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GB/T 13747.27-2020: Methods for chemical analysis of zirconium and zirconium alloys - Part 27: Determination of trace impurities content - Inductively coupled plasma mass spectrometry
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Methods for chemical analysis of zirconium and zirconium alloys - Part 27: Determination of trace impurities content - Inductively coupled plasma mass spectrometry
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GB/T 13747.27-2020
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Basic data | Standard ID | GB/T 13747.27-2020 (GB/T13747.27-2020) | | Description (Translated English) | Methods for chemical analysis of zirconium and zirconium alloys - Part 27: Determination of trace impurities content - Inductively coupled plasma mass spectrometry | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H14 | | Classification of International Standard | 77.120.99 | | Word Count Estimation | 6,639 | | Date of Issue | 2020-03-06 | | Date of Implementation | 2021-02-01 | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration | | Summary | This standard specifies methods for the determination of boron, magnesium, aluminum, titanium, vanadium, chromium, manganese, cobalt, nickel, copper, molybdenum, tin, hafnium, tungsten, lead and uranium content in zirconium and zirconium alloys. This standard applies to the determination of boron, magnesium, aluminum, titanium, vanadium, chromium, manganese, cobalt, nickel, copper, molybdenum, tin, hafnium, tungsten, lead and uranium in sponge zirconium, zirconium and zirconium alloys. Measurement range: 0.00005%~0.010%. When the measurement range overlaps with other parts of GB/T 13747, the method of other parts shall be used as the arbitration method. | GB/T 13747.27-2020: Methods for chemical analysis of zirconium and zirconium alloys - Part 27: Determination of trace impurities content - Inductively coupled plasma mass spectrometry
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Methods for chemical analysis of zirconium and zirconium alloys - Part 27.Determination of trace impurities content - Inductively coupled plasma mass spectrometry
ICS 77.120.99
H14
National Standards of People's Republic of China
Chemical analysis methods of zirconium and zirconium alloys
Part 27.Determination of Trace Impurity Elements
Inductively coupled plasma mass spectrometry
2020-03-06 released
2021-02-01 implementation
State Administration for Market Regulation
Issued by the National Standardization Management Committee
Foreword
GB/T 13747 "Methods for Chemical Analysis of Zirconium and Zirconium Alloys" is planned to be divided into 27 parts.
---Part 1.Determination of the amount of tin potassium iodate titration and phenylfluorone-polyethylene glycol octylphenyl ether spectrophotometry;
---Part 2.Determination of iron content 1,10-phenanthroline spectrophotometry and inductively coupled plasma atomic emission spectrometry;
---Part 3.Determination of nickel content diacetyl oxime spectrophotometry and inductively coupled plasma atomic emission spectrometry;
---Part 4.Determination of chromium content Diphenylcarbazide spectrophotometry and inductively coupled plasma atomic emission spectrometry;
---Part 5.Determination of aluminum content Chromazurol S-tetradecylpyridinium chloride spectrophotometric method;
---Part 6.Determination of copper content 2,9-dimethyl-1,10-phenanthroline spectrophotometry;
---Part 7.Determination of manganese content, potassium periodate spectrophotometry and inductively coupled plasma atomic emission spectrometry;
---Part 8.Determination of Drill Volume Nitroso R Salt Spectrophotometry;
---Part 9.Determination of magnesium content by flame atomic absorption spectrometry;
---Part 10.Determination of Tungsten Content Thiocyanate Spectrophotometric Method;
---Part 11.Determination of molybdenum content thiocyanate spectrophotometric method;
---Part 12.Determination of silicon content molybdenum blue spectrophotometry;
---Part 13.Determination of lead content by polarography;
---Part 14.Polarographic method for the determination of uranium content;
---Part 15.Determination of boron content Curcumin spectrophotometric method;
---Part 16; Determination of chlorine content, silver chloride turbidity method and ion selective electrode method;
---Part 17.Determination of cadmium content by polarography;
---Part 18.Determination of vanadium content Benzoyl phenyl hydroxylamine spectrophotometric method;
---Part 19.Determination of Titanium Content Diantipyrine methane spectrophotometry and inductively coupled plasma atomic emission spectrometry;
---Part 20.Determination of hafnium content inductively coupled plasma atomic emission spectrometry;
---Part 21.Determination of the amount of hydrogen inert gas melting infrared absorption method/thermal conductivity method;
---Part 22.Determination of oxygen and nitrogen content inert gas melting infrared absorption method/thermal conductivity method;
---Part 23.Determination of Nitrogen Content Distillation Separation-Nessler Reagent Spectrophotometry;
---Part 24.Determination of carbon content high frequency combustion infrared absorption method;
---Part 25.Determination of the amount of niobium 5-Br-PADAP spectrophotometry and inductively coupled plasma atomic emission spectrometry;
---Part 26.Determination of alloys and impurity elements inductively coupled plasma atomic emission spectrometry;
--- Part 27.Determination of trace impurity elements inductively coupled plasma mass spectrometry.
This part is part 27 of GB/T 13747.
This section was drafted in accordance with the rules given in GB/T 1.1-2009.
This part was proposed by China Nonferrous Metals Industry Association.
This part is under the jurisdiction of the National Nonferrous Metals Standardization Technical Committee (SAC/TC243).
Drafting organizations of this section. Xi'an Hantang Analysis and Testing Co., Ltd., Baoti Group Co., Ltd., Guangdong Industrial Analysis and Testing Center, Beikuang
Testing Technology Co., Ltd., Youyan Yijin New Materials Co., Ltd., National Nuclear Zirconium and Hafnium Physical and Chemical Testing Co., Ltd., National Standard (Beijing) Inspection and Certification Co., Ltd.
the company.
The main drafters of this section. Wang Jinlei, Ma Xiaomin, Liu Ting, Li Jian, Sun Baolian, Luo Lin, Wang Jin, Liu Chunfeng, Liu Chaofang, Pang Xin, Lu Chao,
Wang Lan, Li Gang, Sun Haifeng, Li Manzhi.
Chemical analysis methods of zirconium and zirconium alloys
Part 27.Determination of Trace Impurity Elements
Inductively coupled plasma mass spectrometry
1 Scope
This part of GB/T 13747 specifies boron, magnesium, aluminum, titanium, vanadium, chromium, manganese, cobalt, nickel, copper, molybdenum, tin, hafnium, tungsten, lead, and lead in zirconium and zirconium alloys.
Method for determination of uranium content.
This section applies to the content of boron, magnesium, aluminum, titanium, vanadium, chromium, manganese, cobalt, nickel, copper, molybdenum, tin, hafnium, tungsten, lead and uranium in sponge zirconium, zirconium and zirconium alloys
The determination. Measuring range. 0.00005%~0.010%. When the measurement range overlaps with other parts of GB/T 13747,
Law is the method of arbitration.
2 Principle
The sample is dissolved in nitric acid and hydrofluoric acid, calibrated with thulium internal standard, and directly measured by inductively coupled plasma mass spectrometer, according to the working curve
The method calculates the mass concentration of each element and expresses the measurement result in mass fraction.
3 reagent
Unless otherwise stated, only reagents and laboratory first-grade water confirmed to be pure superior grade are used in the analysis.
3.1 Hydrofluoric acid (ρ=1.13g/mL).
3.2 Nitric acid (ρ=1.42g/mL).
3.3 Single element standard storage solutions of boron, magnesium, aluminum, titanium, vanadium, chromium, manganese, cobalt, nickel, copper, molybdenum, tin, hafnium, tungsten, lead, uranium and thulium (national standard sample/
National standard material), the mass concentration is 1000μg/mL.
3.4 Mixed standard solution A. Pipette 1.00mL of each element standard stock solution (except thulium element) (3.3) into 100mL plastic volume.
In the bottle, add 2 mL of nitric acid (3.2), dilute to the mark with water, and mix. This solution 1mL contains boron, magnesium, aluminum, titanium, vanadium, chromium, manganese, cobalt, nickel,
Copper, molybdenum, tin, hafnium, tungsten, lead, and uranium each 10μg.
3.5 Mixed standard solution B. Pipette 10.00mL mixed standard solution A (3.4) into a 100mL plastic volumetric flask, add 2mL nitric acid
(3.2), dilute to the mark with water, and mix well. This solution 1mL contains boron, magnesium, aluminum, titanium, vanadium, chromium, manganese, cobalt, nickel, copper, molybdenum, tin, hafnium, tungsten, lead and
Uranium is 1μg each, ready to use when used.
3.6 Thulium internal standard solution. pipette 1.00mL thulium element standard stock solution (3.3) into a 1000mL plastic volumetric flask, and add 2mL nitric acid
(3.2), dilute to the mark with water, and mix well. This solution 1mL contains 1μg thulium.
3.7 Liquid argon or high-purity argon (purity≥99.99%).
4 Instruments
4.1 Inductively coupled plasma mass spectrometer. mass resolution is better than 0.8u±0.1u (at 10% peak height); equipped with hydrofluoric acid resistant injection system
System; equipped with components that can eliminate interfering ions such as 38Ar1H, 40Ar and 40Ar16O.
4.2 The isotope determination of each element is shown in Table 1.
5 samples
Process the sample into chips with a length not greater than 5mm.
6 Test procedure
6.1 Sample
Weigh 0.10g sample (Chapter 5), accurate to 0.0001g.
6.2 Number of determinations
Do two tests in parallel and take the average value.
6.3 Blank test
Make a blank test with the sample.
6.4 Preparation of analysis test solution
Place the sample (6.1) in a 100mL polytetrafluoroethylene beaker, blow a small amount of water along the wall of the cup, add 3mL nitric acid (3.2), 1mL
Hydrofluoric acid (3.1), heat at low temperature until the sample is completely dissolved, cool, transfer to a 100mL plastic volumetric flask, add 1.00mL thulium internal standard solution
(3.6), dilute to the mark with water, and mix well.
6.5 Preparation of working curve solution
Pipette 0mL, 0.10mL, 0.50mL, 1.00mL, 2.00mL, 5.00mL, 10.00mL mixed standard solution B (3.5) in a series
In a 100mL plastic volumetric flask, add 1.00mL Thulium internal standard solution (3.6), dilute to the mark with water, and mix.
6.6 Determination
6.6.1 On the inductively coupled plasma mass spectrometer, after the instrument is running stably, under the selected instrument working conditions, perform the same position as recommended in Table 1.
Prime mass number, use the prepared standard series solution (6.5) to calibrate the calibration working curve, the correlation coefficient of the working curve of each element should be 0.999
Above, otherwise it is necessary to re-standardize or re-formulate standard series solutions for standardization.
6.6.2 Determination of analysis test solution (6.4) and blank test solution (6.3). The instrument automatically processes data according to the working curve, calculates and outputs each element
Element mass concentration.
7 Test data processing
The content of each element is calculated by mass fraction wx, expressed in %, and calculated according to formula (1).
Where.
ρx --- the mass concentration of the element to be tested in the test solution, in nanograms per milliliter (ng/mL);
ρ0 --- The mass concentration of the element to be tested in the blank test solution, in nanograms per milliliter (ng/mL);
V ---The volume of the analysis test solution, in milliliters (mL);
m ---The mass of the sample, in grams (g).
Analysis results Magnesium, aluminum, titanium, vanadium, chromium, manganese, cobalt, nickel, copper, molybdenum, tin, hafnium, tungsten, lead and uranium elements should be expressed to four decimal places; boron element
It should be expressed to five decimal places.
8 tolerance
The difference between the analysis results between the laboratories should not be greater than the relative tolerance listed in Table 2.
9 Test report
The test report should include the following.
---Test object;
---This standard number;
---result;
--- Anomalies observed;
---Test date.
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