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GB/T 5687.12-2020: Ferrochromium - Determination of phosphorus, aluminum, titanium, copper, manganese, calcium content - Inductively coupled plasma atomic emission spectrometric method
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Ferrochromium - Determination of phosphorus, aluminum, titanium, copper, manganese, calcium content - Inductively coupled plasma atomic emission spectrometric method
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GB/T 5687.12-2020
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Basic data | Standard ID | GB/T 5687.12-2020 (GB/T5687.12-2020) | | Description (Translated English) | Ferrochromium - Determination of phosphorus, aluminum, titanium, copper, manganese, calcium content - Inductively coupled plasma atomic emission spectrometric method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H11 | | Classification of International Standard | 77.100 | | Word Count Estimation | 14,186 | | Date of Issue | 2020-06-02 | | Date of Implementation | 2020-09-01 | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration | GB/T 5687.12-2020: Ferrochromium - Determination of phosphorus, aluminum, titanium, copper, manganese, calcium content - Inductively coupled plasma atomic emission spectrometric method
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Ferrochromium - Determination of phosphorus, aluminum, titanium, copper, manganese, calcium content - Inductively coupled plasma atomic emission spectrometric method
ICS 77.100
H11
National Standards of People's Republic of China
Chromium iron phosphorus, aluminum, titanium, copper, manganese, calcium
Inductively coupled plasma
Atomic emission spectrometry
2020-06-02 released
2020-09-01 Implementation
State Administration for Market Regulation
Issued by the National Standardization Management Committee
Foreword
GB/T 5687 is divided into the following parts.
---GB/T 5687.2 Determination of the content of ferrochromium, silicon-chromium alloy and chromium-iron-silicon nitride perchloric acid dehydration gravimetric method;
---GB/T 5687.4 Determination of Nitrogen Content of Ferrochromium Nitride and High Nitrogen Chromium Iron Distillation-Neutralization Titration Method;
---GB/T 5687.10 Determination of chromium, iron and manganese content by flame atomic absorption spectrometry;
---GB/T 5687.11 Determination of chromium iron titanium content Diantipyrine methane spectrophotometric method;
---GB/T 5687.12 Determination of chromium iron phosphorus, aluminum, titanium, copper, manganese, calcium content inductively coupled plasma atomic emission light
Spectrum method;
This part is Part 12 of GB/T 5687.
This section was drafted in accordance with the rules given in GB/T 1.1-2009.
This part was proposed by the China Iron and Steel Association.
This part is under the jurisdiction of the National Pig Iron and Ferroalloy Standardization Technical Committee (SAC/TC318).
Drafting organizations of this section. Benxi Steel Plate Co., Ltd., Inner Mongolia Ordos Power Metallurgical Group Co., Ltd., Liuzhou, Guangxi
Iron and Steel Group Co., Ltd., Anhui Changjiang Iron and Steel Co., Ltd., Jiangsu Yinxin Iron and Steel Group Co., Ltd., Shougang Co., Ltd. Qian'an Steel
Iron Company, Beijing MCC Equipment Research and Design Institute Co., Ltd., Jiaocheng Yiwang Ferroalloy Co., Ltd., China Metallurgical Construction Research Institute Co., Ltd.
Company, Metallurgical Industry Information Standard Research Institute.
The main drafters of this section. Yang Weixiu, Wang Yapeng, Tang Yu, Tian Yuwei, Chen Rong, Lin Zhiwang, Chen Hai, Zhang Xianfeng, Ma Ning, Bo Fenghua,
Gu Hongqin, Yu Shurong, Du Shiyi, Tan Danliu, Wang Lixia, Sun Juan, Cui Yuwen, Liu Feiyu, Huang Zhimin, Lu Chunsheng.
Chromium iron phosphorus, aluminum, titanium, copper, manganese, calcium
Inductively coupled plasma
Atomic emission spectrometry
Warning---The personnel using this section should have formal laboratory work experience. This section does not point out all possible security issues.
The user is responsible for taking appropriate safety and health measures to ensure compliance with the conditions stipulated by relevant national laws and regulations.
1 Scope
This part of GB/T 5687 specifies the use of inductively coupled plasma atomic emission spectrometry (ICP-AES) for the determination of phosphorus, aluminum, titanium,
Method for the content of copper, manganese, calcium and other elements.
This section applies to the determination of phosphorus, aluminum, titanium, copper, manganese, calcium content in ferrochromium, and the determination of the corresponding elements of silicon-chromium alloy is also applicable to this section.
The measurement range of each element is shown in Table 1.
Table 1 Elements and measurement range
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article
Pieces. For undated references, the latest version (including all amendments) applies to this document.
GB/T 4010 Collection and preparation of samples for chemical analysis of ferroalloys
GB/T 6682 Analytical laboratory water specifications and test methods
GB/T 8170 Numerical rounding rules and the expression and determination of limit values
GB/T 12806 Laboratory glassware single mark volumetric flask
GB/T 12807 Laboratory Glass Apparatus Indexing Pipette
GB/T 12808 Single-marked pipette for laboratory glassware
JJG768 Emission Spectrometer Verification Regulations
3 Principle
The low-carbon sample is decomposed by hydrochloric acid, hydrogen peroxide, hydrofluoric acid and perchloric acid, and in a smoking state, hydrochloric acid is added dropwise to volatilize chromium and prepared into hydrochloric acid solution
Liquid; high-carbon sample is melted in a nickel crucible with sodium peroxide, leached with acid, and diluted to a certain volume. Use high salt resistant atomizer and corresponding fog
In the chemical chamber, use the inductively coupled plasma atomic emission spectrometer (ICP-AES) to measure the emission spectrum intensity of the analytical elements in the test solution, or to yttrium
On the calibration curve, calculate the mass fraction of the analysis element.
4 reagent
In the analysis, unless otherwise specified, only use reagents of superior grade and above purity and laboratory grade two and laboratory grades that comply with GB/T 6682
Above water.
4.1 Pure chromium, the content of the element to be tested is less than 0.001% (mass fraction).
4.2 Pure iron (≥99.98% or known analytical elements).
4.3 Sodium peroxide.
4.4 Perchloric acid, ρ=1.67g/mL.
4.5 Hydrofluoric acid, ρ=1.15g/mL.
4.6 Hydrogen peroxide (30%).
4.7 Hydrochloric acid, ρ=1.19g/mL.
4.8 Hydrochloric acid, 1 1.
4.9 Nitric acid, 1.42g/mL.
4.10 Nitric acid, 1 1.
4.11 Standard solution
4.11.1 Phosphorus standard stock solution
4.11.1.1 Phosphorus standard stock solution, 0.50mg/mL
Weigh 2.1968g of potassium dihydrogen phosphate ( >99.95%) which has been dried to constant weight at 105℃±5℃ in advance and cooled to room temperature. Use appropriate amount of water
Dissolve, transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix.
4.11.1.2 Phosphorus standard solution, 100.00μg/mL
Dilute 20.00mL phosphorus standard stock solution (see 4.11.1.1), add 20mL hydrochloric acid (see 4.7) in a 100mL volumetric flask, and dilute with water
Release to the mark and mix well.
4.11.1.3 Phosphorus standard solution, 10.00μg/mL
Aliquot 10.00mL phosphorus standard stock solution (see 4.11.1.1), add 20mL hydrochloric acid (see 4.7) in a 500mL volumetric flask, and dilute with water
Release to the mark and mix well.
4.11.2 Aluminum standard solution
4.11.2.1 Aluminum standard stock solution, 1.00mg/mL
Weigh 1.0000g metal aluminum (≥99.95%) into a 250mL PTFE beaker, add 30mL hydrochloric acid (see 4.8), add at low temperature
Heat to dissolve, cool to room temperature, transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix.
Note. (Weigh 1.0000g metal aluminum (≥99.95%) in a polytetrafluoroethylene beaker, add 30mL sodium hydroxide solution (200g/L), heat and dissolve at low temperature,
Add 100mL water, add hydrochloric acid (see 4.7) dropwise to acidify and excess 10mL, cool to room temperature, transfer to a 1000mL volumetric flask, dilute to the mark with water,
Mix well).
4.11.2.2 Aluminum standard solution, 100.00μg/mL
Dispense 10.00mL aluminum standard stock solution (see 4.11.2.1) into a 100mL volumetric flask, add 20mL hydrochloric acid (see 4.7), and dilute with water
To the mark, mix well.
4.11.2.3 Aluminum standard solution, 10.00μg/mL
Dilute 5.00mL aluminum standard stock solution (see 4.11.2.1) into a 500mL volumetric flask, add 20mL hydrochloric acid (see 4.7), and dilute with water
To the mark, mix well.
4.11.3 Titanium standard solution
4.11.3.1 Titanium standard stock solution, 0.50mg/mL
Weigh 0.5000g spectral pure titanium metal, add 10mL hydrofluoric acid (see 4.5) and 20mL sulfuric acid (11) in a 100mL platinum dish.
Decompose, heat and evaporate until sulfuric acid fumes are emitted, rinse the platinum dish with water, and continue to heat until sulfuric acid fumes are emitted to drive off the fluorine. Cool to room temperature, add about 50mL water to dissolve
To dissolve salts, transfer to a 1000mL volumetric flask, wash the platinum dish with sulfuric acid (1 9), merge the washing liquid into the volumetric flask, and dilute with sulfuric acid (1 9)
To the mark, mix well.
4.11.3.2 Titanium standard solution, 100.00μg/mL
Take 20.00mL titanium standard stock solution (see 4.11.3.1), add 20mL hydrochloric acid (see 4.7) in a 100mL volumetric flask, dilute with water
Release to the mark and mix well.
4.10.3.3 Titanium standard solution, 10.00μg/mL
Take 10.00mL titanium standard stock solution (see 4.11.3.1), add 20mL hydrochloric acid (see 4.7) in a 500mL volumetric flask, dilute with water
Release to the mark and mix well.
4.11.4 Copper standard solution
4.11.4.1 Copper standard stock solution, 1.00mg/mL
Weigh 1.000g of metallic copper (≥99.95%), add 30mL of nitric acid (see 4.10) in a 250mL beaker, dissolve at low temperature, and cook.
Boil to drive off nitrogen oxides, cool to room temperature, transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix.
4.11.4.2 Copper standard solution, 100.00μg/mL
Take 10.00mL copper standard stock solution (see 4.11.4.1), add 20mL hydrochloric acid (see 4.7) in a 100mL volumetric flask, dilute with water
Release to the mark and mix well.
4.11.4.3 Copper standard solution, 10.00μg/mL
Take 5.00mL copper standard stock solution (see 4.11.4.1), add 20mL hydrochloric acid (see 4.7) in a 500mL volumetric flask, and dilute with water
To the mark, mix well.
4.11.5 Manganese standard solution
4.11.5.1 Manganese standard stock solution, 1.00mg/mL
Weigh 1.000g electrolytic manganese (≥99.95%), add 30mL nitric acid (see 4.10) in a 250mL beaker, heat to dissolve, and boil to drive it away
Nitrogen oxides, cool to room temperature, transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix.
4.11.5.2 Manganese standard solution, 100.00μg/mL
Aliquot 10.00mL manganese standard stock solution (see 4.11.5.1), add 20mL hydrochloric acid (see 4.7) in a 100mL volumetric flask, and dilute with water
Release to the mark and mix well.
4.11.5.3 Manganese standard solution, 10.00mg/mL
Take 5.00mL manganese standard stock solution (see 4.11.5.1), add 20mL hydrochloric acid (see 4.7) in a 500mL volumetric flask, and dilute with water
To the mark, mix well.
4.11.6 Calcium standard solution
4.11.6.1 Calcium standard stock solution, 0.50mg/mL
Weigh 2.4973g of calcium carbonate ( >99.95%) which has been dried at 105℃±5℃ and cooled to room temperature in a desiccator in 250mL
In the beaker, add 20 mL of water, mix well, cover with a watch glass, and slowly add 20 mL of hydrochloric acid (see 4.8) until the calcium carbonate is dissolved, then add 20 mL of salt
Acid (see 4.8), boil to remove carbon dioxide, cool to room temperature, transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix.
4.11.6.2 Calcium standard solution, 100.00μg/mL
Take 20.00mL calcium standard stock solution (see 4.11.6.1), add 20mL hydrochloric acid (see 4.7) in a 100mL volumetric flask, dilute with water
Release to the mark and mix well.
4.11.6.3 Calcium standard stock solution, 10.00μg/mL
Dispense 10.00mL calcium standard stock solution (see 4.11.6.1), add 20mL hydrochloric acid (see 4.7) in a 500mL volumetric flask, and dilute with water
Release to the mark and mix well.
4.11.7 Yttrium standard stock solution,.200.0μg/mL
Weigh 0.2540g of yttrium oxide ( >99.95%) which has been burned at 750℃±5℃ for 30 minutes and cooled to room temperature in 250mL.
In the cup, add 30mL hydrochloric acid (see 4.8), heat to dissolve, cool to room temperature, transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix.
5 Instruments
5.1 Single-mark pipettes, graduated pipettes and single-mark volumetric flasks
Comply with GB/T 12806, GB/T 12807 and GB/T 12808 regulations.
5.2 Inductively coupled plasma (ICP) atomic emission spectrometer
5.2.1 Need to be equipped with a high-salt resistant atomizer and corresponding atomization chamber.
5.2.2 Inductively coupled plasma (ICP) atomic emission spectrometer should meet the detection limit (DL) and background equivalent concentration specified in Table 2
(BEC), short-term precision (RSD) performance requirements. When the element concentration in the sample solution is higher than 5000×DL, only the RSD needs to be satisfied.
1.Performance parameter requirements. The detection limit (DL), background equivalent concentration (BEC), and short-term accuracy (RSD) tests are carried out in accordance with Appendix A, and the results
Should be lower than the value in Table 2.
Table 3 lists the recommended analysis spectral lines, which are not significantly interfered by matrix elements. This method does not limit the analysis spectrum
According to the regulations, other analysis lines can also be used. Before using these analysis lines (including recommended analysis lines), carefully evaluate the spectral interference,
Background and ionization, if the recommended performance parameters cannot be met, it indicates that there may be interference.
Table 2 Recommended equivalent concentration and detection limit
5.2.3 Short-term stability
Determine the average value of the absolute intensity or intensity ratio of the standard solution with the highest concentration of each element for 10 times, and calculate the relative standard deviation.
Meet the requirements of JJG768.
5.2.4 Long-term stability
Determine the average value of the absolute intensity or intensity ratio of the standard solution with the highest concentration of each element three times, and calculate the standard deviation of the 7 average values
The relative standard deviation of the absolute strength method should meet the requirements of JJG768, and the relative standard deviation of the internal standard method should meet the requirements of JJG768.
5.2.5 Linearity of the curve
The linearity of the calibration curve is checked by the correlation coefficient, which should be greater than 0.999.
6 Sample
6.1 Laboratory samples used for analysis are prepared in accordance with the requirements of GB/T 4010.
6.2 High-carbon ferrochrome, medium-carbon ferrochrome (powder samples), and silicon-chromium alloy samples should pass through a 0.125mm mesh.
6.3 The micro-carbon, low-carbon, and medium-carbon ferrochrome samples (drilled samples) should pass through a 1.68mm sieve.
7 Analysis steps
7.1 Number of determinations
Each sample should be analyzed at least twice.
7.2 The amount of sample
Weigh 0.20g, accurate to 0.0001g.
7.3 Blank test
Do a blank test in parallel with the sample.
7.4 Determination
7.4.1 Sample decomposition
7.4.1.1 Medium-carbon, low-carbon, and micro-carbon ferrochrome (swarf-like samples) acid solution decomposition method
Place the sample in a 300mL glass beaker, add 20mL of hydrochloric acid (see 4.7), add 5mL of hydrogen peroxide (see 4.6), slightly heat to melt
When the sample has no obvious reaction, continue heating until the intense reaction stops, add about 5mL perchloric acid (see 4.4), cover with a watch glass, and heat to
Perchloric acid smokes. When chromium is oxidized, add 5mL~10mL hydrochloric acid (see 4.7) dropwise in 3~4 times to volatilize chromium until there is no yellow, and heat at low temperature
Blow off perchloric acid fumes (about 2mL~3mL solution), remove, cool slightly, rinse the cup wall and watch glass with water, add 20mL hydrochloric acid (see 4.8), drop
Add 2mL hydrogen peroxide (see 4.6), heat to dissolve, and cool to room temperature. Transfer the test solution into a 100mL volumetric flask, dilute to the mark with water, and mix
uniform. As measured by the internal standard method, before dilution, add 5.00mL yttrium standard solution (see 4.11.7).
7.4.1.2 Medium carbon ferrochrome (powder sample), silicochromic acid solution decomposition method
Place the sample in a.200mL polytetrafluoroethylene beaker, add 20mL hydrochloric acid (see 4.7), add 5mL hydrogen peroxide (see 4.6),
Dissolve the sample with slight heat until there is no obvious reaction, use a plastic tube to carefully add about 5mL of hydrofluoric acid (see 4.5), until the violent reaction stops, add about 5mL
Perchloric acid (see 4.4), cover with a polytetrafluoroethylene watch glass, and heat at low temperature until the perchloric acid emits smoke. The following is the same as 7.4.1.1.
7.4.1.3 Alkali fusion decomposition of high-carbon ferrochrome
Weigh 1.5g of sodium peroxide (see 4.3) and spread it evenly on the bottom of the nickel crucible, then weigh the sample, and stir the sample and sodium peroxide thoroughly.
Then weigh 0.5g of sodium peroxide (see 4.3) to evenly cover the surface. Put the nickel crucible with the sample into the muffle furnace and slowly heat it to
Melt the sample at 760℃, shake it every 5 minutes, until the sample melts to bright red, close the door for 15 minutes, and wait until the sample is completely dissolved.
Take it out and cool naturally, put the crucible into a 400mL glass beaker, add 50mL hot water, 5mL hydrochloric acid (see 4.7), 10mL nitrate
Acid (see 4.9), heat and boil, wash out the nickel crucible, continue heating to boiling, after the salt is dissolved, remove it and cool to room temperature, transfer to
Dilute to the mark with water in a 100mL volumetric flask and mix well. If measured by internal standard method, add 5.00mL yttrium standard solution before dilution
(See 4.11.7).
7.4.2 Preparation of calibration solution
Replace the sample with pure chromium (see 4.1) and pure iron (see 4.2) equivalent to the amount of chromium and iron in the sample, operate according to 7.4.1, and finally dilute to
Before 100mL, add each analysis element, it is recommended to add the standard solution of the measured element according to Table 4.Its concentration range should cover all analytical elements
For the concentration range of the element, each calibration curve needs more than 5 points (including 5 points) of calibration solution to form a suitable step. To separate the calibration solution
The subconcentrations are basically the same. A certain calibration solution should not be the highest or the lowest for each analysis element. If the concentration is too high, the calibration curve becomes
Non-linear, use the sub-sensitive line or appropriately dilute the sample solution and calibration solution.
Table 4 Recommended standard solutions for making standard curves
7.4.3 Adjustment of the spectrometer
Start the inductively coupled plasma emission spectrometer, and optimize the instrument according to the operating instructions. Choose suitable analysis conditions and prepare to use
Software for calibration curve drawing, measurement and statistical calculation.
Turn on the ignition key, and after ignition, confirm that the operating parameters of the instrument are within the determined range, the atomization system and the plasma flame are working normally, and the number is stable.
minute.
7.4.4 Measurement
7.4.4.1 Calibration solution
First use the zero calibration solution, measure the calibration solution from low to high, and inhale deionized water between each inhalation of the solution. At least repeat the measurement
2 times, take the average of the two readings.
7.4.4.2 Test solution
After the calibration solution is measured, measure the test solution immediately, and suck in deionized water between each measurement. The test solution should be measured at least twice.
8 Result calculation and presentation
8.1 Result calculation
Draw a calibration curve for the corresponding mass concentration of the element from the measured spectral intensity value of the calibration solution.
Calculate the respective mass concentration values from the calibration curve according to the spectral intensity value of the test solution, and calculate the analytical element according to formula (1)
content.
8.2 Presentation of analysis results
The analysis result is the average of 2 independent analysis results, rounded according to GB/T 8170.
When the analysis result is greater than or equal to 0.10%, round the value to two decimal places; when the analysis result is less than 0.10%, round the value
To three decimal places.
9 tolerance
The results of two independent analyses in the laboratory should not exceed the allowable error shown in Table 5.If it exceeds, it should be dealt with according to the process in Appendix B.
Table 5 Allowable difference%
10 Experiment report
The experiment report should include the following.
a) Laboratory name and address;
b) The date of issuance of the experiment report;
c) The standard number of this part;
d) Identify the details of the sample;
e) Analysis results;
f) The number of the result;
g) Any characteristics noticed during the measurement and not specified in this standard may affect the results of samples and certified reference materials.
Any operation that has an impact.
Appendix A
(Normative appendix)
Performance test of inductively coupled plasma spectrometer
A.1 Purpose
The purpose of the performance test given in this appendix is to use different types of instruments to properly determine the performance of the plasma spectrometer.
Different instruments are allowed to use different operating conditions, but the plasma spectrometer can eventually produce consistent results.
The whole performance test procedure is assessed with three basic parameters. detection limit (DL), background equivalent concentration (BEC), and short-term precision (RSD).
Note. When the element concentration in the sample solution is higher than 5000×DL, it only needs to meet the performance parameter requirements of RSD.
A.2 Definition
This appendix applies the following definitions.
A.2.1 Detection limit (DL)
A.2.2 Background equivalent concentration (BEC)
A.2.3 Short-term precision (RSD)
A.3 Calibration solution
The concentration levels of the elements to be tested shall be 0×DL (blank), 10×DL and 1000×DL detection limit solutions. These melt
The solution should contain acids, solvents, and matrix elements with similar concentrations of the sample to be tested.
The DL value of the prepared detection limit solution can be a laboratory value or an estimated value.
A.4 Procedure
This procedure is used for the operation of each test element.
The plasma spectrometer should be initially adjusted according to the manufacturer’s recommendations and the laboratory’s practical experience in quantitative analysis. Inhale blank
Liquid and take 10 intensity readings. Repeat this operation for the other two reference solutions.
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