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ISO 13547-1-2014 pdf free download
ISO 13547-1-2014 pdf free download.Copper, lead, zinc and nickel sulfide concentrates — Determination of arsenic — Part 1:Iron hydroxide concentration and inductively coupled plasma atomic emission spectrometric method
Concentrés sulfurés de cuivre, de p10mb et de zinc — Dosage de l’arsenic — Partie 1: Méthode par digestion acide, co-precipitation avec lefer et plasma induit par haute fréquence.
If the residue appears dark (indicating the presence of carbon). slowly add a small amount of nitric acid (4k) to the hot solution until the solution becomes colourless, then heat until strong white fumes have evolved.
Add 50 ml of water and bring to boil, then allow cooling.
Filter the solution through an Insoluble filter paper (5A) in a 250 ml conical beaker. Wash the 300 ml conical beaker and filter paper thoroughly with dilute sulphuric acid (4.12) and collect the filtrate in the same 250 ml conical beaker.
If acid-insoluble material is present, treat this residue as the procedure in Z5 otherwise proceed to step Z.
In the case of lead concentrates, proceed to step L4.
7.4 Removal of lead sulfate
Quantitatively, transfer the precipitate into a 250 ml conical beaker with small amount of water. Add 15 ml of ammonium acetate solution (41.9) and place the conical beaker on the hotplate and heat until dissolution of the PbSO4.
Cool the solution to room temperature and filter through an insoluble filter paper (SA), then wash the insoluble residue with dilute sulphuric acid (412). Reject the filtrate and washing solution. If acid Insoluble material is present, then treat this residue as the procedure in Z5. otherwise proceed to step
7.5 Dissolution of the insoluble residue
Quantitatively, transfer the insoluble residue into a 200 ml polytetrafluoroethylene beaker (5.6) with
a small quantity of deionised water. Add 5 ml of nitric acid (4.6), 2 ml of dilute sulphuric acid (411) and
3 ml to 5 ml of hydrof luoric acid (4.8). Heat the solution until the evolution of white sulphuric acid fumes
to remove silicon dioxide then allow to cool. Dissolve the soluble salts with 10 ml of deionised water and
10 ml of nitric acid (4.6). Proceed to step 7.6.
7.6 Separation of arsenic
Quantitatively, transfer the solution from step 7.5 and the filtrate from step 2.3 into a 300 ml conical beaker and dilute to approximately 150 ml with water. Add 5 g of ammonium chloride (4A) to the solution and agitate to dissolve. Add sufficient iron chloride solution (4.16) to give a total mass of 150 rng of iron in the filtrate.
If the mass of iron from the test portion Is above 150 mg, then do not add any iron chloride solution (41.6). Add sufficient aqueous ammonia (4.14) to effect complete precipitation then add an extra 10 ml of aqueous ammonia. Bring it to boil and leave boiling for 1 mm.ISO 13547-1-2014 pdf free download.
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