Sovellukset
- 410000051-BIdentification of microplastics with Raman microscopy
Research laboratories must expand their capabilities to routinely analyze candidate microplastics from environmental samples to determine their origin and help predict biological impacts. Spectroscopic techniques are well suited to polymer identification. Laboratory Raman spectroscopy is an alternative to confocal Raman microscopes and Fourier transform infrared (FTIR) microscopes for quick identification of polymer materials. Raman microscopy was used to identify very small microplastic particles in this Application Note.
- 8.000.6005Hyphenated techniques as modern detection systems in ion chromatography
The coupling of highly efficient ion chromatography (IC) to multi-dimensional detectors such as a mass spectrometer (MS) or an inductively coupled plasma mass spectrometer (ICP/MS) significantly increases sensitivity while simultaneously reducing possible matrix interference to the absolute minimum. By means of IC/MS several oxyhalides such as bromate and perchlorate can be detected in the sub-ppb range. Additionally, organic acids can be precisely quantified through mass-based determination even in the presence of high salt matrices. By means of IC-ICP/MS different valence states of the potentially hazardous chromium, arsenic and selenium in the form of inorganic and organic species can be sensitively and unambiguously identified in one single run.
- 8.000.6016Advantages of multidimensional ion chromatography for trace analysis
The analytical challenge treated in the present work consists in detecting trace concentrations (ppb) of bromide in the presence of a strong chloride matrix. This problem was overcome by separating the bromide ions from the main fraction of the early eluting chloride matrix (several g/L) by applying two sequential chromatographic separations on the same column. After the first separation, the main fraction of the interfering chloride matrix is flushed to waste, while the later eluting anions are diverted to an anion-retaining preconcentration column. After elution in counter flow, the bromide ions are efficiently separated from the marginal chloride residues. The four-point calibration curves for bromide and sulfate are linear in the range of 10…100 µg/L and 200…800 µg/L and yield correlation coefficients of 0.99988 and 0.99953 respectively. For the method shown here, a second injection valve and a preconcentration column are the only additional devices needed to master this demanding separation problem.
- 8.000.6033Analysis of energetic materials in various water and soil samples using HPLC and LC-MS
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.
- 8.000.6053Trace-level determination of perfluorinated compounds in water by suppressed ion chromatography with inline matrix elimination
This poster describes a simple and sensitive method for the determination of perfluorooctanoate (PFOA) and perfluorooctane sulfonate (PFOS) in water samples by suppressed conductivity detection. Separation was achieved by isocratic elution on a reversed-phase column thermostated at 35 °C using an aqueous mobile phase containing boric acid and acetonitrile. The PFOA and PFOS content in the water matrix was quantified by direct injection applying a 1000 μL loop. For the concentration range of 2 to 50 μg/mL and 10 to 250 μg/mL, the linear calibration curve for PFOA and PFOS yielded correlation coefficients (R) of 0.99990 and 0.9991, respectively. The relative standard deviations were smaller than 5.8%.The presence of high concentrations of mono and divalent anions such as chloride and sulfate has no significant influence on the determination of the perfluorinated alkyl substances (PFAS). In contrast, the presence of divalent cations, such as calcium and magnesium, which are normally present in water matrices, impairs PFOS recovery. This drawback was overcome by applying Metrohm`s Inline Cation Removal. While the interfering divalent cations are exchanged for non-interfering sodium cations, PFOA and PFOS are directly transferred to the sample loop. After inline cation removal, PFAS recovery in water samples containing 350 mg/mL of Ca2+ and Mg2+ improved from 90…115% to 93…107%.While PFAS determination of low salt-containing water samples is best performed by straightforward direct-injection IC, water rich in alkaline-earth metals are best analyzed using Metrohm`s Inline Cation Removal.
- 8.000.6093Determination of arsenic in water with the gold electrode (scTRACE Gold)
Because of its toxicity, the World Health Organization recommends a maximum arsenic content in drinking water of 10 μg/L. Anodic stripping voltammetry with the scTRACE Gold offers a straightforward, highly affordable alternative to spectroscopic determination.
- 8.000.6101Analysis of Anions and Oxoanions using Ion Chromatography Mass Spectrometry (IC-MS)
Ion chromatography tackles difficult separation problems of various ionic species and typically works with conductivity detection. Mass detection as a secondary independent detector significantly lowers the detection limits and confirms the identity of analytes even when coeluting. This poster describes how the combination of IC-MS and automated sample preparation techniques cope with the analysis of anions and oxoanions in challenging matrices such as soil or explosion residues.
- 8.000.6103Speciation of Cr(III) and Cr(VI) by IC-ICP-MS and Empower 3
This poster demonstrates the feasibility of coupling a Metrohm IC system to a PerkinElmer NexION ICP-MS, operated under Empower 3 Software.Using a Metrosep Carb 2 column, the chromatographic separation of both species was achieved with a high resolution. Low background and high sensitivity allow determination in the low ng/L range.Optimal separation and full complexation of Cr(III) is already possible with EDTA concentrations from 40 μmol/L in low matrix solutions and may need to be increased depending on the sample matrix.Handling of the system was easy and user friendly. It was shown that speciation of Cr(III) and Cr(VI) can be carried out on this system utilizing a professional data system for acquisition, processing, and reporting.
- AB-027Potentiometric titration of chloride and bromide in the presence of each other
If chloride and bromide are present in approximately equal molar concentrations they can be titrated directly with silver nitrate solution after addition of barium acetate. If, however, the molar ratio n(Br-) : n(Cl-) changes from 1 : 1 to 1 : 5, 1 : 10, 5 : 1 or 10 : 1 then greater relative errors must be expected with this method. The Bulletin describes an additional titration method that allows bromide to be determined in the presence of a large excess of chloride. The determination of small chloride concentrations in the presence of a large excess of bromide is not possible by titration.
- AB-046Potentiometric determination of cyanide
The determination of cyanide is very important not only in electroplating baths and when decontaminating wastewater but, due to its high toxicity, also in water samples in general. Concentrations of 0.05 mg/L CN- can already be lethal for fish.This Bulletin describes the determination of cyanide in samples of different concentrations by potentiometric titration.Chemical reactions:2 CN- + Ag+ → [Ag(CN)2]-[Ag(CN)2]- + Ag+ → 2 AgCN
- AB-053Determination of ammonium or Kjeldahl nitrogen
The potentiometric titration of Kjeldahl nitrogen is one of the most common analytic procedures. It is referenced in numerous standards, ranging from the food and animal feed industries through sewage and waste analysis and all the way to the fertilizer industry. As a rule, the samples are digested with concentrated sulfuric acid with the addition of a catalyst. The ammonium sulfate that is formed is distilled as ammonia in alkali solution, collected in an absorption solution and titrated there.This Bulletin provides a detailed description of potentiometric nitrogen determination following distillation of the digestion solution, followed by a discussion of the possibilities of coulometric titration (without distillation).
- AB-057Polarographic determination of nicotine
The quantitative determination of the alkaloid nicotine, which is an essential constituent of the tobacco plant, can be carried out by polarography. The quantification limit is less than 0.1 mg/L in the polarographic vessel.
- AB-070Polarographic determination of nitrate in water samples, soil and plant extracts, vegetable juices, meat and sausages, fertilizers, liquid manure, etc.
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.
- AB-074Determination of antimony, bismuth, and copper by anodic stripping voltammetry
This Application Bulletin describes the voltammetric determination of the elements antimony, bismuth, and copper. The limit of detection for the three elements is 0.5 ... 1 µg/L.
- AB-076Polarographic determination of nitrilotriacetic acid (NTA) and ethylenediaminetetraacetic acid (EDTA) according to DIN 38413 part 5
According to the described method, NTA and EDTA can be determined in mass concentrations of 0.05 mg/L up to 25 mg/L in polluted water and wastewater.At first NTA and EDTA are converted to the corresponding Bi complexes by addition of Bi3+ ions at a pH value of 2.0. As these Bi complexes have significantly different peak potentials, they can be determined simultaneously by DP polarography. The interfering anions nitrite, sulfite, and sulfide are removed from the sample by acidification and purging. Interfering cations are removed by cation exchange; any NTA or EDTA heavy metal complexes present in the sample are disintegrated during this procedure. To remove surfactants and other organic components interfering with the analysis, the sample solution is run through a column filled with non-polar adsorber resin.
- AB-083Sodium analysis by ion-selective electrode
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.
- AB-096Determination of mercury at the rotating gold electrode by anodic stripping voltammetry
This Application Bulletin describes the determination of mercury by anodic stripping voltammetry (ASV) at the rotating gold electrode. With a deposition time of 90 s, the calibration curve is linear from 0.4 to 15 μg/L; the limit of quantification is 0.4 μg/L.The method has primarily been drawn up for investigating water samples. After appropriate digestion, the determination of mercury is possible even in samples with a high load of organic substances (wastewater, food and semi-luxuries, biological fluids, pharmaceuticals).
- AB-102Conductometry
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;
- AB-110Determination of free cyanide by polarography
This Application Bulletin describes a polarographic method for the determination of cyanide that allows to determine free cyanide fast and accurately. The determination also succeeds in solutions containing sulfides, where other methods fail. Cyanide concentrations in the range b(CN–) = 0.01...10 mg/L cause no problems. Interference caused by anions and complexed cyanides has been investigated.
- AB-113Determination of cadmium, lead and copper in foodstuffs, waste water and sewage sludge by anodic stripping voltammetry after digestion
Cadmium, lead, and copper can be determined simultaneously in oxalate buffer by anodic stripping voltammetry (ASV) after digestion with sulfuric acid and hydrogen peroxide. Tin present in the sample does not interfere with the determination of lead.For the voltammetric determination of tin please refer to Application Bulletin no. 176.
- AB-114Determination of copper, nickel, cobalt, zinc, and iron in a single operation by polarography
Cu2+, Co2+, Ni2+, Zn2+, and Fe2+/Fe3+ are determined simultaneously. Interference due to the presence of other metals is mentioned, and methods given to eliminate it. The threshold of determination is ρ = 20 µg/L for Co and Ni, and ρ = 50 µg/L each for Cu, Zn, and Fe.
- AB-116Determination of chromium in small quantities by polarography and adsorptive stripping voltammetry after digestion
This Application Bulletin describes methods for the polarographic and voltammetric determination of small quantities of chromium in water, effluent water and biological samples. Methods for the sample preparation for various matrices are given.
- AB-117Determination of selenium by cathodic stripping voltammetry
In the past, selenium determinations have always been either unreliable or have required complicated methods. However, as selenium is on the one hand an essential trace element (vegetable and animal tissues contain about 10 μg/kg), while on the other hand it is very toxic (threshold value 0.1 mg/m3), it is very important to cover determinations in the micro range. Cathodic stripping voltammetry (CSV) enables selenium to be determined in mass concentrations down to ρ(Se(IV)) = 0.3 μg/L.
- AB-119Potentiometric determination of trace bromide and iodide in chlorides
Bromide is removed from the sample as BrCN by distillation. The BrCN is absorbed in sodium hydroxide solution and decomposed with concentrated sulfuric acid, then the released bromide ions are determined by potentiometric titration with silver nitrate solution. Iodide does not interfere with the determination.Iodide is oxidized to iodate by hypobromite. After destruction of the excess hypobromite, the potentiometric titration (of the iodine released from iodate) is carried out with sodium thiosulfate solution. Bromide does not interfere, even in great excess.The described methods allow the determination of bromide and iodide in the presence of a large excess of chloride (e.g., in brine, seawater, sodium chloride, etc.).
- AB-121Determination of nitrate with the ion-selective electrode
It has been known for years that consuming too much nitrates from foodstuffs can result in cyanosis, particularly for small children and susceptible adults. According to the WHO standard, the hazard level lies at a mass concentration c(NO3-) ≥ 50 mg/L. However, more recent studies have shown that when nitrate concentrations in the human body are too high, they can (via nitrite) result in the formation of carcinogenic and even more hazardous nitrosamines.Known photometric methods for the determination of the nitrate anion are time-consuming and prone to a wide range of interferences. With nitrate analysis continually increasing in importance, the demand for a selective, rapid, and relatively accurate method has also increased. Such a method is described in this Application Bulletin. The Appendix contains a cselection of application examples where nitrate concentrations have been determined in water samples, soil extracts, fertilizers, vegetables, and beverages.
- AB-123Determination of manganese in water samples by anodic stripping voltammetry
"A sensitive methods to determine manganese is described. It is primarily suitable for the investigation of ground, drinking and surface waters, in which the concentration of manganese is important. The method can naturally also be used for trace analysis in other matrices.Manganese is determined in an alkaline borate buffer by the anodic stripping voltammetry (ASV). Interference by intermetallic compounds is prevented by the addition of zinc ions in the sample. The limit of determination lies at b(Mn) = 2 µg/L."
- AB-125Simultaneous determination of calcium, magnesium, and alkalinity by complexometric titration with potentiometric or photometric indication in water and beverage samples
This bulletin describes the determination of calcium, magnesium, and alkalinity in water by complexometric titration with EDTA as titrant. It is grouped into two parts, the potentiometric determination and the photometric determination.There are multiple definitions of the different types of water hardness. In this Application Bulletin, the following definitions are used: alkalinity, calcium hardness, magnesium hardness, total hardness, and permanent hardness. Explanations of these definitions and other expressions are provided in the Appendix.Determination of alkalinity during the photometric part is carried out in a separate acid-base titration before the complexometric titration of calcium and magnesium in water. Permanent hardness can be calculated from these values. The determination of calcium and magnesium in beverages (fruit and vegetable juices, wine) is also described.The photometric part includes the determinations of total and calcium hardness and thereby indirectly magnesium hardness using Eriochrome Black T and calconcarboxylic acid as indicators (in accordance with DIN 38406-3).
- AB-129Potentiometric determination of orthophosphates, metaphosphates, and polyphosphates
After acid digestion, the sample solution is neutralized with sodium hydroxide to form sodium dihydrogen phosphate. An excess of lanthanum nitrate is added and the released nitric acid is then titrated with sodium hydroxide solution.NaH2PO4 + La(NO3)3 → LaPO4 + 2 HNO3 + NaNO3This determination method is suitable for higher phosphate concentrations.
- AB-133Determination of ammonia with the ion-selective electrode – Tips and tricks for a reliable determination according to common standards
Although the known photometric methods for the determination of ammonia/ammonium are accurate, they require a considerable amount of time (Nessler method 30 min, indophenol method 90 min reaction time). A further disadvantage of these methods is that only clear solutions can be measured. Opaque solutions must first be clarified by time-consuming procedures. These problems do not exist with the ion-selective ammonia electrode. Measurements can be easily performed in waste water, liquid fertilizer, and urine as well as in soil extracts. Especially for fresh water and waste water samples several standards, such as ISO 6778, EPA 350.2, EPA 305.3 and ASTM D1426, describe the analysis of ammonium by ion measurement. In this Application Bulletin, the determination according to these standards is described besides the determination of other samples as well as some general tips and tricks on how to handle the ammonia ion selective electrode. Determination of ammonia in ammonium salts, of the nitric acid content in nitrates, and of the nitrogen content of organic compounds with the ion-selective ammonia electrode is based on the principle that the ammonium ion is released as ammonia gas upon addition of excess caustic soda:NH4+ + OH- = NH3 + H2OThe outer membrane of the electrode allows the ammonia to diffuse through. The change in the pH value of the inner electrolyte solution is monitored by a combined glass electrode. If the substance to be measured is not present in the form of an ammonium salt, it must first be converted into one. Organic nitrogen compounds, especially amino compounds are digested according to Kjeldahl by heating with concentrated sulfuric acid. The carbon is oxidized to carbon dioxide in the process while the organic nitrogen is transformed quantitatively into ammonium sulfate.
- AB-134Determination of potassium with an ion-selective electrode
Potassium is one of the most common elements and can be found in many different minerals and other potassium compounds. It is of importance for humans, animals and plants as it is an essential mineral nutrient and involved in many cellular functions like cell metabolism and cell growth. For these reasons, it is important to be able to declare the potassium content of food or soil to reduce problems that may arise by a potassium deficiency or extensive consumption.This bulletin describes an alternative to flame photometric method using an ion selective electrode and direct measurement or standard addition technique. Several potassium determinations in different matrices using the combined potassium ion-selective electrode (ISE) are presented here. Additionally, general hints, tips and tricks for best measurement practice are given.
- AB-146Determination of trace amounts of molybdenum (or tungsten) in water by polarography
"Molybdenum is an essential trace element for plant growth. Since it occurs in natural waters only in trace amount, a very sensitive method of determination is needed. Using the following polarographic method, it is possible to determine 5·10-10 mol/L resp. 50 ng/L.The principle of the method is based on the reaction between the molybdate ion MoO42- and the complexing agent 8-hydroxy-7-iodo-quinoline-5-sulfonic acid (H2L) to form a MoO2L22- complex, which is adsorbed on the mercury electrode. The adsorbed Mo(VI) is reduced electrochemically to the Mo(V) complex. The hydrogen ions present in the solution oxidize Mo(V) again spontaneously to form the Mo(VI) complex, which is thus newly available for electrochemical reduction. This catalytic reaction is the reason for the high sensitivity of the method.Tungsten W(VI) exhibits practically the same electrochemical behavior as molybdenum, but is not described in detail in this Application Bulletin."
- AB-176Determination of lead and tin by anodic stripping voltammetry
In most electrolytes the peak potentials of lead and tin are so close together, that a voltammetric determination is impossible. Difficulties occur especially if one of the metals is present in excess.Method 1 describes the determination of Pb and Sn. Anodic stripping voltammetry (ASV) is used under addition of cetyltrimethylammonium bromide. This method is used when:• one is mainly interested in Pb• Pb is in excess• Sn/Pb ratio is not higher than 200:1According to method 1, Sn and Pb can be determined simultaneously if the difference in the concentrations is not too high and Cd is absent.Method 2 is applied when traces of Sn and Pb are found or interfering TI and/or Cd ions are present. This method also uses DPASV in an oxalate buffer with methylene blue addition.
- AB-178Fully automated analysis of water samples
The determination of the physical and chemical parameters as electrical conductivity, pH value, p and m value (alkalinity), chloride content, the calcium and magnesium hardness, the total hardness, as well as fluoride content are necessary for evaluating the water quality. This bulletin describes how to determine the above mentioned parameters in a single analytical run.Further important parameters in water analysis are the permanganate index (PMI) and the chemical oxygen deman (COD). Therefore, this Bulletin additionally describes the fully automated determination of the PMI according to EN ISO 8467 as well as the determination of the COD according to DIN 38409-44.
- AB-186Determination of aluminum in water samples by adsorptive voltammetry
This Bulletin describes the voltammetric determination of aluminum in water samples down to a concentration of 1 μg/L. An aluminum complex is formed with alizarin red S (DASA) and enriched at the HMDE. The following determination employs differential pulse adsorptive stripping voltammetry (DP-AdSV). Disturbing Zn ions are eliminated by addition of CaEDTA.
- AB-188pH measurement technique
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.
- AB-199Determination of sulfide and sulfite by polarography
Sulfide and sulfite can be determined polarographically without any problems. For sulfide, polarography is performed in an alkaline solution, for sulfite in a slightly acidic primary solution. The method is suitable for the analysis of pharmaceuticals (infusion solutions), wastewater/flue gas water, photographic solutions, etc.
- AB-207Determination of silver by anodic stripping voltammetry at the carbon RDE
This Application Bulletin describes the stripping analysis of Ag at the rotating disk electrode (RDE) with glassy carbon tip (GC) or Ultra Trace graphite tip. In routine operation, the determination limit lies at approx. 10 μg/L Ag, with careful work 5 μg/L Ag can be obtained. After appropriate digestion, silver determination is also possible with samples containing a relatively high proportion of organic substances (e.g. wine, foodstuffs etc.). The method has been developed primarily for water samples (well, ground and wastewater, desilvering solutions of the photographic industry).
- AB-220Determination of platinum and rhodium in the ultratrace range by adsorptive stripping voltammetry
This Application Bulletin describes …
- AB-221Standard methods in water analysis
This Bulletin gives a survey of standard methods from the field of water analysis. You will also find the analytical instruments required for the respective determinations and references to the corresponding Metrohm Application Bulletins and Application Notes. The following parameters are dealt with: electrical conductivity, pH value, fluoride, ammonium and Kjeldahl nitrogen, anions and cations by means of ion chromatography, heavy metals by means of voltammetry, chemical oxygen demand (COD), water hardness, free chlorine as well as a few other water constituents.
- AB-226Determination of arsenic by stripping voltammetry at the rotating gold electrode
This Bulletin describes the determination of arsenic by anodic stripping voltammetry (ASV) at the rotating gold electrode. A determination limit of 0.5 μg/L can be achieved with 10 mL sample solution. A differentiation between the As(III) concentration and the total arsenic concentration can be made by appropriate selection of the deposition potential. The analyses are performed with a special gold electrode whose active surface is located laterally; c(HCl) = 5 mol/L is used as supporting electrolyte. For the determination of the total arsenic content, As(III) and As(V) are reduced at -1200 mV by nascent hydrogen to As0, which is preconcentrated on the electrode surface. If the deposition is carried out at -200 mV then only As(III) is reduced; this allows the differentiation between total arsenic and As(III). During the subsequent voltammetric determination the preconcentrated As0 is again oxidized to As(III).
- AB-231Determination of zinc, cadmium, lead, copper, thallium, nickel and cobalt in water samples by anodic and adsorptive stripping voltammetry according to DIN 38406-16
The standard method postulated by DIN 38406 Part 16 describes the determination of Zn, Cd, Pb, Cu, Tl, Ni, and Co in drinking, ground, surface and precipitation (e.g. rain) water. Because the presence of organic substances in the water samples can strongly interfere with the voltammetric determination, a pretreatment with UV digestion using hydrogen peroxide is necessary. This digestion ensures the elimination of all organic substances without introduction of blank values. These methods can, of course, also be applied for trace analysis in other materials, e.g. trace analysis in the production of semiconductor chips based on silicon. Zn, Cd, Pb, Cu, and Tl are determined on the HMDE by means of anodic stripping voltammetry (ASV), Ni and Co by means of adsorptive stripping voltammetry (AdSV).
- AB-241Determination of cadmium and lead by anodic stripping voltammetry at a mercury film electrode
This Application Bulletin describes the determination of cadmium and lead at a mercury film electrode (MFE) by anodic stripping voltammetry (ASV). The mercury film is plated ex situ on a glassy carbon electrode and can be used for up to one day. With a deposition time of 30 s, the limit of detection is ß(Cd2+) = 0.02 µg/L and ß(Pb2+) = 0.05 µg/L. The linear working range for both elements goes up to approx. 50 μg/L using the same deposition time.
- AB-242Determination of tungsten by anodic stripping voltammetry at the Ultra Trace graphite RDE
The method described allows the determination of W(VI) traces in the range 0.2 to 50 µg/L (ppb). Traces of organic compounds present in the samples (e.g. natural waters) interfere. They have to be removed by UV digestion (e.g. 705 UV Digester). Interference by Fe(III) up to a concentration of 100 mg/L is eliminated by reduction to Fe(lI) with ascorbic acid. If the amount of Cu(II) in the sample exceeds the amount of W(VI) by a factor of 200 or more, the Cu ions have to be bound with thiourea. Moreover, the concentration of Cu(II) should not exceed 5 mg/L. The determination is made by adsorptive stripping analysis in the DP mode.
- AB-243Determination of chromium by adsorptive stripping voltammetry at the Ultra Trace graphite RDE
The method describes the determination of Cr traces in a range between 1 ... 250 μg/L. The method is based on the adsorption of a Cr(lll)-diphenylcarbazonate complex on the Ultra Trace graphite rotating disk electrode (RDE). Organic compounds present in samples (e.g. natural waters) have a strong interfering effect. So they have to be removed by e.g. UV digestion. The determination is made by adsorptive stripping voltammetry in the DC (direct current) measuring mode. Purging with nitrogen is not necessary. The determinations work well also in high salt concentration solutions.
- AB-249Determination of free and residual chlorine based on DIN EN ISO 7393-1 and APHA 4500-Cl
Chlorine is frequently added to drinking water for disinfection. Depending on the reactivity and the concentration of chlorine, toxic disinfection by-products (DBPs) can thereby be released. Therefore, it is necessary to strictly control the chlorine concentration in the drinking water. This Application Bulletin shows how to determine the chlorine concentration according to three standard methods: DIN EN ISO 7939-1, APHA 4500-Cl Method B, and APHA 4500-Cl Method I.
- AB-254Determination of zinc, cadmium and lead by anodic stripping voltammetry at a mercury film electrode
This Application Bulletin describes the determination of zinc at a mercury film electrode (MFE). Zinc can also be determined simultaneously with cadmium and lead. The determination of copper at the MFE is not possible. The mercury film is plated ex-situ on a glassy carbon electrode and can be used for half a day up to one day.Zinc can be determined at the mercury film electrode by anodic stripping voltammetry (ASV). The presence of copper, which is naturally present in many samples, affects the determination of zinc due to the formation of an intermetallic compound. As a result the determined concentrations of zinc are too low. The addition of gallium can eliminate the interference to a certain extent since the intermetallic complex of gallium and copper is more stable than the complex of zinc and copper.With a deposition time of 10 s, the limit of detection is β(Zn2+) = 0.15 μg/L. The linear working range goes up to approx. 300 μg/L.With the deposition time of 10 s the method is suitable for samples between 10 μg/L and 150 μg/L Zn content. For samples with lower concentrations the results are more reliable if the deposition time is increased to e.g. 30 s. Samples with higher concentrations have to be diluted.
- AB-266Determination of titanium by adsorptive stripping voltammetry
This Application Bulletin describes the determination of titanium by adsorptive stripping voltammetry (AdSV) using mandelic acid as complexing agent. The method is suitable for the analysis of ground, drinking, sea, surface and cooling waters, in which the concentration of titanium is of importance. The methods can, of course, also be used for the trace analysis in other matrices.The limit of detection is approx. 0.5 µg/L.
- AB-317Determination of iron in the µg/L-range by polarography
This Application Bulletin describes two methods for the determination of iron at the Multi Mode Electrode.Method 1, the polarographic determination at the DME, is recommended for concentrations of β(Fe) > 200 μg/L. For this method the linear range is up to β(Fe) = 800 μg/L.For concentrations < 200 μg/LMethod 2, the voltammetric determination at the HMDE, is to be preferred. The detection limit for this method is β(Fe) = 2 μg/L, the limit of quantification is β(Fe) = 6 μg/L. The sensitivity of the method cannot be increased by deposition.Iron(II) and iron(III) have the same sensitivity for both methods.These methods have been elaborated for the determination of iron in water samples. For water samples with high calcium and magnesium concentrations such as, for example, seawater, a slightly modified electrolyte is used in order to prevent precipitation of the corresponding metal hydroxides. The methods can also be used for samples with organic loading (wastewater, beverages, biological fluids, pharmaceutical or crude oil products) after appropriate digestion.
- AB-416Determination of arsenic in water with the scTRACE Gold
This Application Bulletin describes the determination of arsenic in water samples by anodic stripping voltammetry using the scTRACE Gold sensor. This method makes it possible to distinguish between As(total) and As(III). With a deposition time of 60 s, the limit of detection for As(total) is 0.9 µg/L, for As(III) it is 0.3 µg/L.
- AB-422Determination of mercury in water using scTRACE Gold
This Application Bulletin describes the determination of inorganic mercury in water samples by anodic stripping voltammetry using the scTRACE Gold sensor. With a deposition time of 90 s, calibration is linear up to a concentration of 30 µg/L; the limit of detection lies at 0.5 µg/L.
- AB-429Determination of copper in water with the scTRACE Gold
Copper is one of the few metals which is available in nature also in its metallic form. This and the fact that it is rather easy to smelt led to intense use of this metal already in the so-called Copper and Bronze Age. Nowadays, it is more important than ever, because of its good electrical conductivity and its other physical properties. For plants and animals, it is an essential trace element; for bacteria, in contrast, it is highly toxic.This Application Bulletin describes the determination of copper by anodic stripping voltammetry (ASV) using the scTRACE Gold electrode. With a deposition time of 30 s, the limit of detection is about 0.5 μg/L.
- AB-430Determination of uranium by adsorptive stripping voltammetry according to DIN 38406-17
This Application Bulletin describes the methods for the determination of uranium by adsorptive stripping voltammetry (AdSV) according to DIN 38406 part 17. The method is suitable for the analysis of ground, drinking, sea, surface and cooling waters, in which the concentration of uranium is of importance. The methods can, of course, also be used for the trace analysis in other matrices.Uranium is determined as chloranilic acid complex. The limit of detection in samples with low chloride concentration is about 50 ng/L and in seawater about 1 µg/L. Matrices with high chloride content can only be analyzed after reduction of the chloride concentration by means of a sulfate-loaded ion exchanger.
- AB-431Determination of iron, copper and vanadium by adsorptive stripping voltammetry
This Application Bulletin describes the voltammetric determination of the elements iron, copper and vanadium. Fe as well as Cu and V can be determined as catechol complex at the HMDE by adsorptive stripping voltammetry (AdSV). Fe(II) and Fe(III) are determined as Fe(total) with the same sensitivity for both species in either phosphate buffer or PIPES electrolyte. Cu and V can be determined in PIPES buffer.The methods are primarily suitable for the investigation of ground, drinking and surface waters, in which the concentration of these metals is important. But the methods can naturally also be used for trace analysis in other matrices.The limit of detection for all three elements in PIPES buffer is 0.5 ... 1 µg/L, for iron in phosphate buffer it is approx. 5 µg/L.
- AB-433Determination of lead in water with the scTRACE Gold modified with a silver film
Lead is known to be highly toxic and lead salts are easily absorbed by creatures. By interfering with enzyme reactions,lead can affect all parts of the human body. It can cause severe damage to brain and kidneys and can cross the bloodbrain barrier. Cases of chronic lead poisoning caused by lead metal used in the water piping system are well known. Therefore, the control of drinking water for lead content is of utmost importance. In many countries (e.g., EU, USA), the limit for lead in drinking water is between 10 and 15 μg/L. These concentrations can reliably be determined with the method described in this Application Bulletin. The determination is carried out by anodic stripping voltammetry at a silver film applied to the scTRACE Gold electrode.
- AB-438Determination of cadmium and lead in water samples by anodic stripping voltammetry with a Bi drop electrode
Heavy metals, particularly cadmium and lead, are known to be highly toxic to humans. Therefore, controlling the cadmium and lead content in drinking water is of utmost importance. In many countries, the limit in drinking water for cadmium is between 3–5 µg/L, and for lead it is between 5–15 µg/L. These trace concentrations can reliably be determined with the method described in this Application Bulletin. The determination is carried out by anodic stripping voltammetry (ASV) using the non-toxic Bi drop electrode in a slightly acidic electrolyte.
- AB-439Voltammetric determination of iron in water samples with a Bi drop electrode
Iron is an essential element in the human diet and is found in many natural and treated waters. Therefore, the World Health Organization (WHO) does not issue a health-based guideline value for iron. Higher concentrations of iron in surface waters can indicate the presence of industrial effluents or outflow from other operations and sources of pollution. Because of this, precise, rapid, and accurate iron determination at low concentrations in environmental and industrial samples is of great importance. This can be achieved with the method described in this Application Bulletin.
- AB-440Determination of nickel and cobalt in water samples by adsorptive stripping voltammetry with a Bi drop electrode
Cobalt is an essential element for humans because it is a component of vitamin B12. While small overdoses of cobalt compounds are only slightly toxic to humans, larger doses from 25–30 mg per day may lead to skin, lung, and stomach diseases, as well as liver, heart, and kidney damage, and even cancerous growths. The same is valid for nickel, which can lead to inflammation at higher concentrations. Drinking a large amount of water containing nickel can cause discomfort and nausea. In the EU the legislation specifies 0.02 mg/L as the limit value for the nickel concentration in drinking water. This concentration can be reliably determined with the method described in this Application Bulletin.
- AN-C-060Magnesium, strontium, and barium in produced water (11 g/L sodium)
Determination of magnesium, strontium, and barium in produced water using cation chromatography with direct conductivity detection.
- AN-C-066Four cations in the water soluble fraction of a washing powder
Determination of sodium, potassium, calcium, and magnesium in the water soluble fraction of a washing powder using cation chromatography with direct conductivity detection.
- AN-C-071Choline in a saline solution
Determination of sodium, potassium, DMEA (dimethylethanolamine), calcium, choline, and magnesium in a saline solution using cation chromatography with direct conductivity detection.
- AN-C-103Standard cations in lake water on the Metrosep C 3 - 250/4.0 column
Determination of lithium, sodium, potassium, magnesium, and calcium in lake water using cation chromatography with direct conductivity detection.
- AN-C-130Cations in offshore effluent
Determination of lithium, sodium, ammonium, potassium, manganese, calcium, magnesium, strontium, and barium in an offshore effluent using cation chromatography with direct conductivity detection.
- AN-C-143Ammonia in addition to standard cations in maritime pore water
Maritime pore water contains sodium in the percentage range. The analysis of ammonia in this kind of sample requires a high column capacity and an exceptionally good separation of sodium and ammonia. These requirements are completely fulfilled by a 2 µL injection to the high-capacity Metrosep C 6 - 250/4.0 column.
- AN-C-172Cations in snow from an open field
Cation content in snow is greatly dependent on sampling site. Samples from remote areas are expected to exhibit lower cation concentrations. This application shows the analysis of a snow sample from an open field in an agricultural zone. Separation is performed on a microbore Metrosep C 6 - 100/2.0 column with direct conductivity detection. The relatively high ammonia content can be explained by animal husbandry in the vicinity of the sampling site.
- AN-C-173Cations in roadside snow
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.
- AN-C-195Cation quantification with increased performance using microbore IC
Microbore ion chromatography offers better sensitivity, shorter retention times, and consumes less eluent, increasing sample throughput and reducing running costs.
- AN-CIC-033Monitoring PFASs in water sources
AOF (adsorbable organic fluorine) is used to screen for per- and polyfluorinated alkyl substances in aqueous matrices via pyrohydrolytic combustion and ion chromatography.
- AN-CIC-034Fast analysis of AOX in waters by CIC
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.
- AN-EC-015Metrohm 663 VA stand for Heavy Metal Ions detection in Water Sample
The determination of heavy metal ions in a solution is one of the most successful application of electrochemistry. In this application note, anodic stripping voltammetry is used to measure the presence of two analytes, in a sample of tap water.
- AN-EC-038Measuring ionic conductivity using screen-printing technology
Using disposable 11COND screen printed electrodes and electrochemical impedance spectroscopy, conductivity in drinking water can be measured using only 100 µL samples.
- AN-H-034Determination of calcium and magnesium in process samples
Determination of calcium and magnesium in process solutions.
- AN-H-065Determination of salts of carboxylic acids by aqueous acidometric titration
Determination of sodium and potassium salts of carboxylic acids in aqueous media. May be used for analysis of reagent purity.
- AN-H-074Determination of calcium and magnesium in seawater
Determination of calcium and magnesium in seawater. The method is suitable for determining the effect of caustic soda and alumina refinery aluminate solutions on the calcium and magnesium content of seawater.
- AN-H-077Determination of sodium in brines by aluminum titration
Determination of sodium in seawater and similar brines. This procedure is suitable for the analysis of sodium in seawater contaminated with sodium aluminate solutions emanating from alumina refineries, and seawater which has been used for the neutralization of alumina refinery waste («red mud») slurries.
- AN-H-078Determination of total halides in brines
Determination of total halides (Cl- + Br- +I-) in seawater and similar brines. This procedure is suitable for the analysis of total halides in seawater contaminated with sodium aluminate solutions emanating from alumina refineries, and seawater which has been used for the neutralization of alumina refinery waste («red mud») slurries. Given the small concentration of bromine andiodine in seawater, the total halide content approximates the chloride concentration.
- AN-H-130Determination of nitrite using sulfamic acid
This Application Note describes the determination of nitrite using thermometric endpoint titration with sulfamic acid. The nitrite content of a solution can be analyzed down to 0.2 mmol/L.
- AN-I-002Low levels of ammonia in distilled water
Determination of ammonia (ammonium) in distilled water by direct potentiometry using the NH3-ISE.
- AN-I-006Chloride content of water samples
Determination of chloride in water by direct potentiometry using the Cl-ISE.
- AN-I-009Cyanide in water
Cyanides are used in some industrial processes, but if not handled carefully, they could contaminate the wastewater. In an acidic or neutral environment, this contaminated wastewater can form highly toxic hydrogen cyanide gas. Furthermore, the cyanide salts could also poison the environment and enter the ground water system. Therefore, it is essential to monitor the content of cyanide in effluent water. Cyanides can be easily determined with a cyanide ion-selective electrode. This application note presents a method for cyanide analysis according to APHA Method 4500-CN and ASTM D2036.
- AN-I-013Sulfide in ground and waste water
Even in low concentration, sulfide ions cause odor and corrosion problems in ground water and waste water. They can release hydrogen sulfide in acidified water, which is toxic in even minuscule amounts. This Application Note describes the determination of sulfide concentration in water via direct measurement with the Ag/S-ISE in accordance with ASTM D4658.
- AN-I-014Bromide in water
Bromide is ubiquitous in sea water, where it is present in concentrations of around 65 mg/L. By contrast, the maximum bromide concentration in drinking and ground water is usually less than 0.5 mg/L. A higher bromide content may indicate a contamination of the water caused by fertilizer, road salt or industrial waste water. This Application Note describes the determination of the bromide content in water via direct measurement with a Br ion-selective electrode in accordance with ASTM D1246.
- AN-I-022Potassium in surface water – Fast and inexpensive determination by direct measurement
Potassium is naturally occurring in surface water caused by weathering of stones and soil. As potassium in drinking water is regulated and should not exceed a certain threshold value, it is necessary to assess the potassium concentration.This can easily be done by direct measurement using a potassium selective electrode. First, a calibration is performed, afterwards, the samples are measured within tens of seconds. This is a fast, inexpensive and reliable method to determine the potassium content in various water samples.
- AN-I-024Nitrate in surface water – Fast and inexpensive determination by direct measurement
Nitrate is naturally present in the environment. However, excessive concentrations of nitrate in surface and ground water are problematic as such concentrations have a negative effect on the water quality. Usually, excessive levels of nitrate area direct result of extensive usage of fertilizers in agriculture. Nitrate is easily washed from soils and can end up in surface or ground water. As the nitrate content is regulated in many countries, a quick and inexpensive assessment of its concentration is required to monitor the water quality.The nitrate concentration can easily be obtained by direct measurement using a nitrate ion selective electrode. First, a calibration is performed, afterwards, the samples are measured in less than a minute.This is a fast, inexpensive and reliable method to determine the nitrate content in various water samples.
- AN-I-026Fluoride in leachate – Fast determination of fluoride using direct measurement
Increased fluoride concentrations in water may cause tooth damage, growth disorders, and bone deformation. According to the World Health Organization (WHO), concentrations above 1.5 mg/L are critical.One possible source of fluoride is landfills. Rain washes out harmful substances from landfills which can enter the groundwater. The leachate from landfills should thus be monitored for the fluoride concentration.Ion measurement is a fast and inexpensive method to determine the fluoride content in water samples compared to other methods such as ion chromatography. This Application Note describes a reproducible and accurate measurement of the fluoride content using the fluoride ion-selective electrode with an OMNIS system.
- AN-I-028Dissolved oxygen in surface water
Oxygen diffuses into water sources from the air via aeration, however several factors can reduce the dissolved oxygen (DO) content in water. First, as water warms up, oxygen is released into the atmosphere. Secondly, oxygen is consumed by bacteria and other microorganisms which feed on organic material. Finally, plants can also consume oxygen in certain situations.Human-induced alterations can have a negative influence on surface water when DO values fall below crucial limits for maintaining the life supporting capacity of freshwater ecosystems. Therefore, monitoring the DO content in surface water by an optical sensor to assess its quality is important.
- AN-M-003Phosphate in produced water using IC/MS coupling after sample preparation by inline dialysis
Determination of phosphate in produced water containing up to 100 g/L chloride as well as crude oil using anion chromatography with conductivity and MS detection after inline dialysis.
- AN-M-008Determination of chromate in water using IC-ICP/MS detection
Hexavalent chromium, also referred to as chromate or Cr(VI), is considered toxic and potentially carcinogenic, which is why its concentrations in drinking water should be kept as low as possible. Determination of Cr(VI) is performed by combining ion chromatography with ICP/MS. Separation takes place on the Metrosep A Supp 1 Guard/4.6.
- AN-M-013Chromium speciation by IC-ICP-MS
Differentiation between Cr(III) and Cr(VI) is possible following ISO 24384 guidelines by combining ion chromatography with inductively coupled plasma mass spectrometry.
- AN-M-016Resolving haloacetic acids in water
During drinking water disinfection with chlorine, chloramine, or ozone, potentially toxic halogenated byproducts can be formed. The disinfectants can react with naturally occurring bromide and/or organic matter in the source water and form one of the most common and highly toxic disinfection byproducts (DBPs): haloacetic acids (HAAs). To protect human health, maximum tolerable levels of HAA in drinking waters are regulated (EPA 816-F-09-004). The EPA Method 557 specifies the analysis of HAAs beside bromate and dalapon by ion chromatography coupled to tandem mass spectroscopy (IC-MS/MS) with LODs varying from 0.02–0.11 µg/L. However, even with single MS, a high sensitivity is achieved to determine the current MCLs within an adequate accuracy. This Application Note describes the analysis of bromate, chlorite, monochloroacetic acid (MCAA), monobromoacetic acid (MBAA), bromochloroacetic acid (BCAA), bromodichloroacetic acid (BDCAA), dibromoacetic acid (DBAA), dichloroacetic acid (DCAA), tribromoacetic acid (TBAA), chlorodibromoacetic acid (CDBAA), and trichloroacetic acid (TCAA) with IC/MS. The Metrohm Driver 2.1 for EmpowerTM offers the analysis as a single software solution with EmpowerTM.
- AN-M-017IC-MS/MS analysis of trifluoroacetic acid according to DIN 38407-53
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.
- AN-N-025Traces of nitrite, thiosulfate, and iodide using amperometric detection
Determination of traces of nitrite, thiosulfate, and iodide using anion chromatography with amperometric detection at the carbon paste electrode.
- AN-N-037Perchlorate in process water
Determination of perchlorate in process water using anion chromatography with direct conductivity detection.
- AN-N-058LOD and LOQ for silicate and borate determination according to EPA (MDL procedure)
Determination of silicate and borate and their limits of determination (LOD) and quantification (LOQ) according to the EPA procedure for method detection limit (MDL) using anion chromatography with direct conductivity detection and Metrohm Inline Calibration.
- AN-N-064Sodium dodecylsulfate (SDS) in water
Determination of sodium dodecylsulfate (SDS, sodium laurylsulfate) using anion chromatography with direct conductivity detection.
- AN-O-040Borate in seawater
Determination of borate in seawater using ion-exclusion chromatography with suppressed conductivity detection after inline matrix elimination.
- AN-P-051Cyanide and sulfide on Metrosep A Supp 10 - 100/2.0 using amperometric detection
The determination of cyanide and sulfide in the trace range requires an alkali eluent and amperometric detection. This Application Note describes a new column/eluent combination for optimized separation. The combination consists of the Metrosep A Supp 10 - 100/2.0 Microbore Column and a sodium hydroxide eluent that contains traces of EDTA for the complexation of the transition metals. This yields a better peak shape and detection limits below 0.05 µg/L.
- AN-RA-010SERS detection of pesticides using screen-printed electrodes
EC-SERS enhances Raman sensitivity using electrochemically activated gold SPEs, enabling rapid, simplified pesticide detection without complex prep or instrumentation.
- AN-RS-018Trace Detection of Malachite Green in Stream Water
Malachite green (MG) is a textile dye with effective fungicidal properties, however it is acutely toxic and its metabolites persist in the flesh of fish and mammals, making it a threat to the human food chain. The EU has concluded that contaminated foods containing levels higher than 2 μg/g MG constitute a credible health risk, and several countries have banned malachite green as an aquaculture additive. Despite tight regulation, seafood products contaminated with MG continue to find their way to consumers.Using Misa (Metrohm Instant SERS Analyzer) to ensure food safety, the rapid and highly sensitive detection of malachite green is achieved in a facile assay format.
- AN-S-008Six standard anions in surface water
Determination of fluoride, chloride, nitrite, bromide, nitrate, and sulfate in surface water using anion chromatography with conductivity detection after chemical suppression.
- AN-S-017Chloride, bromide, and sulfate in seawater
Determination of chloride, bromide, and sulfate in synthetic seawater using anion chromatography with conductivity detection after chemical suppression.
- AN-S-028ppb levels of anions
Determination of 1 (3) µg/L of chloride, nitrite, bromide, nitrate, phosphate, and sulfate after direct injection using anion chromatography with conductivity detection after chemical suppression.
- AN-S-033Five anions in surface water (nitrite with ELCD)
Determination of fluoride, chloride, nitrate, phosphate, and sulfate in surface water using anion chromatography with conductivity detection after chemical suppression; nitrite with electrochemical detection (conductivity and ELCD detectors in series).
- AN-S-039Bromide and phosphate in waste dump drainage water using dialysis for sample preparation
Determination of bromide and phosphate in waste dump drainage water in the presence of very high concentrations of other ions and organic substances using anion chromatography with conductivity detection after chemical suppression and dialysis for sample preparation.
- AN-S-052Anions in rainwater
Determination of fluoride, chloride, nitrite, nitrate, and sulfate in rainwater using anion chromatography with conductivity detection after chemical suppression.
- AN-S-058Iodide in the presence of the standard anions in a leach solution
Determination of fluoride, chloride, bromide, nitrate, sulfate, and iodide in rock leachant using anion chromatography with conductivity detection after chemical suppression.
- AN-S-071Traces of chlorite and nitrite using amperometric detection
Determination of chlorite and nitrite using anion chromatography with amperometric detection at the carbon paste electrode after chemical suppression.
- AN-S-072Acetate, propionate, and formate in the presence of chloride in water
Determination of acetate, propionate, formate, and chloride in water using anion chromatography with conductivity detection after chemical suppression.
- AN-S-073Determination of three anions in seawater
Determination of chloride, bromide, and sulfate in seawater using anion chromatography with conductivity detection after chemical suppression.
- AN-S-135Eight anions in river water
Determination of fluoride, chloride, nitrite, bromide, nitrate, phosphate, sulfite, and sulfate in river water using anion chromatography with conductivity detection after chemical suppression.
- AN-S-1522-Fluorobenzoate in water deposits
Determination of 2-fluorobenzoate in a water deposit from the oil production industry using anion chromatography with conductivity detection and chemical suppression.
- AN-S-196Anions in water from an agricultural irrigation systems
Determination of fluoride, chloride, nitrite, bromide, nitrate, phosphate, and sulfate in water from an agricultural irrigation system using anion chromatography with conductivity detection after chemical suppression.
- AN-S-217Ultratrace-level perchlorate in reagent water, ground water, surface water, and water containing 3000 ppm of total dissolved solids (USEPA method 314.0)
Determination of perchlorate in water containing 3 g/L of total dissolved solids (TDS) using anion chromatography with conductivity detection after chemical suppression.
- AN-S-222Anions in borate effluent
Determination of fluoride, chloride, nitrate, phosphate, and sulfate in a borate effluent using anion chromatography with conductivity detection after chemical suppression.
- AN-S-237Phosphor species in process water
Determination of hypophosphite, phosphite, and phosphate in the presence of fluoride, chloride, and sulfate in process water using anion chromatography with suppressed conductivity detection.
- AN-S-261Chloride, nitrate, and sulfate in produced water
Determination of chloride, nitrate, and sulfate in produced water using anion chromatography with conductivity detection after chemical suppression.
- AN-S-272Column-switching method for anions in water samples with two different analytical requirements
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.
- AN-S-280Ten anions in an offshore effluent
Determination of acetate, chloride, nitrite, bromide, nitrate, phosphate, sulfate, oxalate, fumarate, and molybdate using anion chromatography with conductivity detection after chemical suppression.
- AN-S-298Arsenate in high-chloride and high-sulfate matrix by sample reinjection technique
The anion column Metrosep A Supp 15 - 150/4.0 is a pretty high-capacity column. The direct determination of arsenate in a matrix of 180 mg/L chloride and 320 mg/L sulfate is not possible, as the arsenate is hardly detectable under the sulfate peak tail. Sample reinjection cuts off the majority of the matrix and therefore allows an accurate determination of the arsenate.
- AN-S-301Comprehensive water analysis with VoltIC pro I
VoltIC pro I is the perfect combination of voltammetry and ion chromatography for the fully automated analysis of anions, cations, and heavy metals (e.g., Zn, Cd, Pb, Cu): comprehensive water analysis on a single system.
- AN-S-326Oxyhalides in addition to standard anions in swimming pool water
Swimming pool water needs to be thoroughly disinfected and this is often accomplished with ozonization. This process can generate harmful oxyhalides, the concentration of which must be monitored. Here the separation and determination of oxyhalides as well as standard anions are carried out using a column of the Metrosep A Supp 5 - 250/4.0 type. Quantification takes place using conductivity detection in accordance with sequential suppression.
- AN-S-347Comprehensive water analysis with VoltIC Professional 1
VoltIC Professional 1 is the perfect combination of voltammetry and ion chromatography for the fully automated, simultaneous analysis of anions, cations, and heavy metals (e.g., Zn, Cd, Pb, Cu). The multiple-parameter analysis uses the same "Liquid Handling" elements and a shared sample changer, thus saving on space and costs.
- AN-S-349High-low calibration technique: large calibration range with intelligent Partial Loop Injection Technique
In ion chromatography with suppressed conductivity detection, calibration curves quite often are not really linear. Especially, if a calibration has to cover a large concentration range, results will be more accurate when multiple calibration curves for different concentration ranges are applied. The MagIC Net software allows to apply multiple calibration curves within one single determination. This means that for every ion the optimal calibration is applied, improving the accuracy of the results. This method is applied to rainwater samples.
- AN-S-358Total Nitrogen, Total Kjeldahl Nitrogen, and Total Phosphorus as per ASTM D8001
Kjeldahl nitrogen is a typical titration application that follows digestion and ammonia distillation. The ASTM Standard D8001 now offers an alternative applying persulfate digestion followed by IC determination. No distillation is required. In addition, the method enables the determination of total nitrogen and total phosphorus. We show the results of control samples containing organic substances. As these substances are dissolved in ultrapure water, the nitrogen concentration found corresponds to Total Nitrogen and Kjeldahl Nitrogen.
- AN-S-364Dissolved anions in water according to EN ISO 10304-1 applying Inline Ultrafiltration
EN ISO 10304-1 is one of the most important standards for the determination of the seven standard anions in water samples. Many other standards refer to EN ISO 10304-01 if anion determination by IC is required. This standard asks for a membrane filtration for samples to avoid bacteria and solids, if required. This application shows the determination of anions according EN ISO 10304-1 applying Inline Ultrafiltration. This setup avoids tedious manual sample filtration and handles any samples fully automatically.
- AN-SENS-002Detection of heavy metals with differential pulse voltammetry
This Application Note presents DPV as a sensitive, selective method for detecting heavy metals in water, detailing setup, parameters, and advantages over other techniques.
- AN-T-032Sulfide and hydrogen sulfide in water
This Application Note presents a potentiometric titration method for trace H2S analysis in water on an OMNIS system using silver nitrate and an Ag Titrode.
- AN-T-057Calcium in aqueous solutions by photometric titration
Determination of calcium in aqueous solutions by photometric titration with EDTA using the 610 nm Spectrode.
- AN-T-062Analysis of nitrite solutions
Determination of nitrite in aqueous solutions by potentiometric back-titration of the added permanganate excess with ammonium iron(II) sulfate using the Pt-Titrode.
- AN-T-084Total, calcium, and magnesium hardness in water samples
ASTM D8192 describes the photometric titration of the total hardness, calcium hardness, and magnesium hardness in water with an optical sensor for objective endpoint indication, increasing precision and reliability. The method is suitable for both colored and colorless samples such as groundwater, surface water, wastewater, and drinking water. Using a fully automated OMNIS system equipped with an Optrode ensures that the sample preparation and analysis are repeatable.
- AN-T-085Photometric determination of sulfate
This Application Note describes the photometric determination of sulfate using the Optrode (610 nm). Sulfate is titrated with a lead nitrate solution; dithizone is used as indicator.
- AN-T-094Fully automated determination of the permanganate index according to EN ISO 8467
The automated system MATi 13 determines the permanganate index in all kind of water samples according to EN ISO 8467. The high degree of automation (e.g., automated sample addition, automated titer and blank value determination) minimizes errors and guarantees robust and reproducible results.
- AN-T-116Automatic sulfate determination in aqueous solution using a combined ion-selective calcium electrode (Ca ISE)
This Application Note describes automatic sulfate determination using a combined ion-selective calcium electrode. Sulfate is precipitated with an excess of barium chloride solution. Excess barium is subsequently back-titrated with a standard EGTA solution.
- AN-T-131Calcium, magnesium, and total hardness in water
Water hardness is often determined photometrically using two different indicators and while performing the determination at two different pH values. Additionally, the determination itself is subjective, as the color change is determined by the analyst and not by an analytical device.This application note introduces a more robust option to easily assess calcium, magnesium, and total hardness in water by using the Cu-ISE and two different titrants. Sample preparation is identical for both analyses and can therefore be automated without any issues.
- AN-T-172Determination of alkalinity in brackish water, seawater and brine in accordance with ASTM D3875
Alkalinity is well-suited as a means of describing the capacity of a body of water to neutralize acid contaminations. It is therefore an important indicator for estimating the influence of contaminations on the ecological system.
- AN-T-204Permanganate index in water
The permanganate index (PMI) is a sum parameter that indicates the total load of oxidizable organic and inorganic matter in water. The substances concerned are mainly humic materials/acids that are primarily formed when dead organic material present in soil is further broken down and released into water sources. As it is an indicator of the water quality, testing of the PMI for drinking water is obligatory in many countries.For the determination, it is necessary to heat the stabilized water sample to 95 °C and higher for a stipulated time. Afterwards, the amount of permanganate that has remained after the reaction with the sample is determined titrimetrically. This sample preparation step requires considerable manual effort.In this Application Note, a fully automated procedure for the determination of the PMI according to GB/T 11892 is described, including all sample preparation steps. The gains in productivity because of a reduced manual workload are considerable.
- AN-T-213Ozone in water
Water treatment with ozone (O3) is a common procedure for the disinfection of swimming pools. It is important that a sufficient but not excessive amount of O3 is produced to disinfect the water. Otherwise, the remaining ozone could enter the swimming water, which could irritate the respiratory system or the skin of bathers.Ozone is also used in drinking and waste water treatment because it is significantly more effective than chlorine at inactivating or killing viruses and bacteria. This application note describes a method to determine the ozone concentration in water by potentiometric titration according to DIN 38408-3.
- AN-T-233Determination of pyrophosphates by titration
Titration is an accurate and precise method that can be used to determine the pyrophosphate content in aqueous products. The OMNIS Titrator equipped with a dUnitrode delivers reliable determinations.
- AN-T-238Determination of the alkalinity (p-value and m-value) in water
Alkalinity defines the acid-binding capacity of natural water. A distinction is made between total alkalinity (m-value) and carbonate alkalinity (p-value). This Application Note presents the determination of pH and alkalinity in water with a titration method conforming to EPA 310.1, Standard Methods 2320 B (Titration Method), ASTM D1067, EN ISO 9963-1, and EN ISO 9963-2.
- AN-U-002Bromide and nitrate in 1% sodium chloride
Determination of bromide and nitrate in 1% sodium chloride solution using anion chromatography with UV/VIS detection (205 nm) after chemical suppression.
- AN-U-010Nitrite, nitrate, and phosphate in seawater from a shrimp farm
Determination of nitrite, nitrate, and phosphate in seawater from a shrimp farm using anion chromatography with conductivity detection after chemical suppression and subsequent UV/VIS detection.
- AN-U-018Bromate determination using post-column reaction (o-dianisidine method)
Determination of bromate in water using anion chromatography with UV/VIS detection after post-column reaction (PCR) with o-dianisidine reagent (described in EPA 317.0).
- AN-U-023Nitrite, bromide, nitrate, and iodide in 10 g/L sodium chloride with UV detection
Determination of nitrite, bromide, nitrate, and iodide in 10 g/L sodium chloride using anion chromatography with UV detection.
- AN-U-053Chromate with 887 Professional UV/VIS Detector and 886 Professional Thermostat / Reactor
Chromate (Cr(VI)) or hexavalent chromium is carcinogenic. Its use is restricted. Chromate has to be analyzed in a large range of products starting with drinking water, wastewater (e.g., from leather production), over toys to RoHS-regulated substances. Besides ion chromatographic determination applying conductivity detection, the method described here is suitable especially for lower concentrations.
- AN-U-056Nitrite, bromide, and nitrate in artificial sea water applying direct UV/VIS detection
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.
- AN-U-069Chromate using post-column reaction and UV/VIS detection in accordance with EPA 218.7
Hexavalent chromium (Cr(VI)) is regarded as being toxic and potentially carcinogenic. Its concentration in drinking water should therefore be kept as low as possible. The determination of Cr(VI) is performed using ion chromatography. The separation takes place on the Metrosep A Supp 10 - 250/2.0 separation column. The presence of Cr(VI) is determined photometrically following post-column reaction (PCR) with diphenylcarbazide.
- AN-U-071Nitrite, bromide and nitrate in artificial seawater with the aid of UV/VIS detection
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.
- AN-V-068Cadmium and lead in seawater
Cd and Pb can be determined in seawater samples in the ng/L concentration range by anodic stripping voltammetry on a mercury film electrode (MFE).
- AN-V-069Nickel and cobalt in seawater
Nickel and cobalt can be determined in seawater by adsorptive stripping voltammetry (AdSV) at the HMDE.
- AN-V-082Different chromium species in sea water
Cr(III) forms an electrochemically active complex with diethylenetriaminepentaacetic acid (DTPA), so does Cr(VI) after in situ reduction on the surface of the HMDE. Depending on the sample preparation procedure and the waiting time after the addition of the complexing agent, the different chromium species can be differentiated:Total active chromium [total concentration of Cr(VI) and free Cr(III)]:The measurement is carried out immediately after the addition of DTPA.; Cr(VI): Between the addition of DTPA and the start of the analysis a minimum waiting time of 30 min is necessary. During this waiting time the Cr(III)-DTPA complex becomes electrochemically inactive.; Cr(III): The difference between the total active Cr and Cr(VI).; Totalchromium: Determination of total active Cr after UV digestion.;
- AN-V-122Iron (total) in deionized water (triethanolamine-bromate-method)
The concentration of Fe(total) is determined in deionized water. The method is suitable for iron concentrations down to the mid µg/L range. Electrochemical deposition is not applicable for this method. A subtraction of the reagent blank is recommended. Fe(II) and Fe(III) give signals with the same sensitivity.
- AN-V-130Aluminum in the ppb range in aqueous eluates of filter layers (Solochrome violet RS method)
The concentration of Al is determined by adsorptive stripping voltammetry at the HMDE. The method is suitable for Al in concentrations in the range of 0.1 ppb to approx. 40 ppb Al3+. Pb2+ ions do not interfere up to a concentration ratio Pb:Al = 10:1. Due to the slow complex formation of Al with solochrome violet RS the measuring solution was heated to 40 °C for 10 min prior to the determination. For standard addition a solution of Al with solochrome violet RS complex was used. All reagents have to be added in the order as listed below.
- AN-V-178Copper in seawater with the Mercury Film Electrode (MFE)
The concentration of Cu in seawater is determined by anodic stripping voltammetry (ASV) in acetate buffer on a mercury film electrode (MFE). Gallium is added to overcome zinc interferences.
- TA-020IC-MS and IC-ICP/MS analysis in the environment
This article describes the coupling of ion chromatography with mass spectrometry (IC-MS) and plasma mass spectrometry (IC-ICP/MS) for the trace analysis of potentially hazardous compounds in the environment.
- TA-044pH value, conductivity and titration in water and soil analysis
The rapid growth of the Earth's population has led to massive increases in the consumption of energy and resources and in the production of consumer products and chemicals. It is estimated that 17 million chemical compounds are currently on the market, of which 100,000 are produced on a large industrial scale. Many of these enter the environment. This leads to a demand for sensitive analytical procedures and high-performance analytical instruments.pH value, conductivity and oxygen requirement are important characteristics in water and soil analysis. The first two of these can be determined rapidly; for the third, the titration that is used is also the one used in numerous single determinations. This article describes several important standard-compliant determinations in water and soil analysis.
- WP-004Electrochemistry in the environmental sciences
This Metrohm White Paper presents the important role of electrochemistry in the environmental sciences. The applications have to do with basic research for the fuel cell that yields energy from wastewater, the electrical clean-up of contaminated soil and electrochemical CO2 reduction of greenhouse gases for isolating chemical raw materials.
- WP-014High productivity and profitability in IC environmental analysis
Brad Meadows is Vice President and Lab Director at the US company BSK Labs, which runs a number of environmental laboratories and service centers. Brad is an analytical chemist and has been working in the management of analysis laboratories for 15 years. He shared his experiences with Metrohm ion chromatography with us in the form of some concrete facts and figures.
- WP-021Water analysis in the field: Determining arsenic, mercury, and copper
Heavy metals such as arsenic and mercury find their way into the ground water in many regions of the world, either through natural processes or as the result of human activities. Limit values are exceeded many times over, particularly for arsenic in drinking water, in many areas. This calls for a rigorous monitoring of water quality. The present whitepaper focuses on field determinations of arsenic, mercury, and copper – directly at the sampling site.
- WP-039Ion chromatography – addressing the latest challenges in environmental analysis
The analytical challenges of environmental analysis increase in difficulty from year to year. As well as analysis of particularly toxic types of metals such as chromium(VI), highly diverse and partially persistent organic fluorine compounds (e.g., trifluoroacetic acid) are presently in focus. The analysis of toxic oxohalides such as bromate and perchlorate is also a current subject of investigation.
- WP-045When HPLC fails: IC in food, water, and pharmaceutical analysis
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.
- WP-056Determining dissolved oxygen in water – Titration or direct measurement?
«Dissolved oxygen» describes the amount of oxygen molecules (O2) which are dissolved in a liquid phase under certain conditions. In this white paper, two different methods for the analysis of dissolved oxygen, titration and direct measurement, are compared and contrasted to help analysts determine which method is more suitable for their specific applications. Here, we primarily focus on the determination of dissolved O2 in water. However, the same principle applies for other liquid phases such as non-alcoholic or alcoholic beverages.
- WP-062Overcoming difficulties in ion measurement: Tips for standard addition and direct measurement
Ion measurement can be conducted in several different ways, e.g., ion chromatography (IC), inductively coupled plasma optical emission spectrometry (ICP-OES), or atom absorption spectroscopy (AAS). Each of these are well-established, widely used methods in analytical laboratories. However, the initial costs are relatively high. In contrast, ion measurement by the use of an ion-selective electrode (ISE) is a promising alternative to these costly techniques. This White Paper explains the challenges which may be encountered when applying standard addition or direct measurement, and how to overcome them in order for analysts to gain more confidence with this type of analysis.
- WP-078Adsorbable organic fluorine (AOF) for screening of PFAS in waters
Learn about PFAS, their impact on water quality, EU Directive 2020/2184, and the benefits of AOF measurement using combustion ion chromatography (CIC).
- WP-081Fast determination of AOX in waters according to DIN 38409-59
Monitor adsorbable organic halogens (AOX) in water using combustion ion chromatography (CIC) for precise analysis of AOCl, AOBr, AOI, and total AOX.
- WP-087Green alternative methods for voltammetric analysis in different water matrices
This White Paper presents four different «green» sensors: the scTRACE Gold, screen-printed electrodes, the glassy carbon electrode, and the Bi drop electrode from Metrohm that can be used to determine low concentrations of heavy metals in different sample matrices, such as boiler feed water, drinking water, and sea water.
- WP-090Automated water hardness determination according to ASTM D8192
The ASTM D8192 standard allows analysts to determine water hardness in different water matrices by complexometry with automated photometric endpoint recognition, increasing the reproducibility and the precision of the results.
- WP-097Why switch to OMNIS Client/Server (C/S)?
OMNIS Client/Server boosts business performance with scalable server management, cutting costs by reducing hardware, energy use, and maintenance across locations.