Low-level measurement of the cosmogenic 22Na radionuclide in fresh water by ultra low-background gamma-ray spectrometry after simple radiochemical separation

A simple analytical method was developed for the determination of cosmogenic ²²Na radionuclide in fresh water samples by ultra low-background g-ray spectrometry after radiochemical separation. The method consists in pre-concentration of ²²Na(Na) by a ion exchange resin column from a large volume of ca. 500-liter water samples, elution with 4M HCl from the resin, and removal of the main metal components such as Ca and Mg as carbonate precipitates and of ⁴⁰K(K) as potassium tetraphenylborate K[B(C₆H₅)₄]. The obtained ²²Na fraction was successfully measured by an ultra low-background Ge detector installed in the Ogoya Underground Laboratory.     

The advantage of anti-Compton counting in the measurement of low-level radioactivity by gamma-ray spectrometry

The inherent advantage of anti-Compton counting of low-level radioactivity is defined in terms of changes in the limits of decision, detection and determination. It appears that the advantage factor can be expressed in the experimentally observed reductions of peak area, compton continuum and natural background. For an array equipped with a sample changer, the advantage factor for interference by the compton continuum is 4, while that for interference by the natural background amounts to 3. By sacrificing the sample changer and closing its gap with NaI-plug, additional factors of 1.5 and 2 can be obtained for compton and natural background, respectively.     

Determination of54Mn in foods

⁵⁴Mn is analyzed in complex food ash of high cationic environment. The initial step is an extraction atpH 2.7 with hexane containing di(2-ethylhexyl) phosphoric acid (HDEHP) to complex the⁵⁴Mn and other nuclides. The manganese is reextracted into an alkaline EDTA buffer which is washed with 1% 8-hydroxyquinoline in chloroform containing 5% isoamyl alcohol. The⁵⁴Mn is determined by gamma spectrometry with recoveries ranging from 96.6 to 99.4%.     

Determination of plutonium-241 in low-level radwastes using radiochemical separation combined with LSC,alpha spectrometer and ICP-MS

Two kinds of measuring methods were described for the determination of Plutonium-241 in low level wastes in this study. Plutonium isotopes were separated and purified by highly selective UTEVA and TRU resin. LSC, alpha spectrometry, and ICP-MS were applied and compared for determination of Plutonium-241. There is a good agreement with the analytical results and also shows that the different analytical methods have high chemical recovery yields.

     

Determination of rare earth elements in soils and sediments by inductively coupled plasma atomic emission spectrometry after cation-exchange separation

The influence of matrix elements such as Ba, Ca, Fe, K, Na and Ti, on the inductively coupled plasma atomic emission spectrometry determination of the rare earth elements in soils and sediments is investigated and analytical lines with minimal interferences are chosen. The analysis of certified reference materials by two calibration methods (pure rare earth solutions and IAEA-Soil 5) and after cation-exchange proved that calibrations with IAEA-Soil 5 increase the number of accurately determined rare earth elements (REE), permitting the instrumental determination of Ce, Eu, La, Nd, Tb, Yb and Y in soils and some sediments. The cation-exchange procedure permits the determination of 12 REE with very good accuracy (below 10%) and detection limits varying between 0.05 (Eu, Tb, Yb) and 0.5 (Er) mg kg(-1).     

Determination of nitrogen in steels by alpha-induced prompt gamma-ray spectrometry

The prompt gamma-ray of 871 keV emitted during the bombardment of steels by 5 MeV alpha particles were used to determine nitrogen by means of the reaction¹⁴N(α, pγ)¹⁷O. The method is non-destructive, rapid and experimentally simple. It has a sensitivity of about 7 μg·g⁻¹. In the nitrogen concentration range of 10¹–10² μg·g⁻¹ the relative precision of the method is about 3%. The accuracy of the method compares with that of other nuclear methods. Presented at the 5th Symposium on Recent Developments in Activation Analysis, Oxford, 17–21 July, 1978.     

Determination of metals in alloys by neutron capture gamma-ray spectrometry

A collimated neutron beam capable of providing a thermal neutron flux of 4.75·10⁷ n·cm⁻²·sec⁻¹ has been used to analyze alloy samples of 1–5 g during relatively short irradiation times of 30 min by the use of neutron capture gamma-ray spectrometry. The analyses were performed by using a mathematical treatment that relates the count ratio of every constituent present in the matrix with the concentration and thus it requires no standards. The technique was applied to the analysis of steel and gold alloy samples. Errors ranged from 0.8%–10%.     

Determination of beryllium in Pt-Be alloy by atomic-absorption spectrometry after ion-exchange separation

Traces of beryllium in platinum have been determined by graphite-furnace atomic-absorption spectrometry, the graphite furnace being coated with lanthanum or titanium carbide. The coating improves the reproducibility, sensitivity and detection limit. Platinum interferes in the beryllium determination, and an ion-exchange separation is used in the determination of beryllium in Pt-Be alloy.     

Determination of oxygen in alkali halide salts by proton activation and radiochemical separation

A lanthanum fluoride precipitation method for the separation of¹⁸F produced from the¹⁸O(p,n)¹⁸F reaction in alkali halide salts is described. This radiochemical separation method minimizes interferences from other positron emitters produced by proton bombardment and makes the accurate determination of ppm-level¹⁸O in complex alkali halide systems feasible. The interference from the¹⁹F(p,d)¹⁸F reaction is eliminated by keeping the proton energy less than 8.2 MeV. Applications of this technique to studies of dissolved oxide species in molten alkali halide salts are discussed.     

Determination of vanadium in titanate-based ferroelectrics by INAA with discriminating gamma-ray spectrometry

Instrumental neutron activation analysis was used for determination of vanadium mass fraction in crystals of incipient ferroelectric strontium titanate and ferroelectric barium titanate. In order to improve vanadium limit of detection, discriminating gamma-ray spectrometry was used by inserting an absorption filter between the samples and an HPGe detector. The use of the absorption lead filter 6-mm thick yielded improvement of the vanadium limit of detection by a factor of two. The vanadium mass fraction determined in a quality control sample, which was NIST standard reference material SRM 1648 Urban Particulate Matter, was in close agreement with the certified value.

     

Determination of Cu in minerals by 14-MeV neutron activation analysis and radiochemical separation

14-MeV neutron activation analysis /NAA/ and radiochemical separation technique were used for the determination of Cu in Hungarian minerals. The separation of Cu from other elements is a possibility to avoid the interferences in the 511 keV -line.     

Determination of small amounts of tungsten by atomic absorption spectrometry after extraction separation

Small amounts of tungsten can be determined by atomic absorption spectrometry, after reduction with tin(II) and separation of the thiocyanate complex into methyl isobutyl ketone. The organic phase is aspirated into an acetylene-nitrous oxide flame There are no interferences from 1000-fold amounts of Zr or Cr(III), 200-fold amounts of U or Ti. 100-fold V or 10-fold Mo. Interference from large amounts of iron(III) is avoided by prior reduction. The method was successfully applied to the determination of tungsten in steels and zirconium alloys.     

On the determination of226Ra in soils and uranium ores by direct gamma-ray spectrometry

The evaluation of the source term in facilities related to the first stages of nuclear fuel involves the determination of radium concentration, as well as those from other radionuclides members of the uranium series. These activities are often required within a short time period, making impossible the use of radiochemical methods or the gamma-ray spectrometry of radium daughters. In those situations it can be very convenient to determine the²²⁶Ra activity by means of its 186 keV gamma-ray line. For this purpose it is necessary to estimate the interference due to²³⁵U, also present in natural samples. This method has been applied successfully to several soil samples from an old uranium factory in Southern Spain.     

超高效液相色谱-串联质谱法测定牛奶中糠氨酸

采用超高效液相色谱-串联质谱法建立了检测牛奶中糠氨酸含量的分析方法。试样经10.6 mol/L盐酸水解,纯水稀释后,糠氨酸在C18色谱柱上以0.1%甲酸水溶液和乙腈为流动相,进行液相色谱分离;质谱检测采用电喷雾正离子化模式和多反应监测模式(MRM)。结果表明,糠氨酸在0.01~0.5 mg/L范围内线性关系良好,相关系数(R2)为0.9996,定量限(LOQ)为0.5 mg/100 g蛋白。在生牛乳空白样品中添加浓度为10,100,300 mg/100 g蛋白时,糠氨酸的平均回收率为93.1%~95.7%,相对标准偏差(RSDs)为1.2%~1.7%(n=6)。     

超高效液相色谱-串联质谱法测定果汁中的展青霉素

建立了超高效液相色谱-电喷雾串联三重四极杆质谱(UPLC-ESI-MS/MS)联用技术分析果汁中展青霉素的方法。浓缩果汁样品经酶解,乙酸乙酯提取,Oasis HLB固相萃取(SPE)小柱净化后(澄清果汁直接进行SPE净化),以C18色谱柱为分离柱,以水和乙腈作为流动相进行梯度洗脱,电喷雾离子源电离、负离子多反应监测模式质谱进行定性和定量分析。展青霉素在1.0～500.0 μg/L质量浓度范围内线性关系良好,相关系数为0.999,方法的定量限为5.0 μg/kg;加标水平为5.0、25.0和100.0 μg/kg时,加标回收率为80.6%～91.8%,相对标准偏差为1.5%～7.3%。实验结果表明,该方法简单、灵敏、准确,各项技术指标均满足国内外法规要求,可用于果汁中展青霉素的检测。     

Determination of uranium by neutron activation and radiochemical separation of the tellurium fission product

After irradiation and dissolution of the samples (minerals, rocks etc.), elemental tellurium is precipitated, redissolved, extracted for its diethyldithiocarbamate, and finally reduced again for measurement of the ¹³²Te 228-keV γ-peak. The chemical yield is 75% and the lower limit of determination is 2 × 10^-7 g U.     

阴离子交换树脂分离-原子荧光法测定色母粒中的镉

采用微波消解溶样,结合离子交换法对色母粒样品进行待测元素的提取及净化处理,利用原子荧光光度计进行镉含量的测定。研究了717型阴离子交换树脂对色母粒样品中镉的吸附及分离条件,解决了样品中铅、铜等元素的干扰问题。方法加标回收率在92.4%～117.4%之间,相对标准偏差小于3.0%。     

Determination of selenium in foods by pseudo-cyclic neutron activation and anti-coincidence gamma-ray spectrometry

A pseudo-cyclic instrumental neutron activation analysis method in conjunction with anti-coincidence gamma-ray spectrometry (PC-INAA-AC) has been developed for the determination of ppb levels of Se. The method consists of repetitions of the irradiation-decay-counting cycles of a sample using the rapid transfer cyclic system at the Dalhousie University SLOWPOKE-2 reactor facility. The 162-keV γ-ray of ^77mSe (t _1/2 = 17.4 s) has been found to be highly selective. The precision and detection limits are significantly improved and the total experimental time drastically reduced by this method. Detection limits are between 2 and 9 ng. The accuracy of the method has been evaluated by analyzing a number of nutritional reference materials. The PC-INAA-AC method has been applied for the routine determination of Se to the composites of 135 food samples with values ranging from as low as 1 ng g⁻¹ for tea to 1,045 ng g⁻¹ for organ meats on fresh weight basis.     

Detection of background thermal neutrons in a modified low-background germanium gamma-ray spectrometer

Journal of Radioanalytical and Nuclear Chemistry - The paper presents the detection of background neutrons using the 558.4 keV gamma line emitted from excited 114Cd nuclei after neutron...