YS/T 928.3-2013Methods for chemical analysis of nickel cobalt manganese composite hydrogenoxide. Part 3: Determination of nickel, cobalt, manganese content. Inductively coupled plasma atomic emission spectromertric (English PDF)

3.1 Hydrochloric acid (rho = 1.19 g/mL).

3.2 Nitric acid (rho = 1.42 g/mL).

3.3 Hydrochloric acid (1 + 1).

3.4 Nitric acid (1 + 1).

Element Determination Scope/%

3.7 Nickel standard stock solution. weigh-take 2.0000 g of pure nickel (wNi >= 99.99%) in a 300

mL beaker, add 40 mL of hydrochloric acid (3.1) and 5 mL of nitric acid (3.2); heat to dissolve

it. Boil to remove nitrogen oxides, remove and cool it, then, use water to wash the watch glass

and beaker wall. Transfer to a 500 mL volumetric flask, use water to dilute to the scale and mix

it well. 1 mL of this solution contains 4 mg of nickel.

3.10 Nickel cobalt manganese standard solution 955.accurately transfer-take 15.00 mL, 20.00

mL and 30.00 mL of nickel standard stock solution (3.7), and 2.00 mL, 3.00 mL and 5.00 mL

of cobalt standard stock solution (3.8) and manganese standard stock solution (3.9) in a group

of 200 mL volumetric flasks. Respectively add 2.00 mL of yttrium internal standard solution A

(3.5), use water to dilute to the scale and mix it well.

3.11 Nickel cobalt manganese standard solution 811.accurately transfer-take 15.00 mL, 20.00

mL and 25.00 mL of nickel standard stock solution (3.7), and 5.00 mL, 7.00 mL and 10.00 mL

of cobalt standard stock solution (3.8) and manganese standard stock solution (3.9) in a group

of 200 mL volumetric flasks. Respectively add 2.00 mL of yttrium internal standard solution A

(3.5), use water to dilute to the scale and mix it well.

3.12 Nickel cobalt manganese standard solution 523.accurately transfer-take 10.00 mL, 15.00

mL and 18.00 mL of nickel standard stock solution (3.7), and 10.00 mL, 12.00 mL and 15.00

mL of cobalt standard stock solution (3.8), and 10.00 mL, 15.00 mL and 20.00 mL of manganese

standard stock solution (3.9) in a group of 200 mL volumetric flasks. Respectively add 2.00 mL

of yttrium internal standard solution A (3.5), use water to dilute to the scale and mix it well.

3.13 Nickel cobalt manganese standard solution 424.accurately transfer-take 10.00 mL, 12.00

mL and 15.00 mL of nickel standard stock solution (3.7) and cobalt standard stock solution

(3.8), and 15.00 mL, 25.00 mL and 30.00 mL of manganese standard stock solution (3.9) in a

group of 200 mL volumetric flasks. Respectively add 2.00 mL of yttrium internal standard

solution A (3.5), use water to dilute to the scale and mix it well.

5.1 Test Portion

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

5.2 Blank Test

Along with the specimen, conduct the blank test.

5.3 Treatment of Test Portion

Place the test portion (5.1) in a 300 mL beaker, add 20 mL of hydrochloric acid (3.3), use a

watch glass to cover it; completely dissolve it at low temperature. Remove and cool it, then,

use water to wash the watch glass and beaker wall.

5.4 Drawing of Working Curve

On the ICP optical spectrometer, in accordance with the condition parameters provided in Table

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

repeatability limit (r) does not exceed 5%. The repeatability limit (r) is calculated using the

linear interpolation method and the extrapolation method in accordance with the data in Table

4.