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GB/T 34208-2017 (GB/T34208-2017)

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GB/T 34208-2017: PDF in English (GBT 34208-2017)
GB/T 34208-2017
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.080.01
H 11
Iron and steel – Determination of antimony and tin
content – Inductively coupled plasma atomic emission
spectrometric method
ISSUED ON. SEPTEMBER 7, 2017
IMPLEMENTED ON. JUNE 1, 2018
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of the People's Republic of China;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative References ... 4 
3 Principle ... 4 
4 Reagents and materials ... 5 
5 Instruments and equipment ... 6 
6 Sampling and preparation of specimen ... 7 
7 Analytical procedure ... 7 
8 Calculation of results ... 8 
9 Precision ... 9 
10 Test report ... 10 
Annex A (Normative) Standard operation of measuring instruments ... 11 
Annex B (Informative) Additional data of joint precision test ... 1 
Iron and steel – Determination of antimony and tin
content – Inductively coupled plasma atomic emission
spectrometric method
1 Scope
This Standard specifies the method for the determination of antimony and tin content
using the inductively coupled plasma atomic emission spectrometric method.
This Standard applies to the determination of antimony and tin content in carbon steel
and low alloy steel of chromium content (mass fraction) less than 1.50% and nickel
content (mass fraction) less than 2.00%. the measuring range of antimony (mass
fraction) is 0.002 0% ~ 0.12%; the measuring range of tin (mass fraction) is 0.002 0%
~ 0.13%.
2 Normative References
The following referenced documents are indispensable for the application of this
document. For dated references, only the edition dated applies to this document. For
undated references, the latest edition of the referenced documents (including all
amendments) applies to This Standard.
GB/T 6379.2, Accuracy (trueness and precision) of measurement methods and
results – Part 2. Basic method for the determination of repeatability and
reproducibility of a standard measurement method
GB/T 6682, Water for analytical laboratory use – Specification and test methods
GB/T 20066, Steel and iron – Sampling and preparation of samples for the
determination of chemical composition
3 Principle
Use the mixed acid of hydrochloric acid and nitric acid to dissolve specimen; dilute to
a certain volume. After atomizing the specimen solution, introduce into the inductively
coupled plasma atomic emission spectrometer; measure the spectral intensity of all
measured elements’ analytical lines. In accordance with the calibration curve
established, calculate the mass fraction of all analytical elements.
4 Reagents and materials
Unless specified otherwise, only use certified analytically pure reagents and grade II
water specified in GB/T 6682 in the analysis.
4.1 High-purity iron, ρ about 1.19 g/mL.
4.2 Nitric acid, ρ about 1.42 g/mL.
4.3 Nitric acid, ρ about 1.42 g/mL, diluted to be 1 + 1.
4.4 Antimony standard solution
4.5 Antimony stock solution, 500 μg/mL
Weigh 1.371 5 g of antimony potassium tartrate (C4H4KOSb·ଵଶ H2O) pre-dried in a
desiccator; dissolve in hydrochloric acid (1 + 9); transfer to a 1,000 mL volumetric flask;
use hydrochloric acid (1 + 9) to dilute to scale; mix up.
1 mL of the solution contains 500 μg of antimony.
A merchant certified antimony standard solution can also be used.
4.5.1 Antimony standard solution, 10.0 μg/mL
Transfer 2.00 mL of antimony stock solution (4.5.1) to a 100 mL volumetric flask; use
hydrochloric acid (1 + 9) to dilute to scale; mix up.
1 mL of the solution contains 10.0 μg of antimony.
4.5.2 Tin standard solution
4.6 Tin standard solution
4.6.1 Tin stock solution, 500 μg/mL
Weigh 0.500 0 g of high-purity tin (mass fraction not less than 99.9%); place into a 200
mL beaker. Add 40 mL of hydrochloric acid (1 + 1); heat to dissolve. After cooling to
room temperature, transfer the solution into a 1,000 mL volumetric flask; use
hydrochloric acid to dilute to scale; mix up.
1 mL of the solution contains 500 μg of tin.
A merchant certified antimony standard solution can also be used.
4.6.2 Tin standard solution, 10.0 μg/mL
Spray in blank test solutions for about 10 s; measure 10 times using the preset integral
time.
Spray in 10 times detection limit solutions about 10 s; measure 10 times using the
preset integral time.
Based on the readings of intensity obtained from blank solutions and 10 times
detection limit solutions, calculate the average intensity of blank solutions Xഥ b, the
average intensity of 10 times detection limit solutions Xഥ1 and the standard deviation of
blank sb.
Calculate the net average intensity of 10 times detection limit solutions (Xഥ n1) in
accordance with Equation (A.1).
Calculate the detection limit of tested elements (DL) in accordance with Equation (A.2).
where.
ρ1 – the concentration of 10 times detection limit solutions, in μg/mL;
It shall be indicated that, because of limited number of repeated measurements, the
errors of detection limit calculated using this method are within a wide range.
A.2.3 Determination of background equivalent concentration
Calculate the background equivalent concentration (BEC) in accordance with Equation
(A.3).
A.3 Spectral line interferences
Spectral line inferences make the intensities of tested elements’ analytical lines on the
high side, so spectral interference calibration needs to be done.
Prepare respectively one solution containing 1 mg/L of tested elements and one
solution containing 1,000 mg/L of interfering elements.
Spray in respectively water, 1 mg/L tested element solution and 1,000 mg/L interfering
element solution; measure the absolution intensities of the tested elements’ analytical
lines.
Obtain the net analytical intensity In by subtracting the absolute intensity of 1 mg/L
tested element solution by the intensity of water.
......
 
(Above excerpt was released on 2018-06-02, modified on 2021-06-07, translated/reviewed by: Wayne Zheng et al.)
Source: https://www.chinesestandard.net/PDF.aspx/GBT34208-2017