatically using potentiometric titration. The excess DCTA is back-titrated with copper(II) sulfate solution after the addition of 1,2-diaminocyclohexanetetraacetic acid (DCTA) and complex formation. The ion-selective copper electrode is used here as the indicator electrode. First, the aluminum is determined in acidic solution and then the magnesium in alkali solution.

This Bulletin, using practical examples, indicates how the user can achieve optimum pH measurements. As this Bulletin is intended for actual practice, the fundamentals - which can be found in numerous books and publications - are treated only briefly.

This Bulletin provides an overview of the potentiometric titer determination of current titrants. Many publications only describe methods with color indicators. However, the titration conditions chosen for the titer determination should resemble those used for the actual analysis as closely as possible. The tables contain suitable titrimetric standard substances and electrodes for selected titrants as well as additional information. Following this, an example is given to show what an SOP for a titer determination could look like.

This Bulletin describes the determination by ion chromatography of anions, particularly fluoride, chloride, nitrite, bromide, nitrate, and sulfate using the Hamilton PRPX100 IC anion column without chemical suppression.

Determination of aluminum using cation chromatography, post-column reaction and UV detection.

Determination of mono-, di-, and trimethanolamine (MMA, DMA, TMA respectively), in the presence of lithium, sodium, ammonium, potassium, magnesium, cesium, calcium, and strontium using cation chromatography with direct conductivity detection.

Determination of traces of methylamine, isopropylamine diethylethanolamine, and diethylamine in the presence of lithium, sodium, ammonium, potassium, magnesium, and calcium using cation chromatography with direct conductivity detection.

Determination of traces of lutetium, ytterbium, thulium, erbium, terbium, gadolinium, samarium, neodymium, praseodymium, cerium, and lanthanum using cation chromatography with direct conductivity detection.

Determination of traces of lutetium, ytterbium, thulium, erbium, terbium, gadolinium, samarium, neodymium, praseodymium, cerium, and lanthanum using cation chromatography with gradient elution and UV/VIS detection after post-column reaction with Arsenazo III.

Determination of methylamine in the presence of sodium, ammonium, potassium, magnesium, and calcium using cation chromatography with direct conductivity detection.

Determination of monoethanolamine (MEA), diethanolamine (DEA), and triethanolamine (TEA) in the presence of lithium, sodium, ammonium, potassium, calcium, and magnesium 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 lithium, sodium, ammonium, potassium, manganese, calcium, magnesium, strontium, and barium using cation chromatography with direct conductivity detection.

Determination of lithium, sodium, ammonium, and monoethanolamine (MEA) using cation chromatography with direct conductivity detection and Metrohm Inline Preconcentration and Inline Calibration.

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 required eluent concentration. The use of eluent concentrates is suitable for any eluent. This facilitates unattended operation of the system over several weeks (see AN S-296 for anion eluent preparation).

Metrohm intelligent Partial Loop Technique (MiPT) is a versatile injection mode in IC. In this application, injection volumes range from 4 to 200 µL (corresponding to 0.5 - 10 mg/L) using the 250 µL loop. Here, the use of 2 and 5 mL Dosing Units are compared.

The Metrosep C 6 columns have a higher capacity than those of the Metrosep C 4. The present Application Note describes the exceptional separating efficiency for standard cations with the three Metrosep C 6 column lengths available. The outstanding sodium-ammonia separation is particularly noteworthy.

マトリックス除去を伴うメトローム インライン前濃縮技術 (MiPCT-ME) は、前濃縮、マトリックス除去、およびマルチレベル校正を組み合わせた強力な方法です。このアプリケーション ノートでは、この方法論が 2 mg/L アンモニアに加えて微量のナトリウムの測定に適用されます。Metrosep C 6 - 250/4.0 カラムは、選択性の理由から使用されます。

Sample dilution is a work-intensive routine task in the analysis laboratory. An automatic two-step dilution exponentiates the dilution factor – 1:100 – thus incorporating a dilution factor of 10,000. The intelligent dilution is made possible by MagIC Net, which calculates the essential dilution steps, and by the dosing properties of the 800 Dosino and the Liquid Handling Station. The Application Note shows statistical results of a 1:10,000 dilution.

Fast IC means short run times on separation columns with a relatively high flow rate and the standard eluent. Here the standard cations are separated within eleven minutes on the Metrosep C 4 - 250/2.0. The sodium and ammonium peaks are separated from one another under these conditions.

Fast IC means short run times on separation columns with a relatively high flow rate. Separation with the Metrosep C 4 - 150/2.0 is even quicker than that in the AN-C-150 at 1.1 mL/min. Here, the standard cations are separated within five minutes. Under the selected conditions, sodium and ammonium are no longer completely separated.

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 tri-ethanolamine are separated with the Metrosep C 4 - 150/2.0 within 2.5 minutes.

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.

Metrosep C 6 - 250/4.0のカラムの安定性に関して、長期間に渡るラボ試験による調査が行われました。6日間連続で、各日2セットのインジェクションが行われました。それぞれのセットは水道水のインジェクション9回、検査基準のインジェクション3回、そして水道水のインジェクション6回から構成されています。それぞれ7日目には、ICシステムをシャットダウンしました。システムは計10週間以上稼働し、計2150回のインジェクションが行われました。その結果は傑出した再現性を示し、カラムの高度な安定性が立証されました。

インラインマトリックス除去を伴うインテリジェントなインライン濃縮（MiPCT-ME）は、亜鉛やジエチルアミンなどといった6つの基本陽イオンの微量測定に使用されます。Metrosep C 4 - 250/2.0 のマイクロボアカラムでは、24分で分析が完了します。回収率は95％を超えます。ソフトウェア MagIC Net によって算出される検出限界は、濃縮量が4ｍLの場合、より低いng/Lレベルにまで及びます。

医薬用の酒石酸水素カリウムは、USP要件に適合している必要があります。現行のモノグラフ (USP 42) では、アンモニウム不純物の測定に比色メソッドを用いています。イオンクロマトグラフィーにより、カリウムのアッセイ (AN-C-181を参照) に使用されるのと同じ条件において、シングル測定で測定できます。USP モノグラフの近代化の過程では、このイオンクロマトグラフィーによるアプローチによりこのタイプの分析がより容易になっています。

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

連続サプレッションを伴う陽イオンクロマトグラフィにより、その炭酸水素塩中の陽イオンを測定することが可能です。溶離剤（大抵の場合硝酸が使われる）は、炭酸に変化します。二酸化炭素および水の中の炭酸が分解した後、CO2 サプレッサにより前者は連続的に除去されます。このようにベースラインノイズの減少が達成されると、検出限界値を下げることができ、また陽イオン濃度が非常に低い場合でも再現性が改良されます。この 技術資料は、算出された陽イオン濃度 10 µg/L の再現性が示されています。

この技術資料では、イソクラティック条件下におけるアルキルアミン、エタノールアミンに加えて、標準陽イオンをMetrosep C Supp 1 - 250/4.0カラム で測定しています。イオンクロマトグラフは、連続サプレッション後、電気伝導度検出器を使用しています。

Metrosep C Supp 2カラムシリーズは、ポリスチレン/ジビニルベンゼンを基材としており、そのため連続陽イオンサプレッションを適用できます。このANは、連続陽イオンサプレッションに後続する電気伝導度検出を用いた150mmバージョンのカラムにおける異なるアミンの分離および検出について紹介するものです。

短いMetrosep C Supp 2 - 100/4.0により、高い溶離液流量を適用できます。より濃度の高い溶離液 (5.0 mmol/Lの代わりに7.0mmol/Lの硝酸) を用いると、ナトリウム、カリウム、マグネシウム、およびカルシウムの4種の陽イオンの処理時間を5分間に短縮することができます。連続サプレッションの後に電気伝導度検出が行われます。

溶液中の重金属イオンの測定は、最も成功を収めた電気化学のアプリケーションの1つです。この Application Note では、水道水のサンプル中の2つの検体の存在を測定するのにアノーディックストリッピングボルタンメトリーが用いられています。

電解質の電気伝導度を計算するには、電池のセル定数を知る必要があります。FRA32M モジュールを装備した Metrohm Autolab PGSTAT204 と Autolab Microcell HC セットアップとの組み合わせが、温度管理された電気化学セル TSC1600 の電気伝導度セル定数の測定に使われました。

TEMPO の電気酸化反応における動態パラメータならびに質量移動パラメータは、Autolab Microcell HC システムのための TSC Surface 測定セルを用いて測定されます。この電池により、温度管理下での3つの電極コンフィグレーションにおける液体電解質中の電気化学プロセスの研究が可能となります。

このApplication Noteでは、電気化学電池における様々な接続のタイプや装置のセッティングなど、EISを実施するための準備について説明されています。

Here, the most common circuit elements for EIS are introduced which may be assembled in different configurations to obtain equivalent circuits used for data analysis.

Explore how to construct simple and complex equivalent circuit models for fitting EIS data in this Application Note. Nyquist plots are shown for each example.

このApplication Noteでは、電気化学インピーダンス測定中の個々の周波数のための生のタイムドメインデータの記録の長所について説明されています。