Alkali metals, sampling

The alkali-metal sample ions were converted to the highly conducting metal hydroxide, e.g.. 

Analytical methods to determine carbon in the light alkali metals have to be highly sensitive, as there are only very low concentrations present in the molten metals. Therefore, monitoring of the chemical activities of carbon seems to be more favourable than the classical analysis of combustion and determination of the carbon dioxid evolved. This method is based oh an analytical vacuum distillation of the dissolving alkali metal samples collected in alumina crucibles. The sensitivity of the method is not sufficient to estimate the carbon contents in unsaturated solutions of carbon in lithium or sodium. The hydrolysis and evolution of acetylene has also been applied for the estimation of the lithium acetylide contents. This method may be disturbed by side reactions, which occur in the presence of higher amounts of nitrogen. 

Whereas the emission spectrum of the hydrogen atom shows only one series, the Balmer series (see Figure 1.1), in the visible region the alkali metals show at least three. The spectra can be excited in a discharge lamp containing a sample of the appropriate metal. One series was called the principal series because it could also be observed in absorption through a column of the vapour. The other two were called sharp and diffuse because of their general appearance. A part of a fourth series, called the fundamental series, can sometimes be observed. 

The chemical resistance of PTFE is exceptional. There are no solvents and it is attacked at room temperature only by molten alkali metals and in some cases by fluorine. Treatment with a solution of sodium metal in liquid ammonia will sufficiently alter the surface of a PTFE sample to enable it to be cemented to other materials using epoxide resin adhesives. 

Other possibilities are the reduction of nitro groups by applying the sample solutions to adsorbent layers containing zinc dust and then exposing to hydrochloric acid vapors [110] 3,5-Dinitrobenzoates and 2,4-dinitrophenylhydrazones can also be reduced in the same way on tin-containing silica gel phases [111] Cellulose layers are also suitable for such reactions [112] Seiler and Rothweiler have described a method of trans-salting the alkali metal sulfates to alkali metal acetates [113]... 

Doping of alkali-metals into CNTs has been examined [11]. The X-ray powder diffraction (XRD) patterns of the K- or Rb-doped CNTs show that alkali-metals are intercalated between the CNT layers. The hexagonal unit cell is essentially the same as that of the stage-1 alkali-metal intercalated graphite ACg (A=K, Rb). For a sample doped with Rb, the observed lattice parameter of the perpendicular... 

Reviews of analytical methods for impurities in alkali metals are largely devoted to Na and K owing to their use as liquid coolants in fast-breeder nuclear reactors ". These methods may be extended to Rb and Cs except the analysis for oxygen. In analytical work with the alkali metals, care is necessary during sampling and handling to avoid contamination in transit. The impurities usually considered are O, C, N, H and metals. 

The relatively impure crude Ca obtained from both thermal reduction and electrolytic sources (97-98%) is distilled to give a 99% pure product. Volatile impurities such as the alkali metals are removed in a predistillation mode at 800°C subsequent distillation of the bulk metal at 825-850°C under vacuum removes most of the involatile impurities, such as Al, Cl, Fe and Si. The N content is often not reduced because of atmospheric contamination after distillation. Unfortunately, these commercial methods have no effect on Mg, which is the major impurity (up to 1 wt%). Typical analytical data for Ca samples prepared by electrolysis, thermal reduction (using Al) and distillation are collated in Table 1. 

The first column of the periodic table, Group 1, contains elements that are soft, shiny solids. These alkali metals include lithium, sodium, potassium, mbidium, and cesium. At the other end of the table, fluorine, chlorine, bromine, iodine, and astatine appear in the next-to-last column. These are the halogens, or Group 17 elements. These four elements exist as diatomic molecules, so their formulas have the form X2 A sample of chlorine appears in Figure EV. Each alkali metal combines with any of the halogens in a 1 1 ratio to form a white crystalline solid. The general formula of these compounds s, AX, where A represents the alkali metal and X represents the halogen A X = N a C 1, LiBr, CsBr, KI, etc.). 

Next, a series of runs was conducted to determine the effect of various alkali metal hydroxide additions along with the sponge nickel catalyst. The 50 wt. % sodium hydroxide and 50 wt. % potassium hydroxide caustic solution used in the initial test was replaced with an aqueous solution of the alkali metal hydroxide at the level indicated in Table 2. After the reaction number of cycles indicated in Table 2, a sample was removed for analysis. The conditions and results are shown in Table 2. The results reported in Table 2 show the level of 2° Amine in the product from the final cycle. The level of NPA in all of the mns was comparable to the level observed in the initial test. No significant levels of other impurities were detected. 

The experimental system for measuring the sonoluminescence spectrum of alkali-metal atom emission from an aqueous solution is similar to that for measuring the MBSL spectrum from water. Degassing the solution is an important procedure because the presence of dissolved air affects the emission intensity. In an air-saturated solution, no observation of alkali-metal atom emission has been reported, whereas continuum emission can be observed. A typical experimental apparatus using ultrasonic standing waves is shown in Fig. 13.3 [8]. The cylindrical sample container is made of stainless steel, and its size is 46 mm in diameter and 150 mm in... 

To test this approach, 5 g samples -300 mesh Tyler, of a low-rank vitrinite, were stirred for 6 hrs in liquid ammonia (150 ml -33°C) containing 5 gms of potassium amide and 5 g of sodium amide. (The amides were formed in the medium, before introducing the coal, by action of anhydrous ferric oxide (1 g) or ferric chloride (1.5 g) on alkali metals.) Thereafter, 100 ml of anhydrous ethyl ether was added, the suspended coal material ethylated with C2H5Br (32 ml), and the reaction mixture stirred until all ammonia and ether had evaporated. Following... 

Like tetrasulfur tetranitride, salts of trisulfur trinitride and of pentasulfur tetran-itride (particularly alkali-metal salts) are heat- and friction-sensitive explosives. Preparation on a scale limited to 1 g, and care in use of spatulae or in preparation of samples for IR examination is recommended. 

Orren [663] used atomic absorption spectrometry to determine these elements in seawater in both their soluble and insoluble forms. The alkali metals are determined directly, but the other elements are first concentrated by solvent extraction. The particulate matter content is derived by dissolving the membranes used to filter the sample and determine the metals in the resulting solution. For organic standards of known metal content, the efficiency of the technique was almost 100%. 

Greenberg and Kingston [821,822] used a solid Chelex 100 resin to preconcentrate these elements from 100-500 ml of estuarine and seawater prior to their determination. A procedure is described for the preconcentration of 100 ml of estuarine and seawater into a solid sample using Chelex 100 resin. This solid sample weighs less than 0.5 g, and contains the transition metals and many other elements of interest, but is essentially free of alkali metals, alkaline earth metals, and halogens. 

A second type of interference is ionization interference. Certain elements, particularly the alkali metals in high temperature flames, become partially ionized in the flame. This event causes a decrease in the number of neutral atoms and hence, a decrease in the sensitivity. For example, an appreciable fraction of sodium atoms will be ionized. Now if another easily ionized element such as potassium is added to the sodium solution, it will contribute free electrons to the flame and cause the equilibrium for the sodium ionization to shift toward the formation of a larger fraction of neutral atoms. This is, therefore, a positive interference. It can be overcome by adding the same amount of interfering element to the standard solution. Or, more simply, a large amount of an ionizable element such as potassium (200 to 1000 ppm) can be added to both sample and standard solutions this will effectively suppress ionization to a small and constant value and at the same time increase the sensitivity. 

A similar type of catalyst including a supported noble metal for regeneration was described extensively in a series of patents assigned to UOP (209-214). The catalysts were prepared by the sublimation of metal halides, especially aluminum chloride and boron trifluoride, onto an alumina carrier modified with alkali or rare earth-alkali metal ions. The noble metal was preferably deposited in an eggshell concentration profile. An earlier patent assigned to Texaco (215) describes the use of chlorinated alumina in the isobutane alkylation with higher alkenes, especially hexenes. TMPs were supposed to form via self-alkylation. Fluorinated alumina and silica samples were also tested in isobutane alkylation,... 

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