BS ISO 7530-1:2015 pdf download – Nickel alloys — Flame atomic absorption spectrometric analysis Part 1 : Determination of cobalt, chromium, copper, iron and manganese
4.12 Copper standard solution, 1,000 g/l. Weigh 1 g ± 0,001 g of copper (Cu ≥ 99,9 %) and transfer it into a 400 ml beaker. Add 50 ml of nitric acid (4.2), cover with a watch glass, and allow to stand until the reaction ceases. Heat to complete dissolution, boil to remove nitrogen oxides, and evaporate just to dryness. Cool, add 25 ml of hydrochloric acid (4.3), and evaporate just to dryness. Add again 25 ml of hydrochloric acid (4.3) and repeat the evaporation. Dissolve the salts in 50 ml of hydrochloric acid (4.4) and heat if necessary. Cool, transfer into a 1 000 ml one-mark volumetric flask, dilute to the mark with water, and mix well. 1 ml of this solution contains 1,000 mg of copper.
4.13 Copper standard solution, 0,100 g/l.
Transfer 10,0 ml of copper standard solution (4.12) into a 100 ml one-mark volumetric flask and add 5 ml of hydrochloric acid (4.3). Dilute to the mark with water and mix well.
Prepare this solution immediately prior to use.
1 ml of this solution contains 0,100 mg of copper.
4.14 Copper standard solution, 0,025 g/l.
Transfer 5,0 ml of copper standard solution (4.12) into a 200 ml one-mark volumetric flask and add 10 ml of hydrochloric acid (4.3). Dilute to the mark with water and mix well.
Prepare this solution immediately prior to use.
1 ml of this solution contains 0,025 mg of copper.
4.15 Iron standard solution, 1,000 g/l.
Weigh 1 g ± 0,001 g of iron (Fe ≥ 99,9 %) and transfer it into a 400 ml beaker. Add 30 ml of hydrochloric acid (4.4) and cover with a watch glass. Heat to initiate the reaction and complete dissolution. Cool to about 50 °C, cautiously add 1 ml of hydrogen peroxide (4.7), and bring to the boil to oxidize the iron. Cool,transfer into a 1 000 ml one-mark volumetric flask, and add 35 ml of hydrochloric acid (4.3). Dilute to the mark with water and mix well.
1 ml of this solution contains 1,000 mg of iron.
4.16 Iron standard solution, 0,050 g/l.
Transfer 10,0 ml of iron standard solution (4.15) into a 200 ml one-mark volumetric flask and add 10 ml of hydrochloric acid (4.3). Dilute to the mark with water and mix well.
Prepare this solution immediately prior to use.
1 ml of this solution contains 0,050 mg of iron.
4.17 Manganese standard solution, 1,000 g/l.
Weigh 1 g ± 0,001 g of manganese (Mn ≥ 99,9 %) and transfer it into a 400 ml beaker. Add 30 ml of hydrochloric acid (4.4) and 2 ml of nitric acid (4.1). Cover with a watch glass and heat to initiate the reaction and complete dissolution. Add 0,5 ml of hydrogen peroxide (4.7). Cool, transfer into a 1 000 ml one-mark volumetric flask, and add 50 ml of hydrochloric acid (4.3). Dilute to the mark with water and mix well.
1 ml of this solution contains 1,000 mg of manganese.
4.18 Manganese standard solution, 0,100 g/l.
Transfer 10,0 ml of manganese standard solution (4.17) into a 100 ml one-mark volumetric flask and add 2,5 ml of hydrochloric acid (4.3). Dilute to the mark with water and mix well.
Prepare this solution immediately prior to use.
1 ml of this solution contains 0,100 mg of manganese.
4.19 Manganese standard solution, 0,010 g/l.
Transfer 5,0 ml of manganese standard solution (4.17) into a 500 ml one-mark volumetric flask and add 12,5 ml of hydrochloric acid (4.3). Dilute to the mark with water and mix well.
Prepare this solution immediately prior to use.
1 ml of this solution contains 0,010 mg of manganese.
5 Apparatus
All volumetric glassware shall be class A in accordance with ISO 385, ISO 648, or ISO 1042 as appropriate.
Ordinary laboratory apparatus and the following.
5.1 Atomic absorption spectrometer.
WARNING — The manufacturer’s recommendations should be closely followed and particular attention is drawn to the following safety points.
a) The explosive nature of acetylene and regulations concerning its use.
b) The need to shield the eyes of the operator from ultraviolet radiation by means of tinted glass.
c) The need to keep the burner clear of deposits because a badly clogged burner can cause a flashback.
d) The need to ensure that the liquid trap is filled with water.