Graphite analyser

Electrodes. For arc and spark analyses, graphite electrodes are commonly used as sample and counter electrodes some standardized electrode shapes are presented in Figure 11.4 [11]. The purity of these electrodes must be high, and most suppliers provide a quantitative DC-arc analysis for at least 15 elements with each box of electrodes. Electrodes are generally guaranteed to have a total ash content of less than 1 ppm, a maximum allowable impurity per element of 2 ppm, and total maximum impurities of 6 ppm. 

Einely divided samples may be identified further by analyses of the graphite ash, and identification of the minerals associated with the graphite and comparison with graphites from known sources. Owing to its softness and opaqueness, most of the graphitic carbon must be removed from the sample before analysis by either method. There are two general ways of accomplishing this. 

On the other hand, TED patterns can assign the fine structure. In general, the pattern includes two kinds of information. One is a series of strong reflexion spots with the indexes of (00/), 002, 004 and 006, and 101 from the side portions of MWCNTs as shown in Eig. 1(b). The indexes follow those of graphite. The TED pattern also includes the information from the top and bottom sheets in tube. The helieity would appear as a pair of arcs of 110 reflexions. In the case of nano-probed TED, several analyses in fine structures have been done for SWCNT to prove the dependence on the locations [11,12]. 

The solution of the sample to be analysed (1-100 pL) is introduced by inserting the tip of a micropipette through a port in the outer (water) jacket, and into the gas inlet orifice in the centre of the graphite tube. The graphite cylinder is then heated by the passage of an electric current to a temperature... 

Another point of contention has been the extent to which, if any, SbFj is reduced to SbFs upon intercalation. Although chemical analyses have shown an F Sb ratio of 5 1 (Lll, M5), Sb Mossbauer measurements (B24) indicated partial reduction of Sb(V) to Sb(III). On the other hand, mass-spectral measurements as a function of temperature (S15) showed only SbFs, evolved in stages, with no fluorocarbons emitted at any time. The latter are usually an indication of partial reduction of the intercalant and fluorination of the graphite host. Wide-line, F-NMR chemical-shifts are consistent with either SbFj or SbFe, but not with SbFs, but the occurrence of fluorine exchange could produce minor amounts of trivalent species (FI 1) this point is thus still controversial, and will be alluded to again. 

The second analytical method uses a combustion system (O Neil et al. 1994) in place of reaction with BrF,. This method was used for the crocodiles because they were represented by very thin caps of enamel. The enamel was powdered and sieved (20 mg), pretreated in NaOCl to oxidize organic material and then precipitated as silver phosphate. Approximately 10-20 mg of silver phosphate were mixed with powdered graphite in quartz tubes, evacuated and sealed. Combustion at 1,200°C was followed by rapid cooling in water which prevents isotopic fractionation between the CO2 produced and the residual solid in the tube. Analyses of separate aliquots from the same sample typically showed precisions of 0.1%o to 0.4%o with 2 to 4 repetitive analyses even though yields are on the order of 25%. 

TEM-EDS and XPS analyses were conducted on Co/MgO catalysts. The results of surface analyses showed that Co metal is not supported on the MgO as particles, but covers MgO surface in the case of 12 wt.% Co/MgO calcined at 873 K followed by reduction. After the reduction of catalyst at 1173 K, both cobalt oxide and CoO-MgO solid solution are observed on the surface of catalyst. In the steam reforming of naphthalene, two types of coke deposited on the surface of catalyst are observed. These are assigned to film-like and graphite type carbon by TPO analysis. 

Aqueous standard solutions are a source of certain difficulties In electrothermal atomic absorption spectrometry of trace metals In biological fluids The viscosities and surface tensions of aqueous standard solutions are substantially less than the viscosities and surface tensions of serum, blood and other proteln-contalnlng fluids These factors Introduce volumetric disparities In pipetting of standard solutions and body fluids, and also cause differences In penetration of these liquids Into porous graphite tubes or rods Preliminary treatment of porous graphite with xylene may help to minimize the differences of liquid penetration (53,67) A more satisfactory solution of this problem Is preparation of standards In aqueous solutions of metal-free dextran (50-60 g/llter), as first proposed by Pekarek et al ( ) for the standardization of serum chromium analyses This practice has been used successfully by the present author for standardization of analyses of serum nickel The standard solutions which are prepared In aqueous dextran resemble serum In regard to viscosity and surface tension Introduction of dextran-contalnlng standard solutions Is an Important contribution to electrothermal atomic absorption analysis of trace metals In body fluids. 

Danielson et al. [119] have described a method for the determination of cadmium in seawater. The samples were analysed by graphite furnace atomic... 

Klinkhammer [432] has described a method for determining manganese in a seawater matrix at concentrations ranging from about 30 to 5500 ng/1. The samples are extracted with 4 nmol/1 8-hydroxyquinoline in chloroform, and the manganese in the organic phase is then back-extracted into 3 M nitric acid. The manganese concentrations are determined by graphite furnace atomic absorption spectrophotometry. The blank of the method is about 3.0 ng/1, and the precision from duplicate analyses is 9% (1 SD). 

When the samples were returned to the laboratory the pH was adjusted to approximately pH 8 using concentrated ammonia (Ultrapure, G. Frederick Smith). Chelating cation exchange resin in the ammonia form (20 ml Chelex 100,100 - 200 mesh, Bio-Rad) was added to the samples and they were batch extracted on a shaker table for 36 hours. The resin was decanted into columns, and the manganese eluted using 2N nitric acid [129]. The eluant was then analysed by graphite furnace atomic absorption spectrophotometry. Replicate analyses of samples indicate a precision of about 5%. 

The sensitivity achieved should enable seawater samples to be analysed for molybdenum, because the concentration of molybdenum in seawater is usually 2.1 -18.8 pg/1. The selected temperature of 1700-1850 °C during the charring stage permits separation of the seawater matrix from the analyte prior to atomisation with the Perkin-Elmer Model 603 atomic absorption spectrometer equipped with a heated graphite atomiser (HGA-2100). 

The concentration of nickel in natural waters is so low that one or two enrichment steps are necessary before instrumental analysis. The most common method is graphite furnace atomic absorption after preconcentration by solvent extraction [122] or coprecipitation [518]. Even though this technique has been used successfully for the nickel analyses of seawater [519,520] it is vulnerable to contamination as a consequence of the several manipulation steps and of the many reagents used during preconcentration. 

The flow injection AAS system with online preconcentration will challenge the position of the graphite furnace technique, because it yields comparable sensitivity at much lower cost by using simpler apparatus and separation mode. The method offers unusual advantages when matrices with high salt content (e.g., seawater) are analysed, because the matrix components do not reach the nebuliser. 

The samples were analysed by injecting 25 pi aliquots into an HGA 2000 Perkin-Elmer graphite furnace attached to a Jarrell-Ash 82-800 double beam atomic absorption spectrophotometer. Graphite tubes in the furnace were replaced after 75-100 analyses. Metal concentrations were determined by comparing the peak heights of the samples to the standard curve established by the determination of at least five known standards. The detection Emits of this technique for 1% absorption were 0.9 pmol/1 (Fe), and 0.2 pmol/1 (Mn). The coefficient of variation was 11% at 6.5 pmol/1 for iron and +12% at 11.8 pmol/1 for manganese. 

Bruland et al. [122] have shown that seawater samples collected by a variety of clean sampling techniques yielded consistent results for copper, cadmium, zinc, and nickel, which implies that representative uncontaminated samples were obtained. A dithiocarbamate extraction method coupled with atomic absorption spectrometry and flameless graphite furnace electrothermal atomisation is described which is essentially 100% quantitative for each of the four metals studied, has lower blanks and detection Emits, and yields better precision than previously published techniques. A more precise and accurate determination of these metals in seawater at their natural ng/1 concentration levels is therefore possible. Samples analysed by this procedure and by concentration on Chelex 100 showed similar results for cadmium and zinc. Both copper and nickel appeared to be inefficiently removed from seawater by Chelex 100. Comparison of the organic extraction results with other pertinent investigations showed excellent agreement. 

Hayase et al. [684] first extracted the seawater sample with chloroform to remove dissolved organic matter prior to analysis of the aqueous phase by graphite furnace atomic absorption spectrometry. Seawater samples at pH 3 and at pH 8 were extracted with chloroform, evaporated to dryness, and the residue treated with nitric acid. Acid solutions were subjected to metal analyses by graphite furnace atomic absorption spectrometry. 

---