The　surface　properties　of　mixed　solutions　containing　an　anionic　polyelectrolyte,　carboxymethylchitosan　(CMCH),　and　a　cationic　gemini　surfactant,　1,2-bis(dodecyldimethlyammonio)hexane　dibromide　(C12C6C12),　were　studied　by　measuring　the　surface　tension　and　the　dynamic　surface　elasticity.　The　association　behaviors　in　the　solutions　were　also　measured　by　fluorescence　probe　technique.　The　results　showed　that　the　adsorption　layer　transformed　from　pure　elastic　2D　layer　to　visco-elastic　3D　layer　with　increase　in　surfactant　concentration.　The　microparticles　in　the　3D　layer　were　adsorbed　from　the　adjacent　bulk　to　the　surface　but　not　formed　directly　in　the　surface　layer　as　it　was　sometimes　assumed　in　other　polyelectrolyte/surfactant　systems.　The　stress　relaxation　mechanism　were　supposed　to　be　the　mass　exchange　between　the　unstructured　thinner　film　surrounding　the　microparticles　and　the　adjacent　bulk　during　the　surface　compression　or　expansion.　These　surface　properties　of　CMCH/C12C6C12　solutions　were　influenced　strongly　by　the　association　in　the　bulk　solution.　©　2019,　©　2019　Taylor　&　Francis　Group,　LLC.