Calibration of AA finish fire assays

fireguy

fireguy

Supermoderator
#1
Higher production labs get a hugh productivity increase by using an AA finish for gold values rather than gravimetric finish. However, the calibration process is much move involved than most people initially realize.

You cannot just use the stock calibration solutions to make standards as this will produce a bias in almost all results.

One way to overcome this problem is by using a metallic gold standard which travels through the assay process. The method is something like this:

1) Weigh a piece of pure gold on the microbalance. You can record the weight by wrapping the gold in a piece of tape and writing the weight on the tape. This piece of gold should be approximately the correct weight to match your liquid AA standard used for calibration.

2) Assay this piece of gold along with your other assays. Make sure and use a new crucible so there is less chance of contamination.

3) After digesting the dore beads in aqua regia (I will discuss this further in another thread) use the digested gold piece to check the value of the liquid standard. You can note the "actual" value of the liquid standard and use it for further calibration. Example: if your 0.5 ppm standard reads 0.48 ppm against the gold piece, use the value of 0.48 ppm to standardize.

4) Make sure and have at least 2 gold pieces (one of them could be a flyer).

5) You should have a gold piece periodically (every 48 assays?).

6) You can generate the gold pieces from gravimetric finish assays.
 
J

JonSnow

New Member
#2
Could you please explain what you meant when you said.

"You cannot just use the stock calibration solutions to make standards as this will produce a bias in almost all results. "


Thanks,

Jon
 
fireguy

fireguy

Supermoderator
#3
JonSnow said:
Could you please explain what you meant when you said.

"You cannot just use the stock calibration solutions to make standards as this will produce a bias in almost all results. "


Thanks,

Jon
You can buy, or make, stock solutions. 1000 ppm standards are common to purchase. However, if you dilute these standards and calibrate with these solutions you will have a bias. You need to run a metallic standard completely through the assay and use this for calibration- not the liquid standard. You can set the value of the liquid standard against the metallic standard and use this for calibration on a short term basis. For instance, if you add metallic gold to a crucible that will generate a final solution concentration of 0.1 ppm gold, you can run this against your 0.1 ppm gold liquid standard- and then record the result. Perhaps it will run 0.095 ppm gold. You can then use this liquid standard in your calibration at the 0.095 ppm value for a short time. Maybe an hour. It is best to run one metallic standard per furnace load and use this to verify the concentration of your liquid standard. The variation could be caused by a combination of viscosity differences, temperature, percent dissolved solids, etc.
 
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