hi G, are you now getting solid double-zero readings for ammonia and nitrite(NO2) at the 24-hour test?
One thing you look for is that the 24-hour tests become very consistent with not showing blips, whereas you may still be struggling to get double-zeros on the 12-hour tests.
Tom has stated the core of our procedure very clearly. We try for 4-5ppm doses at the "add-hour" to be dropped to zero ppm ammonia and zero ppm nitrite(NO2) when tested 12 hours after the add-hour and if the biofilter can do this for a week we know it's very solid and very unlikely to mini-spike on us after fish introduction.
Now, that being said, the process can get into a bit of a vicious little circle itself toward the very end where one keeps seeing little blips of nitrite (typically 0.25ppm) at 12 hours and it can go for weeks like that. That sort of "sticking syndrome" is not productive. While we know that eventually it -will- reach the double-zero point with extra time, we also know that most real-world stocking plans will not fully stock and these "sticking syndrome" fishless cycles will transition to a running tank with initial stock without mini-spiking. It's just a question of degree and yours doesn't, unfortunately, sound like it's down to that kind of small blipping yet. You've just reported a 5ppm nitrite spike at 12 hours if I'm reading you right.
The issue of very high nitrates(NO3) pulling the nitrite(NO2) test result artificially up is usually not consistent over a weeks worth of test results in my experience. It also seems to be a bit worse with the Nutrafin tests than the API tests. It's one of multiple reasons we sometimes do the large down-to-the-gravel water changes near the end of the fishless cycle, but that carries it's own problems in that the sudden change also can cause the bacteria to seem to "pause" in their processing for a day or two. It's all rather more ugly trying to interpret things near the end but you just have to look down a long page of daily results and hope for general trends to reveal themselves.
~~waterdrop~~
ps. (I'm very late to this thread, maybe you already have fish

)