XLO Test CD, track no. 3, is the best for setting up speakers, accurate to within 1/8 inch. No substitute.
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A Sterephile test CD and a Radio Shack meter for the bass works well, a Cardas Disc for set up (includes a "walk about" which I find helpful), and I use an Opus 3's "Depth of Image" to fine tune, as well as other ordinary disc's with which I'm very familiar and which have borderline problems if the room set up and the electronics are not ideal. In the end though you're still likely to have some compromise somewhere. The bass can be a bitch to get smoothed out as there usually are some room problems you can't correct.
Ditto on the Rives CD - grand shtuff. Though it does become a love/hate thing, you know? I'd gone through some other discs & done the (trivial, in retrospect) calibration to the RS meter by hand, etc. Then I broke down and got Rives and got a bit more thorough. I also became acutely aware of nodes and stuff like that. Wound up turning the whole room 90 degrees, researching treatments (and doing entry-level stuff), and in the end it was the nodes and the math that kinda led me to just throw up my hands, kick back, and just listen. I did learn a lot with the Rives, though.
You do have to guard against becoming way too anal about it all - I mean, it's not like I've outlined the exact spot for my butt in the "A" listening position or anything like that...
I worked out a procedure to locate speakers (nearly full range floor standers) with a Stereophile Test CD and RS SPL meter. My meter is placed on a tripod at ear height at the listening seat position. I record response throughout the 200 to 40 Hz range (after setting level for 80 dB at 1K Hz) for each position, moving speakers forward in 2" increments from the front wall. I then add up the deviations from the 80 dB reference and compare totals for each speaker position. This is to locate the smoothest bass response, not necessarily the deepest range. I've found this quite satisfactory.
Regarding the Rives Test CD, I believe their supposed correction for RS meter readings assumes too much precision from the RS meter. I doubt very much if at that price, RS could offer a meter with such consistency from one to another that an absolute correction is possible.
And so I consider any readings I make with my RS meter to represent relative data rather than absolute.
Lots of good suggestions above. If you still can't get things dialed in completely to your satisfaction, or maybe even if you can, I'd recommend finding a way to demo something like the DSpeaker Anti-Mode Dual Core room correction device. It may yield even further improvements above integrating bass and save you time and headaches. Best of luck.
First, ask GIK Acoustics for help. Best products at the lowest prices and great advice.
Once you have taken all their advice, you'll need OmniMic or Room EQ Wizard. The reviewers at Stereophile have been using OmniMic more often, but they don't know what they are looking at yet. :)
Anyway, the Room EQ forums are filled with good advice about sub placment AND EQ.
Look at miniDSP for your subwoofer EQ.
That is all.