YS/T 1006.2-2014Methods for Chemical Analysis of Lithium Nickel Cobalt Manganese Oxide - Part 2: Determination of Lithium, Nickel, Cobalt, Manganese, Sodium, Magnesium, Aluminum, Potassium, Copper, Calcium, Iron, Zinc and Silicon Content - Inductively Coupled Plasma Atom (English PDF)

3.5 Internal standard solution. weigh-take 2.5400 g of yttrium trioxide [w(Y2O3) >= 99.99%]

in a beaker; add 30 mL of hydrochloric acid (3.3). Heat it up to dissolve it, then, remove

it and cool it down. Use water to wash the watch glass and the wall of the beaker;

transfer it into a 1,000 mL volumetric flask. Use water to dilute it to the scale, then, mix

it up. 1 mL of this solution contains 2 mg of yttrium.

3.8 Cobalt standard stock solution. weigh-take 1.0000 g of pure cobalt [w(Co) >= 99.99%]

in a beaker; add 50 mL of hydrochloric acid (3.3). Heat it up to dissolve it, then, remove

it and cool it down. Use water to wash the watch glass and the wall of the beaker;

transfer it into a 500 mL volumetric flask. Use water to dilute it to the scale, then, mix it

up. 1 mL of this solution contains 2.0 mg of cobalt.

3.9 Manganese standard stock solution. weigh-take 1.0000 g of pure manganese [w(Mn)

>= 99.99%] in a beaker; add 50 mL of hydrochloric acid (3.3). Heat it up to dissolve it,

then, remove it and cool it down. Use water to wash the watch glass and the wall of

the beaker; transfer it into a 500 mL volumetric flask. Use water to dilute it to the scale,

then, mix it up. 1 mL of this solution contains 2.0 mg of manganese.

3.10 Sodium standard stock solution. weigh-take 2.5420 g of dried reference sodium

chloride [w(NaCl) >= 99.99%] in a beaker; slowly add 100 mL of water and cover the watch

glass. Conduct low-temperature dissolution, then, cool it down. Use water to wash the

watch glass and the wall of the beaker; transfer it into a 1,000 mL volumetric flask. Use

water to dilute it to the scale, then, mix it up; immediately transfer it to a dry plastic

bottle. 1 mL of this solution contains 1.0 mg of sodium.

3.11 Magnesium standard stock solution. weigh-take 1.6580 g of dried magnesium

oxide [w(MgO) >= 99.99%] in a beaker; slowly add 50 mL of hydrochloric acid (3.3) and

cover the watch glass. Conduct low-temperature dissolution, then, cool it down. Use

water to wash the watch glass and the wall of the beaker; transfer it into a 1,000 mL

volumetric flask. Use water to dilute it to the scale, then, mix it up. 1 mL of this solution

contains 1.0 mg of magnesium.

3.13 Potassium standard stock solution. weigh-take 1.9068 g of dried reference

potassium chloride [w(KCl) >= 99.99%] in a beaker; slowly add 100 mL of water and cover

the watch glass. Conduct low-temperature dissolution, then, cool it down. Use water

to wash the watch glass and the wall of the beaker; transfer it into a 1,000 mL

volumetric flask. Use water to dilute it to the scale, then, mix it up; immediately transfer

it to a dry plastic bottle. 1 mL of this solution contains 1.0 mg of potassium.

3.16 Iron standard stock solution. weigh-take 1.0000 g of pure iron [w(Fe) >= 99.99%] in

a beaker; slowly add 50 mL of hydrochloric acid (3.3) and cover the watch glass.

Conduct low-temperature dissolution, then, remove it and cool it down. Use water to

wash the watch glass and the wall of the beaker; transfer it into a 1,000 mL volumetric

flask. Use water to dilute it to the scale, then, mix it up. 1 mL of this solution contains

1.0 mg of iron.

3.17 Zinc standard stock solution. weigh-take 1.0000 g of pure zinc [w(Zn) >= 99.99%] in

a 400 mL beaker; slowly add 50 mL of nitric acid (3.4) and cover the watch glass.

Conduct low-temperature dissolution to drive off nitrogen oxides, then, remove it and

cool it down. Use water to wash the watch glass and the wall of the beaker; transfer it

into a 1,000 mL volumetric flask. Use water to dilute it to the scale, then, mix it up. 1

mL of this solution contains 1.0 mg of zinc.

3.18 Silicon standard stock solution. weigh-take 2.1395 g of pure silicon oxide [w(SiO2)

>= 99.99%] in a platinum crucible; add 15 g of anhydrous sodium carbonate; mix it up

and cover it. Then, transfer it into a 400 °C muffle furnace; raise the temperature to

3.19 Mixed standard solution A. respectively transfer-take 10.00 mL of sodium

standard stock solution (3.10), magnesium standard stock solution (3.11), aluminum

standard stock solution (3.12), potassium standard stock solution (3.13), copper

standard stock solution (3.14), calcium standard stock solution (3.15), iron standard

stock solution (3.16) and zinc standard stock solution (3.17); place it in a 100 mL

volumetric flask. Use hydrochloric acid (5 + 95) to dilute it to the scale, then, mix it up;

immediately transfer it to a dry plastic bottle. 1 mL of this solution contains 100 µg of

sodium, magnesium, aluminum, potassium, copper, calcium, iron and zinc.

3.20 Mixed standard solution B. transfer-take 10.00 mL of mixed standard solution A

(3.19); place it in a 100 mL volumetric flask. Use hydrochloric acid (5 + 95) to dilute it

to the scale, then, mix it up; immediately transfer it to a dry plastic bottle. 1 mL of this

solution contains 10 µg of sodium, magnesium, aluminum, potassium, copper, calcium,

iron and zinc.

4.1 Inductively Coupled Plasma Atomic Emission Spectrometer

4.2 Analytical Spectrums

Table 2 lists out the recommended analytical spectrums.

4.4 Linearity of Working Curve

In terms of the linearity of the working curve, the correlation coefficient shall be greater

than 0.999.

5.1 The specimen shall pass through a 50 µm sieve.

5.2 Before analysis, the specimen shall be dried at 110 °C ± 5°C for 2 h and placed in

a desiccator to cool down to room temperature.

6.1 Specimen

Weigh-take 0.20 g of specimen, accurate to 0.0001 g.

6.2 Number of Determinations

Independently conduct two determinations; take the average value.

6.3 Blank Test

Conduct a blank test on the accompanying specimen.

6.4 Determination

6.4.1 Processing of specimen

6.4.2 Preparation of a series of standard solutions

6.4.2.1 Respectively transfer-take 0 mL, 0.60 mL, 2.00 mL, 5.00 mL, 10.00 mL, 20.00

mL, 30.00 mL and 40.00 mL of standard solution (3.20); place it in a 200 mL volumetric

flask. Use water to dilute to the scale, then, mix it up; immediately transfer it to a dry

plastic bottle.

6.4.3 Measurement

After the instrument stably operates, in accordance with the optimized operating

conditions of the instrument and the recommended analytical spectrum wavelengths

(see Table 2), use the series of standard solutions (6.4.2.1) to determine the light

emission intensity of sodium, magnesium, aluminum, potassium, copper, calcium, iron

and zinc; use the standard series of solution (6.4.2.2) to determine the light emission

intensity of silicon; use the standard series of solution (6.4.2.3) to determine the light

emission intensity of lithium, nickel, cobalt and manganese. From low to high,

determine the light emission intensity of the measured element in the standard series

of solution.

8.1 Repeatability

In terms of the measured value of two independent test results obtained under

repeatability conditions, the absolute difference between the two test results shall not

exceed the repeatability limit (r), and the circumstance of exceeding the repeatability

limit (r) shall not exceed 5%. The value of the repeatability limit (r) shall comply with

the data in Table 3.

8.2 Allowable Difference

The difference of the inter-laboratory analysis results shall be not greater than the

values shown in Table 4.