This chapter describes technical aspects of neutron-stimulated gamma ray analysis of soil carbon. The introduction covers general principles, different modifications of neutron-gamma analysis, measurement system configuration, and advantages of this method for soil carbon analysis. Problems with neutron-gamma technology in soil carbon analysis and methods of investigations including Monte-Carlo simulation of neutron interaction with soil elements are discussed further. Based on the investigation results, a method of extracting the "soil carbon net peak" from the raw acquired data was developed. The direct proportional dependency between the carbon net peak area and average carbon weight percent in the upper 10 cm soil layer for any carbon depth profile was shown. Calibration of the measurement system using sand-carbon pits and field measurements of soil carbon are described. Measurement results compared to chemical analysis (dry combustion) data demonstrated good agreement between the two methods. Thus, neutron-stimulated gamma ray analysis can be used for in situ determination of near-surface soil carbon content and is applicable for precision geospatial mapping of soil carbon.