Thanks for the reply WD. On the 12hr/24hr thing, I am putting no. of hours since adding NH3 in the post after you suggested it. It's often not 12 or 24hrs though-just depends when I'm free to test.
On the point about pH, up until this week, I was measuring it with an electronic probe from work. Then I bought a master kit with pH and high pH tests in. Sometimes, it's right at the top of pH or right at the bottom of high pH, so I do the other test to make sure. I can't remember what I did when it went up a point, but, as I mentioned, I think the 4ppm was a little low. I'd added 1ml and got 2ppm, so added some more. On the calculator, 1.3ml is meant to get me up to 5ppm from 0.
Anyway, had a bit of a breakthrough last night. I broke my NH3 test tube soon after buying the kit. I replaced it with a new tube from work and a rubber bung. When I came to do the test last night, I noticed there was a white cloudiness in the test tube, so decided to use a spare one from the master kit. NH3 was 0ppm

This morning, I've done the test in both tubes to compare and they are both 0ppm. So not sure if it's coincidence or what, but either way, I'm happy!
Day 27 24hrs
NH3-0ppm
NO2-0ppm
pH-7.5
added 1.5ml NH3 > 4ppm
Day 28 14.5hrs
NH3-0ppm

NO2-0ppm

pH-7.5