Fluorine determination, analytical methods

Dynamar Polymer Processing Additive Technical Information, Parr Bomb Analytical Method for Determining Total Organic Fluorine Concentration in Polyethylene, Dyneon, Oakdale, MN (n.d.). 

The fact that fluorination had taken place was established by various analytic methods ESCA, IR and FTIR spectroscopy, bulk anlaysis,NMR, and DSC. The presence of chemically bonded fluorine in the surface layer of treated samples were uniquely determined by analysis data. Further details can be found elsewhere.22... 

The aim of this section is to present a concise overview of separation, concentration and decomposition methods for sample pre-treatment and an overview of the analytical methods available for determining free inorganic fluoride and total fluorine in the environment (natural and drinking water, air and soil), biological and related materials, and fluoride supplements and dental products. 

Numerous analytical methods have been described for determining fluorine in a variety of samples. 

In 1935, the Committee was renamed the Analytical Methods Committee (AMC) but the main analytical work was carried out by sub-committees composed of analysts with specialised knowledge of the particular application area. The earliest topics selected for study were milk products, essential oils, soap and the determination of metals in food colourants. Later applications included the determination of fluorine, crude fibre, total solids in tomato products, trade effluents and trace elements, and vitamins in animal feeding stuffs. These later topics led to the publication of standard methods in a separate booklet. All standard and recommended methods were collated and published in a volume entitled Bibliography of Standard, Tentative and Recommended or Recognised Methods of Analysis in 1951. This bibliography was expanded to include full details of the method under the title Official, Standardised and Recommended Methods of Analysis in 1976 with a second edition in 1983 and a third edition in 1994. 

An analytical method for ultra-trace determination (down to 0.1 4g/L) of 15 fluorinated aromatic carboxylic acids, used as water tracers, was described [290]. The method comprised off-line extraction of the acids with Isolute ENV-f at pH 1. 5, elution with acetonitrile, and GC-MS quantification. The examination of the behavior of the fluorinated benzoic acids on the hypercrosslinked extracting material showed that with increasing acidity the breakthrough volume of the acid decreases, while increasing its molecular size increases the breakthrough volume because of more effective dispersion interactions with sorbent material. 

DPP is often superior to other techniques in the control of chemical production, e.g. the synthesis of steroids with a fluorine atom in C-6 (a) is always linked with the formation of a smaller amount of the 3-isomer, which can be detected easily by its more positive peak in DPP (see Figure 1). No other analytical method is known for the determination of this impurity with such accuracy. 

When other fluorochemicals are present, the fluorinated surfactant has to be separated and determined by a specific analytical method. Some of the conventional methods for the analysis of hydrocarbon-type surfactants [ 1 ] are also... 

The trend of discovering the analytical field of environmental analysis of surfactants by LC-MS is described in detail in Chapters 2.6-2.13 and also reflected by the method collection in Chapter 3.1 (Table 3.1.1), which gives an overview on analytical determinations of surfactants in aqueous matrices. Most methods have focused on high volume surfactants and their metabolites, such as the alkylphenol ethoxylates (APEO, Chapter 2.6), linear alkylbenzene sulfonates (LAS, Chapter 2.10) and alcohol ethoxylates (AE, Chapter 2.9). Surfactants with lower consumption rates such as the cationics (Chapter 2.12) and esterquats (Chapter 2.13) or the fluorinated surfactants perfluoro alkane sulfonates (PFAS) and perfluoro alkane carboxylates (PFAC) used in fire fighting foams (Chapter 2.11) are also covered in this book, but have received less attention. 

The GC/MS procedures for methamphetamine are described in Table 4. The papers published in Japanese - have corresponding reports in English. - - Methamphetamine was detected and determined by mass fragmentography in rat hair after administration of the substance. Nine methods also detected the metabolite amphetamine or amphetamine alone. Suzuki et al. determined methamphetamine also in nail, sweat and saliva. The workup (EX after acid or alkaline hydrolysis) and derivatization technique (methanol-trifluoroacetic acid [TEA]) is rather uniform in most procedures. Nakahara et al. ° used methoxyphenamine excretion into beard hair to discuss several washing procedures. Alkaline or methanolic extraction are used with one exception. Derivatization is mainly made by fluorinated anhydrides. A review ° gives details on analytical procedures, incorporation rates of amphetamines from blood to hair, and relationship between drug history and drug distribution in hair. 

Abstract In the past years, elucidation of transformation products of per- and polyfluorinated chemicals (PFC) has been a task frequently approached by analytical chemists. PCT, such as perfluorooctane sulfonate (PFOS) and perfluorooctanoic acid (PFOA) are persistent and thus, the analytical quest to detect transformation products has failed so far. Their prominence as contaminants is mainly due to their extreme persistence, which is linked to their perfluoroalkyl chain length. Molecules that are less heavily fluorinated can show very complex metabolic behavior, as is the case for fluorotelomer alcohols. These compounds are degraded via different but simultaneous pathways, which produce different stable metabolites. Biotransformation processes of PFC may occur when these compounds enter the environment, and thus known and unknown PFC may be generated in these compartments. Therefore, it is essential to determine metabolic pathways of such compounds in order to entirely understand their fate in the environment. This chapter summarizes methodological approaches and instmmental setups which have been implemented in biotransformation studies of PFC and focuses on mass spectrometric methods and the separation techniques coupled to the mass spectrometer (MS). Valuable MS approaches that have not been frequently used in studies on PFC are presented as well. Since compounds carrying C-F bonds exhibit unique properties, these will be initially presented to address the meaning of these properties both for analytical tasks and for the setup of biotransformation experiments. 

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