Nanjing Kirin Analytical Instrument-Analysis Method of Ore

Nanjing Kirin Analytical Instrument-Analysis Method of Ore

1. Preparation of mother liquor

Weigh 100mg sample through 100 mother sieve in 50ml volumetric flask, add 20ml hydrochloric acid, 5-10ml ammonium fluoride, depending on the content of silicon, dissolve under low temperature heating, if not complete, add stannous chloride dropwise to dissolve Cool, dilute to the mark.

Two; analysis

1. Determination of iron

Draw 5ml into a 100ml volumetric flask, add 10ml Edta, heat and boil, add 15ml ammonia water while hot, cool with running water, add 2ml hydrogen peroxide, and bring to volume. Colorimetric at a specific wavelength.

2. Determination of silica

Draw 2ml into the measuring flask, add 15ml of ammonium molybdate, let it sit for 20 minutes, or water bath for 40 seconds, add 10ml of oxalic acid, and quickly add 2ml of ferrous ammonium sulfate. Colorimetric at a specific wavelength. (For reference)

3. Determination of manganese

Pipette 20ml into a 50ml measuring flask, add 10ml of nitric acid, 10ml of ammonium persulfate, boil for 30 seconds, cool and set the volume. Colorimetric at a specific wavelength.

4. Determination of phosphorus

Pipette 10ml into a 60ml separating funnel, add a few drops of 6% ferrous ammonium sulfate, add 2-3 drops of hydrofluoric acid with a plastic dropper, 1ml of sodium thiosulfate, shake well, put it for 1-2 minutes, 25 Put it for 2-5 minutes, add 5ml of ammonium molybdate 4%, shake it, immediately add 20ml of butyl acetate, shake and extract for 1 minute, after still separation, separate the aqueous phase into another separating funnel (measure (For arsenic), add 5% ascorbic acid to the organic phase, and 5 drops of bismuth nitrate 10% (1 + 9 nitric acid), shake for 2 minutes, 25 degrees for 3 minutes, discard the aqueous phase after static layering, add 10ml of ethanol The water phase sinks and is discarded, and the color is compared at a specific wavelength.

5. Determination of arsenic

In the aqueous phase for extracting phosphorus, shake and keep the red color for 30 seconds when adding potassium permanganate (4%) dropwise, add 20ml of n-butanol, shake for 1-2 minutes, discard the aqueous phase after static stratification, in the organic phase Add 2ml of ascorbic acid and 5 drops of bismuth nitrate, shake for 2 minutes, discard the phase after static stratification. Add 1ml of ethanol to the organic phase, shake until the water phase condensate sinks, and discard the water phase at a specific wavelength.

6. Determination of aluminum oxide

Divide 1.0ml into a 100ml bottle, add about 50ml of water, 4ml of mixed color reagent, shake well, add 10ml of buffer solution, shake well, colorimetric at a specific wavelength.

Mixed developer

1), chrome azure S solution

2), Zn-Edta solution, mixed developer; mix the two in equal volume.

3), Hexamethylenetetramine buffer solution, take 100g and dissolve with appropriate amount of water, add 5ml 1 + 1 hydrochloric acid, dilute to 500ml.