Nice tip about making up your own reference solutions. Any guidance as to how you did it?
Sure. I have a microgram balance and a set of voumetric flasks so I can work in smaller quantities relatively easily. The principles scale however.
Starting with deionised water and whatever powder I was using, I'd dry the powder out on a hot plate, measure it out on the scale and dump it in the water. Transfer the lot to a bottle. Salt was easy as I was aiming for 4600ppm, so 4.6g of salt in 1L. From memory I used un-iodised table salt.
CYA was a bit harder. From memory I had the flask on a mag stirrer for a day or two to make sure it was all dissolved.
I made a 2800ppm solution, divided that by 2 to get a 1400ppm solution and then used a 50ml pipette to take 50ml of that into a 1L flask to give me 70ppm. I still have the 3 bottles (70/1400/2800) which is how I remember the sequence. I *think* after a few experiments 2.8g/l was about all I could get to cleanly dissolve and I was clearly over-egging the desire for accuracy.
I have 2 CYA standards. One just CYA in water and the other is pH balanced, but I would have used bicarb and HCl to ensure it was all "pool compatible". I don't recall why I did that. I did spend a lot of time playing with them trying to read that test reliably. Not a fan of opacity testing.
I did a similar thing with Boric acid, although that was a lot easier to dissolve. I just wanted to be sure I had a firm grip on the borate titration test and since I had the gear it was just another measure/dissolve/dilute.
You don't have to go to the extent I did with the measuring equipment. Larger volumes help compensate for less accurate measuring. If I weighed out 20kg of water on a bathroom scale and I got 92g of salt on a kitchen scale I get ~4600ppm.
CYA would be more of a challenge in a bucket. I'm waiting on some fresh reagent to actually check to see how well the CYA standard has held up, but the salt, hardness and boric acid are all fine.
Memory is a little hazy, that was all done in early 2019 and I've had a bit of stuff going on since then. I've really only had time to get back to it in the last couple of months.