Depending on the application, you may or may not have done it right.
Like Borek: said, liquid volumes may or may not be additive. That is simply the way the physical chemistry works. The effect may be negligible, or significant, and which can depend on the application.
If a solution has a change in temperature on mixing, the volume can also change. And again, this can be significant, or not depending on the application. Funny, I'd expect mixing sulfuric and water to get very hot, and increase in volume slightly, then contract as cooled.
Hrm ... did you mix 50 ml sulfuric and 150 ml water, measured separately and then mixing, to get your solution? Because that's how I'd do it. Or did you mix them in one measuring vessel, and then let it cool, because that's what would give what you've seen.
The protocol you're using should tell you exactly how its done. This is definitely the case for a pharmacopeia method, may or may not be the case for ASTM or other methods.
Possibly, its not a significant part of the assay, 1:3 is a pretty general sort of solution, maybe this reagent is used, in an assay, to just keep the pH low? You can describe the assay for us better so we can be sure.
If this is a titrant, or other quantitative reagent, then it should be defined better in the procedure, and prepared by you more carefully, you can let us know about that as well.