Sodium samples containing

Description of Method. Salt substitutes, which are used in place of table salt for individuals on a low-sodium diet, contain KCI. Depending on the brand, fumaric acid, calcium hydrogen phosphate, or potassium tartrate also may be present. Typically, the concentration of sodium in a salt substitute is about 100 ppm. The concentration of sodium is easily determined by flame atomic emission. Because it is difficult to match the matrix of the standards to that of the sample, the analysis is accomplished by the method of standard additions. 

Quantitatively, sulfur in a free or combined state is generally determined by oxidizing it to a soluble sulfate, by fusion with an alkaH carbonate if necessary, and precipitating it as insoluble barium sulfate. Oxidation can be effected with such agents as concentrated or fuming nitric acid, bromine, sodium peroxide, potassium nitrate, or potassium chlorate. Free sulfur is normally determined by solution in carbon disulfide, the latter being distilled from the extract. This method is not useful if the sample contains polymeric sulfur. 

FIGURE 7.17 Separation of a complex mixture on Fractogel EMD BioSEC (S) with a column dimension of 1000 X 50 mm (Superformance glass column). The sample contained ferritin (I), immunoglobulin G (2), transferrin (3), ovalbumin (4), myoglobin (5), aprotinin (6), and vitamin B, (7). Five milliliters of the mixture was injected onto the column at a flow rate of 3 ml/min (eluent 20 mAI sodium phosphate buffer, 0.1 M NaCI, pH 7.2). 

A 1.500-g sample containing sodium nitrate was heated to form NaN02 and 02. The oxygen evolved was collected over water at 23°C and 752 mm Hg its volume was 125.0 mL. Calculate the percentage of NaN03 in the sample. The vapor pressure of water at 23°C is 21.07 mm Hg. 

More straightforwardly, the sample may be titrated potentiometrically using hydrochloric acid to two points of inflexion. The first represents sodium hydroxide plus sodium carbonate the second sodium bicarbonate. Clearly there cannot be bicarbonate in the sample if there is sodium hydroxide present. Any second inflexion in this case can be used to determine the carbonate content. Should the titer from the first inflexion to the second be greater than that from start to the first inflexion, then the sample contains only carbonate and bicarbonate. The titer to the first inflexion can be used to estimate carbonate and the difference between twice this titer and the total titer to the second inflexion is a measure of bicarbonate. 

Molar mass is important when we need to know the number of atoms in a sample. It would be impossible to count out 6 X ID23 atoms of an element, but it is very easy to measure out a mass equal to the molar mass of the element in grams. Each of the samples shown in Fig. E.2 was obtained in this way each sample contains the same number of atoms of the element (6.022 X 1023), but the masses vary because the masses of the atoms are different (Fig. E.4). The same rule applies to compounds. Flence, if we measure out 58.44 g of sodium chloride, we obtain a sample that contains 1.000 mol NaCl formula units (Fig. E.5). 

FIGURE E.5 Each sample contains 1 mol of formula units of an ionic compound. From left to right are 58 g of sodium chloride (NaCl), 100 g of calcium carbonate (CaCO,), 278 g of iron(ll) sulfate heptahydrate (FeS04-7H.0), and 78 g of sodium peroxide (Na. O,). 

Le Corre and Treguer [49] developed an automated procedure based on oxidation of the ammonium ion by hypochlorite in the presence of sodium bromide followed by spectrophotometric determination of the nitrite. The standard deviation on a set of samples containing 1 p,g NH -N per litre was 0.02. This method was compared with an automated method for the determination of ammonia as indophenol blue. The results from the two methods are in good agreement. 

In similar work, Sturgeon et al. [125] compared direct furnace methods with extraction methods for cadmium in coastal seawater samples. They could measure cadmium down to 0.1 pg/1. They used 10 pg/1 ascorbic acid as a matrix modifier. Various organic matrix modifiers were studied by Guevremont [116] for this analysis. He found citric acid to be somewhat preferable to EDTA, aspartic acid, lactic acid, and histidine. The method of standard additions was required. The standard deviation was better than 0.01 pg/1 in a seawater sample containing 0.07 pg/1. Generally, he charred at 300 °C and atomised at 1500 °C. This method required compromise between char and atomisation temperatures, sensitivity, heating rates, and so on, but the analytical results seemed precise and accurate. Nitrate added as sodium nitrate delayed the cadmium peak and suppressed the cadmium signal. 

In the indirect amperometric method [560], saturated uranyl zinc acetate solution is added to the sample containing 0.1-10 mg sodium. The solution is heated for 30 minutes at 100 °C to complete precipitation. The solution is filtered and the precipitate washed several times with 2 ml of the reagent and then five times with 99% ethanol saturated with sodium uranyl zinc acetate. The precipitate is dissolved and diluted to a known volume. To an aliquot containing up to 1.7 mg zinc, 1M tartaric acid (2-3 ml) and 3 M ammonium acetate (8-10 ml) are added and the pH adjusted to 7.5-8.0 with 2 M aqueous ammonia. The solution is diluted to 25 ml and an equal volume of ethanol added. It is titrated amperometrically with 0.01 M K4Fe(CN)6 using a platinum electrode. Uranium does not interfere with the determination of sodium. 

Conditions columns, Asahipak GS320 (vinyl alcohol copolymer gel), 50 cm x 7.6 mm i.d. eluent, 0.1 M sodium phosphate containing 0.3 M sodium chloride pH 7.0 flow rate, 1 ml min-1 detection, UV 250 nm direct injection of sample. Peaks l, protein, 2, orotidine 3, creatinine, and 4, uric acid. 

Figure 4.11 Direct injection analysis of haemoglobin in red blood cells. Column, Asahipak ES-502C eluent, 32 min linear gradient from 25% 30 mM sodium phosphate buffer to 65% 30 mM sodium phosphate containing 300 mM sodium chloride pH 5.5 flow rate, 1.0 ml min-1 detection, 425 nm. Samples. A, normal subject and B, diabetic patient.

Figure 12.1 Clearance of small-molecule impurities from process buffers in a formulated protein product. Trace A the NMR spectrum of a control sample containing a mixture of three components (succinate, tetraethylammonium, and tetramethylammonium) in the final formulation buffer (sodium acetate). These three components were used in the recovery process for a biopharmaceutical product. Traces B and D the proton NMR spectra of the formulated protein product. No TEA or TMA were detected, but a small amount of succinate was observed in this sample. Traces C and E the proton NMR spectra of a formulated protein product spiked with 10 jag/ml of succinate, TEA, and TMA. Traces D and E were recorded with CPMG spin-echo method to reduce the protein signals. The reduction of NMR signals from the protein allows for better observation of the small-molecule signals.

Throughout this discussion, we have been considering pure substances, i.e. substances composed of a single material, whether element or compound. A compound may be molecular or ionic, or both. A compound is a single chemical substance. To anticipate slightly, sodium chloride is an ionic compound that contains two atomic species, Na" and d . If a sample of sodium chloride is formally manipulated to remove some Cl ions and replace them by Br ions in equivalent number, the resultant material is a mixture. The same is true of a sample containing neutral species such as P4, Sg and CsHg. 

S.2.2.2 ICLS Example 2 This example discusses the determination of sodium hydroxide (caustic) concentration in an aqueous sample containing sodium hydroxide and a salt using NIR spearoscopy. An example of this problem in a chemical process occurs in process scrubbers where CO, is converted to Na,CO and H,S is converted to Na,S in the presence of caustic. Although caustic and salts have no distinct bands in the NIR, it has been demonstrated that they perturb the shape of the water bands (Watson and Baughman, 1984 Phelan et al., 1989)-Near-infrared spectroscopy is therefore a viable measurement technique. This method also has ad tages as an analytical technique for process analysis because of the stability of the instrumentation and the ability to use fiber-optic probes to multiplex tlie interferometers and Icx ate them rcm< >tely from the processes. 

Two polarographic methods have been developed for the determination of cohalt(II) at concentrations ranging from approximately 1 to 80 mM in an aqueous sample. For the first method [15], which is suitable for samples containing large amounts of nickel]11), the cobalt(II) is oxidized to Co(NH3)6 in an ammoniacal medium with the aid of sodium perborate, after which the cobalt(III) species is determined. A second procedure [16] entails the use of lead dioxide in an acetic acid-acetate buffer containing oxalate to convert cobalt(II) to the 0(0204)3 ion, which can be subjected to polarographic reduction. This latter approach is well suited to the determination of cobalt in the presence of copper(II), iron(III), nickel(II), tin(IV), and zinc(II), whereas the chief interferences are cerium, chromium, manganese, and vanadium. 

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