Determination of lead in household refuse fly-ash by X-ray fluorescence spectrometry and a modified standard-addition technique

Lead in fly-ash from a garbage incinerator has been determined by X-ray fluorescence spectrometry (XRFS) and a modified standard-addition method. To keep the attenuation properties of the spiked samples constant, decreasing amounts of an attenuation modifier [mercury (II) acetate] were added together with increasing amounts of the standard (lead nitrate). Linearity between fluorescence intensity and amount of lead was thus obtained, so the amount of lead in the sample could be evaluated by linear regression. The amount of modifier needed could be calculated from a simple expression. The method was validated by comparison with the results obtained by applying atomic-absorption spectrometry (AAS) to solutions made by leaching the fly-ash with strong acid. For 8 fly-ash samples, containing between 0.8 and 1.35% lead, the largest absolute difference between the two sets of results was 0.03%. Theoretical calculations based on a simplified version of the Sherman equation were performed to confirm the linearity of the modified standard-addition curves.     

Determination of thallium in cadmium and lead by graphite-furnace atomic-absorption spectrometry with sample vaporization from a platform

When the sample is vaporized from the wall of a graphite furnace it is not possible to determine thallium in cadmium and lead by AAS without matrix matching of the standards. In the case of a lead matrix and vaporization from the wall, the thallium signal is barely distinguishable from the base-line. When the sample is vaporized from a platform, and the peak area is used for measurement, pure aqueous standards may be used for instrument calibration. The peak heights and areas of the thallium signals are considerably enhanced by vaporization from a platform (peak height 1.7-fold and peak area 2.6-fold in pure aqueous solutions as compared to vaporization from the wall). The enhancement factors are larger in presence of the cadmium or lead matrix since here the reduced interference also makes a contribution.     

Determination of total sulphur in coal by x-ray fluorescence spectrometry

A precise x-ray fluorescence method for the determination of sulphur in coat. The sample is mixed with calcium oxide and active carbon and is gradually heated to 900°C. After coding, lithium tetraborate and lead oxide are added and a prepared. The Pb M_α line is used as an internal standard for the KK_α line. The results for coal have a relative standard deviation of approximately 1% and exhibit.     

Determination of cadmium and lead in urine and other biological samples by graphite-furnace atomic-absorption spectrometry

A method for determining cadmium and lead in urine and other biological samples by graphite-furnace atomic-absorption spectrometry is reported. Samples were analysed after wet or dry ashing and without extraction or matrix-modification techniques, in laminar-flow clean-room; negligible blank contributions were found. Matrix interference effects were observed only for lead and were resolved by the method of standard additions. Five NBS biological reference materials were used as internal quality-control standards. The urinary levels for non-exposed volunteers ranged from 0.16 +/- 0.01 to 1.65 +/- 0.20 and from 6 +/- 1 to 31 +/- 6 ng/ml for cadmium and lead, respectively; this corresponds to 0.15 +/- 0.02 to 2.01 +/- 0.16 and 7 +/- 1 to 31 +/- 3 mug/day. The average relative standard deviation for 60 urine samples was 10% for cadmium and 13% for lead.     

Determination of lead in carbonate rocks by carbon-furnace atomic-absorption spectrometry after dissolution in nitric acid

A simple and rapid method for the determination of 1-100 ppm of lead in carbonate rocks is described. Dissolution of the rock samples in 10% v v nitric acid is shown to give precise and accurate results even though silicates in the samples remain undissolved. A more time-consuming but complete dissolution of the sample with hydrofluoric acid may be used if preferred. The increase in sensitivity and freedom from matrix interference obtained by the use of a carbon-furnace atomizer eliminate the necessity for preconcentration of the lead, saving time and preventing errors from contamination or losses derived from inefficient extraction procedures. The detection limit and precision of the method are 0.4 ppm and 6% (relative standard deviation at the 3-ppm lead level) respectively and accurate results were obtained for the analysis of standard rock samples.     

Determination of germanium by graphite-furnace atomic-absorption spectrometry

The premature loss of germanium as volatile GeO results in low sensitivity and poor reproducibility in the determination of germanium by graphite-furnace atomic-absorption spectrometry. This interference can be eliminated by suppressing the premature reduction of GeO(2) to GeO during the ashing step, and dissociating the germanium oxides into the atoms simultaneously with their vaporization during the atomization step. The premature reduction of GeO(2) to GeO has been successfully prevented by several approaches: (1) diminishing the reducing activity of the graphite furnace by (a) oxidizing the graphite surface and intercalating oxygen into the graphite lattice with oxidizing acids, such as nitric or perchloric, in the sample solution, or (b) using a tantalum-treated graphite furnace; (2) keeping the analyte as germanium (IV) by addition of sodium or potassium hydroxide to the sample solutions.     

Determination of tin in lead/tin solder leachates from copper piping by graphite platform furnace atomic-absorption spectrometry

A stabilized-temperature platform furnace/atomic-absorption spectrophotometric(STPF-AAS) method has been developed for the determination of tin leached from lead/tin-soldered copper pipes. The method involves the use of a modifier composed of diammonium hydrogen phosphate, magnesium nitrate and nitric acid. Aqueous tin standards in the composite matrix modifier are used for calibration. The characteristic mass and detection limit (three standard deviations of the blank) for peak-height measurement of tin are 5 pg and 1.7 microgl., respectively. The corresponding peak-area values are 26.8 pg and 12.8 microgl., respectively. The accuracy, precision, and interferences (especially of sulphate) have been assessed.     

Determination of lead in stainless steel by atomic-absorption spectroscopy

A method has been developed for the determination of lead in stainless steels by atomic-absorption spectrometry after removal of iron by solvent extraction and volatilization of chromium as chromyl chloride. The method proposed is suitable for the determination of lead in the range from 5 to 100 ppm.     

Determination of lead in propellant samples by atomic-absorption spectrophotometry

A procedure is described for the determination of lead in different types of propellant samples by atomic-absorption spectrophotometry. The method is simple, rapid and avoids the use of strong acids and prior sample digestion. Complete lead extraction is achieved with 10% acetic acid. The results obtained by the proposed method are compared with those obtained by the gravimetric chromate method. The variation of the efficiency of lead extraction with sample type is discussed.     

Determination of trace metals in water using x-ray fluorescence spectrometry

A simple, rapid and accurate method for water analysis is proposed. The analytical procedure for the determination of Fe, Mn, Zn, Cu, Cd, As, Pb and Se in water in concentrations as low as a few ppM involves precipitation with a carrier of the metals by diethyldithiocarbamate (DDTC) or 1-(2-pyridylazo)-2-naphthol (PAN) and filitration through a Millipore filter. The precipitates collected on the filter disc are examined by X-ray fluorescence analysis. PAN is excellent for the determination of several metal ions at the ppM level, and DDTC can be used with tartrate as a masking agent if water samples contain large amounts of iron(III).     

Determination of arsenic, cadmium, lead and selenium in highly mineralized waters by graphite-furnace atomic-absorption spectrometry

A graphite-furnace AAS method using the stabilized-temperature platform furnace (STPF) concept, mixed palladium and magnesium nitrates as chemical modifier and Zeeman background correction has been applied to the direct determination of As, Cd, Pb and Se in highly mineralized waters used for medicinal purposes. These contain 20-40 g/l. concentrations of salts, mainly sodium and magnesium chlorides, bicarbonates and sulphates. The use of a pre-atomization cool-down step to 20 degrees in the graphite-furnace programme reduced the background absorption. Increasing the mass of magnesium nitrate modifier to 5 times that originally proposed improved the analyte peak shape. Under these conditions, no interference was found in analysis of the chloride/bicarbonate type of water, but the sodium and magnesium sulphate type of water had to be diluted, and even then an interference remained. Calibration with matrix-free standard solutions was used, but use of spike recovery is strongly recommended for testing the accuracy. The limits of determination (4.65sigma) of the proposed method for undiluted samples are 2.0 mug/l. for As, 0.05 mug/l. for Cd, 1.0 mug/l. for Pb and 1.5 mug/l. for Se.     

Determination of gold in silver, copper, lead, selenium and anode slime by atomic-absorption spectrometry

A simple and sensitive combined solvent-extraction and atomic-absorption spectrometric method has been developed for the determination of gold in silver, copper, lead, selenium and anode slime. Samples are decomposed with hydrochloric and nitric acids, and gold is extracted as the trioctylmethylammonium-gold bromide complex and determined by atomic-absorption spectrometry by direct spraying of the extract into the flame. Optimal conditions for the extraction and determination of gold have been established. As little as 0.5 mug of gold in a sample can be determined. The extraction of gold from hydrochloric or hydrobromic acid solution with trioctylamine or trioctylmethylammonium chloride (or bromide) has also been investigated.     

Determination of aluminium in aerosols by flameless atomic-absorption spectrometry

A method is reported for the determination of aluminium in aerosols collected on Whatman 41 cellulose filters. In the destruction procedure, provision was made to eliminate silica by hydrofluoric acid treatment. Analysis of the solutions was performed by the flameless atomic-absorption technique. The accuracy was checked by using data from instrumental neutron-activation analysis (INAA) and standard reference materials. An analogue integrator gave a better linearity and detection limit than conventional peak-reading.     

Determination of gold in tissue by carbon-furnace atomic-absorption spectrometry

A sensitive and reproducible technique is reported for the determination of gold in tissue by carbon-furnace atomic-absorption spectrometry. Results are compared with those obtained by using a flame-atomization procedure and by neutron-activation analysis. The method is used to analyse samples of kidney, liver, spleen, nails and hair from human subjects. A possible correlation between gold levels in nails and plasma is suggested.     

Determination of indium by hydride generation and atomic-absorption spectrometry

Conditions are presented for the determination of indium by atomic-absorption spectrometry following hydride generation. Indium hydride produced by addition of sodium borohydride to a solution of indium in 3M hydrochloric acid is flushed with argon into an electrically heated silica tube. The mass of indium giving 1 % absorption is 0.3 mug.     

Determination of trace elements in the water cycle by total-reflection x-ray fluorescence spectrometry

The determination of trace elements in the various stages of the water cycle is very important. Economic procedures for multi-element determinations of trace elements in various matrices are needed. The applications of total-reflection x-ray fluorescence spectrometry in this general area are reviewed briefly, with examples relating to rain, river and sea waters, sediments, particulate matter and manganese nodules and crusts, as well as mussel tissue. Up to 25 elements can be determined; these are S, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Pb, Se, Rb, Sr, Y, Zr, Mo, Ag, Cd, Sb and Ba. Preliminary treatments of the various matrices are described. Accuracy checks by analysis of reference standards and by application of independent techniques are reported.     

Determination of selenium and tellurium in air by atomic-absorption spectrometry

Elemental selenium and tellurium, and gaseous inorganic forms of Se(IV), Se(VI), Te(IV) and Te(VI) have been determined after their adsorption on gold-coated beads. After leaching, with water and dilute hydrochloric and nitric acids, the different chemical species in each acid fraction were separated with an anion-exchange resin (Bio-Rad AG-1X8) and a cation-exchange resin (Amberlite IR-120 Plus) by varying the acidity of the leaching agent. Subsequent analysis was by graphite-fumace atomic-absorption spectrometry. The lower detection limit for Se and Te was 0.03 ng/M(3) with a precision of +/- 5%. The average amounts of selenium in interior and exterior air samples were about 4.73 and 1.93 ng/m(3) respectively. For tellurium the corresponding values were about 0.78 and 0.24 ng/m(3).     

氢化物发生-原子荧光法测定绞股蓝中痕量铅

建立了以重铬酸钾为氧化剂、碱性铁氰化钾为络合剂, 丙二酸为掩蔽剂, 在盐酸介质中进行铅的氢化物发生的反应体系. 样品经HNO3-H2O2体系高压消解后, 采用断续流动氢化物发生器, 对测定铅的各种条件进行了优化和探讨. 在选定条件下, 方法检出限为3.76×10-7 g/L, 线性范围为0.01～2.00 ×10-4 g/L, 相对标准偏差为1.3%. 方法用于绞股蓝中铅的测定, 回收率为90.5%～101.4%.