This may or may not apply to your situation, but the same thing was happening to me. I had killed Althok once and redeived the head, but went LD afterwards and didn't get a chance to hail the last cleansed worshipper. Halsey wouldn't take the items in any combination or respond to hails.
After killing Althok again but hailing the worshipper this time, the sarge took my head, vial, etc. and allowed me to complete the quest. This was last night.