Technical Abstract: Near Infrared (NIR) Reflectance spectroscopy has established itself as an important analytical technique in the field of food and agriculture. It is quicker and easier to use and does not require processing the samples with corrosive chemicals such as acids or hydroxides. However, for a long time the samples had to be grounded into powder form before making any measurements. Thanks to the development of new soft ware packages for use with NIR instruments, NIR techniques could be used in the analysis of intact grains and seeds. While most of the commercial instruments presently available work well with small grain size materials such as wheat and corn, they were found to be not suitable for large kernel size products such as shelled or in-shell peanuts. In this chapter principles of NIR Reflectance spectroscopy are discussed in particular reference to the water and oil bands, and the application of NIR in the rapid and nondestructive measurement of moisture and total oil contents in shelled and in-shell peanuts. Also discussed is the applicability, and limitations of NIR reflectance method in the analysis of fatty acid composition of different varieties of peanuts while they are in their shells. Ability to rapidly and nondestructively measure the water and total oil content, and analyze the fatty acid composition, will be immensely useful in the grading process of grains and nuts.