BS ISO 13933 pdf download

BS ISO 13933 pdf download Steel and iron — Determination of calcium and magnesium — Inductively coupled plasma atomic emission spectrometric method
Scope
This Internationa Standard specifies a method for determination of calcium and magnesium contents iniron, castiron,steel, and alloyed steel byinductively coupled plasma(lCP) atomic emission spectrometry
The method is applicable to the determination of calcium and magnesium contents (mass fraction) inthe range of 0,000 5 % to 0,006 % and 0,000 5 % to 0,20 %, respectively.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and areindispensable for its application, For dated references, only the edition cited applies. For undatedreferences, the latest edition of the referenced document (including any amendments) applies.
ISO 385, Laboratory glassware — Burettes
ISO 648, Laboratory glassware — Single-volume pipettes
ISO 1042, Laboratory glassware – One-mark volumetric flasks
ISO 3696, Water for analytical laboratory use – Specification and test methods
ISO 14284, Steel and iron – Sampling and preparation of samples for the determination of chemicalcomposition
3 Principle
A test portion is dissolved in a hydrochloric, nitric and hydrofluoric acid mixture and fumed withperchloric acid.Hydrochloric acid, nitric acid, and an internal standard element (if used) are added andthe solution is diluted to a known volume. The solution is filtered if necessary, nebulized into an ICpspectrometer and the intensity of the emitted light from each element measured simultaneously withthe intensity of the light emitted by the internal standard element.
4 Reagents
During the analysis, unless otherwise stated, use only reagents of recognized analytical grade with verylow calcium and magnesium contents and only grade 2 water as specified in ISO 3696.
4.1 Pure iron, containing less than 0,5 ug/g of calcium and magnesium.
4.2 Hydrochloric acid, p about 1,19 g/ml.
4.3Hydrochloric acid, p about 1,19 g/ml, diluted 1 + 1.
4.4Hydrochloric acid, p about 1,19 g/ml, diluted 1 + 4.
4.5 Hydrochloric acid, p about 1,19 g/ml, diluted 1 + 100.
4.6 Nitric acid, ρ about 1,42 g/ml.
4.7 Hydrofluoric acid, ρ about 1,14 g/ml.
4.8 Perchloric acid, ρ about 1,67 g/ml.
4.9 Acid mixture.
Mix two volumes of hydrochloric acid (4.2), one volume of nitric acid (4.6), and three volumes of water.
4.10 Calcium standard solutions.
4.10.1 Calcium stock solution, corresponding to 1 000 mg of calcium per litre.
Dry several grams of calcium carbonate [purity ≥99,9 % (mass fraction)] in an oven at 100 °C ± 5 °C for at least 1 h and cool to room temperature in a desiccator. Weigh, to the nearest 0,000 1 g, 2,497 g of the dried product into a 400 ml beaker, add 20 ml of hydrochloric acid (4.3), cover with a watch-glass and heat gently until the product is completely dissolved. Cool to room temperature and transfer the solution into a 1 000 ml one-mark volumetric flask. Dilute to the mark with water and mix.