An EDTA-polarographic method for the determination of tellurium in lead alloys

A procedure is described for the polarographic determination of tellurium in lead alloys, without resorting to prior separative techniques. Interference by Cu, Cd, Tl, As, and Sb is discussed.     

The determination of magnesium in the presence of large amounts of zinc: A spectrophotometric method

The spectrophotometric determination of magnesium in the presence of large amounts of zinc is described. Zinc as well as some other interfering metals are removed by mercury cathode electrolysis and aluminium is removed by a chloroform extraction with 8-hydroxyquinoline.     

Trace amounts determination of lead,zinc and copper by adsorptive stripping voltammetry in the presence of dopamine

A selective and sensitive method for simultaneous determination of lead, zinc and copper by adsorptive differential pulse cathodic stripping voltammetry is presented. The method is based on adsorptive accumulation of the complexes of Pb(II), Zn(II), and Cu(II) ions with dopamine onto hanging mercury drop electrode (HMDE), followed by reduction of adsorbed species by differential pulse cathodic stripping voltammetry. The effect of experimental parameters such as pH, dopamine concentration, accumulation time and potential and scan rate were examined. Under the optimized conditions, linear calibration curves were established for the concentration of Pb, Zn, and Cu in the ranges of 5–150, 5–250, and 1–150 ng/mL, respectively. Detection limits of 0.06, 0.25, and 0.04 ng/mL for Pb, Zn, and Cu were obtained. An application of the proposed method is reported for the determination of these elements in some real samples such as natural waters and alloys.     

Simultaneous determination of trace amounts of zinc, lead and copper in rum by anodic stripping voltammetry

The determination of traces of Zn, Pb and Cu in rum samples by anodic stripping voltammetry without previous treatment or addition of a supporting electrolyte, using a hanging mercury drop electrode, is described. The choice of an appropriate stripping voltammetric method and deposition potential minimizes the influence of the organic content and ensures good reproductibility of the measurements. The reliability of the method was tested by comparing the results with those given by absorption spectrometry, the differences being about 10%. The method allows heavy metal ions to be determined in the mug l(-1) concentration range.     

A micro-sampling method for the determination of blood lead

The analytical micromethod discussed here has been found to be very rapid, accurate, and relatively inexpensive for the determination of blood and urine leads. It has the distinct advantage in that a determination can be repeated. The sensitivity of the method is 1.37 × 10^?10 g per 1% absorption at 283.3 nm. Our laboratories have analyzed 7353 specimens in duplicate or more from March 17, 1971 to April 30, 1972.Considering the many possible sources of contamination (the mobile unit being more so than a clinic) it is the Division of Chemistry's conclusion that an agreement of 84% is good and that a finger-stick method is feasible, and therefore, a complete micro-screening for blood lead is possible.     

The chromatomembrane method used for sample preparations in the spectrophotometric determination of zinc and copper in pharmaceuticals

The chromatomembrane cell (CMC) was used to extract zinc and copper and to preconcentrate them for their separation from pharmaceutical preparations. The method performance was evaluated at the determination of the enrichment factor, the linearity of response, the reproducibility, the accuracy and the sensitivity. In practice a five-fold enrichment has been enough provided that sample sizes of 0.825 ml were introduced. Good linearities for zinc and copper (r² > 0.99) were observed under this condition. The relative standard deviation (<3%) proved the good reproducibility of the method. The accuracy has been verified using model solutions, which were prepared from a certified reference. Recoveries of 98.8, 99.5 and 100.3% were achieved with solutions containing 0.1, 0.3 and 0.5 μg ml⁻¹ Zn(II), respectively. In case of copper 101.2, 99.6 and 100.6% recovery were obtained for 0.1, 0.4 and 0.7 μg ml⁻¹ Cu(II), respectively. The detection limits (three-fold of the signal-to-noise ratio) were estimated at 0.04 μg ml⁻¹ for both. The proposed method was applied on pharmaceutical preparations and the results were found to be in a good agreement with the contents guaranteed by the producers.     

A rapid iodometric method for the determination of copper and zinc

A method has been described for the iodometric simultaneous determination of zinc and copper. Copper is determined in the presence of sufficient KCNS and a small amount of KI. This is followed by the titration of the iodine equivalent to the zinc, which is liberated by the addition of potassium ferricyanide solution.Interference is eliminated completely by keeping the solution neutral or just acid with phosphoric acid.Within the range under investgation, results are obtained which are accurate to ± 0.7%.     

beta-Correction as a preprocessing method for partial least squares in simultaneous determination of zinc and lead

An error analysis of predicted values using spectral correction matrix and partial least squares (PLS) modeling is applied for the determination of Zn²⁺ and Pb²⁺ with methylthymol blue (MTB) as a metallochromic indicator. The concentration ranges for Pb²⁺ and Zn²⁺ in standard solution sets are 0.5-5.2 and 0.1-2.5 μg ml⁻¹, respectively. The experimental calibration set was composed of 20 sample solutions using a random design for two component mixtures. The absorption spectra were recorded from 400 to 700 nm. The two wavelengths, which exert the minimum error in prediction of two metal ion concentrations, are chosen according to an error analysis of different pairs of wavelengths. The effect of the pH on the sensitivity in determination of Zn²⁺ and Pb²⁺ using MTB was studied in order to choose the optimum pH (pH=6) for determination. The values of root mean square difference (RMSD) for lead and zinc using β-correction partial least squares were 0.0977 and 0.1266, respectively. The effect of diverse ions and several experimental parameters were studied. The method was used for the determination of lead and zinc in alloy samples.     

A method for the determination of the uranium content in U-Al alloys

The paper describes a method for the determination of uranium content in enriched U–Al alloys. The mass-spectrometric isotope dilution method was proposed and verified for the determination of uranium in these materials. A solution of natural uranylnitrate, prepared by dissolution of standard reference material NBS-U-960, was used as a spike. Uranium was separated from aluminium in the form of chloro complexes by sorption on anion exchange resin Dowex 1-X8 from 9M HCl. The error of determination lies in an interval 0.03–0.07% rel. for uranium contents 18.2–22.8 wt%.     

A sensitive flow-injection method for determination of trace amounts of nitrite

A new sensitive colour reaction for nitrite determination is presented. In acidic medium, nitrite was reacted with safranine to form a diazonium salt which caused the reddish-orange dye colour of the solution to change to blue. The carrier stream, into which the sample solution was injected, was doubly distilled water. The reagent solution stream, which contained safranine dye, hydrochloric acid and potassium chloride, was mixed with the carrier in a 3-m length of silicon tubing (bore 0.5 mm) maintained at 30°C in a thermostatic bath. The absorbance intensity was measured at 520 nm. The detection limit was 20 ng ml⁻¹ and the RSD% of 20 injections of 1 μg ml⁻¹ of nitrite was 0.65%. Analysis can be done at a rate of up to 30 h⁻¹. Under the optimum conditions in the concentration range of 30–4000 ng ml⁻¹ of nitrite ion, a linear calibration graph was obtained (r=0.9999). The method was applied successfully to the determination of nitrite in sausages.     

Rapid EDTA determination of lead in binary alloys of lead and tin

Binary alloys of lead and tin were dissolved in nitric acid (1 + 1) containing 10% sodium fluoride. The tin(IV) was effectively masked by the fluoride. The lead was quickly and accurately titrated with EDTA in a hexamine-buffered solution, with Xylenol Orange as indicator.     

A rapid spectrophotometric method for determination of zinc in milk

1-(2',3'-Dihydroxypyridyl-4'-azo)benzene-4-sulphonic acid and the corresponding 5'-chloro-substituted acid are proposed as sensitive reagents for zinc. Cyanide masking and selective demasking of zinc can be used to deal with the interference of many metal ions, cadmium can be masked with semithiocarbazide, and thiosulphate can be used for masking Hg(II), Pd(II) and Os(VIII). The molar absorptivities are about 1.3 x 10(5) 1.mole(-1).cm(-1). The method has been used for determinating zinc in milk.