Atomic absorption digestion-flame

Acid digestion or extraction, atomic absorption spectrometry (flame, cold vapor, hydride generation, and electrothermal), emission spectroscopy (plasma and flame), spectrophotometry, anodic stripping voltametry... 

Description of Method. Copper and zinc are isolated by digesting tissue samples after extracting any fatty tissue. The concentration of copper and zinc in the supernatant are determined by atomic absorption using an air-acetylene flame. 

Potassium is analyzed in chemicals that are used in the fertilizer industry and in finished fertilizers by flame photometric methods (44) or volumetric sodium tertraphenylboron methods (45) as approved by the AO AC. Gravimetric deterrnination of potassium as K2PtClg, known as the Lindo-Gladding method (46), and the wet-digestion deterrnination of potassium (47) have been declared surplus methods by the AO AC. Other methods used for control purposes and special analyses include atomic absorption spectrophotometry, inductively coupled plasma (icp) emission spectrophotometry, and a radiometric method based on measuring the radioactivity of the minute amount of the isotope present in all potassium compounds (48). 

ASTM. 1998a. ASTME1613. Standard test method for analysis of digested samples for lead by inductively coupled plasma atomic emission spectrometry (ICP-AES). Flame Atomic Absorption (FAAS), or Graphite Furnace Atomic Absorption (GFAA) Techniques. American Society for Testing and Materials. 

Tbe metal may most conveniently be analyzed in tbe aqueous phase by atomic absorption spectrophotometry using flame or a graphite furnace or by ICP emission spectrophotometry at wavelength 206.83 or 217.58 nm. Such measurements are accurate at trace concentration levels. The metal or its ore is digested with hot nitric acid and the acid extract is appropriately diluted and measured. 

Elemental composition Ba 58.89%, Ti 20.53%, O 20.58%. The sobd is digested with a mixture of concentrated H2SO4 and HNO3, diluted and the aqueous solution is analyzed for the metals Ba and Ti by flame or furnace atomic absorption or ICP emission spectrophotometry. The compound in the crystalline powdered form may be identified by various x-ray techniques. 

Cadmium in acidified aqueous solution may be analyzed at trace levels by various instrumental techniques such as flame and furnace atomic absorption, and ICP emission spectrophotometry. Cadmium in solid matrices is extracted into aqueous phase by digestion with nitric acid prior to analysis. A much lower detection level may be obtained by ICP-mass spectrometry. Other instrumental techniques to analyze this metal include neutron activation analysis and anodic stripping voltammetry. Cadmium also may be measured in aqueous matrices by colorimetry. Cadmium ions react with dithizone to form a pink-red color that can be extracted with chloroform. The absorbance of the solution is measured by a spectrophotometer and the concentration is determined from a standard calibration curve (APHA, AWWA and WEF. 1999. Standard Methods for the Examination of Water and Wastewater, 20th ed. Washington, DC American Public Health Association). The metal in the solid phase may be determined nondestructively by x-ray fluorescence or diffraction techniques. 

Manganese in aqueous solution may be analyzed by several instrumental techniques including flame and furnace AA, ICP, ICP-MS, x-ray fluorescence and neutron activation. For atomic absorption and emission spectrometric determination the measurement may be done at the wavelengths 279.5, 257.61 or 294.92 nm respectively. The metal or its insoluble compounds must be digested with nitric acid alone or in combination with another acid. Soluble salts may be dissolved in water and the aqueous solution analyzed. X-ray methods may be applied for non-destructive determination of the metal. The detection limits in these methods are higher than those obtained by the AA or ICP methods. ICP-MS is the most sensitive technique. Several colorimetric methods also are known, but such measurements require that the manganese salts be aqueous. These methods are susceptible to interference. 

Molybdenum may be identified at trace concentrations by flame atomic absorption spectrometry using nitrous oxide-acetylene flame. The metal is digested with nitric acid, diluted and analyzed. Aqueous solution of its compounds alternatively may be chelated with 8—hydroxyquinobne, extracted with methyl isobutyl ketone, and analyzed as above. The metal in solution may also be analyzed by ICP/AES at wavelengths 202.03 or 203.84 nm. Other instrumental techniques to measure molybdenum at trace concentrations include x-ray fluorescence, x-ray diffraction, neutron activation, and ICP-mass spectrometry, this last being most sensitive. 

Rhodium may be analyzed by flame atomic absorption spectrophotometry using the direct air-acetylene flame method. The metal, its oxide and insoluble salts may be solubilized by digesting with sulfuric acid—hydrochloric acid mixture. Rhodium also may by analyzed by ICP-AES and ICP/MS techniques. ICP/MS is the most sensitive method. Also, it may be analyzed by neutron activation analysis. 

Flame atomic absorption spectrometry can be used to determine trace levels of analyte in a wide range of sample types, with the proviso that the sample is first brought into solution. The methods described in Section 1.6 are all applicable to FAAS. Chemical interferences and ionization suppression cause the greatest problems, and steps must be taken to reduce these (e.g. the analysis of sea-water, refractory geological samples or metals). The analysis of oils and organic solvents is relatively easy since these samples actually provide fuel for the flame however, build-up of carbon in the burner slot must be avoided. Most biological samples can be analysed with ease provided that an appropriate digestion method is used which avoids analyte losses. 

Mn(II) and Fe(II) were determined by differential pulse voltammetry (9, 30). The determinations were carried out within a few hours after sampling. Total dissolved and particulate Fe and Mn (after digestion of the particulate matter in a microwave digestion unit with HN03-HC1) were measured by flame or graphite furnace atomic absorption spectrometry. 

In an interlab oratory study involving 160 accredited hazardous materials laboratories reported by Kimbrough and Wakakuwa [28], each laboratory performed a mineral acid digestion on five soils spiked with arsenic, cadmium, molybdenum, selenium and thallium. Analysis of extracts was carried out by atomic emission spectrometry, inductively-coupled plasma mass spectrometry, flame atomic absorption spectrometry and hydride generation atomic absorption spectrometry. 

Evans et al. [98] has described a method for the determination of total copper, iron, manganese and zinc in various plant materials. Organic matter is destroyed by wet oxidation and measurement is made directly upon the sulfuric acid digests by flame atomic absorption spectrophotometry. In the measurement, direct interferences from the inorganic species found in plant... 

Liquid or digested samples are atomized by direct aspiration in a flame atomic absorption (FLAA) instrument or in an electrically heated flameless furnace in a GFAA instrument. 

The optimization of the atomic absorption method of determining metals in particulates found in the air of workplace is described. The Plackett-Burman Youden-Steiner balanced incomplete block designs as well as single-factor experiments were utilized with ten metals Be, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, and Pd. Of the parameters tested, perchloric acid digestion, flame-stoichiometry, and the composition of the calibration standards were the most significant. Perchloric acid affected the recoveries of chromium. This was attributed to the formation of volatile chromylchloride. Flame-related phenomena and interelemental effects were brought under control using lanthanum flame buffer. 

Carbonell, V., de la Guardia, M., Salvador, A., Burguera, J.L., Burguera, M. On-line microwave oven digestion flame atomic absorption analysis of solid samples. Anal. Chim. Acta 238, 417 21 (1990)... 

Haswell, S.J., Barclay, D. On-line microwave digestion of slurry samples with direct flame atomic absorption spectrometric elemental detection. Analyst 117, 117-120 (1992)... 

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