Analysis of Purity

For very high temperatures, or if only very small amoimts of material are available, 

Measurement of vapor pressure of low-boiling substances has already been treated in the discussion of Stock s apparatus. With substances boiling above room temperature, a heated manometer must be used. For instance, molten tin can be used as the manometer liquid and the flask containing the substance together with the short manometer lowered into the heated bath, while the second leg of the manometer is connected to a manometer and a surge vessel. The pressure is then compensated for imtil the tin in both legs is at the same level, and the pressure is read off on the manometer. 

The best device, however, is the quartz coil manometer, the coil of which can be heatedto500°C(in special cases to 600-700°C). In all cases the null point of the instrument must be checked after each measurement. Therefore the manometer should be provided with a heating coil, which doe snot need to be at the test temperature but must nevertheless be at a sufficiently high temperature to prevent condensation in the coil and in the capillary connections (which are likewise provided with a heating coil). With compensation to zero, the pressure is read off on the Hg manometer. In those cases where it cannot be ascertained by the usual method (with a thermometer and distillation flask) the boiling point is determined more accurately by extrapolation of the vapor pressure curve. 

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Two-dimensional electrophoresis is normally run so that proteins are separated from each other on the basis of a different molecular property in each dimension. The most commonly utilized method entails separation of proteins by isoelectric focusing (see below) in the first dimension, with separation in the second dimension being undertaken in the presence of SDS, thus promoting band separation on the basis of protein size. Modified electrophoresis equipment that renders two-dimensional electrophoretic separation routine is freely available. Application of biopharmaceuti-cal finished products to such systems allows rigorous analysis of purity. 

In theory, if the net charge, q, on a molecule is known, it should be possible to measure / and obtain information about the hydrodynamic size and shape of that molecule by investigating its mobility in an electric field. Attempts to define /by electrophoresis have not been successful, primarily because Equation 4.3 does not adequately describe the electrophoretic process. Important factors that are not accounted for in the equation are interaction of migrating molecules with the support medium and shielding of the molecules by buffer ions. This means that electrophoresis is not useful for describing specific details about the shape of a molecule. Instead, it has been applied to the analysis of purity and size of macromolecules. Each molecule in a mixture is expected to have a unique charge and size, and its mobility in an electric field will therefore be unique. This expectation forms the basis for analysis and separation by all electrophoretic methods. The technique is especially useful for the analysis of amino acids, peptides, proteins, nucleotides, nucleic acids, and other charged molecules. 

MEKC-ESI-MS method in the analysis of purity of galantamine hydrobromide and degradation products of ipratropium hydrobromide [80]... 

Beaudet and Caskey (1973) have reported the binding of HGPRT derived from cultured Chinese hamster fibroblasts to anti-HGPRT Sepharose activated by cyanogen bromide. However, the small amount of antisera available precluded isolation of a sufficient quantity of HGPRT for analysis of purity. We believe that the successful application of this technique will allow a rapid and quantitative isola-... 

Gas chromatography is a commonly used analytical technique for the analysis of purity and composition of solvents that is very sensitive, rapid and simple to execute. It gives both qualitative and quantitative information from very small sample sizes of only a few microliters. 

Stem layer adsorption was involved in the discussion of the effect of ions on f potentials (Section V-6), electrocapillary behavior (Section V-7), and electrode potentials (Section V-8) and enters into the effect of electrolytes on charged monolayers (Section XV-6). More speciflcally, this type of behavior occurs in the adsorption of electrolytes by ionic crystals. A large amount of wotk of this type has been done, partly because of the importance of such effects on the purity of precipitates of analytical interest and partly because of the role of such adsorption in coagulation and other colloid chemical processes. Early studies include those by Weiser [157], by Paneth, Hahn, and Fajans [158], and by Kolthoff and co-workers [159], A recent calorimetric study of proton adsorption by Lyklema and co-workers [160] supports a new thermodynamic analysis of double-layer formation. A recent example of this is found in a study... 

To determine the purity of a sample of Na2HP04, a 2.469-g sample is dissolved and diluted to volume in a 100-mL volumetric flask. Analysis of the resulting solution gives an absorbance of 0.135. What is the purity of the Na2HP04 ... 

Analysis of Standards The analysis of a standard containing a known concentration of analyte also can be used to monitor a system s state of statistical control. Ideally, a standard reference material (SRM) should be used, provided that the matrix of the SRM is similar to that of the samples being analyzed. A variety of appropriate SRMs are available from the National Institute of Standards and Technology (NIST). If a suitable SRM is not available, then an independently prepared synthetic sample can be used if it is prepared from reagents of known purity. At a minimum, a standardization of the method is verified by periodically analyzing one of the calibration standards. In all cases, the analyte s experimentally determined concentration in the standard must fall within predetermined limits if the system is to be considered under statistical control. 

The pubHcations detailing standards (5—8) generally include both specifications and methods of analysis for the substances. The estabHshment of standards of quaHty for chemicals of any kind presupposes the abiHty to set numerical limits on physical properties, allowable impurities, and strength, and to provide the test methods by which conformity to the requirements may be demonstrated. Tests are considered appHcable only to the specific requirements for which they were written. Modification of a requirement, especially if the change is toward a higher level of purity, often necessitates revision of the test to ensure the test s vaHdity. 

Direct deterruination of the formamide content by gc methods proves to be inaccurate because of its tendency to decompose at elevated temperatures. This also limits the accuracy of the classical Kjehldahl deterruination. The purity of formamide is, therefore, more reUably deterrnined by analysis of its impurities and substraction of the combined contents from 100%. 

Table 4 lists the specifications set by Du Pont, the largest U.S. producer of DMF (4). Water in DMF is deterrnined either by Kad Fischer titration or by gas chromatography. The chromatographic method is more rehable at lower levels of water (<500 ppm) (4). DMF purity is deterrnined by gc. For specialized laboratory appHcations, conductivity measurements have been used as an indication of purity (27). DMF in water can be measured by refractive index, hydrolysis to DMA followed by titration of the Hberated amine, or, most conveniendy, by infrared analysis. A band at 1087 cm is used for the ir analysis. 

The conventional method for quantitative analysis of galHum in aqueous media is atomic absorption spectroscopy (qv). High purity metallic galHum is characteri2ed by trace impurity analysis using spark source (15) or glow discharge mass spectrometry (qv) (16). 

Analysis of refined germanium products is done in a wide variety of ways, including several methods that have become ASTM standards (47). Electronic-grade Ge02 is analyzed using an emission spectrograph to determine its spectrographic purity. Its volatile content is measured in accord with ASTM F5 and its bulk density with F6. Other ASTM standards cover the preparation of a metal biHet from a sample of the oxide (F27), and the determination of the conductivity type (F42) and resistivity (F43) of the biHet. 

Instmmental methods of analysis provide information about the specific composition and purity of the amines. QuaUtative information about the identity of the product (functional groups present) and quantitative analysis (amount of various components such as nitrile, amide, acid, and deterruination of unsaturation) can be obtained by infrared analysis. Gas chromatography (gc), with a Hquid phase of either Apiezon grease or Carbowax, and high performance Hquid chromatography (hplc), using siHca columns and solvent systems such as isooctane, methyl tert-huty ether, tetrahydrofuran, and methanol, are used for quantitative analysis of fatty amine mixtures. Nuclear magnetic resonance spectroscopy (nmr), both proton ( H) and carbon-13 ( C), which can be used for quaHtative and quantitative analysis, is an important method used to analyze fatty amines (8,81). 

Fig. 2. An SPC control chart of the purity analysis of a reference standard where (—) represents the average value and UCL and LCL are the upper and...

In the sugar industry, where the goal is to determine the exact amount of sucrose present, the analysis of other components is essential to determine purity. The most important of these, besides reducing sugars discussed, are moisture, ash, and color. Also relevant are methods used to determine particle-size distribution and insoluble matter. 

D. I. Ryabchikov, L. L. Na2arenko, and I. P. Alimarin, eBs., Analysis of High Purity Materials, Israel Program for Scientific Information, Jemsalem, 1968. 

Arsenic trioxide may be made by burning arsenic in air or by the hydrolysis of an arsenic trihaUde. Commercially, it is obtained by roasting arsenopyrite [1303-18-0] FeAsS. It dissolves in water to a slight extent (1.7 g/100 g water at 25°C) to form a weaMy acidic solution which probably contains the species H AsO, orthoarsenous acid [36465-76-6]. The oxide is amphoteric and hence soluble in acids and bases. It is frequendy used as a primary analytical standard in oxidimetry because it is readily attainable in a high state of purity and is quantitatively oxidized by many reagents commonly used in volumetric analysis, eg, dichromate, nitric acid, hypochlorite, and inon(III). 

Analysis and purities of the metal or compounds are determined by difference, subtracting the sum of the analyzed levels of all impurities from 100%. Analysis of impurity levels is carried out by the most appropriate technique, which may include spectroscopy, atomic absorption, and photometry. 

Specifications, Analysis, and Toxicity. Dicyandiamide is identified quaHtatively by paper chromatography and quantitatively by ultraviolet spectrometry of the chromatogram. More commonly, total nitrogen analysis is used as a purity control or the dicyandiamide is converted by hydrolysis to guanylurea, which is determined gravimetrically as the nickel salt (50). Methods based on the precipitation of silver dicyandiamide picrate are sometimes used (51). Dicyandiamide can also be titrated with tetrabutylammonium hydroxide ia pyridine solution. Table 4 gives a typical analysis of a commercial sample. Dicyandiamide is essentially nontoxic. It may, however, cause dermatitis. 

The other analytical methods necessary to control the typical specification given in Table 5 are, for the most part, common quality-control procedures. When a chemical analysis for purity is desired, acetylation or phthalation procedures are commonly employed. In these cases, the alcohol reacts with a measured volume of either acetic or phthalic anhydride in pyridine solution. The loss in titratable acidity in the anhydride solution is a direct measure of the hydroxyl groups reacting in the sample. These procedures are generally free from interference by other functional groups, but both are affected adversely by the presence of excessive water, as this depletes the anhydride reagent strength to a level below that necessary to ensure complete reaction with the alcohol. Both procedures can be adapted to a semimicro- or even microscale deterrnination. 

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