noninvasive way. Therefore, several online and inline methods in combination with flow chemistry have emerged during the last years. They range from analytic devices like size exclusion chromatography (SEC), [6,7] electrospray ionization mass spectroscopy [8] or NMR [9,10] to inline spectroscopic methods like IR [11,12] or UV-vis. [13] Most of these techniques are known from batch analytics, where especially NMR and SEC are obligatory for characterization of polymeric intermediates and products. Incorporation of these devices into flow reactors makes the life of every synthetic polymer chemist easier. It provides real-time and continuous information and makes optimization of any polymerization procedure less elaborate and, hence, more effective.In order to optimize homopolymerizations with certain desired molecular weights via controlled radical polymerizations, for instance, the experimentalist usually starts with an arbitrary set of intuitively chosen reaction conditions. Full monomer conversion is rarely targeted to suppress termination events and ensure a high chain end livingness. Consequently, it becomes inevitable to find the right conversion target and hence reaction time that yields the desired chain length. A widely used workflow to make such a kinetic screening in flow reactors is to set a specific flow rate (yielding the desired residence time) and collect the sample after equilibrating the reactor for a few residence times. [4] With a single run of this stationary approach, information about monomer conversion is obtained only at one individual reaction time, coincidently wasting a few reactor volumes of material. Complete kinetic screening is hence a brute force task and-discarding more material into waste than collectionhardly economically feasible. To gather information about all reaction times in a kinetic screening at once, the flow reactor needs to be operated in a nonstationary mode. Therefore, the whole volume is filled at a high flow rate and abruptly set to the desired rate. At this point, the sample collection can be started, and the residence time can be linearly calculated from the elapsed time. Although this approach has been widely used in academia, it is controversially discussed lately on the micro-and mesoscale. [9,10] Real-time data from inline SEC or NMR analysis are particularly helpful to find the desired molar mass as well as monomer conversion. Recently, notable studies showed how these methods can be automated to yield tailored polymer products with a minimum of experimentalist interaction. [7,10] However, the measurement volume of low-field NMR spectrometers is still big compared to other spectroscopic techniques, so that the reactor volume should be on the milliliter scale (or bigger) as well.Gapless monitoring of polymerization reactions is of paramount interest for academia and the polymer industry, allowing for efficient reaction screening and precise tailoring of the polymeric products. Herein, UV-visible spectroscopy (UV-vis) is employed as an operando measurement tech...