The Puncoviscana Formation, largely cropping out in NW Argentina, is mainly composed of a pelite-greywacke turbidite sequence affected by incipient regional metamorphism and polyphase deformation. Metapelites, composed mainly of quartz, albite, dioctahedral mica and chlorite, were sampled in the Lules-Puncoviscana and Choromoro belts. Lattice-fringe images, selected area electron diffraction and analytical electron microscopy analyses, coupled with previous data from white mica crystallinity index, indicate a state of reaction progress for Puncoviscana slates consistent with medium anchizone- to epizone-grade metamorphism. The 2M polytype prevails in dioctahedral micas, coexisting in a few cases with the 1Md polytype as a consequence of lack of equilibrium. The 2Mpolytype coexists with 3T in two slates and long-range four-layer and ten-layer stacking sequences were identified in another sample. Samples with 3T and long-range stacking sequences present b values characteristic of intermediate–high pressure metamorphism and ordered chlorites (1L, 2L, 3L and 7L) prevail.

Based on the Si contents of dioctahedral micas and considering peak temperatures of ∼350 –400ºC, pressures from 5 kbar and 5 –7 kbar were derived for metapelites from the Lules- Puncoviscana and Choromoro belts, respectively. These values agree with facies series derived from the b values. Micas with a wide range of phengitic substitution, as evidenced by Fe + Mg and Si contents, coexist. These variations could not arise from the disturbing effect of detrital white K-mica because TEM evidence indicates that they are absent or represent <10% of the mica population. Thus, compositional variations suggest that dioctahedral micas of individual slates crystallized at different pressure conditions in response to the P-T path of the metamorphism. Moreover, in several biotite-free slates the illite crystallinity (IC) values lead to an underestimation of the metamorphic grade attained in these rocks.

The coexistence of IC corresponding to anchizone and the occurrence of biotite in some slates and felsic metavolcanic rocks intercalated in the Puncoviscana metasediments are interpreted to be the result of a metamorphic path including a relatively high-pressure/ low-temperature (HP/LT) event, followed by a lower-pressure overprint possibly at higher temperatures than the HP/LTevent. Small micas formed during the high-pressure stage would prevail in the <2 mm fraction, producing anchizone IC.

Mica-chlorite mixed-layering was identified by X-ray diffraction (XRD) as a major or subordinate constituent in several slates of the Puncoviscana Formation from Sierra de Mojotoro (Eastern Cordillera, NW Argentina). In order to determine the crystallochemical characteristics of these mixed-layered sequences and interpret their petrological meaning, anchizonal slate P90 was chosen for TEM observations. In this slate, dioctahedral mica and chlorite form interleaved phyllosilicate grains (IPG) or stacks, up to 110 um long, preferentially oriented with (001) planes at a high angle to the slaty cleavage but also oblique to S0.

In agreement with XRD results, the main phyllosilicates identified by transmission electron microscopy (TEM) were dioctahedral mica and random mixed-layer muscovite-chlorite, with chlorite in subordinate amounts and scarce smectite. In the lattice-fringe images of mixed-layer packets, a sequence of irregular stacking that produced apparent 24 Å (10 + 14) layers was observed, but it was frequently possible to distinguish the 10 Å layers from adjacent 14 Å layers. In nearly all packets, 14 Å layers prevail, exhibiting 14 Å:10 Å ratios between 1:1 and 3:1. Some elongated lenticular fissures which are probably a consequence of layer collapse caused by the TEM vacuum were identified in these packets. The straight, continuous appearance of lattice fringes plus the scarce evidence of collapsed layers identified suggest that these packets correspond principally to mixed-layer muscovite-chlorite, which is confirmed by analytical electron microscopy analyses. However, smectite-like layers are probably the third component of some of these mixed-layer sequences, which may account for their high Si and low (Fe + Mg) contents, their low interlayer charge in relation to theoretical interlayer muscovite-chlorite, and for the presence of Ca in the interlayer site.

Textural relationships between chlorite and muscovite packets in IPG along with the observed transformations from 14 Å to 10 Å along the layer, is compatible with a prograde metamorphic replacement of chlorite in stacks by dioctahedral mica layers, probably in the presence of an aqueous fluid.