Radiochemical determination of caesium-137 in liquid milk

Summary A simple and rapid method is described for the radiochemical determination of a caesium-137 in liquid milk. After the addition of caesium carrier the milk sample is deproteinized with nitric acid, filtered and alkaline earths removed by oxalate precipitation. From the decanted solution caesium is precipitated with sodium cobaltinitrite, separated from potassium as caesium silicotungstate and finally counted as dipicrylaminate by an anticoincidence beta counter. The radiochemical yields for caesium amount to about 65%. Good agreement is found between results obtained by the present method and by the gamma spectrometry. The results for caesium-137 content may be obtained within 6 hours.

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Zusammenfassung Es wird eine einfache und schnelle Methode zur radiochemischen Bestimmung von Caesium-137 in flüssiger Milch beschrieben. Die zu untersuchende Milch wird nach Zusatz des Caesiumträgers mit Salpetersäure enteiweißt. Aus der dekantierten Lösung werden die Erdalkalien als Oxalate abgeschieden. Das Radiocaesium wird mit Natriumnitritocobaltat gefällt, von Kalium mit Silicowolframsäure getrennt und endlich als Caesiumdipikrylaminat in einem Beta-Antikoinzidenzzähler gemessen. Die Caesiumträgerrückgewinnung beträgt durchschnittlich 65%. Die nach der beschriebenen Methode erhaltenen Resultate stehen in guter Übereinstimmung mit denen der gammaspektrometrischen Bestimmung. Der Radiocaesiumgehalt in Milch kann innerhalb von 6 Std bestimmt werden.

     

Radiochemical procedure for the determination of plutonium isotopes in powdered milk

Summary A radiochemical procedure for the determination of alpha-emitting isotopes of plutonium in powdered milk is proposed. The procedure involves sample dissolution (by HNO₃ and HClO₄), separation by ionic-exchange resin, electrodeposition and alpha-spectroscopy. In order to determine the chemical recovery, ²⁴²Pu was employed as a tracer. A reference material (Marine Sediment IAEA 135) was analyzed to validate such procedure, and to show its reliability. Afterwards, some powdered milk, produced for international trade, was analyzed and chemical recovery was found to be around 95%.     

Radioanalytical determination of137Cs and89Sr in milk

Separation of Cs, Sr and Ca from their mixture was studied using solvent extraction and ion exchange techniques. More than 90% separation efficiency was achieved for Ca–Sr separation using ion exchange resin (Doulite C-20) while solvent extraction amounted to 88%. A proposed technique for determination of¹³⁷Cs and⁸⁹Sr in milk (after removal of organic matter) showed more than 80% accuracy for⁸⁹Sr determination and more than 90% for¹³⁷Cs determination.     

A rapid method for the determination of strontium-90 in powdered milk

A method in which⁹⁰Y the daughter product of⁹⁰Sr decay is extracted by tributyl phosphate (TBP) from ashed powdered milk is described. The⁹⁰Y which is in equilibrium with⁹⁰Sr is back-extracted into the aqueous phase and coprecipitated with milligram amounts of ferric hydroxide. The proposed procedure makes it possible to obtain thin planar sources convenient for low level gas counters. The overall detection efficiency of 45.5% for⁹⁰Y (including chemical recovery of yttrium) was achieved. The detection limit for 200 g powdered milk samples and 10 000 s counting time was 0.065 Bq·kg^–1. The concentration of⁹⁰Sr in three-year old samples (after Chernobyl accident) ranged from 0.81 to 1.31 Bq·kg^–1.     

The spectrochemical determination of total strontium in bone,milk and vegetation

Samples of bone ash are mixed with anhydrous copper sulphate and graphite and pelleted A d c. arc is used to excite the spectra which are then evaluated by microphotometry The effective concentration range is 50 – 350 p p. m of strontium in the ash and the coefficient of variation is 6% for single exposures at the 90 p p m levelIn the case of milk and vegetation, strontium and calcium are separated as insoluble oxalates and the strontium content of this fraction determined by a method similar to that used for bones, with a similar range and accuracy. An alternative flame photometric method is described for the determination of strontium in the calcium-strontium oxalate fraction, thc coefficient of variation of the whole analytical operation being 5% per determination     

The spectrographic determination of total barium in bone ash

Samples of bone ash are mixed with graphite and anhydrous copper sulphate as spectrographic buffer and lanthanum oxide as internal standard. The mixture is pressed into 30-mg pellets and burnt in a d.c. arc surrounded by a mantle of oxygen and argon. The spectra are evaluated by non-recording microphotometry. The effective concentration range is 2–25 p.p.m. of barium in the ash, and the coefficient of variation is 8% for single exposures at the 8-p.p.m. level     

Rapid determination of strontium-90 in seawater

It is shown that Y₂O₃, YF₃, LaF₃, and CeF₃ help concentrate ⁹⁰Y from seawater. To determine ⁹⁰Sr, YF₃ is the best reagent because the effect of interfering lead and thorium radioisotopes is minimum in this case. It is proposed to preconcentrate ²¹⁰Bi on PbS to eliminate its interference. To determine ⁹⁰Sr we measure the Cherenkov radiation of ⁹⁰Y concentrated on YF₃ without prior elution.     

Radiochemical determination of ruthenium-106 in urine

The method is based on volatilization of Ru in the form of RuO₄ by distillation of wetashed urine with KMnO₄, precipitation of Ru hydroxide, and β-counting. Before the distillation, most of the organic compounds are destroyed by wet-ashing with H₂SO₄ and 30% H₂O₂ at 140°C, with subsequent evaporation until fuming. The chemical recovery is determined photometrically at 430 nm using the solution of β-counted Ru hydroxide in KIO₄/KOH reagent. The mean recovery is about 70%.     

Radiochemical determination of low unsaturations in polyisobutene

A radiochemical technique involving the use of ³⁶Cl has been described previously for the measurement of butyl rubber unsaturations. This method has now been applied to the estimation of the much lower concentration of double bonds present in polyisobutene prepared by the cationic polymerization of isobutene at a low temperature. The nature of the reaction of polyisobutene with radiochlorine in the absence of air is examined, and the experimental results are discussed in relation to present theories of the mechanisms of chain termination in cationic polymerization.     

Radiochemical determination of Mo in pure tungsten

A radiochemical neutron activation technique for Mo determination in high purity tungsten, based on some specific properties of Mo and W radionuclides has been developed. Al₂O₃ powder has been used as a sorbent. An estimation of the Mo content was carried out via the selectively separated^99mTc daughter radionuclide. Limit of detection was 10 ng g^–1.     

Radiochemical determination of As,Cr, Mo,Sb and Se in foods

A radiochemical neutron activation analysis procedure was applied to the analysis of foods for As, Cr, Mo, Sb and Se. The elements are retained on an inorganic chromatographic resin of hydrated managanese dioxide while interfering elements are removed. Activities from Br, K, Na and P interferences are reduced by up to six orders of magnitude, and detection limits for food analysis are reduced by factors of 100–2000, compared with those normally found for instrumental neutron activation analysis. Detection limits for the foods analyzed are 0.1–0.3 ng/g for As and Sb and 1–10 ng/g for Cr, Mo and Se. Results are presented for various foods and several National Bureau of Standards Standard Reference Materials.     

Radiochemical determination of oxygen traces in selenium

A sensitive method for determination of oxygen in selenium is described. Oxygen is converted into the gaseous compound sulfur dioxide labelled with³⁵S. The β-radiation of³⁵S is measured by liquid scintillation counting. The detection limit is 0.02 ppm. The efficiency of vacuum distillation in the purification of selenium, and the influence of air, dry oxygen and water on the absorption of oxygen by selenium have been investigated.     

Radiochemical analysis of90Sr in milk,soil and plants by solvent extraction

A universal and fast method of⁹⁰Sr determination in environmental matrices (raw and dried milk, plants, soils) has been elaborated. Solvent extraction method of daughter⁹⁰Y by tributyl phosphate was used. The method of strontium determination is compatible with determination of other transuranic elements (americium, plutonium) and there is no need to check the chemical yield of strontium.     

Radiochemical determination of mercury,arsenic, cadmium,zinc and copper in biological materials

Extraction procedure for mercury, arsenic, cadmium, copper and zinc in biological materials is proposed. Mercury and copper are extracted with dithizone followed by the separation of mercury with tri-octyl-amine (TOA). Arsenic, cadmium and zinc are extracted as diethyldithiocarbamates. The procedure is applied for the analysis of some reference materials and autopsy human samples of kidneys, liver, heart, spleen and hair.     

Radiochemical determination of cadmium isotopes in radioactive debris

(109)Cd and (113m)Cd were produced in a high altitude nuclear explosion during 1962. Analysis of filters from aircraft and balloon samplers enables the products of this single detonation to be traced. A radiochemical procedure is presented which allows determination of the cadmium radionuclides in the course of a sequential analysis for fission products and activation products from nuclear weapons tests. The sensitivity, recovery and decontamination from other radionuclides are adequate.     

Radiochemical determination of cobalt-60 in environmental samples

A procedure for the radiochemical determination of (60)Co in low-activity samples of sediment and biological material is described. Cobalt recovery is high and decontamination from tervalent lanthanides and naturally-occurring radionuclides is complete. Cobalt is precipitated with 1-nitroso-2-naphthol, decontaminated from iron by precipitation of the iron as ferric phosphate, extracted into methyl isobutyl ketone, and finally precipitated as cobalt mercury(II) thiocyanate for yield determination and beta-counting.     

Phosphorus determination in milk and bone samples by neutron activation analysis

The determination of phosphorus in milk and bone samples by both radiochemical and instrumental neutron activation analysis is described. The radiochemical method consists of thermal neutron irradiation of samples and standards, sample dissolution, phosphorus precipitation as ammonium phosphomolyb-date, use of zinc holdback carrier and counting of the phosphorus-32 ß-activity. The instrumental method involves thermal neutron irradiation of samples and standards, waiting for a decay time and ß-counting. The methods were applied to commercial samples and reference materials.