Analysis of Sodium Metal

Analysis of Ammonia A612-R A303 Analysis of Sodium Metal A612-R... 

Mercury Determine as directed in the monograph for Iron, Reduced, but use 2 g of sample and 40 mL of Sodium Citrate Solution in preparing the Sample Solution, and prepare the Diluted Standard Mercury Solution as follows Transfer 4.0 mL of Mercury Stock Solution into a 250-mL volumetric flask, dilute to volume with 1 N hydrochloric acid, and mix (1 mL = 4 ig of Hg). Modify the first sentence of the Procedure to read Prepare a control by treating 1.0 mL of Diluted Standard Mercury Solution (4 p,g Hg) in the same manner. Sieve Analysis Determine as directed under Sieve Analysis of Granular Metal Powders, Appendix IIC. 

Zirconocene 1271 (Equation (64)) containing Zr-Ga bonds has been obtained by the reaction of sodium metal with Cp2ZrCl2 and ArGaCl2 in hexane as deep green-black, air-sensitive crystals.959 X-ray diffraction analysis revealed a Zr-Ga bond length of 2.6350(8) A this distance is compared with a sum of the Ga and Zr covalent radii of 2.850 A. Complex 1271 is isoelectronic with the well-known 18-electron zirconocene dicarbonyl complex, Cp2Zr(CO)2, thus formally a Zr(n) species. 

Fig. 3-147. Simultaneous analysis of alkali metals, alkaline-earth metals, and manganese on IonPac CS10. - Eluent 0.04 mol/L HC1 + 0.004 mol/L 2,3-diaminopropionic acid flow rate 1 mL/min detection suppressed conductivity injection volume 20 pL solute concentrations 5 ppm lithium (1), sodium (2), ammonium (3), potassium (4), and magnesium (5), 10 ppm manganese (6), and calcium (7).

Finally, it should be pointed out that until now the application of ion chromatography to the analysis of heavy and transition metals such as iron, copper, nickel, and manganese in the ppb range in 50% sodium hydroxide solution [96, 97] was not possible. A concentration procedure developed by Kingston et al. [98] is used for the AAS analysis of heavy metals in sea water. It is based on the selective concentration of heavy metals on a macroporous iminodiacetic acid resin, where divalent cations are retained by chelation. Their affinity toward the stationary phase decreases in the order... 

An interesting application of a cation exchanger has been given in relation to trace analysis of sodium-, potassium-, barium-, and strontium chlorides [147]. Metal cations are retained by the cation exchanger. Concentrated HCl run onto the column precipitates NaCl, KCl, BaCh, and SrCh, whereas trace metals present are eluted. 

When the same procedure was carried out with a-alumina and sodium hydroxide, sharp peaks of 3 -sodium aluminate were observed in the X-ray analysis of the intermediate solid. In this case, the final product clearly shows the diffraction peak of sodium metal (20 29.6° ). This catalyst exhibited no cataljrtic activity for the olefin isomerization. 

The major serum electrolytes—sodium, potassium, calcium, magnesium, chloride, and bicarbonate (CO2)—are fairly easy to determine. The metals are most readily determined by the use of fiame-spectrophotometiic or atomic absorption methods, although colorimetric methods exist for calcium and magnesium. Calcium and, less frequently, magnesium are also titrated with EDTA. Ion-selective electrodes are used for the routine analysis of sodium, potassium, and calcium. Bicarbonate is analyzed also by titration against standard acid (see Experiment 8) in addition to a manometric method. Chloride is widely determined by automatic coulometric titration with electrogenerated silver ion. 

Figure 10.355 Analysis of transition metals in 50% sodium hydroxide. Separator column lonPac CS5A eluent 6 mmol/L pyridine-2,6-dicarboxylic acid -i- lOmmol/L NaOH -1-40 mmol/L NaOAc-l-50mmol/L HOAc flow rate 1 mL/min detection photometry at 520nm...

In cases where only one of the reactants is a gas, we do need to use the ideal gas equation in our analysis. Recall, for example, the reaction of sodium metal and chlorine gas used to illustrate the Bom-Haber cycle Section 8.2] ... 

Bouchacourt, M.et d. EdF Experience on Analysis of Non-metallic Impurities in Sodium. Proceedings of the Third International Conference on Liquid Metal Engineering and Technology in Energy Production, Oxford, UK, April 1984, 1,45. 

Rubidium metal is commeicially available in essentially two grades, 99 + % and 99.9 + %. The main impurities ate other alkali metals. Rubidium compounds are available in a variety of grades from 99% to 99.99 + %. Manufacturers and suppliers of mbidium metal and mbidium compounds usually supply a complete certificate of analysis upon request. Analyses of metal impurities in mbidium compounds are determined by atomic absorption or inductive coupled plasma spectroscopy (icp). Other metallic impurities, such as sodium and potassium, are determined by atomic absorption or emission spectrograph. For analysis, mbidium metal is converted to a compound such as mbidium chloride. 

A method suitable for analysis of sulfur dioxide in ambient air and sensitive to 0.003—5 ppm involves aspirating a measured air sample through a solution of potassium or sodium tetrachloromercurate, with the resultant formation of a dichlorosulfitomercurate. Ethylenediaminetetraacetic acid (EDTA) disodium salt is added to this solution to complex heavy metals which can interfere by oxidation of the sulfur dioxide. The sample is also treated with 0.6 wt % sulfamic acid to destroy any nitrite anions. Then the sample is treated with formaldehyde and specially purified acid-bleached rosaniline containing phosphoric acid to control pH. This reacts with the dichlorosulfitomercurate to form an intensely colored rosaniline—methanesulfonic acid. The pH of the solution is adjusted to 1.6 0.1 with phosphoric acid, and the absorbance is read spectrophotometricaHy at 548 nm (273). 

Atomic absorption spectroscopy of VPD solutions (VPD-AAS) and instrumental neutron activation analysis (INAA) offer similar detection limits for metallic impurities with silicon substrates. The main advantage of TXRF, compared to VPD-AAS, is its multielement capability AAS is a sequential technique that requires a specific lamp to detect each element. Furthermore, the problem of blank values is of little importance with TXRF because no handling of the analytical solution is involved. On the other hand, adequately sensitive detection of sodium is possible only by using VPD-AAS. INAA is basically a bulk analysis technique, while TXRF is sensitive only to the surface. In addition, TXRF is fast, with an typical analysis time of 1000 s turn-around times for INAA are on the order of weeks. Gallium arsenide surfaces can be analyzed neither by AAS nor by INAA. 

The general reaction procedure and apparatus used are exactly as described in Procedure 2. Ammonia (465 ml) is distilled into a 2-liter reaction flask and to this is added 165mlofisopropylalcoholandasolutionof30g(0.195 mole) of 17/ -estradiol 3-methyl ether (mp 118.5-120°) in 180 ml of tetrahydrofuran. The steroid is only partially soluble in the mixture. A 5 g portion of sodium (26 g, 1.13 g-atoms total) is added to the stirred mixture and the solid dissolves in the light blue solution within several min. As additional metal is added, the mixture becomes dark blue and a solid (matted needles) separates. Stirring is inefficient for a few minutes until the mass of crystals breaks down. All of the sodium is consumed after 1 hr and 120 ml of methanol is then added to the mixture with care. The product is isolated as in Procedure 4h 2. After being air-dried, the solid weighs 32.5 g (ca. 100% for a monohydrate). A sample of the material is dried for analysis and analyzed as described in Procedure 2 enol ether, 91% unreduced aromatics, 0.3%. The crude product may be crystallized from acetone-water or preferably from hexane. 

Compounds of the same stoichiometry type usually have the same type crystal structure within the row of alkali metals K - Rb - Cs rarely the same type structure with sodium-containing analogues and never ciystallize similarly with lithium-containing compounds. The crystal structure analysis of different fluoride and oxyfluoride compounds clearly indicates that the steric similarity between all cations and tantalum or niobium must be taken into account when calculating the X Me ratio. 

Calcium, iron, magnesium, alkali metals, and citrates do not affect the analysis. Ammonium salts interfere and must be eliminated by means of sodium nitrite or sodium hypobromite. The hydrochloric acid normally used in the analysis may be replaced by an equivalent amount of nitric acid without any influence on the course of the reaction. Sulphuric acid leads to high and erratic results and its use should be avoided. 

Analysis of metallic peroxides. A metallic peroxide, such as sodium peroxide, can be analysed in similar manner, provided that care is taken to avoid loss of oxygen during the dissolution of the peroxide. This may be done by working in a medium containing boric acid which is converted to the relatively stable perboric acid upon the addition of the peroxide. 

The effects of pH on electrokinetic velocities in micellar electrokinetic chromatography was studied by using sodium dodecyl sulfate solutions [179]. Micellar electrokinetic capillary chromatography with a sodium dodecyl sulfate pseudostationary phase has been used to determine the partition constants for nitrophenols, thiazolylazo dyes, and metal chelate compounds [180]. A similar technique was used to separate hydroquinone and some of its ether derivatives. This analysis is suitable for the determination of hydroquinone in skin-toning creams [181]. The ingredients of antipyretic analgesic preparations have also been determined by this technique [182], The addition of sodium dodecyl sulfate improves the peak shapes and resolution in chiral separations by micellar electrokinetic chromatography [183]. 

Hi) Specialized Analytical Methods. Analytical methods for metallic impurities are well documented and are not covered here. A major advance in the continuous monitoring of impurities in liquid sodium down to the lowest levels of detection has been the development of analysis using electrochemical cells. Oxygen analysis in sodium may be carried out using a cell of the type... 

In the case of Kryptofix 221D, a cryptand able to complex the alkali metal cations [141-143], it has been observed that it is solubilized mainly in the palisade layer of the AOT-reversed micelles. And from an analysis of the enthalpy of transfer of this solubilizate from the organic to the micellar phase it has been established that the driving force of the solubilization is the complexation of the sodium counterion. In addition, the enthalpy... 

Fofanov GM, Kitaev GA (1969) Analysis of the conditions for the precipitation of metal selenides from aqueous solutions with sodium selenosulphate. Russ J Inorg Chem 14 322-324... 

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