Collocation analysis can be used to extract meaningful linguistic information from large-scale corpus data. This paper reviews the methodological issues one may encounter when performing collocation analysis for discourse studies on Chinese. We propose four crucial aspects to consider in such analyses: (i) the definition of collocates according to various parameters; (ii) the choice of analysis and association measures; (iii) the definition of the search span; and (iv) the selection of corpora for analysis. To illustrate how these aspects can be addressed when applying a Chinese collocation analysis, we conducted a case study of two Chinese causal connectives: yushi ‘that is why’ and yin’er ‘as a result’. The distinctive collocation analysis shows how these two connectives differ in volitionality, an important dimension of discourse relations. The study also demonstrates that collocation analysis, as an explorative approach based on large-scale data, can provide valuable converging evidence for corpus-based studies that have been conducted with laborious manual analysis on limited datasets.