Ombrotrophic peatlands are fed uniquely by atmospheric inputs and therefore have much potential as temporal archives of atmospheric microplastic (MP) deposition, yet the recovery and detection of MP within an almost purely organic matrix is challenging. This study presents a novel peat digestion protocol using sodium hypochlorite (NaClO) as a reagent for biogenic matrix removal. NaClO is more efficient than hydrogen peroxide (H2O2). By using purged air-assisted digestion, NaClO (50 vol%) reached 99% matrix digestion compared with 28% and 75% by H2O2 (30 vol%) and Fenton's reagent, respectively. At a concentration of 50 vol% NaClO did however chemically disintegrate small amounts (<10 mass %) of polyethylene terephthalate (PET) and polyamide (PA) fragments in the millimeter size range. Observation of PA6 in natural peat samples, while not found in the procedural blanks, questions whether PA is fully disintegrated by NaClO. The protocol was applied to three commercial sphagnum moss test samples, in which MP particles in the range of 0.8-65.4 μm were detected by Raman microspectroscopy. The MP mass% was determined at 0.012% corresponding to 129 thousand MP particles/g, of which 62% were smaller than 5 μm and 80% were smaller than 10 μm, yet were accountable for only 0.4% (500 ng) and 3.2% (4 μg) of the total mass of MP, respectively. These findings underline the importance of the identification of particles Ø < 5 μm when investigating atmospheric MP deposition. The MP counts were corrected for MP recovery loss and procedural blank contamination. MP spike recovery following the full protocol was estimated at 60%. The protocol offers an efficient way of isolating and pre-concentrating most aerosol sized MPs in large quantities of refractory vegetal matrices and enables the automated μRaman scanning of thousands of particles at a spatial resolution on the order of 1 μm.