Steels in the condition of temper brittleness are distinguished by an increased tendency toward embrittlement in aggressive hydrogen-containing media. In this study type 20Kh3N chrome-nickel steel, which possesses a high tendency toward temper brittleness, was studied. The specimens, separated into several lots, were aged at 400 °C with a hold time from 1 to 10,000 hours. By varying the hold time different levels of segregation of the impurity elements, primarily phosphorus, at the boundaries of the former austenitic grains were created and evaluated. On the basis of experimental results in this study and on information in the literature, the authors conclude that impurities made up of the group of tin, antimony, and phosphorus are responsible for temper brittleness of steel.