BS EN 15605:2010 pdf download
BS EN 15605:2010 pdf download.Copper and copper alloys Inductively coupled plasma optical emission spectrometry.
7.1.1.2 Test portion solution 5 gil
Transfer the test portion (7.1.1.1) into a 250 ml beaker.
Add 20 ml of hydrochloric acid solution (4.2) and 5 ml of nitric acid (4.3). Cover with a watch glass ani heal gently until the sample is completely dissolved, then heat to boiling. Allow to cool. Rinse the cover and the walls of the beaker with water.
Transfer the dissolved test portion into a 200 ml one-mark volumetric flask containing 10 ml of hydrochloric acid (4.1). Dilute to the mark with water and mix well.
7.1.1.3 Test portion solution 1 g1
In order to obtain solutions with 1 gil concentration, pipette exactly 20 ml of the test portion solution (7.1.1.2)
Into a 100 ml one-mark volumetric flask contairNng 5 ml of hydrodiloric acid (4.1) and 5 ml of yttrium solution
(4.34). Dilute to the mark with water and mix well.
7.12 Check test
Make a preliminary check of the apparatus by preparing a solution of a copper reference material or a synthetic sample containing known amounts of the elements listed in Table 1 and carrying out the procedure specified in 7.1.4.
7.1.3 Establishment of the calibration curves
7.1.3.1 Preparation of the calibration solutions
7.1.3.1.1 General
In all cases the acidity of the calibration solutions shall be similar to that of the test portion solutions,
If. for measurement purposes. a blank is required, prepare a solution containing only the same amounts of acids as In the test solution.
7.1.3.1.2 Preparation of the 5 gil calibration solutions, using mono-elemental solutions
Weigh the quantities of copper (47) shown in Table 7 and introduce them into each of a series of 250 ml beakers.
Add 20 ml of hydrochloric acid solution (4.2) and 5 ml of nitric acid (4.3) to each beaker. Cover with a watch glass arid heat gently in order to dissolve the copper Rinse the cover and the walls of the beaker with water and heat to boiling. Allow to cool and transfer each copper solution into a 200 ml one’rnark volumetric flask containing 10 ml of hydrochloric acid (4.1).
Transfer the volumes of the elemental solutions of Sn, Pb, Zn, Fe, Ni. Mn, P Al, Be, Co and Cd shown in Table 7 to each volumetric flask. Dilute to the mark with water and mix well.
7.1.3.1.3 Preparation of the I gil calibration solutions
Dilute accurately the 5 g/l calibration solutions (7.1.3-12) in order to obtain I g/l calibration solutions.
Pipette exactly 20 ml of the 5 gil calibration solutions (7.1.3,1.2) into 100 ml one-mark volumetric flasks each containing 5 ml of hyêochloric acid (4.1) and 5 ml of yttrium solution (4.34). Dilute to the mark with water and mix well.
7.1.3.2 Acustrnent of the apparatus
Start the inductively coup4ed plasma optical emission speCtrometer and let it run for at least half an hour before performing any measurements.
Adjust aU the instrumental parameters. each gas (outer, intermediate or central) flow rate. lord, position, entrance slits, ekit slits, pliotomultiplier tubes voltages (when appropnate). wavelengths of the analytical lines specrfied in Table 8, pro-spraying time and integrating time, according to the manufacturer’s instructions, while aspirating (for each element) the highest concentration calibration soluhon
Prepare the software for the measurement of the intensity of each analytical line and for the calculation of the corresponding mean value and relative standard deviation.
Each time the internal standard is used (V line 37103 nm) prepare the software to calculate the ratio between each analyte intensity and internal standard intensity
7.1.3.3 Spectrornetrlc measurements of me calibration solutions
Carry out the spectrometric measurements of me I gil solutions identified P1. P2. P3 (see Table 7 and 7.1.3.1.3). For phosphorus use me 5 gil calibration solutions (7.1.3.12). A simultaneous spectrometer shall be available for measurements using yttrium as internal standard (ratio mode)
For phosphorus determination use abso1uIe intensity taking into account mat “Gaussian measunng mode may also be recommended.
For each calibration solution (including the drlft surve( solution) at least three integrations are necessary In order to calculate the mean ratsoed intensities (mean absolute intensity for phosphorus).