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GB/T 38744-2020 English PDF (GBT38744-2020)

GB/T 38744-2020 English PDF (GBT38744-2020)

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GB/T 38744-2020: Methods for chemical analysis of synergistic catalysis elements in automotive exhaust catalysis -- Determination of cerium, lanthanum, praseodymium, neodymium, barium and zirconium contents -- Inductively coupled plasma atomic emission spectrometry

This Standard specifies the method that uses inductively coupled plasma atomic emission spectrometry to determine cerium, lanthanum, praseodymium, neodymium, barium and zirconium contents in motor vehicle exhaust purifier. This Standard is applicable to determination of cerium, lanthanum, praseodymium, neodymium, barium and zirconium contents in exhaust gas purifier for gasoline vehicles, diesel vehicles and motorcycles. See Table 1 for the range of determination.
GB/T 38744-2020
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 77.120.99
H 15
Methods for chemical analysis of synergistic catalysis
elements in automotive exhaust catalysis - Determination
of cerium, lanthanum, praseodymium, neodymium,
barium and zirconium contents - Inductively coupled
plasma atomic emission spectrometry
ISSUED ON: APRIL 28, 2020
IMPLEMENTED ON: MARCH 01, 2021
Issued by: State Administration for Market Regulation;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Method summary ... 4
3 Reagents or materials ... 4
4 Instruments ... 6
5 Sample ... 6
6 Test steps ... 6
7 Processing of test data ... 8
8 Precision ... 9
9 Test report ... 10
Annex A (informative) Recommended instrument operating conditions ... 11 Methods for chemical analysis of synergistic catalysis
elements in automotive exhaust catalysis - Determination
of cerium, lanthanum, praseodymium, neodymium,
barium and zirconium contents - Inductively coupled
plasma atomic emission spectrometry
1 Scope
This Standard specifies the method that uses inductively coupled plasma atomic emission spectrometry to determine cerium, lanthanum, praseodymium, neodymium, barium and zirconium contents in motor vehicle exhaust purifier. This Standard is applicable to determination of cerium, lanthanum,
praseodymium, neodymium, barium and zirconium contents in exhaust gas
purifier for gasoline vehicles, diesel vehicles and motorcycles. See Table 1 for the range of determination.
Table 1 -- Range of determination for each element
Element Range of determination. / %
Ce, Zr 0.10~10.0
La, Pr, Nd, Ba 0.025~5.0
2 Method summary
Use hydrochloric acid, nitric acid, hydrogen peroxide, hydrofluoric acid to heat at a constant temperature to dissolve the test material in a sealed PTFE sample dissolving tank. Use inductively coupled plasma atomic emission spectrometer. Measure and calculate the mass fraction at the wavelength corresponding to each element to be measured.
3 Reagents or materials
Unless otherwise specified, only reagents confirmed to be of superior purity and water equivalent to first-grade purity are used in this Standard.
3.1 Hydrochloric acid (??=1.19g/mL).
3.2 Nitric acid (??=1.42g/mL).
3.3 Hydrogen peroxide (30%).
3.4 Hydrofluoric acid (40%).
3.5 Hydrochloric acid (1+1).
3.6 Nitric acid (1+1).
3.7 Hydrochloric acid (1+9).
3.8 Mixed acid of hydrochloric acid and nitric acid: prepared by 3 portions of hydrochloric acid (3.1), 1 portion of nitric acid (3.2), 4 portions of water. Prepare as needed.
3.9 Cerium standard storage solution: Weigh 0.1228g of high-purity ceria (CeO2) that has been burnt at 850??C. Place in a beaker. Add 20mL of nitric acid (3.6). Slowly add 2mL of hydrogen peroxide. Heat at a low temperature till it is dissolved. After cooling, move into a 100mL volumetric flask. Use water to dilute to the scale. Mix well. 1mL of this solution contains 1000??g of cerium. 3.10 Lanthanum standard storage solution: Weigh 0.1173g of high-purity
lanthanum trioxide (La2O3) that has been burnt at 850??C. Place in a beaker. Use water to moisture. Add 20mL of hydrochloric acid (3.5). Heat at a low temperature till it is dissolved. After cooling, move into a 100mL volumetric flask. Use water to dilute to the scale. Mix well. 1mL of this solution contains 1000??g of lanthanum.
3.11 Praseodymium standard stock solution: Weigh 0.1208g of high-purity praseodymium oxide (Pr6O11). Place in a beaker. Add 30mL of mixed acid of hydrochloric acid and nitric acid (3.8). Heat at a low temperature till it is dissolved. After cooling, move into a 100mL volumetric flask. Use water to dilute to the scale. Mix well. 1mL of this solution contains 1000??g of praseodymium. 3.12 Neodymium standard stock solution: Weigh 0.1166g of high-purity
neodymium trioxide (Nd2O3). Place in a beaker. Add 40mL of hydrochloric acid (3.5). Heat at a low temperature till it is dissolved. After cooling, move into a 100mL volumetric flask. Use water to dilute to the scale. Mix well. 1mL of this solution contains 1000??g of neodymium.
3.13 Barium standard storage solution: Weigh 0.1437g of high-purity barium carbonate (BaCO3) that has been dried at 105??C for 2h. Place in a beaker. Add water and 20mL of nitric acid (3.6). Heat at a low temperature till it is dissolved. After cooling, move into a 100mL volumetric flask. Use water to dilute to the scale. Mix well. 1mL of this solution contains 1000??g of barium.
3.14 Zirconium standard storage solution: Weigh 0.1351g of high-purity
6.3 Blank test
Conduct blank test with test materials.
6.4 Determination
6.4.1 Place the test material (6.1) in a 30mL Teflon digestion tank. Add 12mL of hydrochloric acid (3.1), 3mL of nitric acid (3.2), 2mL of hydrogen peroxide (3.3), 0.3mL (about 8 drops) of hydrofluoric acid (3.4). Tighten the lid. Place in an oven at a constant temperature of 150??C for 12h. Take it out. Open the tank after cooling to room temperature. Use distilled water to transfer all samples into a 200mL beaker. Steam on an electric stove to about 10mL. Move into a 100mL volumetric flask. Use
6.4.2 Preparation methods:
STD-1: Pipette 1.00mL of mixed standard solution I (3.15) and 0.50mL of mixed standard solution II (3.16) respectively into a 100mL volumetric flask. Use hydrochloric acid (3.7) to dilute to the scale. Mix well.
STD-2: Pipette 5.00mL of mixed standard solution I (3.15) and 5.00mL of mixed standard solution II (3.16) respectively into a 100mL volumetric flask. Use hydrochloric acid (3.7) to dilute to the scale. Mix well.
STD-3: Pipette 2.00mL of cerium and zirconium standard stock solutions (3.9, 3.14), 1.00mL of lanthanum, praseodymium, neodymium, and barium standard stock solutions (3.10~3.13) respectively into a 100mL volumetric flask. Use hydrochloric acid (3.7) to dilute to the scale. Mix well.
STD-4: Pipette 5.00mL of cerium and zirconium standard stock solutions (3.9, 3.14), 2.50mL of lanthanum, praseodymium, neodymium, and barium stock
solutions (3.10~3.13) respectively into a 100mL volumetric flask. Use
hydrochloric acid (3.7) to dilute to the scale. Mix well.
STD-5: Pipette 10.00mL of cerium and zirconium standard stock solutions (3.9, 3.14), 5.00mL of lanthanum, praseodymium, neodymium, and barium standard stock solutions (3.10~3.13) respectively into a 100mL volumetric flask. Use hydrochloric acid (3.7) to dilute to the scale. Mix well.
6.4.3 Drawing of working curve: Prepare the standard solution shown in Table 2. Make working curve under selected ICP-AES instrument conditions. The linear correlation coefficient of the working curve of each element shall be ???0.9995.

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