Shpolsky studied at the department of physics of Moscow State University. In the aftermath of the Casso affair of 1911 professors of physics Pyotr Lazarev and Pyotr Lebedev and their assistant Sergey Vavilov resigned and joined the faculty of the fledgling private Shanyavsky University. Shpolsky followed them, remaining de jure a student of Moscow State, and made his first research assignment in Lazarev's private laboratory in Arbat District. He graduated from the department of physics of Moscow State University in 1913 and joined the staff of Shanyavsky University. In 1918 he returned to Moscow State University and lectured there until 1939. In 1932 he also joined the faculty of Moscow State Pedagogical Institute and chaired its department of physics for 46 years. He received the doctorate at MSU in 1933.
After World War II Shpolsky engaged in physical studies of carcinogens. He reasoned that carcinogens should possess physical propertiesdistinct from harmless substances, and although no such link was ever found, his studies led to the discovery of Shpolsky effect. In 1952 Shpolsky, Ilyina and Klimov published an article in Doklady Akademii Nauk asserting that complex organic substances that normally do not have clearly defined spectral lines do, in fact, emit or absorb them at low temperatures when mixed with specific organic solvents. Use of the solvent, forming a snow-like paraffinstructure at 77 K, was a radical departure from an established spectroscopy routine. In the same year Pyotr Kapitsa provided Shpolsky his laboratory to repeat the experiment at lower temperatures. This property became known as Shpolsky effect; Soviet authorities formally recognized it as a discovery only after Shpolsky's death. Organic compounds possessing this effect became known as Shpolsky matrixes and Shpolsky systems. The method, although lacking solid theoretical foundation, provided extreme spectral selectivity and became a major improvement in detecting 3,4-benzapyrene in the 1960s. In 1961 Karl Rebane suggested that Shpolsky effect was an optical analogy to Mössbauer effect. Roman Personov, an alumnus of Shpolsky laboratory, confirmed Karl Rebane hypothesis in 1971. Later studies showed that matrix isolationfluorimetry has significant practical advantages over original Shpolsky methode.
