I don't really understand the chemistry at work here, although Radu: seems to be on the right track -- the spatula may have reduced the sample, either because of what it was made of, or. You really shouldn't use a metal spatula with reactive reagents. You can try a disposable plastic spatula. My favorite thing is to cut the bulb of a polypropylene dropper in half. That give me a spoon that I know has never touched another reagent ... because it was never a spoon in the first place.