Copper electroplating was studied based on cyclic voltammetry combined with a new type of acoustic microgravimetry. The instrument operates similarly to a quartz crystal microbalance with dissipation monitoring (EQCM-D), meaning that it reports shifts in resonance frequency, Δf, and half bandwidth, ΔΓ, on several overtones. Compared to the existing instruments, the time resolution was improved by a factor of 10 down to 10 ms using multifrequency lockin amplification. The frequency noise after accumulation was reduced below 10 mHz ≙ 0.12 ng/cm2 ≙ 0.14 pm (assuming ρ = 8.96 g/cm3) by modulating the electrode potential and averaging of Δf and ΔΓ. Mostly, Δf and ΔΓ are in line with the Sauerbrey prediction (Δf/n ≈const. and ΔΓ/n < -Δf/nwith n the overtone order). Small unsystematic deviations between overtones due to compressional wave effects are seen but no evidence for strong roughness or viscoelasticity. Further, the Faraday efficiency is almost unity, meaning that Δf is close to the expectations derived from the electrical current. The improved sensitivity enables to determine the time derivative of the frequency shift, which is equal to an apparent mass transfer rate that can be compared to the current directly. Again, small deviations are seen for bulk deposition and stripping. These go back to weak roughness effects most pronounced in the initial phase of bulk deposition and, also, to the presence of a Cu(I) intermediate during dissolution. When adding benzotriazole (BTA) or thiourea (TU) as plating additives, the gravimetric and the voltammetric response changes. For BTA, the deviations between mass transfer rate and current vanish indicative of decreased roughness. For TU additional features appear, related to a potential-dependent adsorption of TU and to increased underpotential deposition (UPD). In the presence of TU, the electrode-electrolyte interface displays viscoelasticity, evident by the bandwidth increases during deposition.[1] Caption: Currents, time derivatives of the frequency shift, and bandwidth shift obtained during copper electrodeposition without additives (A), in the presence of 10 µM benzotriazole (B), and in the presence of 10 µM thiourea (C). Reprinted with permission from Reference [1].