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In Situ Compensation Method for Precise Integral SQUID Magnetometry of Miniscule Biological, Chemical, and Powder Specimens Requiring the Use of Capsules

Steadily growing interest in magnetic characterization of organic compounds for therapeutic purposes or of other irregularly shaped specimens calls for refinements of experimental methodology to satisfy experimental challenges. Encapsulation in capsules remains the method of choice, but its applicability in precise magnetometry is limited. This is particularly true for minute specimens in the single milligram range as they are outweighed by the capsules and are subject to large alignment errors. We present here a completely new experimental methodology that permits 30-fold in situ reduction of the signal of capsules by substantially restoring the symmetry of the sample holder that is otherwise broken by the presence of the capsule. In practical terms it means that the standard 30 mg capsule is seen by the magnetometer as approximately a 1 mg object, effectively opening the window for precise magnetometry of single milligram specimens. The method is shown to work down to 1.8 K and in the whole range of the magnetic fields. The method is demonstrated and validated using the reciprocal space option of MPMS-SQUID magnetometers; however, it can be easily incorporated in any magnetometer that can accommodate straw sample holders (i.e., the VSM-SQUID). Importantly, the improved sensitivity is accomplished relying only on the standard accessories and data reduction method provided by the SQUID manufacturer, eliminating the need for elaborate raw data manipulations.