YS/T 1085-2015 PDF in English
YS/T 1085-2015 (YS/T1085-2015, YST 1085-2015, YST1085-2015)
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Refined nickel. Determination of Silicon, manganese, phosphorus, iron, copper, cobalt, magnesium, aluminum, zinc, chromium. Inductively coupled plasma atomic emission spectrometric method
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Standards related to (historical): YS/T 1085-2015
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YS/T 1085-2015: PDF in English (YST 1085-2015) YS/T 1085-2015
YS
NONFERROUS METAL INDUSTRY STANDARD
OF THE PEOPLE'S REPUBLIC OF CHINA
ICS 77.120.40
H 13
Refined nickel - Determination of Silicon, manganese,
phosphorus, iron, copper, cobalt, magnesium, aluminum,
zinc, chromium - Inductively coupled plasma atomic
emission spectrometric method
ISSUED ON: APRIL 30, 2015
IMPLEMENTED ON: OCTOBER 1, 2015
Issued by: Ministry of Industry and Information Technology of the People's
Republic of China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Method principle ... 5
3 Reagents ... 5
4 Instruments ... 6
5 Samples ... 7
6 Analysis steps ... 8
7 Calculation of analysis results ... 9
8 Precision ... 10
9 Test report ... 12
Appendix A (Normative) Operation of determining instrument performance
specifications ... 14
Refined nickel - Determination of Silicon, manganese,
phosphorus, iron, copper, cobalt, magnesium, aluminum,
zinc, chromium - Inductively coupled plasma atomic
emission spectrometric method
WARNING - Personnel using this standard shall have practical experience in
regular laboratory work. This standard does not address all possible safety issues.
Users are responsible for taking appropriate safety and health measures and
ensuring compliance with the conditions stipulated in relevant national
regulations.
1 Scope
This standard specifies the method for the determination of silicon, manganese,
phosphorus, iron, copper, cobalt, magnesium, aluminum, zinc and chromium content in
refined nickel by using an inductively coupled plasma atomic emission spectrometric
method.
This method is applicable to the analysis of silicon, manganese, phosphorus, iron,
copper, cobalt, magnesium, aluminum, zinc and chromium content in refined nickel.
The measuring range of each element is shown in Table 1.
2 Method principle
A certain amount of the sample is weighed and decomposed by the nitric acid; an
inductively coupled plasma atomic emission spectrometer is used to measure the
spectral intensity of the spectral line of the element to be measured in the solution; the
spectral line is corrected by subtracting the background to eliminate the influence of the
matrix nickel; the elemental content is obtained from the calibration curve drawn
according to the standard solution.
3 Reagents
Unless otherwise stated, the reagents used in this standard are all of analytical grade,
and the water used is first-grade water.
3.1 Nitric acid (ρ=1.42 g/mL).
3.2 Nitric acid (1+1).
3.3 Hydrofluoric acid (ρ=1.15 g/mL).
3.4 Silicon standard stock solution: Heat high-purity silica (the content is greater than
99.9%) at a temperature of 1100 °C until its mass is constant, and cool to room
temperature in a desiccator; weigh 2.1393 g and put it into a platinum crucible, add
about 5 g of sodium carbonate, heat and melt for 15 minutes. Take it out and cool it
slightly, place it in a 500 mL beaker, dissolve the melt with water, and wash out the
platinum crucible; then, transfer the solution into a 1000 mL volumetric flask, wash the
beaker with water and pour the washing liquid into the volumetric flask, add water to
the scale of the volumetric flask, mix well, and store in a plastic bottle. This solution
contains 1000 μg of silicon in 1 mL.
3.5 Manganese standard stock solution: Weigh 1.0000 g of high-purity manganese
metal (the content is greater than 99.9%), put it into a (300 mL) beaker with a glass
cover, add 30 mL of nitric acid, and heat it carefully to decompose it. After the solution
cools to room temperature, transfer it to a 1000 mL volumetric flask, clean the beaker
with water, and pour the washing liquid into the volumetric flask. Add water to the scale
of the volumetric flask and mix well. This solution contains 1000 μg of manganese in
1 mL.
3.6 Phosphorus standard storage solution: Weigh 4.3936 g of the standard dipotassium
hydrogen phosphate dried at 105 ℃~110 ℃, dissolve it in water, transfer the solution
to a 1000 mL volumetric flask, dilute it with water to the mark, and mix well. This
solution contains 1000 μg of phosphorus in 1 mL.
3.7 Iron standard stock solution: Weigh 1.0000 g of high-purity iron powder (the content
is above 99.95%), add 30 mL hydrochloric acid (1+1) to dissolve it with slight heat,
transfer the solution to a 1000 mL volumetric flask, dilute it with water to the mark, and
shake well. 1 mL of this solution contains 1000 μg of Fe.
3.8 Copper standard stock solution: Weigh 1.0000 g of high-purity copper (the content
is greater than 99.9%), put it into a 300 mL beaker, add 30 mL of nitric acid, and heat
it at low temperature to decompose it. After the solution cools to room temperature,
transfer it to a 1000 mL volumetric flask, dilute to volume with water, and mix well.
This solution contains 1000 μg of copper in 1 mL.
3.9 Cobalt standard stock solution: Weigh 1.0000 g of high-purity cobalt (the content is
greater than 99.9%), pour into a 500 mL beaker, then add 40 mL of nitric acid, and heat
to completely dissolve; boil slightly to discharge nitrogen oxides, cool and pour it into
a 1000 mL volumetric flask containing 160 mL of nitric acid. Dilute to volume with
water and mix well. This solution contains 1000 μg of cobalt in 1 mL.
3.10 Magnesium standard stock solution: Weigh 1.0000 g of metallic magnesium (the
content is above 99.9%), add 60 mL of hydrochloric acid (1+5) to dissolve, cool and
transfer the solution to a 1000 mL volumetric flask, dilute to the mark with water, and
shake well. This solution contains 1000 μg of magnesium in 1 mL.
3.11 Aluminum standard stock solution: Weigh 1.0000 g of pure metal aluminum (the
content is above 99.9%), add 30 mL of hydrochloric acid (1+1), drop a small amount
of nitric acid, heat to dissolve, and drive out the nitrogen compounds; cool and transfer
to a 1000 mL volumetric flask, dilute to volume with water, and shake well. 1 mL of
this solution contains 1000 μg of Al.
3.12 Zinc standard stock solution: Weigh 1.0000 g of pure metallic zinc (the content is
above 99.9%), add 30 mL of hydrochloric acid (1+1) and slowly heat to dissolve,
transfer the solution to a 1000 mL volumetric flask, dilute to the mark with water, and
shake well. 1 mL of this solution contains 1000 μg of Zn.
3.13 Chromium standard stock solution: Weigh 1.0000 g of pure metal chromium (the
content is above 99.9%), add 30 mL of hydrochloric acid (1+1) and heat to dissolve,
then transfer the solution to a 1000 mL measuring bottle, dilute to the mark with water,
and mix well. This solution contains 1000 μg of chromium in 1 mL.
4 Instruments
4.1 Single-scale pipettes and single-scale volumetric flasks.
4.2 Analytical balance, capable of weighing accurately to 0.0001 g.
4.3 Inductively coupled plasma atomic emission spectrometer
6 Analysis steps
6.1 Specimen
Weigh 0.2 g of the sample (Chapter 5), accurate to 0.0001 g.
6.2 Blank test
Perform a blank test along with sample analysis.
6.3 Pretreatment of specimens
Place the specimen (6.1) into a 200 mL Erlenmeyer flask, add 15 mL of nitric acid (3.2),
and heat at low temperature until the specimen is completely dissolved. Remove the
flask and cool to room temperature, transfer the solution into a 200 mL volumetric flask,
dilute to volume with water, and mix well. This solution is the solution to be tested.
NOTE: If the content of P and Al elements in the sample is < 0.01%, a 100 mL volumetric flask can be
selected.
6.4 Determination
On the adjusted inductively coupled plasma spectrometer, according to the optimized
working conditions of the instrument and the wavelengths given in Table 2, measure
the spectral line intensity, from which the spectral line background is subtracted, of the
sample solution (6.3) and blank test solution (6.2). The mass concentration of the
corresponding element in the liquid to be tested is obtained on the working curve drawn
by the instrument according to (6.5).
6.5 Drawing of working curve
6.5.1 Mix standard solution: Respectively pipette 60.00 mL of cobalt standard stock
solution (3.9), 40.00 mL of iron standard stock solution (3.7), 20.00 mL each of silicon
standard stock solution (3.4), manganese standard stock solution (3.5) and copper
standard stock solution (3.8), 2.00 mL each of phosphorus standard stock solution (3.6),
magnesium standard stock solution (3.10), aluminum standard stock solution (3.11),
zinc standard stock solution (3.12) and chromium standard stock solution (3.13) in a
1000 mL volumetric flask, dilute with water to the mark and mix well. This solution
contains 60 μg of cobalt, 40 μg of iron, 20 μg each of silicon, manganese, and copper,
and 2 μg each of phosphorus, zinc, chromium, aluminum, and magnesium per milliliter.
6.5.2 Preparation of working curve series calibration solutions: Pipette 0 mL, 1.00 mL,
5.00 mL, 10.00 mL, 25.00 mL, 50.00 mL of mixed standard solutions (6.5.1) into a set
of 100 mL volumetric flasks, add 7.5 mL of nitric acid (3.2), dilute to volume with water,
and shake well. The concentrations of each element in the calibration curve standards
Appendix A
(Normative)
Operation of determining instrument performance specifications
A.1 Overview
The purpose of the performance tests given in this appendix is to use different types of
instruments to appropriately determine the detection limit (DL) and background
equivalent concentration (BEC) of the inductively coupled plasma spectrometer, and to
perform appropriate spectral line background correction. Different operating conditions
are allowed to be used for different models of instruments, but the final measurement
results shall meet the requirements of this standard.
A.2 Detection limit of background equivalent concentration
Prepare 3 solutions, containing the concentration of the test substance at 0 concentration
level, 10 times the detection limit, and 1000 times the detection limit. These solutions
contain acids and matrix elements with similar concentrations to the samples to be
tested.
Spray the 1000 times detection limit solution and wait 10 seconds after the solution
enters the plasma to ensure stable atomization. Set operating and instrument conditions
for the element to be measured.
Carefully position the selected wavelength at the highest peak and select an appropriate
photomultiplier tube (if not automatically selected) to ensure that the measured light
intensity has 4 significant digits. Set the integration time to 3 s.
A.2.1 Detection limit
Spray the blank solution for about 10 seconds and measure 10 times with the preset
integration time.
Spray the 10 times detection limit solution for about 10 seconds and measure 10 times
with the preset integration time.
According to the intensity readings obtained from the blank test solution and 10 times
the detection limit solution, calculate the average value 𝑋 1, 𝑋 b and the standard
deviation Sb of the blank solution.
The net average intensity (𝑋n1) of the 10 times detection limit solution according to
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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