Aplikasi

A new Raman system design is presented that expands the applicability of Raman to See Through diffusely scattering media such as opaque packaging materials, as well as to measure the Raman spectrum and identify thermolabile, photolabile, or heterogeneous samples.

Edible oils are not only a major source of nutrition but also a key basic material in the food industry. Vegetable oils are increasingly important because of their high content in mono- and polyunsaturated fatty acids in comparison with animal fats. In this application note, the main ingredients of olive oil, camellia oil, arachis oil, sunflower seed oil, and colza oil are analyzed using a portable Raman spectrometer combined with chemometrics software.

See through Raman Spectroscopy (STRaman®) is a newly developed technology that expands the capability of Raman spectroscopy to measure samples beneath diffusely scattering packaging material. The STRaman technology features a much larger sampling area than the confocal approach. This design enhances the relative intensity of the signal from the deeper layers, thereby increasing the effective sampling depth, allowing the measurement of material inside visually opaque containers. The larger sampling area has the additional advantage of preventing sample damage by reducing the power density, as well as improving measurement accuracy by eliminating heterogeneous effect.

Botanicals are derived from plant materials and used for their medicinal and therapeutic properties in the nutraceuticals market. They are not as heavily regulated by the U.S. Food and Drug Administration (FDA) like the pharmaceuticals drug market, but they are required to follow Good Manufacturing Practice (GMP Requirements).The NanoRam®-1064 is an asset for pharmaceutical identity testing, minimizing fluorescence generated by typical handheld Raman systems with 785 nm lasers. As such, the NanoRam®-1064 is used here to identify botanicals that would normally fluoresce with a 785 nm laser.

Although the process of building, validating and using a method is well-defined through software, the robustness of the method is dependent on proper practice of sampling, validation, and method maintenance. In this document, we will detail the recommended practices for using the multivariate method with NanoRam-1064. These practices are recommended for end users who are in the pharmaceutical environment, and can expand to other industries as well. This document aims to serve as a general reference for NanoRam-1064 users who would like to build an SOP for method development, validation and implementation.

Raman spectroscopy’s use for process analytics in the pharmaceutical and chemical industries continues to grow due to its nondestructive measurements, fast analysis times, and ability to do both qualitative and quantitative analysis. Spectral preprocessing algorithms are routinely applied to quantitative spectroscopic data in order to enhance spectral features while minimizing variability unrelated to the analyte in question. In this technical note we discuss the main preprocessing options pertinent to Raman spectroscopy with real applications examples, and to review the algorithms available in B&W Tek and Metrohm software so that the reader becomes comfortable applying them to build Raman quantitative models.

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.

Compared to the classical Epton titration, potentiometrically indicated two-phase titrations using organic-solvent-resistant Surfactrodes can be easily automated and require no toxic and environmentally hazardous chloroform. Even challenging matrices such as fats and oils in bath oils and hair conditioners or strong oxidizing agents in washing powder and industrial cleaners do not interfere with the titration of the ionic surfactants. Results obtained show excellent agreement to those of the Epton titration. Irrespective of the matrix, relative standard deviations of threefold determinations are all below 2.1%. While the Surfactrode Resistant is mainly used for oil-containing formulations, the Surfactrode Refill is ideal for washing powders and soaps. Both electrodes excel by their ruggedness and allow the rapid and precise determination of anionic and cationic surfactants.

Fluoride is commonly used in dental products to help prevent tooth decay. When fluoride is present in high concentrations, these products are regulated by 21 CFR 355. Three fluoride compounds used in over the counter (OTC) anti‐cavity dental products are sodium fluoride, stannous fluoride and sodium monofluorophosphate (MFP). The assay of fluoride in these active ingredients and finished formulations are determined by manual titration, or by ion‐selective electrodes. As a part of USP’s global monograph modernization initiative, an alternative selective and sensitive method has been developed and validated – ion chromatography (IC). The proposed IC method can also be used for the identification test as an alternative to the wet chemistry method.

This Bulletin is a supplement to Application Bulletin no. 36 (Half-wave potentials of inorganic substances) in the sense that the half-wave potentials of 100 different organic substances are listed. At the same time the supporting electrolytes used and the limits of determination are given.The various substances are listed in alphabetical order. The most important polarographically active functional groups are taken into consideration. This means that substances for related structures can also be determined polarographically in the same or similar supporting electrolytes, although they may not appear in the list.Unless otherwise stated, the half-wave potentials refer to a temperature of 20 °C, and the potentials are given in volts, measured with a sat. KCI-Ag/AgCl electrode assembly.The determination limits give the smallest concentrations which can be measured without risking serious errors in the results. In all cases, the limit of detection lies below the limit of determination.

This Application Bulletin gives an overview of the volumetric water content determination according to Karl Fischer. Amongst others, it describes the handling of electrodes, samples, and water standards. The described procedures and parameters comply with the ASTM E203.

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.

This Application Bulletin gives an overview of the coulometric water content determination according to Karl Fischer.Amongst others, it describes the handling of electrodes, samples, and water standards. The described procedures and parameters comply with the ASTM E1064.

Application Bulletin AB-076 contains a description of the polarographic determination of low concentrations (1–100 mg/L) of NTA and EDTA in bodies of water. NTA, EDTA and citrate have gained in importance as complexing agents and builders due to the fact that the laws of some countries have made it necessary to find a substitute for phosphates in detergents.This Bulletin describes the determination of larger quantities of complexing agents in detergents using potentiometric titration. The ion-selective copper electrode (Cu-ISE) is used here as the indicator electrode. The determination of complexing agents is not disturbed by the other constituents often present in detergents.

The Rancimat method is an accelerated ageing test. Air is conducted through the sample in the reaction vessel at a constantly increased temperature. The fatty acids are oxidized during this process. Volatile secondary reaction products are formed at the end of the test that are conducted by air flow into a measuring vessel, where they are absorbed by a measuring solution (distilled water). The continually recorded electrical conductivity increases as a result of the absorption of the ionic reaction products. The time up to which the secondary reaction products arise is called the induction time. It characterizes the oxidation stability of oils and fats.This Application Bulletin provides a detailed description of the method, in particular also of the required sample preparation.

The titrimetric determination of nonionic surfactants on the basis of polyoxyethylene adducts (POE adducts) is described in the Bulletin. The basis for the determination is the transfer of the nonionic surfactant into a pseudo-cation compound and its precipitation titration with sodium tetraphenylborate (Na-TPB). The NIO electrode is used for the indication of the potentiometric titration. This Bulletin describes determinations in raw products, formulations and wastewater and draws attention to special features, possibilities, limits and disruptions.

Anionic surfactants can be titrated with cationic surfactants and vice-versa. The Bulletin describes a multitude of substances that can be determined in this fashion and specifies the respective working conditions and parameters. In contrast to the classic two-phase titration in accordance with Epton, the titration with the anionic and cationic surfactants electrodes can be performed without chloroform. Furthermore, the equivalence point of the titration is difficult to determine in some cases with the Epton method and the titration cannot be automated.In many cases, a surfactant ISE is a remedy that is both environmentally friendly and suitable here. It was developed specially for application with potentiometrically indicated surfactant determinations.

The two potentiometric titration methods described here allow the determination of the content of commercial betaine solutions. Neither method is suitable for determining the betaine content of formulations. The possibilities and limits of both methods are described and distinctive features and possible sources of interference are mentioned. The Bulletin explains the most important theoretical principles and is intended to help users to develop their own product-specific titration methods.

The present Bulletin offers an overview of the multitude of surfactants and pharmaceuticals that can be determined with potentiometric titration. Metrohm provides five different surfactant electrodes for indicating the titration endpoint: the Ionic Surfactant, the High Sense, the Surfactrode Resistant, the Surfactrode Refill and the NIO Surfactant electrode. The manufacture of the respective titrants and their titer determination are described in detail. In addition to this, the Bulletin contains a tabular overview of more than 170 proven applications from the area of surfactant and pharmaceutical analysis. This guideline leads you reliably to your destination: At a glance you can see from the table which surfactant electrode and which titrant are optimally suitable for your product.

On the basis of a multitude of practical examples, this Bulletin describes the potentiometric two-phase titration of ionic surfactants in raw materials and many other formulations.Two surfactant electrodes – the Surfactrode Resistant and the Surfactrode Refill – make it possible to perform this type of surfactant titration, analogous to the classic "Epton titration", with a high degree of automation. The achieved results correlate very well with those of Epton titration. The toxic, carcinogenic and environmentally hazardous chloroform can be replaced by other solvents such as methyl iosbutyl ketone or n-hexane.

Two-phase titration with potentiometric indication is a universal method for the determination of ionic surfactants in detergents. The results obtained are comparable to those with the classic two-phase titration in accordance with Epton (mixed indicator system disulfine blue / dimidium bromide). The present Bulletin addresses various parameters that could have an influence on potentiometric surfactant titration. The information provided makes it possible for the user to determine precisely the anionic surfactant content in practically all formulations.

This Application Bulletin describes the determination of Sn(II) in presence of Sn(IV) by anodic stripping voltammetry (ASV). Using an electrolyte containing fluoride, Sn(IV) gives no signal, so that a speciation is possible. The limit of detection is 2.5 µg/L.

Eco Titrators provide the capability to send PC/LIMS reports directly to a PC. This feature is mainly used to transfer data to an external LIMS system or to simply store the data in a digitally on the PC. Additionally, it is possible to control the Eco Titrator by RS232 commands if the connection is set up according to the procedure described below.The data transfer from the Eco Titrator to a PC can be done by a software- or a hardware-based option. Additional accessories are needed for the hardware-based option whereas for the software-based option two additional softwares must be installed. Both solutions are described in this document.

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 3-dimethylamino-1-propylamine in cocoamidopropyl betaine using cation chromatography with direct conductometric detection.

Determination of sodium, potassium, calcium, and magnesium in the water soluble fraction of a washing powder using cation chromatography with direct conductivity detection.

Determination of sodium and potassium in toothpaste using cation chromatography with direct conductivity detection.

Palm oil is a vegetable oil that is used not only in the food industry but also for the manufacture of soaps and body care products. It is furthermore an important raw material for the generation of biodiesel. Depending on the degree of refinement, palm oil can be red, reddish or even colorless in appearance. The carotenes responsible for the color are removed during refinement and the oil becomes increasingly clear. In this Note, the chlorine and sulfur content of various palm oils are determined using Combustion IC.Keyword: pyrohydrolysis

AOF (adsorbable organic fluorine) is used to screen for per- and polyfluorinated alkyl substances in aqueous matrices via pyrohydrolytic combustion and ion chromatography.

Determination of a nonionic surfactant of the alkyl propylene oxide derivative type in commercial mixtures containing anionic surfactants.

Determination of sodium lauryl ether sulfate surfactants.

Fluoride protects dental enamel and is an important trace element in toothpaste. A rapid and precise determination is made via standard addition with the help of an ion-selective fluoride electrode (F-ISE).

The water content of moisturising creams is determined according to Karl Fischer. Because of their high water content, the samples are first mixed and prediluted with dry methanol.

In this application note, Karl Fischer titration is used to determine the water content of urea.

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

The water content in panthenol is determined according to Karl Fischer.

This Application Note describes the automated determination of the water content in toothpaste using volumetric Karl Fischer titration (MATi 10).

Karl Fischer reagents contain buffer substances (usually imidazole) since the reaction constant is dependent on the pH value. A constant pH therefore ensures the most repeatable results. In 2015, imidazole was classified by European Union the as a CMR (carcinogenic, mutagenic or toxic) substance and the statement H360D was added, stating possible harm to fertility or a fetus. Meanwhile, other reagents free of imidazole are available for purchase. This Application Note summarizes test measurements with 34433 HYDRANAL™ NEXTGEN Coulomat AG-FI.

Determination of traces of carbonate in urea using anion chromatography with direct conductivity detection.

This Application Note shows how, with the help of Vis-NIR spectroscopy and a special plant library, 46 different medicinal and aromatic plants, e.g., Organicum majoricum and Tilia cordata, can be conveniently identified on the basis of their spectrum. In comparison with alternative methods for the determination of plants, which are elaborate and require experienced scientists for their performance, the Vis-NIR method permits rapid and uncomplicated identification.

Determination of key quality parameters of palm oil, namely free fatty acids (FFA), iodine value (IV), moisture content, deterioration of bleachability index (DOBI), and carotene require the use of several different analytical methods, which are laborious and can lack in accuracy. This application note demonstrates that the XDS RapidLiquid Analyzer operating in the visible and near infrared spectral region (Vis-NIR) provides a cost-efficient and fast solution for the determination of these quality control parameters in palm oil. With no sample preparation or chemicals needed, Vis-NIR spectroscopy allows for the analysis of palm oil in less than a minute and can be used by anyone.

Vis-NIR spectroscopy is used to determine the droplet morphology in hair conditioner. This Application Note shows that near-infrared (NIR) spectroscopy can be used to distinguish between unprocessed and processed hair conditioner and to qualify quality parameters such as the droplet size.

Visible Near-infrared (Vis-NIR) spectroscopy is a valuable chemical analysis tool that can be used to determine quality parameters of hair creams. A qualitative method was developed in order to allow a fast out-of-spec analyses of an active antibacterial ingredient.

Near-infrared spectroscopy (NIRS) was used as an analysis method for quality control of hair spray samples. A model for an active ingredient within hair sprays was developed, enabling fast and reliable out-of-specification analyses.

Near-infrared spectroscopy (NIRS) was used in a preliminary study as a fast and accurate method for the quantification of different preservatives and active ingredients in liquid shampoo. This Application Note shows how this analytical method allows the simultaneous determination of several constituents in shampoo in a single measurement.

Near-infrared spectroscopy (NIRS) was used as an analysis method for quality control of soap noodles. Quantitative models for the determination of Total Fatty Matter, Iodine Number, and C8–C14 were developed, enabling fast and reliable quality control.

Near-infrared spectroscopy (NIRS) was used as an analysis method for quality control of aqueous xanthan gum solutions. Quantitative models for the determination of optical density, glucose, and xanthan gum were developed, enabling fast and reliable quality control.

Determination of sodium laureth sulfate (SLES), cocamidopropyl betaine (CABP), cocamidopropylamine oxide (CAW), cocamide diethanolamine (DEA), and carbopol in shampoo is a cost- and time-intensive process due to the use of large volumes of chemicals per analysis. This application note demonstrates that the DS2500 Solid Analyzer operating in the visible and near-infrared spectral region (Vis-NIR) provides a cost-efficient and fast solution for a simultaneous determination these parameters in shampoo. With no sample preparation or chemicals needed, Vis-NIR spectroscopy allows for the complete analysis in less than a minute.

Near-infrared spectroscopy (NIRS) was used for quality control of skin creams. A model for the quantification of the water content was developed based on Karl Fischer titration (KF), enabling fast and reliable atline analysis and final product quality control.

This Application Note shows that visible near-infrared spectroscopy (Vis-NIRS) can determine the sun protection factor (SPF) of sunscreen products. Thanks to measurement durations of less than 30 seconds, NIR spectroscopy is ideally suited for rapid and reliable quality control.