アプリケーション検索（技術資料）

In this poster a convenient direct injection suppressed ion chromatographic method for determining chloride and sulfate in denatured ethanol samples according to ASTM D7319 is presented.

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.

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

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.

Several testing methods such as the determination of the acid and the iodine numbers in biodiesel as well as the quantification of sulfate and chloride in bioethanol are described.

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.

The analytical challenge treated in the present work consists in the determination of chloride, phosphate and sulfate in the presence of difficult sample matrices that interact with the stationary column phase or even render it unusable. Metrohm`s patented stopped-flow dialysis coupled to the new 881 Compact IC pro ion chromatograph overcomes these drawbacks. Two standard solutions covering the concentration ranges 1.0…3.6 mg/L and 10…36 mg/L as well as two samples, an ultra-high temperature (UHT) processed milk and a baby milk powder, were characterized in terms of analyte concentration, relative standard deviation, calibration quality, carryover and recovery rates. While the five-point calibration curves yielded correlation coefficients (R) better than 0.9999, carryover (between two subsequent injections of a concentrated sample and a blank) was less than 0.49%. Recoveries for the low (10…36 mg/L) and high standard concentrations (1.0…3.6 mg/L) were within 91…99% and 94…100%, respectively. Automated compact stopped-flow dialysis is a leading-edge sample preparation technique that ensures optimum separation performance by effectively protecting the column from detrimental matrix compounds.

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.

This poster provides an overview of ion chromatographic methods combined with inline sample preparation for the determination of anions and water-extractable cations in biofuels. In addition, the determination of the oxidation stability is described.

この研究では、オフラインの手動フィルター抽出とそれに続くイオンクロマトグラフ分析を含むフィルターベースの方法で得られた空気サンプリングデータを、イオンクロマトグラフ（PILS-IC）に接続された自動Particle-Into-Liquid-Samplerで得られたデータと比較します。 -ICは、エアロゾルサンプリング用の簡単な機器であり、長期間の無人操作をほぼリアルタイムで測定できるため、エアロゾル粒子のイオン組成の急激な変化を監視するために不可欠なツールです。

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.

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.

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

Thermometric titration can solve application problems that potentiometry cannot solve at all, or at least not satisfactorily.

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.

イオンクロマトグラフィーは様々なイオン種の困難な分離課題に取り組んでおり、一般的に電気伝導度検出器とともに使用します。独立した二次検出としての質量検出は検出限界を著しく下げるので、たとえ共溶出しても検体の識別を確認することができます。このポスターでは、IC-MS および自動サンプル前処理技術の組み合わせにより、土壌または爆発残渣のような困難なサンプルマトリックスにおける陰イオンおよびオキソ陰イオンの分析がいかに処理されるかについて説明しています。

AAPS会議にてUSPと共同で発表されたこのポスターは、原薬、炭酸水素カリウムならびに炭酸カリウム中の塩化物および硫酸塩の測定のためのICメソッドの検証に弊社が成功したことを紹介するものです。ここで提案されているICメソッドは、比濁法/目視比較メソッドの限界を克服するものです。

This Bulletin describes analysis methods for determining the following parameters: pH value, total titratable acid, ash alkalinity, formol number, total sulfurous acid, chloride, sulfate, calcium, and magnesium. These methods are suitable for the analysis of jams, fruit and vegetable juices, and their concentrates.

This Bulletin describes potentiometric titration methods for checking sulfuric acid and chromic acid anodizing baths. In addition to the main components aluminum, sulfuric acid, and chromic acid, chloride, oxalic acid, and sulfate are determined.

This Bulletin describes three potentiometric, one photometric, one thermometric and one conductometric titration method for sulfate determination. The question of which indication method is the most suitable depends primarily on the sample matrix.Method 1: Precipitation as barium sulfate and back titration of the Ba2+ surplus with EGTA. Use of the ion-selective calcium electrode as indicator electrode.Method 2: As with Method 1, although with the electrode combination tungsten/platinum.Method 3: Precipitation titration in semi-aqueous solution with lead nitrate in accordance with the European Pharmacopoeia using the ion-selective lead electrode as indicator electrode.Method 4: Photometric titration with lead nitrate, dithizone indicator and the Optrode 610 nm, particularly suitable for low concentrations (up to 5 mg SO42- in the sample solution).Method 5: Thermometric precipitation titration with Ba2+ in aqueous solution, particularly suitable for fertilizers.Method 6: Conductometric titration with barium acetate in accordance with DIN 53127

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.

Sulfate can be rapidly and easily titrated thermometrically using a standard solution of Ba2+ as titrant. In industry, the widespread procedure is applied to the determination of sulfate in wet-process phosphoric acid. This bulletin deals with the determination of sulfate in granular fertilizers such as MAP (monoammonium phosphate), DAP (diammonium phosphate) and TSP (triple superphosphate). Results are reported as percentage of elemental sulfur, %S.

Sulfate can be rapidly and easily titrated thermometrically using a standard solution of Ba2+ as titrant. In industry, the widespread procedure is applied to the determination of sulfate in wet-process phosphoric acid.

建築や装飾の用途に使われるポリマー材料は耐炎性が必要です。要求される対炎性の基準に達するため、プレーンポリマーに難燃剤が添加されています。難燃剤にはしばしばハロ有機化合物が用いられます。こういった化合物、および導入されたハロゲンの各濃度は、燃焼イオンクロマトグラフによって測定することができます。全システムのリカバリは認証標準物質 (CRM) によって試験確認済みです。

鉄鉱石は、鉄製品にとって重要な資源です。そのハロゲンの自然含有量は、個々のハロゲン化物の腐食による品質特性です。保護バイアルを使用した燃焼イオンクロマトグラフィは、鉄鉱石中のフッ素および塩素の分析に使われます。SO2の放出と、それによる硫黄回収を改善するためにWO3が通常助燃剤として添加されます。このアプリケーションでは、フッ化物の回収も著しく改善させています。

衣料品に使われるテキスタイルには、フルオロケミカルを様々な処理を行い撥水効果をもたせることがあります。これらの化合物、特にペルフルオロ有機物は、自然環境では極めて分解されにくく、そのため新たな汚染物質に数えられます。熱分解装置とイオンクロマトグラフを組み合わせた燃焼法イオンクロマトグラフィシステムは、織物中のフッ素含有量の分析が行えます。

硫黄はアンモニアガスの危険な汚染物質です。金属の高温の硫化を引き起こし、他の成分と共に刺激性錯体を形成したり、あるいはアンモニアガスが用いられるプロセス工程において反応を起こしたりすることがあります。このような不純物の濃度は極めて低く抑えられていますが、危険なレベルとされる0.5 mg/Lを超えないようにしなければなりません。この基準は、燃焼イオンクロマトグラフィシステムのシステムブランク値に非常に近いですが、試料に含まれれている硫黄が、この危険値を超えていないことを証明するのために使われています。

セルロースエステル膜は、塩化物溶媒を用いて製造されます。製造に用いられた溶媒残留物は数日で蒸発します。残留溶媒は熱分解熱による有機結合した塩素から塩化物への変換させて、燃焼イオンクロマトグラフフィシステムで測定します。最終製品は塩化物系の溶剤が残っていない状態である必要があります。危険な量のこれらの化合物が残っていないかを品質管理分析において測定することができます。このアプリケーションでは、単一の標準試料から正確な自動キャリブレーションカーブ作成もおこなっています。

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

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.

Determination of the sulfate content of wet process phosphoric acid.

Determination of the sulfate content of brines.

Determination of low levels of sulfate (to approximately 20mg/L SO42-) by thermometric titration.

Determination of sulfate and total acids in a nitrating mixture.

この技術資料では、温度滴定法で銅の定量にするチオ硫酸ナトリウムの標定試験の仕方について解説しています。

Standardization of barium acetate titrant used in the determination of sulfate in phosphoric acid. The same procedure is applied if barium chloride is chosen as the titrant.

Sulfate is precipitated by reaction with an acidified barium chromate solution. The excess barium chromate is precipitated by basification with ammonia solution. Residual soluble chromate equivalent to the sulfate content of the sample is titrated with a solution of standard ferrous ion to a thermometrically determined endpoint.

Sulfate is precipitated as barium sulfate by reaction with an acidified barium chromate solution. The excess barium chromate is precipitated by basification with ammonia solution. Residual soluble chromate, equivalent to the sulfate content of the sample, is titrated with a solution of standard ferrous ion to a thermometrically determined endpoint.

This Application Note supplements AN-H-003 with the treatment of the standard addition of sulfate as sulfuric acid. This technique may be contemplated when either sulfate levels are too low for a satisfactory direct titration, or when the sample matrix hinders endpoint detection, leading to poor precision and accuracy.

硫黄は植物のための副次的栄養素であり、葉緑体の生育と機能に不可欠です。肥料には、硫黄は通常、硫酸塩という形態で提供されています。伝統的に、硫酸塩含有量はバリウムを用いた沈殿物による重量測定で測定されます。このメソッドの欠点は、非常に長い時間がかかり、かつ面倒な分析手順を要することです。このApplication Noteでは、硫酸塩を塩化バリウムを用いた沈殿滴定にて測定する代替メソッドが紹介されています。硫黄含有量 1～8% の様々な固形物および液体NPK肥料が分析されました。TETによる肥料中の硫酸塩の分析では、液体NPK肥料の場合はサンプル前処理はまったく不要、固形物NPK肥料の場合必要なのは最小限のサンプル前処理のみです。一回の測定におよそ3分しかかかりません。メソッドの感度を高めるためにサンプルには標準硫酸溶液がスパイキングされ、それは結果計算の際に考慮されます。

This Application Note covers the formation of calcium carbonate from solution.

Determination of anions in solder paste after alcoholic extraction using anion chromatography with direct conductivity detection.

Determination of anions in a Schoeniger absorption solution of a test mixture without decomposition of the H2O2 using anion chromatography with direct conductivity detection.

Determination of chloride, nitrate, phosphate, sulfate, and oxalate in dried potatoes using anion chromatography with direct conductometric detection.

Determination of acetate, formate, chloride, bromide, and sulfate in toluene using anion chromatography with direct conductivity detection.

Determination of chloride, nitrate, phosphate and sulfate in plant leaf extracts using anion chromatography with direct conductometric detection.