YS/T 928.4-2013 English PDF (YS/T928.4-2013)

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YS/T 928.4-2013: Methods for chemical analysis of nickel cobalt manganese composite hydrogenoxide. Part 4: Determination of iron, calcium, magnesium, copper, zinc, silicon, aluminium, sodium contents. Inductively coupled plasma atomic emission spectromertric
YS/T 928.4-2013
YS
NONFERROUS INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.60
H 13
Methods for Chemical Analysis of Nickel Cobalt Manganese
Composite Hydrogenoxide - Part 4: Determination of Iron,
Calcium, Magnesium, Copper, Zinc, Silicon, Aluminum,
Sodium Contents - Inductively Coupled Plasma Atomic
Emission Spectrometric
ISSUED ON: OCTOBER 17, 2013
IMPLEMENTED ON: MARCH 1, 2014
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 Summary ... 4
3 Reagents ... 5
4 Instrument ... 6
5 Analytical Procedures ... 7
6 Calculation and Expression of Analysis Results ... 8
7 Precision ... 8
8 Test Report ... 10
Methods for Chemical Analysis of Nickel Cobalt Manganese
Composite Hydrogenoxide - Part 4: Determination of Iron,
Calcium, Magnesium, Copper, Zinc, Silicon, Aluminum,
Sodium Contents - Inductively Coupled Plasma Atomic
Emission Spectrometric
1 Scope
This Part of YS/T 928 specifies the method for the determination of iron, calcium, magnesium,
copper, zinc, silicon, aluminum and sodium content in nickel cobalt manganese composite
hydrogenoxide.
This Part is applicable to the determination of iron, calcium, magnesium, copper, zinc, silicon,
aluminum and sodium content in nickel cobalt manganese composite hydrogenoxide. See Table
1 for the determination scope.
2 Method Summary
Use hydrochloric acid to dissolve the test portion and adopt an inductively coupled plasma
atomic emission spectrometer to directly conduct the determination. In accordance with the
working curve method, calculate the concentration of each element. Express the determination
results in mass fraction.
3 Reagents
All reagents used in this Part are of top-grade purity, and only pure water with an electrical
resistivity of not less than 18.2 M  cm shall be used in the analysis.
3.1 Hydrochloric acid (ρ = 1.19 g/mL).
3.2 Nitric acid (ρ = 1.42 g/mL).
3.3 Hydrochloric acid (1 + 1).
3.4 Nitric acid (1 + 1).
3.5 Aluminum standard stock solution: weigh-take 0.2000 g of pure aluminum (wAl  99.99%)
in a 300 mL beaker, slowly add 30 mL of hydrochloric acid (3.3), use a watch glass to cover it;
at a low temperature, dissolve it, then, cool it. Use water to wash the watch glass and beaker
wall. Transfer to a 1,000 mL volumetric flask, use water to dilute to the scale and mix it well. 1
mL of this solution contains 200 g of aluminum.
3.6 Magnesium standard stock solution: weigh-take 0.3316 g of dried magnesium oxide (wMgO
 99.99%) in a 300 mL beaker, slowly add 30 mL of hydrochloric acid (3.3), use a watch glass
to cover it; at a low temperature, dissolve it, then, cool it. Use water to wash the watch glass
and beaker wall. Transfer to a 1,000 mL volumetric flask, use water to dilute to the scale and
mix it well. 1 mL of this solution contains 200 g of magnesium.
3.7 Calcium standard stock solution: weigh-take 0.2800 g of dried calcium oxide (wCaO 
99.99%) in a 300 mL beaker, slowly add 30 mL of hydrochloric acid (3.3), use a watch glass to
cover it; at a low temperature, dissolve it, then, cool it. Use water to wash the watch glass and
beaker wall. Transfer to a 1,000 mL volumetric flask, use water to dilute to the scale and mix it
well. 1 mL of this solution contains 200 g of calcium.
3.8 Copper standard stock solution: weigh-take 0.2000 g of pure copper (wCu  99.99%) in a
300 mL beaker, slowly add 30 mL of nitric acid (3.4), use a watch glass to cover it; at a low
temperature, dissolve it and drive out nitrogen oxides, then, remove and cool it. Use water to
wash the watch glass and beaker wall. Transfer to a 1,000 mL volumetric flask, use water to
dilute to the scale and mix it well. 1 mL of this solution contains 200 g of copper.
3.9 Iron standard stock solution: weigh-take 0.2000 g of pure iron (wFe  99.99%) in a 300 mL
beaker, slowly add 30 mL of hydrochloric acid (3.3), use a watch glass to cover it; at a low
temperature, dissolve it, then, remove and cool it. Use water to wash the watch glass and beaker
wall. Transfer to a 1,000 mL volumetric flask, use water to dilute to the scale and mix it well. 1
mL of this solution contains 200 g of iron.
3.10 Zinc standard stock solution: weigh-take 0.2000 g of pure zinc (wZn  99.99%) in a 300
mL beaker, slowly add 30 mL of nitric acid (3.4), use a watch glass to cover it; at a low
temperature, dissolve it and drive out nitrogen oxides, then, remove and cool it. Use water to
wash the watch glass and beaker wall. Transfer to a 1,000 mL volumetric flask, use water to
dilute to the scale and mix it well. 1 mL of this solution contains 200 g of zinc.
3.11 Sodium standard stock solution: weigh-take 0.5084 g of high-purity sodium chloride that
has been dried at 110 C and place it in a 300 mL beaker, slowly add 100 mL of water, use a
watch glass to cover it; at a low temperature, dissolve it, then, cool it. Use water to wash the
watch glass and beaker wall. Transfer to a 1,000 mL volumetric flask, use water to dilute to the
scale, mix it well, and immediately transfer it into a dry plastic bottle. 1 mL of this solution
contains 200 g of sodium.
3.12 Silicon standard stock solution: weigh-take 0.4279 g of silica (wSiO2  99.99%) and place
it in a platinum crucible, add 3 g of anhydrous sodium carbonate, mix it well, cover it, then,
transfer it to a 400 C muffle furnace. Raise the temperature to 900 C, conduct melting for 1
h, then, remove and cool it. Use water to wash the outer wall of the crucible, place it in a 400
mL polytetrafluoroethylene plastic beaker and add 100 mL of hot water. At a low temperature,
dissolve it, cool it, then, transfer to a 1,000 mL volumetric flask. Use water to dilute to the scale,
mix it well, and immediately transfer it into a dry plastic bottle. 1 mL of this solution contains
200 g of silicon.
3.13 Aluminum, magnesium, calcium, copper, iron and zinc standard solutions: accurately
transfer-take 10.00 mL of the standard stock solutions (3.5, 3.6, 3.7, 3.8, 3.9 and 3.10) in a 200
mL volumetric flask. Use water to dilute to the scale and mix it well. 1 mL of this solution
contains 10 g of aluminum, magnesium, calcium, copper, iron and zinc.
3.14 Sodium standard solution: accurately transfer-take 10.00 mL of the standard stock solution
(3.11) in a 200 mL volumetric flask. Use water to dilute to the scale, mix it well, and
immediately transfer it into a dry plastic bottle. 1 mL of this solution contains 10 g of sodium.
3.15 Silicon standard solution: accurately transfer-take 10.00 mL of the standard stock solution
(3.12) in a 200 mL volumetric flask. Use water to dilute to the scale, mix it well, and
immediately transfer it into a dry plastic bottle. 1 mL of this solution contains 10 g of silicon.
4 Instrument
In terms of the inductively coupled plasma atomic emission spectrometer, the spectral lines of
the various element are shown in Table 2; the working parameters of the instrument for sodium
determination are shown in Table 3; the working parameters of the instrument for the
determination of other elements are shown in Table 4.
Table 2 -- Element Spectral Lines
Element
Element
Wavelength/nm
Wavelength/nm
with the condition parameters provided in Table 4, use water and silicon standard solution to
determine the intensity value of silicon, and the instrument automatically fits the working curve.
5.4.2 Accurately transfer-take 0 mL, 2.00 mL, 5.00 mL, 10.00 mL, 20.00 mL and 30.00 mL of
the standard solution (3.14) in a 200 mL volumetric flask. Use water to dilute to the scale, mix
it well, and immediately transfer into a dry plastic bottle. On ICP spectrometer, in accordance
with the condition parameters provided in Table 3, use water and sodium standard solution to
determine the intensity value of sodium, and the instrument automatically fits the working curve.
5.4.3 Accurately transfer-take 0 mL, 2.00 mL, 5.00 mL, 10.00 mL, 20.00 mL and 30.00 mL of
the standard solution (3.13) in a 200 mL volumetric flask. Use water to dilute to the scale and
mix it well. On ICP spectrometer, in accordance with the condition parameters provided in
Table 4, use water and aluminum, iron, calcium, magnesium, copper and zinc standard solutions
to determine the intensity values of aluminum, iron, calcium, magnesium, copper and zinc, and
the instrument automatically fits the working curve.
6 Calculation and Expression of Analysis Results
In accordance with Formula (1), calculate the mass fraction wx of the element being determined
and express it as a percentage.
Where,
wx---respectively the mass fraction of iron, calcium, magnesium, copper, zinc, silicon,
aluminum and sodium, expressed in (%);
ρ---the concentration of the element in the test solution, expressed in (g/mL);
ρ0---the concentration of the element in the blank test solution, expressed in (g/mL);
V---the total volume of the test solution, expressed in (mL);
m---the mass of the test portion, expressed in (g).
The result shall retain two decimal places.
7 Precision
7.1 Repeatability
Under repeatability conditions, obtain the determined values of two independent test results.
Within the average value range provided in Table 5, the absolute difference between the two
test results does not exceed the repeatability limit (r), and the circumstances of exceeding the