GB/T 223.88-2019 English PDF (GBT223.88-2019)

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GB/T 223.88-2019: Iron, steel and alloy -- Determination of calcium and magnesium contents -- Inductively coupled plasma atomic emission spectrometric method
GB/T 223.88-2019
Iron, steel and alloy--Determination of calcium and magnesium contents--Inductively coupled plasma atomic emission spectrometric method
ICS 77.080.01
H11
National Standards of People's Republic of China
Determination of calcium and magnesium in steel and alloys
Inductively coupled plasma atomic emission spectrometry
(ISO 13933.2014, Steelandiron-Determinationofcalciumandmagnesium-
Inductivelycoupledplasmaatomicemissionspectrometricmethod, IDT)
Published on.2019-06-04
2020-05-01 implementation
State market supervision and administration
China National Standardization Administration issued
Foreword
GB/T 223 is divided into several parts.
This part is the 88th part of GB/T 223.
This part is drafted in accordance with the rules given in GB/T 1.1-2009.
This section uses the translation method equivalent to ISO 13933.2014 "Steel calcium and magnesium determination inductively coupled plasma atomic emission
Spectroscopy.
The documents of our country that have a consistent correspondence with the international documents referenced in this part are as follows.
---GB/T 6682-2008 Analytical laboratory water specifications and test methods (ISO 3696.1987, MOD)
---GB/T 12806-2011 Laboratory glass instrument single standard line volumetric flask (ISO 1042.1998, MOD)
---GB/T 20066-2006 Sampling and sample preparation method for samples for determination of chemical composition of steel and iron (ISO 14284.1996,
IDT)
This section has made the following editorial changes.
--- In line with the existing standard series, change the name of this part to "Inductive Coupling Isolation of Determination of Calcium and Magnesium Content in Steel and Alloys"
Daughter atomic emission spectrometry.
This part was proposed by the China Iron and Steel Association.
This part is under the jurisdiction of the National Steel Standardization Technical Committee (SAC/TC183).
This section drafted by. Steel Research Nak Testing Technology Co., Ltd., Baosteel Special Steel Co., Ltd., Anshan Iron and Steel Co., Ltd., Wuhan Steel
Iron Co., Ltd., China Metallurgical Construction Research Institute Co., Ltd.
The main drafters of this section. Luo Qianhua, Liu Zheng, Wang Yujuan, Yu Yuanjun, Yu Lujun, Lin Chunlai, Li Nannan.
Determination of calcium and magnesium in steel and alloys
Inductively coupled plasma atomic emission spectrometry
1 Scope
This part of GB/T 223 specifies the determination of pure iron, cast iron, steel and superalloys by inductively coupled plasma atomic emission spectrometry.
Method of calcium and magnesium content.
This section applies to the magnesium content with a mass fraction of 0.0005%~0.006% and a magnesium content of 0.0005%~0.20%.
Determination.
2 Normative references
The following documents are indispensable for the application of this document. For dated references, only dated versions apply to this article.
Pieces. For undated references, the latest edition (including all amendments) applies to this document.
ISO 385 laboratory glass instrument burette (Laboratoryglassware-Burettes)
ISO 648 laboratory glass instrument single-line pipette (Laboratoryglassware-Single-volumepipettes)
ISO 1042 laboratory glass instrument single line volumetric flask (Laboratoryglassware-Onemarkvolumetricflasks)
ISO 3696 Analytical Laboratory Water Regulations and Test Methods (Waterforanalyticallaboratoryuse-Specification
Andtestmethods)
ISO 14284 Method for sampling and sample preparation of steel and iron chemical constituents (Steelandiron-Samplingand
Preparationofsamplesforthedeterminationofchemicalcomposition)
3 Principle
The sample was dissolved with a mixed acid of hydrochloric acid, nitric acid and hydrofluoric acid, and perchloric acid smoked. The salts are dissolved with hydrochloric acid and nitric acid. If necessary, join inside
Label the element and dilute to a certain volume. The solution is filtered (if necessary) and atomized into an inductively coupled plasma spectrometer, measuring each
The element analyzes the emission intensity of the line while measuring the emission intensity of the internal standard element line.
4 reagents
Unless otherwise stated, only analytically pure reagents identified as low levels of calcium and magnesium and secondary waters specified in ISO 3696 were used in the analysis.
Or water of considerable purity.
4.1 The content of pure iron, calcium and magnesium is less than 0.5μg/g.
4.2 Hydrochloric acid, ρ about 1.19g/mL.
4.3 Hydrochloric acid, ρ approximately 1.19 g/mL, diluted to 1 1.
4.4 Hydrochloric acid, ρ approximately 1.19 g/mL, diluted to 14.
4.5 Hydrochloric acid, ρ approximately 1.19 g/mL, diluted to 1 100.
4.6 Nitric acid, ρ about 1.42g/mL.
4.7 Hydrofluoric acid, ρ about 1.15g/mL.
4.8 Perchloric acid, ρ about 1.67g/mL.
4.9 Mixed acid.
2 parts of hydrochloric acid (4.2), 1 part of nitric acid (4.6) and 3 parts of water were mixed.
4.10 Calcium standard solution.
4.10.1 Calcium stock solution, 1000mg/L.
Dry a few grams of calcium carbonate (mass fraction ≥99.9%) in an oven at 100 °C ± 5 °C for at least 1 h and cool to room in a desiccator
temperature. Weigh 2.497g of dried calcium carbonate to the nearest 0.0001g, place in a 400mL beaker, add 20mL of hydrochloric acid (4.3), cover the table
The dish is slowly heated until completely dissolved. After cooling to room temperature, the solution was transferred to a 1000 mL volumetric flask. Dilute to the mark with water,
Mix well.
This stock solution 1 mL contains 1.000 mg of calcium.
4.10.2 Calcium standard solution A, 100 mg/L.
Transfer 10.00 mL of calcium stock solution (4.10.1) into a 100 mL volumetric flask. Add 10 mL of hydrochloric acid (4.4). Dilute to the mark with water,
Mix well.
1 mL of this standard solution contained 0.100 mg of calcium.
4.10.3 Calcium standard solution B, 10 mg/L.
10.00 mL of calcium standard solution A (4.10.2) was transferred to a 100 mL volumetric flask. Add 10 mL of hydrochloric acid (4.4). Dilute with water to the moment
Degree, mix.
1 mL of this standard solution contained 0.010 mg of calcium.
4.10.4 Calcium standard solution C, 1.0 mg/L.
10.00 mL of calcium standard solution B (4.10.3) was transferred to a 100 mL volumetric flask. Add 10 mL of hydrochloric acid (4.4). Dilute with water to the moment
Degree, mix.
1 mL of this standard solution contained 0.001 mg of calcium.
4.11 Magnesium standard solution.
4.11.1 Magnesium stock solution, 1000mg/L.
1.000 g of pure magnesium (mass fraction ≥ 99.9%) was weighed to the nearest 0.0001 g and placed in a 250 mL beaker. Add 20mL of water, then
After that, hydrochloric acid (4.3) was added dropwise under constant shaking until the reaction was stopped, and hydrochloric acid (4.3) was further added to a total volume of 20 mL. Cover the watch glass, add
Heat boil for 10 min. Cool to room temperature, transfer to a 1000 mL volumetric flask, dilute to the mark with water, and mix.
This stock solution 1 mL contains 1.000 mg of magnesium.
4.11.2 Magnesium standard solution A, 100mg/L.
10.00 mL of magnesium stock solution (4.11.1) was transferred to a 100 mL volumetric flask. Add 10 mL of hydrochloric acid (4.4) and dilute to the mark with water.
Mix well.
1 mL of this standard solution contained 0.100 mg of magnesium.
4.11.3 Magnesium standard solution B, 10 mg/L.
10.00 mL of Magnesium Standard Solution A (4.11.2) was transferred to a 100 mL volumetric flask. Add 10mL hydrochloric acid (4.4), dilute with water until the moment
Degree, mix.
1 mL of this standard solution contained 0.010 mg of magnesium.
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