Dissolving the Sample

The solvent chosen must dissolve the sample, yet be relatively transparent in the spectral region of interest. In order to avoid poor resolution and difficulties in spectrum interpretation, a solvent should not be employed for measurements that are near the wavelength of or are shorter than the wavelength of its ultraviolet cutoff, that is, the wavelength at which absorbance for the solvent alone approaches one absorbance unit. Ultraviolet cutoffs for solvents commonly used are given in Table 7.10. 

When working with a solid sample, it often is necessary to bring the analyte into solution by dissolving the sample in a suitable solvent. Any solid impurities that remain are removed by filtration before continuing with the analysis. 

After dissolving the sample in a beaker, remove any solid impurities by filtering a portion of the solution containing the analyte. Collect and discard the first several milliliters of solution before collecting a sample of approximately 5 mL for further analysis. 

Analytical chemistry is more than a collection of techniques it is the application of chemistry to the analysis of samples. As you will see in later chapters, almost all analytical methods use chemical reactivity to accomplish one or more of the following—dissolve the sample, separate analytes and interferents, transform the analyte to a more useful form, or provide a signal. Equilibrium chemistry and thermodynamics provide us with a means for predicting which reactions are likely to be favorable. 

Because of the risk of lead poisoning, the exposure of children to lead-based paint is a significant public health concern. The first step in the quantitative analysis of lead in dried paint chips is to dissolve the sample. Corl evaluated several dissolution techniques. " In this study, samples of paint were collected and pulverized with a Pyrex mortar and pestle. Replicate portions of the powdered paint were then taken for analysis. Results for an unknown paint sample and for a standard reference material, in which dissolution was accomplished by a 4-6-h digestion with HNO3 on a hot plate, are shown in the following table. 

Dissolve the sample in about 100 mL of H2O, and then dilute to the mark. Using a pipet, transfer a 25-mL aliquot of this solution to a 125-mL Erlenmeyer flask, and add 25-mL of H2O and 2 drops of bromocresol green indicator. Titrate the sample with 0.1 M HCl to the indicator s end point. 

When an analyte is too concentrated, it is easy to overload the column, thereby seriously degrading the separation. In addition, the analyte may be present at a concentration level that exceeds the detector s linear response. Dissolving the sample in a volatile solvent, such as methylene chloride, makes its analysis feasible. 

The syndiotactic polymer configuration is not obtained in pure form from polymerizations carried out above 20°C and, thus has not been a serious concern to most propylene polymerization catalyst designers. Eor most commercial appHcations of polypropylene, a resin with 96+% isotacticity is desired. Carbon-13 nmr can be used to estimate the isotactic fraction in a polypropylene sample. Another common analytical method is to dissolve the sample in boiling xylene and measure the amount of isotactic polymer that precipitates on cooling. 

Some samples were obtained with melting points ranging from 77° to 93°, but on dissolving the samples in chloroform and evaporating the solvent the values rose to 100-102°. This is not believed to be a process of purification. 

Select mobile phases for HPSEC based on their ability to dissolve the sample and their compatibility with the column. Zorbax PSM columns are compatible with a wide variety of organic and aqueous mobile phases (Table 3.4), but analysts should avoid aqueous mobile phases with a pH greater than 8.5. As mentioned earlier, select mobile phases that minimize adsorption between samples and silica-based packings. Sample elution from the column after the permeation volume indicates that adsorption has occurred. If adsorption is observed or suspected, select a mobile phase that will be more strongly adsorbed onto the silica surface than the sample. For example, N,N-dimethyl-formamide (DMF) is often used for polyurethanes and polyacrylonitrile because it eliminates adsorption and dissolves the polymers. When aqueous mobile phases are required, highly polar macromolecules such as Carbowax can be used to coat the silica surface and eliminate adsorption. Table 3.5 provides a list of recommended mobile-phase conditions for some common polymers. 

There is increasing interest in copolymer systems, which, due to their chemical heterogeneity, may require very complex eluent systems in order to dissolve the sample and ensure that the separation ensues hy a pure size exclusion mechanism. In these examples, the PLgel is also compatible with eluent systems containing mixed solvents of different polarity (including water as a cosolvent up to 10% hy volume) and in organic solvents modified with acids or bases (e.g., acetic or formic acid, triethanolamine) as it is stable in the pH range of 1-14. 

Procedure. Dissolve the sample in distilled water and take an aliquot which should contain not more than 50 pg of phenolic compound. Use the aqueous ammonia to adjust the pH of the solution to 9.7-10.3 (pH meter), and then dilute to 500 mL with distilled water. Transfer the solution to a large separatory funnel, add 1.0 mL of solution A followed by 10 mL of solution B. Shake well to ensure thorough mixing, and then carry out three extractions with successive portions of 15 mL, 10 mL and 5 mL of chloroform (trichloromethane). Combine the chloroform extracts and make up the volume to 30 mL. Measure the absorbance of the extract against a blank of chloroform at a wavelength of 460 nm (blue filter), using 1 cm cells. The colour may tend to fade after 10 minutes and so speed is essential. 

Acrylamide impurities (dissolve the sample in a minimum amount of methanol) also separate formamide, acetamide, dimethylformamide, jV-methylacetamide, propionamide, N,N-dimethylacetamide... 

The procedure for determination of neutral oils in AOS measures petroleum spirit-extractable material from an aqueous alcoholic solution. Normally a solution of 1 1 ethanol/water is used as to dissolve the sample prior to extraction. For higher molecular weight materials 2 1 propan-2-ol/water is preferred. The petroleum ether is removed on a steambath and finally under vacuum. The amount of neutral oil is then determined gravimetrically. Due to the slight volatility of alkenes, alkanes, and alcohols, especially in the C,2 materials, the neutral oil tends to be underestimated by these procedures. 

Precondition a Cig (EC) SPE column (l-g/6-mL) with methanol (5mL) followed by another 5 mL of acetonitrile-water (3 7, v/v). Transfer the sample on to the column and allow it to percolate through the column under vacuum, discarding the column eluate. Wash the column with 5 mL of acetonitrile-water (3 7, v/v). Dry the column under high vacuum for 15 min and wash it with hexane (5 mL). Elute the azoxystrobin from the column with 5 mL of ethyl acetate-dichloromethane (11 9, v/v), and evaporate the eluate to dryness under a stream of air in a heating block at 50 °C. Dissolve the sample in 1 mL of acetonitrile-water (1 1, v/v) and filter the solution through a 0.45-p.m syringe filter, transferring the filtrate to an autosampler vial ready for LC/MS/MS analysis. 

A common technique used for polyolefin samples is to dissolve the sample using solvents such as xylene, decalin, toluene and di- or trichlorobenzene heated to temperatures as high as 130-150°C. After the plastic sample has been solvated, the polymeric component is precipitated by cooling and/or by adding a cold nonsolvent such as acetone, methanol or isopropanol. Polypropylene does not completely dissolve in toluene under reflux for 0.5 to 1 h with magnetic stirring (typically, 2g of polymer in 40 mL of toluene), yet the additives may be extracted [603]. In addition to additives, most solvents also extract some low-MW polymer with subsequent contamination of the extract. To overcome this a procedure for obtaining polymer-free additive extracts from PE, PP and PS has been described based on low-temperature extraction with n-hexane at 0°C [100],... 

Metal derivatives (Ti, Zn, Cd, Sn, Sb, Pb) and bromine from additives in recycled thermoplasts from consumer electronic waste were determined by dissolving the samples in an organic solvent, followed by TXRF analysis [56], The procedure proved considerably less time-consuming than conventional digestion of the polymer matrix. Results were validated independently by INAA. 

The Association of Official Analytical Chemists is utilizing atomic absorption spectroscopy for the determination of several trace elements. McBride 274>27s), has conducted collaborative and ruggedness studies for a number of elements in fertilizers. He dissolves the sample in hydrochloric acid, filters, and dilutes to vo-... 

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