Aplikasi

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.

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

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).

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.

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.

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.

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.

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.

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

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

Phosphate can be rapidly and easily titrated thermometrically using a standard solution of Mg2+ as titrant. The phosphate-containing solution is basified and buffered with NH3/NH4Cl solution before titration. The formation of insoluble MgNH4PO4 is exothermic. The method is a titrimetric adaptation of a classical gravimetric procedure. This bulletin deals with the determination of phosphate in phosphoric acid and granular fertilizers such as MAP (monoammonium phosphate), DAP (diammonium phosphate) and TSP (triple superphosphate). Results are reported as percentage of P and P2O5.

The phosphoric acid content can be easily titrated with a standardized solution of 2 mol/L NaOH. The interfering calcium content in phosphoric fertilizer can be eliminated by adding a saturated oxalate solution.

Pyrithione complexes, such as zinc pyrithione (ZnPT), copper pyrithione (CuPT), and sodium pyrithione (NaPT), are used as fungicides and bactericides. ZnPT is used in the treatment of skin conditions such as seborrheic dermatitis or dandruff. Furthermore, ZnPT is sometimes used as an antibacterial agent in paints to prevent algae and mildew growth. CuPT is primarily in use as a biocide to prevent biofouling of surfaces submerged in water. Meanwhile, NaPT is used as antifungal agent for treatment of mycosis, such as athlete’s foot. The different pyrithione complexes are determined by iodometric titration using a maintenance-free Pt Titrode for the indication.

Determination of ammonium, magnesium, and calcium in a fertilizer using cation chromatography with directconductivity detection.

Determination of ammonium, potassium, magnesium, and calcium in a liquid fertilizer using cation chromatography with direct conductivity detection..

Determination of soluble orthophosphate ions, for example soluble phosphate in fertilizers such as DAP.

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

Phosphorus is a primary macronutrient for plants and is a constituent of DNA and adenosine triphosphate (ATP), which is involved in many biological processes requiring energy. In fertilizers, phosphorus is present in the form of phosphate, as the most accessible form of phosphorus for plants is dihydrogen phosphate. Knowledge of the phosphorus content helps to select the right fertilizer for the plants.Traditionally, phosphate is determined gravimetrically (a time consuming procedure) or spectrophotometrically (expensive instrumentation). In this Application Note, an alternative method is presented, where phosphate is determined by a precipitation titration with magnesium. Various solid and liquid NPK fertilizers with phosphorus contents between 6.5 and 17% were analyzed. The analysis by thermometric titration requires no sample preparation in case of liquid NPK fertilizers and only minimal sample preparation in case of solid NPK fertilizers. One determination takes about 5 minutes.

Sulfur is a secondary macronutrient for plants and is essential for chloroplast growth and function. In fertilizers, sulfur is usually provided in the form of sulfate. Traditionally the sulfate content is determined gravimetrically by precipitation with barium. The drawback of this method is that it requires numerous time consuming and laborious analysis steps.In this Application Note, an alternative method is presented, where sulfate is determined by a precipitation titration with barium chloride. Various solid and liquid NPK fertilizers with sulfur contents between 1 and 8% were analyzed. The analysis of sulfate in fertilizers by thermometric titration requires no sample preparation at all for liquid NPK fertilizers, and only minimal sample preparation for solid NPK fertilizers. One determination takes about 3 minutes only. To increase the sensitivity of the method, the samples are spiked with a standard sulfuric acid solution, which is then considered when calculating the result.

Fertilizers are applied in the agricultural sector to provide more essential nutrients to growing plants. The so-called «NPK» fertilizers provide such nutrients to plants with its three main components (N – nitrogen, P – phosphorous, K – potassium). In fertilizers, nitrogen is mainly provided in three forms: as ammonium nitrate (NH4NO3), ammonia (NH3), and urea (H2NCONH2). Determination of the individual nitrogen-contributing components is often laborious work. Thermometric titration offers the possibility to rapidly determine the amount of ammoniacal nitrogen and urea nitrogen in a single titration using sodium hypochlorite as titrant.

Potassium is a primary macronutrient for plants, as it plays an important role in water regulation as well as plant growth. In NPK fertilizers, potassium is present besides nitrogen and phosphorus, which are the other two primary macronutrients. Knowing the quality and content of a NPK fertilizer allows an optimal fertilizer management for a planned culture, saving costs and increasing profitability.Traditionally potassium is determined gravimetrically or by flame photometry. In this Application Note, an alternative method is presented, where potassium is determined a precipitation titration. Various solid and liquid NPK fertilizers with potassium contents between 10 and 27% were analyzed. After the removal of any present ammonia, the potassium can be determined reliably in about 5 minutes.

Potash is commonly mined from ore, deposited after ancient inland oceans evaporated. The potassium salt is then purified in evaporation ponds. At the end of this process, the potash is typically obtained as potassium chloride. Potash is mainly used as fertilizer, providing potassium—an essential nutrient—to plants. Additionally, it is used in the chemical industry and to produce medicine. Potassium content in potash is typically determined by flame photometry (F-AES) or ICP-OES. However, these techniques have high investment and running costs. By applying the historically used gravimetric precipitation reaction as a thermometric titration, it becomes possible to rapidly and inexpensively determine the potassium content in potash within minutes.

As nitrogen is essential nutrient for plants, it is an essential constituent of many fertilizers. It is present there in different forms, mainly as ammonium or nitrate. Knowing the nitrogen concentration and the form in which is present helps to select the right fertilizer for the plants. For producers of fertilizers, it is therefore necessary to indicate the concentration of ammonium nitrogen in their product.This Application Note shows how to determine ammonium in liquid fertilizers by means of a standard addition.

NPK fertilizers are mainly comprised of three primary nutrients required for a healthy plant growth (nitrogen, phosphorous, potassium). They are available as liquid, or granular form, whereof the last is the most common used one. Knowing the quality and content of a fertilizer allows an optimal utilization for a planned culture and optimizing the amount of used fertilizer. This helps to reduce costs and to improve plant growth and with it, a better harvest follows.To assess potassium, several methods like flame photometry, titration, or ion measurement can be used. In this work, the potassium content is measured by standard addition which is a fast, inexpensive, and easy to use method.

This Application Note describes the determination of water content in pesticides using Karl Fischer titration.

This Application Note shows that visible near-infrared spectroscopy (Vis-NIRS) can be used for the quantification of five effective insecticide and herbicide components (Abamectin emulsifiable concentrate (EC), Emamectin EC, Cyhalothrin EC, Cypermethrin and Glyphosate) in pesticides. Vis-NIRS is an excellent alternative to conventional lab methods, saving both cost and time.

Specialty chemicals have to fulfill multiple quality requirements. One of these quality parameters, which can be found in almost all certificates of analysis and specifications, is the moisture content. The standard method for the determination of moisture content is Karl Fischer titration.This method requires reproducible sample preparation, chemicals, and waste disposal. Alternatively, near-infrared spectroscopy (NIR) can be used for the determination of moisture content. With this technique, samples can be analyzed without any preparation and without using any chemicals.

Moisture content is one of the most commonly measured properties of fertilizers. Globally, regulations for different fertilizers vary, but local legal limits ensure that the maximum amount of water must not be exceeded. Next to gravimetric methods, Karl Fischer titration is often used for accurate moisture determination.Compared to these methods, near-infrared spectroscopy (NIRS) offers unique advantages: it generates reliable results within seconds, and at the same time does not create chemical waste. This Application Note explains how NIRS can offer fast, reagent-free analysis of moisture content in various fertilizer products.

Spectroelectrochemistry is a multi-response technique that provides both electrochemical and spectroscopic information about a chemical system in a single experiment, i.e., it offers information from two different points of view. Spectroelectrochemistry focused on the UV/VIS region is one of the most important combinations because this allows us to obtain not only valuable qualitative information, but also outstanding quantitative results. In this application note, the degradation kinetics for 4-nitrophenol, a known pollutant, were determined using SPELEC.

Determination of nitrate and sulfate in a fertilizer after acid digestion using anion chromatography with conductivity detection after chemical suppression.

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

Determination of chloride, sulfite, sulfate, and thiosulfate in metam potassium (potassium N-methyldithiocarbamate) using anion chromatography with conductivity detection after chemical suppression.

Determination of fosetyl-aluminum in a formulation using anion chromatography with conductivity detection after sequential suppression.

Determination of phosphate, HEDP (etidronic acid), and pyrophosphate in a biocide sample using anion chromatography with conductivity detection after sequential suppression.

The FOS/TAC value, sometimes referred to as VFA/TA, is a meaningful parameter for assessing both the current condition and the development of anaerobic digestion processes in a digester of a biogas plant. Knowledge of this value can help decrease the risk of acidification problems, which can result in a costly crash of the entire digestion process. Therefore, an accurate and reliable determination of the FOS/TAC value is important for both efficient and cost-effective production operations. This value is determined by an acid-base titration. Using the Eco Titrator from Metrohm equipped with an Ecotrode plus electrode, a reproducible and accurate determination of the FOS/TAC value is possible.

Complexing agents are used in fertilizers to bind trace nutrients such as cobalt, iron, manganese, etc. EN 13368-1 describes the determination of EDTA, HEDTA, and DTPA. As sample preparation, Fe3+ is added to build complexes with the three agents. The complexes are separated on an anion-exchange column and detected by UV/VIS after addition of perchloric acid.

Hexavalent chromium (chromate) in soil needs to be minimized as it acts cancerogenic. Chromate may be introduced to soil by applying fertilizers containing Cr(VI). Most of this chromate is reduced to Cr(III) by oxidizing organic matter. The remaining chromate is determined according to EN ISO 15192 by alkaline digestion followed by ion chromatography with post-column reaction with 1,5-diphenylcarbazide and subsequent visible detection at 538 nm. Procedure B of EN 16318 applies the alkaline digestion and the same analytical procedure to fertilizers.

Determination of cadmium and lead in herbicide powder containing 37% copper after digestion.

Agriculture at significant scale without fertilizers is no longer possible in the modern world. To grow a sufficient amount of produce for nearly 8 billion people as well as for domesticated animals and industrial uses, fertilizers of different nutrient compositions are available to cater to the unique needs of various soil types. Information on the fertilizer’s composition (e.g., total nitrogen, phosphorus, and potassium) is available to help select the ideal fertilizer for a specific soil. Conventionally these constituents are determined either gravimetrically (e.g., phosphorus, potassium, or sulfate) or with ICP-OES (e.g., phosphorus or potassium). These methods either have the disadvantages of long analysis times combined with laborious sample preparation (gravimetry), or require expensive instrumentation with high running costs (ICP-OES). This White Paper elaborates how thermometric titration is a fast and inexpensive alternative method to provide information on the content of various nutrients in different fertilizers.

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.