This paper develops a methodology of crosstalk analysis/measurement techniques for the design and fabrication of the MEMs (Micro-ElectroMichanical system) probe card. By introducing more ground pins into the connector pins, the crosstalk characteristics can be enhanced and a design guide for the parameters, such as pin's size and pitch is proposed to satisfy the given crosstalk limitation of -30 dB for reliable high speed signal transfer. The paper also presents a novel method to characterize scattering parameters of multiport interconnect circuits with a 4-port VNA (Vector Network Analyzer). By employing the re-normalization of scattering matrices with different reference impedances at other ports, data obtained from 4-port configuration measurements can be synthesized to build a full scattering matrix of the DUT (Device-Under-Test, MEMs probe connector pins). In comparison to the conventional 2-port VNA re-normalization method, proposed technique has two advantages: saving of measuring time, and enhanced accuracy even with open-ended unmeasured ports. A good agreement of the estimated and correct S parameters verifies the validness of the proposed algorithm.