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Neutron Activation Analysis

Introduction

Neutron activation analysis (NAA) is an analytical technique that relies on the measurement of gamma rays emitted from a sample that was irradiated by neutrons. The rate at which gamma rays are emitted from an element in a sample is directly proportional to the concentration of that element. The major advantages of NAA are that:

Principle

The process for analyzing samples by NAA involves irradiating them with a neutron source. Neutrons are captured by elements in the sample to produce unstable radioactive isotopes (radionuclides). Beta particles, and in most cases gamma rays, are emitted from the radionuclides as they decay. The energies of these gamma rays are, in general, distinct for a specific nuclide and the rate at which these photons are emitted with a particular energy can be measured using high–resolution semiconductor detectors. Because the production and decay rate of gamma radiation are dependent on the half–life of the nuclide, elemental measurements can be optimized by varying the irradiation and the decay times (i.e., how long the sample is near a neutron source and when the sample is analyzed).

Procedure

The most common procedure for NAA involves encapsulating the samples and suitable standards in heat–sealed polyethylene or quartz vials and simultaneously irradiating them. Ideally, the samples are irradiated in a "lazy susan" facility that revolves around the core thereby ensuring that the samples and standards experience the same neutron fluence. Following sequential decay periods, each standard sample is analyzed utilizing high resolution germanium detectors coupled to a multi–channel analyzer system. Gamma ray counts accumulated in an energy region above the background counts produce photopeaks. After counting analysis is complete, these data are processed using sophisticated computer programs that smooth the spectral data and determine the net areas of gamma ray photopeaks. The program then translates the area into count rates (counts per minute or cpm). These programs are capable of resolving overlapping and complex photopeak energy regions. Additional data for decay time differences, electronic dead time losses and unresolved interferences and compares the sample data (cpm/weight) to the standard data (cpm/μg) to calculate elemental abundance in the sample.

Errors in Analysis

The principal error in the analysis of materials by NAA is the counting statistic error, which is based on the signal to background ratio at the gamma ray energy region of interest. A one sigma error for a photopeak area determination is approximately equal to the square root of the total counts (background plus net counts) divided by the net counts. For example, a peak area determination with 2000 total counts and a net area of 1000 counts produces a counting error of about 4.5%.

An additional source of error for some elemental determinations is due to unresolved interferences. The most serious interferences are those that result when identical radionuclides are produced from different nuclear reactions. For example, high concentrations of U fission products can interfere with the accurate determination of La, Ce, Nd, Mo, and Zr abundances. In addition, the determinations of some elements can suffer because the photopeaks produced by gamma rays emitted by two or more radionuclides is not readily resolved. In these cases, empirical corrections are integrated into the data reduction procedure.

Self–shielding is a phenomenon that occurs when the neutron flux experienced by a sample is attenuated, thereby reducing the neutron activation of the nuclides in self–shielded samples. This effect occurs when a sample contains high concentrations of elements with very high probabilities that a neutron will be captured, which is measured in terms of a target area, or cross section.

Detection Limits

Elemental detection limits for NAA are variable because some elements become very radioactive–, and can be determined at very low levels while other elements do not become very radioactive or have very short half–lives (less than 10 seconds). Activation analysis determines the total mass of an element in a sample. A certain amount of an element, like arsenic–, is needed in the sample for detection. For arsenic, under ideal conditions, 5 ng is required. To determine 5 ppb of arsenic, 1 g of sample is sufficient. To determine 0.5 ppb of arsenic, 10 g of sample is necessary, etc. The production of radioactive nuclides depends on the cross sections of the specific elements. Also important is the number of gamma rays that are emitted by a radionuclide. In some cases, only a small fraction of the total emissions from a specific nuclide is in the form of gamma rays. Samples with high concentrations of elements that are readily activated and emit a considerable number of gamma rays, such as Na and Sc, can generate high background count rates and raise the detection limits for the element(s) of interest. The following table shows the best case minimum detection levels (MDL) for the 70 elements that NAA is capable of identifying.

element 

MDL

(μg

element 

MDL

(μg

element 

MDL

(μg

Ag  0.004  Hf  0.0006  Re  0.0008 
Al 0.004 Hg 0.003 Rh 0.005
Ar 0.002 Ho 0.003 Ru 0.04
As 0.005 I 0.002 Sb 0.007
Au 0.0005 In 0.00006 Sc 0.001
Ba 0.02 Ir 0.0003 Se 0.01
Br 0.003 K 0.2 Sm 0.001
Ca 4 Kr 0.01 Sn 0.03
Cd 0.005 La 0.005 Sr 0.005
Ce 0.2 Lu 0.0003 Ta 0.1
Cl 0.05 Mg 0.5 Tb 0.03
Co 0.01 Mn 0.0001 Te 0.03
Cr 0.3 Mo 0.1 Th 0.2
Cs 0.001 Na 0.004 Ti 0.1
Cu 0.002 Nb 3 Tm 0.2
Dy 0.00003 Nd 0.03 U 0.003
Er 0.002 Ne 2 V 0.002
Eu 0.0001 Ni 0.7 W 0.004
F 0.4 Os 1 Xe 0.1
Fe 2 Pd 0.03 Y 0.4
Ga 0.002 Pr 0.03 Yb 0.02
Gd 0.007 Pt 0.1 Zn 0.1
Ge 0.1 Rb 0.02 Zr 0.8

 

Applications

Neutron activation analysis remains at the forefront of techniques for the quantitative multi–element analyses of major, minor and trace elements in hundreds of different types of materials. The following list includes some of the materials that can be readily analyzed by NAA:

 

References

  • Ameil, S. (Editor), 1981. Non Destructive Activation Analysis. Studies in Analytical Chemistry, Vol. 3, Elsevier, Amsterdam.
  • De Soete, D., Gijbels, R. and Hoste J., 1972. Neutron Activation Analysis, Wiley, New York.
  • Hoffman, E.L., 1992. Instrumental neutron activation analysis. Journal of Geochemical Exploration, Special Issue: Geoanalysis (Editor: G. E. M. hall) volume 44:297–320.
  • Reeves, R.D. and Brooks, R.R., 1978. Trace Element Analysis of Geologic Materials, Wiley, New York.


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