Aplikace

100% starting materials identification testing is one of the FDA’s directives as per 211.84 for FDA regulated industries such as Pharmaceutical, Vaccines, Cosmetics, Tobacco, Animal veterinary products, Food, etc. STRam®-1064 is a Raman analyzer uniquely suited for this purpose. It measures samples through thick packaging materials such as plastics, multilayer kraft paper sacks, and HDPE containers. A long wavelength laser is used to suppress fluorescence. The ID algorithm isolates the sample signature by subtracting that of the packaging material and compares that with library spectra to achieve identification.

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.

This Bulletin describes fluoride determination in various matrices with the help of the ion-selective fluoride electrode (F-ISE). The F-ISE is comprised of a lanthanum fluoride crystal and exhibits a response in accordance with the Nernst equation across a wide range of fluoride concentrations.The first part of this Bulletin contains notes regarding the handling and care of the electrode and the actual fluoride determination itself. The second part demonstrates the direct determination of fluoride with the standard addition technique in table salt, toothpaste and mouthwash.

Determination of calcium and magnesium in high-purity sodium chloride using cation chromatography with direct conductivity detection.

Determination of nickel, zinc, cobalt, iron(II), and manganese in lithium bromide using cation chromatography with UV/VIS detection (520 nm) after post-column reaction with PAR.

Determination of sodium, potassium, DMEA (dimethylethanolamine), calcium, choline, and magnesium in a saline solution using cation chromatography with direct conductivity detection.

Within the scope of the USP monograph modernization, potassium is determined in potassium bitartrate applying cation chromatography with direct conductivity detection. The USP41 monograph for “Potassium bitartrate” does not yet mention an assay for potassium. The separation is performed on a Metrosep C 6 - 150/4.0 column (L76). The assay of potassium is performed with two commercially available products according to USP definitions. All acceptance criteria are fulfilled.

Within the scope of the USP monograph modernization, potassium is determined in potassium sodium tartrate applying cation chromatography with direct conductivity detection. The USP41 monograph for “Potassium sodium tartrate” does not yet mention an assay for potassium. The separation is performed on a Metrosep C 6 - 150/4.0 column (L76). The assay of potassium is performed with two commercially available products according to USP definitions. All acceptance criteria are fulfilled.

Lanthanum (La) is a transition metal which oxidizes easily in air to lanthanum(III) oxide. This oxide, as well as salts resulting from its dissolution in acid and recrystallization, is a component of different catalysts. Here, a lanthanum(III) acetate solution prepared by dissolution of lanthanum(III) oxide in acetic acid, has to be tested for a sodium contamination. The high concentration of La3+ is complexed by the dipicolinic acid in the eluent and forms anionic complexes. These complexes are eluted in the front and therefore do not interfere with the sodium impurity as well as other cations such as ammonium and calcium.

Lithium hexafluorophosphate (LiPF6) is used as an electrolyte in rechargeable batteries. Its high solubility in non-polar solvents and its non-coordinating character in particular make lithium hexafluorophosphate the ideal salt for use in lithium-ion cells. This Application describes the determination of cation traces in LiPF6 with conductivity detection following sequential suppression.

This Application Note presents the Mott-Schottky measurement, an extension of electrochemical impedance spectroscopy (EIS), on a popular semiconducting material.

Determination of sodium, potassium, and silica values in sodium and potassium silicates.

Determination of Na, P, and [Na]/[P] in precursor solutions and solids in the manufacture of sodium tripolyphosphate.

Determination of sodium in salts, process solutions, and foods.

Automated determination of the zirconium content of zirconium acetate, as well as other zirconium compounds which can be rendered soluble as zirconium acetate.

A measured amount of salt is titrated directly with a solution of 1 mol/L tetrasodium EDTA to thermometrically determined endpoints for Ca and Mg. Acetylacetone is added to alter the Ca and Mg EDTA stability constants for better endpoint sharpness.

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

This Application Note 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.

The water content of ammonium and potassium peroxodisulphate is determined according to Karl Fischer using two-component reagents. To prevent unwanted side reactions the determinations are carried out at -20 °C. Because the potassium salt is insoluble in the solvent, a high-frequency homogenizer is used to disintegrate the salt particles.

The water content of lime is determined according to Karl Fischer using the oven method (150 °C).

The water content of bismuth subnitrate is determined according to Karl Fischer.

The water content in Ca carbonate is determined by volumetric Karl Fischer titration.

In this application note, Karl Fischer titration is used to determine water content in sodium acetate trihydrate. The MATi 10 allows this determination to be automated, saving users time in the laboratory.

Determination of acetate and methansulfonate in an organic salt using anion chromatography with direct conductivity detection.

Pure sodium chloride contains much less iodide than e.g., table salt which usually is fortified with it. Trace determination of iodide is easily performed applying ion chromatography with amperometric detection. This detection mode is particularly selective and sensitive. The actual separation is achieved using a Metrosep A Supp 5 - 250/4.0 column. The detection happens at a silver working electrode. LOQ is at approximately 1.0 μg/L (in solution) and 50 μg/kg in the sample. The use of a shorter column might further improve the LOQ.

Determination of citric acid and tartaric acid in fruit salt using ion-exclusion chromatography with direct conductivity detection.

Fentanyl, a powerful synthetic opioid, is illegally distributed worldwide. Overdosing can be fatal, causing symptoms like stupor, pupil changes, cyanosis, and respiratory failure. Just 2 mg of fentanyl can be lethal, depending on factors like body size and past usage. Given its severe impact, identifying and detecting fentanyl is crucial, as it has become a major public health crisis. Combining electrochemical surface-enhanced Raman spectroscopy (EC-SERS) with screen-printed electrodes (SPEs) offers a fast, effective, and precise method for detecting fentanyl.

This Application Note documents the suitability of hand-held Raman spectrometers, e.g., the Mira M-1, for the identification and differentiation of salts such as carbonates, phosphates, and sulfates. The focus of the work was the rating of the influence of the cationic part and of the crystal water on the Raman spectroscopy identification of the salts.

Determination of fluoride, chloride, bromide, and sulfate in bath salts (sea salt) using anion chromatography with conductivity detection after chemical suppression.

Determination of iodide in common salt using anion chromatography with amperometric detection at the silver electrode.

Determination of bromide in NaCl crystals using anion chromatography with conductivity detection after chemical suppression.

Determination of chloride and sulfate in potassium tetraborate (KB4O7 * 4 H2O) using anion chromatography with conductivity detection after chemical suppression.

Determination of nitrate and sulfate in sodium phosphinate (sodium hypophosphite) using anion chromatography with conductivity detection after chemical suppression.

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

Determination of fluoride, chloride, nitrate, phosphate, sulfate, trimetaphosphate, and tripolyphosphate in tetrasodium pyrophosphate using anion chromatography with a high pressure gradient and conductivity detection after chemical suppression.

Determination of chloride, nitrite, nitrate, phosphate, sulfate, trimeta-, and pyrophosphate in tripolyphosphate using anion chromatography with a high pressure gradient and conductivity detection after chemical suppression.

Determination of iodide in a table salt using anion chromatography with conductivity detection after chemical suppression.

Determination of traces of chloride in a quaternary ammonium hydroxide using anion chromatography with conductivity detection after chemical suppression and inline cation exchange to remove the matrix cations.

Determination of molybdate in 2.5% NaCl using anion chromatography with conductivity detection after chemical suppression and inline matrix elimination by molybdate preconcentration after the first separation and subsequent reinjection.

Poly(3,4-ethylenedioxythiophene) (PEDOT) is one of the most promising ICPs due to its high conductivity, electrochemical stability, catalytic properties, high insolubility in almost all common solvents and interesting electrochromic properties (transparent in the doped state and colored in the neutral state). In this Application Note, PEDOT film is evaluated by spectroelectrochemical techniques.

Determination of free alkali in sodium hypochlorite by potentiometric titration with hydrochloric acid using a combined glass electrode.

In accordance with the European Pharmacopoeia, sodium sulfate is determined with the PB ISE.

The composition of salts with laxative and expectorant effects must be determined precisely in medications. The sulfate content is determined using automatic potentiometric titration with EGTA as titrant in accordance with Ph. Eur. 8.0.

Potassium carbonate and potassium bicarbonate are important raw materials in the pharmaceutical industry. As APIs, both can be used in effervescent tablets and powders as supplements to help patients with low potassium levels in their blood.For both species, the other species is the most important contamination. For the assay, a selective method is thus required. Separation of both species by ion chromatography is not possible as the eluent changes the ratio of carbonate and bicarbonate falsifying the result. Due to their different pKa values, carbonate and hydrogen carbonate can be selectively determined by titration, which is therefore the method of choice for pharmacopeias, such as the USP and Ph.Eur.Using potentiometric autotitration instead of manual titration increases the accuracy and reliability of results. Furthermore, the use of an autotitrator ensures that crucial requirements of regulatory compliance guidelines such as dataintegrity are met.

Lithium salts (e.g., lithium carbonate and lithium hydroxide) are used in myriad applications. Lithium hydroxide is used for the production of lithium stearate, an important engine lubricant. In addition, it is utilized as an air purifier due to its ability to bind carbon dioxide. While the majority of lithium carbonate is used for aluminum production, it is also used for the glass and ceramic industry. It lowers the melting point of these materials, lowering the associated electricity costs and making it cheaper to produce them.For all of these applications, it is important to know the quality of the pure lithium salts used in the various production processes. This Application Note presents an easy method for the assay of lithium hydroxide and lithium carbonate on an automated OMNIS system.

Lithium nitrate is an oxidizing agent used in the manufacture of red-colored fireworks and flares. In addition, the lithium nitrate trihydrate compound absorbs heat well and can be used for thermal energy storage. Since lithium nitrate is a hygroscopic substance, its purity must first be verified before it is used for synthesis or other applications. The purity assay is done by a fully automated precipitation titration between lithium and fluoride in an ethanolic solution. The benefit of titration is that the lithium nitrate does not need to be diluted after dissolving in ethanol as with other techniques such as ICP-MS.

Determination of nickel, zinc, iron(II), and manganese in lithium bromide using cation chromatography with UV/VIS detection (520 nm) after post-column reaction.

Determination of bromide and nitrate in 1% sodium chloride solution using anion chromatography with UV/VIS detection (205 nm) after chemical suppression.

Determination of traces of fluoride, bromide, nitrate, phosphate, and sulfate using anion chromatography with conductivity detection after chemical suppression and subsequent UV/VIS detection.

Determination of bromide in calcium chloride using anion chromatography with UV/VIS detection.