アプリケーション検索（技術資料）

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.

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 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.

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.

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.

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.

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.

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.

The photometric determination of nitrate is limited by the fact that the respective methods (salicylic acid, brucine, 2,6-dimethyl phenol, Nesslers reagent after reduction of nitrate to ammonium) are subject to interferences. The direct potentiometric determination using an ion-selective nitrate electrode causes problems in the presence of fairly large amounts of chloride or organic compounds with carboxyl groups. The polarographic method, on the other hand, is not only more rapid, but also practically insensitive to chemical interference, thus ensuring more accurate results. The limit of quantification depends on the matrix of the sample and is approximately 1 mg/L.

食品から硝酸塩を過剰に摂取すると、特に小さな子供や感受性の高い大人にチアノーゼが起こることが以前から知られています。WHO の規格では、人が c(NO3-) ≥ 50 mg/L の硝酸塩を摂取すると危険とされています。しかし、最近の研究では、人体内の硝酸塩濃度が高すぎると、（亜硝酸塩を介して）発がん性が指摘され、さらに危険なニトロソアミンが生成される可能性があることが明らかになりました。硝酸アニオンを測定するための既知の測光メソッドは、時間がかかり、広範囲にわたる干渉を受けやすくなります。硝酸塩分析の重要性がますます高まる中、選択的かつ迅速で、比較的正確な分析法の要求も高まっています。この技術資料では、水サンプル、土壌抽出物、肥料、野菜、飲料の硝酸塩濃度を迅速測定した応用例を紹介しています。

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.

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.

Advances in polymeric membranes and screen-printed technologies have enabled miniaturized, portable potentiometric sensors ideal for point-of-care analysis.

Determination of nitrate in a copper plating bath after conversion of nitrate to ammonium. Direct potentiometric measurement using the NH3-ISE.

硝酸塩はあらゆる一般的な農産物に含まれており、また肥料において広範囲に用いられることから、硝酸塩は野菜や、ジュースなどのその加工製品に驚くほどの高濃度で含有されていることがあります。硝酸塩含有量は、ヒトの体内でニトロソアミンを形成する恐れがあることから、多くの国で規制されています。ニトロソアミンは、癌を引き起こす可能性があるため、世界保健機関 (WHO) は一日の許容摂取量 (ADI) を 3.7 mg/kg と定めています。ジュースなどに含まれる硝酸塩含有量を管理すべく、その濃度の迅速かつ低コストな査定が、硝酸イオン選択性電極を用いた標準添加によって行われます。メソッドは自動化することができ、また競合するクロマトグラフ法または分光法メソッドと比較して、より早く低価格です。

窒素は環境中に自然に存在します。しかしながら、表面水や地下水の窒素濃度が過剰であると、水質に悪影響を及ぼす恐れがあるため問題になります。たいていの場合、過剰な窒素量は農業における肥料の広範囲な用法に直接的に起因します。窒素は土壌から流れ出やすいため、最終的に表面水や地下水にたどり着くことがあります。窒素含量は多くの国で制限されているので、品質管理のため、その濃度の迅速かつ安価な調査法が求められます。窒素濃度は、窒素イオン選択性電極を用いた直接測定によって簡単に知ることができます。最初に校正が行われ、その後サンプルが1分未満で測定されます。これは、様々な水サンプル中の窒素含量を測定するための迅速かつ安価で信頼性の高いメソッドです。

ルシゲニンは最も頻繁に使われる化学発光試薬の1つであり、例えばスーパーオキシドアニオン基の存在指標などとして用いられることがあります。ルシゲニンは購入するには比較的高価でありますが、その合成はアクリダノンから出発する2段階の合成を含むのみです。1段階目にはメチル化が含まれ、2段階目の形態は最終的に硝酸ルシゲニンに変換される塩化ルシゲニンです。合成されたルシゲニンの純度を確認するため、硝酸塩選択性電極を用いてイオン測定が実施されます。これは、イオンクロマトグラフィーなどといった競い合うメソッドと比較すると、迅速かつ安価なメソッドであります。

Determination of NO3- and ClO4- in the presence of a large excess of HCl using anion chromatography with direct conductivity detection (using time program for full scale change after 18 min).

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 chloride, nitrate, phosphate and sulfate in plant leaf extracts 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 fluoride, chloride, nitrite, nitrate, and sulfate in an effluent sample using anion chromatography with direct conductometric detetction.

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

Determination of nitrate in a nickel plating bath using anion chromatography with UV/VIS detection (205 nm).

Determination of sulfite, nitrite, nitrate, sulfate, imidodisulfonate, and peroxodisulfate using ion-pair chromatography with conductivity detection after suppression.

Measures to monitor or prevent corrosion are crucial in nuclear power plants, where significant risks to health and safety can occur if corrosion is left unchecked. Anions corrode metals under high temperature and pressure, therefore their concentrations must be monitored at all times. The analytical challenge in the primary circuit is detection of anions in the μg/L range alongside gram quantities of boric acid and lithium hydroxide. Precise, reliable trace analysis requires the method to be automated as much as possible. The 2060 IC Process Analyzer from Metrohm Process Analytics can measure several anions from a single injection, with combined Inline Preconcentration and Inline Matrix Elimination to measure low anion concentrations precisely and reliably time after time.

基礎化学工業界は、数千種もの原料の非常に大規模な生産に対する責任を負っています。一定レベルの不純度は様々なプロセスにおいて重大な問題を引き起こす可能性がある一方、下流産業は自社製品を製造するのに、一定レベルの化学的純度に依存しています。基礎化学物質である NaOH および KOH の製造中、皮膜セルを用いた飽和食塩水の電気分解後、蒸発によって更に濃縮された製品が生産されます。食塩水に用いられている塩からの不純物もまた濃縮されます。一般的に、こういった不純物の分析は、多様な保存期間を有する様々な有害化学物質を用いてオフラインで行われます。プロセスイオンクロマトグラフは、ASTM E1787-16に従って測定をオンラインで行うことができ、時間をかけることなく、またラボでの危険な実験を行わずに、製品の質を保証することができます。

Determination of trace levels of chloride, nitrate, phosphate, and sulfate in boiler feed water using anion chromatography with conductivity detection after chemical suppression.

この技術資料では、可変濃縮とInline Matrix Elimination ( MiPCT-ME ) を組み合わせたInline Neutralization（ インライン中和 ）を使用することにより、注入前にほう酸を自動除去してからイオンクロマトグラフで微量アニオンを直接分析しています。

940 Professional IC Vario、942 Extension Module Vario LQH、941 Eluent Preparation Module の組み合わせにより、イオンクロマトグラフィーを使用したプロセス監視が可能となります。ProfIC Vario 12 Anion の名称を持つこの組み合わせは、Metrohm Process IC の陰イオンバージョンです。サンプル前処理には、マトリックス除去機能を備えたインテリジェント濃度調整技術が使用されます。ELGA PURELAB® Flex 6 の使用により、特にサンプル量が多い場合でも、最高品質の超純水の供給を保証します。

Determination of the anions in potable water using anion chromatography with conductivity detection after chemical suppression.

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

Determination of chloride, nitrate, phosphate, and sulfate in wastewater using anion chromatography with conductivity detection after chemical suppression.

電気伝導度検出器付きイオンクロマトグによる地表水中のフッ化物、塩化物、亜硝酸塩、臭化物、硝酸塩、硫酸塩の測定アプリケーションです。

Determination of fluoride, chloride, nitrite, nitrate, and sulfate in soil eluates using anion chromatography with conductivity detection after chemical suppression.

Determination of lactate, chloride, nitrate, sulfite, and phosphate in wine using anion chromatography and conductivity detection after chemical suppression.

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

Determination of nitrite and nitrate in wastewater using anion chromatography with conductivity detection after chemical suppression.

Determination of fluoride, chloride, and nitrate in a solution of NiSO4, ZnSO4 in sulfuric acid using anion chromatography with conductivity detection after chemical suppression.