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钢铁 锑、锡含量的测定 电感耦合等离子体原子发射光谱法
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GBT 34208-2017
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标准编号: GB/T 34208-2017 (GB/T34208-2017)
中文名称: 钢铁 锑、锡含量的测定 电感耦合等离子体原子发射光谱法
英文名称: Iron and steel -- Determination of antimony and tin content -- Inductively coupled plasma atomic emission spectrometric method
行业: 国家标准 (推荐)
中标分类: H11
字数估计: 11,138
发布日期: 2017-09-07
实施日期: 2018-06-01
起草单位: 鞍钢股份有限公司
归口单位: 全国钢标准化技术委员会(SAC/TC 183)
提出机构: 中国钢铁工业协会
发布机构: 中华人民共和国国家质量监督检验检疫总局、中国国家标准化管理委员会
GB/T 34208-2017: 钢铁 锑、锡含量的测定 电感耦合等离子体原子发射光谱法
GB/T 34208-2017 英文名称: Iron and steel -- Determination of antimony and tin content -- Inductively coupled plasma atomic emission spectrometric method
1 范围本标准规定了用电感耦合等离子体原子发射光谱法测定锑、锡含量的方法。本标准适用于铬含量(质量分数)小于1.50%,镍含量(质量分数)小于2.00%的碳素钢、低合金钢中锑、锡含量的测定,锑的测定范围(质量分数):0.0020%~0.12%;锡的测定范围(质量分数):0.0020%~0.13%。
2 规范性引用文件下列文件对于本文件的应用是必不可少的。凡是注日期的引用文件,仅注日期的版本适用于本文件。凡是不注日期的引用文件,其最新版本(包括所有的修改单)适用于本文件。
GB/T 6379.2 测量方法与结果的准确度(正确度与精密度) 第2部分:确定标准测量方法重复性与再现性的基本方法GB/T 6682 分析实验室用水规范和试验方法
GB/T 20066 钢和铁 化学成分测定用试样的取样和制样方法
3 原理试料用盐酸和硝酸混合酸溶解,并稀释至一定体积。将试料溶液雾化后引入电感耦合等离子体原子发射光谱仪中,测定各被测元素分析线的光谱强度。根据建立的校准曲线,计算各分析元素的质量分数。
4 试剂与材料除非另有说明,在分析中仅使用认可的分析纯试剂和符合GB/T 6682规定的二级水。
4.1 高纯铁,质量分数大于99.98%,且锡、锑质量分数不超过0.0001%。
4.2 盐酸,ρ约1.19g/mL。
4.3 硝酸,ρ约1.42g/mL。
4.4 硝酸,ρ约1.42g/mL,稀释为1+1。
4.5 锑标准溶液
4.5.1 锑贮备溶液,500μg/mL称取1.3715g预先在干燥器中干燥过的酒石酸锑钾(C4H4KO7Sb·2H2O),溶于盐酸(1+9)中,移入1000mL容量瓶中,用盐酸(1+9)稀释至刻度,混匀。此溶液1mL含500μg锑。也可使用市售的有证锑标准溶液。
4.5.2 锑标准溶液,10.0μg/mL将2.00mL锑贮备溶液(4.5.1)移入100mL容量瓶中,用盐酸(1+9)稀释至刻度,混匀。此溶液1mL含10.0μg锑。
4.6 锡标准溶液
4.6.1 锡贮备溶液,500μg/mL称取0.5000g高纯锡(质量分数不小于99.9%),置于200mL烧杯中。加入40mL盐酸(1+1),加热溶解。冷却至室温后,将溶液移入1000mL容量瓶中,用盐酸(1+4)稀释至刻度,混匀。此溶液1mL含500μg锡。也可使用市售的有证锡标准溶液。
4.6.2 锡标准溶液,10.0μg/mL将2.00mL锡贮备溶液(4.6.1)移入100mL容量瓶中,用盐酸(1+4)稀释至刻度,混匀。此溶液1mL含10.0μg锡。
5 仪器与设备通常的实验室设备及电感耦合等离子体原子发射光谱仪(ICP-AES)。
5.1 电感耦合等离子体原子发射光谱仪(ICP-AES)光谱仪按仪器厂家提供的操作程序和指南优化后,符合5.1.2~5.1.5的性能指标,就达到使用要求。光谱仪既可是同时型的,也可是顺序型的。
5.1.1 分析线本标准推荐使用的分析线列于表1。在使用时,应仔细检查谱线的干扰情况,优先使用灵敏度高,干扰少的谱线。
5.1.2 光谱仪的实际分辨率按A.1,计算所使用的每条分析线的带宽。带宽应小于0.030nm。
5.1.3 短期稳定性连续测量10次每个分析元素浓度最高的校准溶液的光谱强度,计算其相对标准偏差(RSD),RSD应不超过1.0%。
5.1.4 长期稳定性在3h中,每隔30min测量每个分析元素浓度最高的校准溶液的光谱强度3次,共得到7个测量平均值。计算7个测量平均值的相对标准偏差(RSD),RSD应不超过2.0%。
5.1.5 背景等效浓度和检出限背景等效浓度和检出限见A.2,对仅含被测元素的溶液,计算分析线的背景等效浓度(BEC)和检出限(DL),其结果应低于表2中的数值。
5.1.6 曲线的线性校准曲线的线性通过计算相关系数进行检查,相关系数应大于0.995。
6 取制样按GB/T 20066或适当的国家标准取制样。
7 分析步骤
7.1 试料称取0.50g试料,精确至0.1mg。
7.2 空白试验(相当于零号)称取0.500g高纯铁(4.1),随同试料做空白试验。
7.3 试料溶液的制备将试料(7.1)置于150mL三角烧瓶或烧杯(加盖表面皿)中,加入10mL硝酸(4.4),低温加热至停止反应,加入5mL盐酸(4.2),继续加热至试料溶解完全。取下,冷却至室温,移入100mL容量瓶中,用水稀释至刻度,混匀。如浑浊,干过滤后测量。
7.4 校准曲线的绘制
7.4.1 标准溶液系列称取0.500g高纯铁(4.1)6份分别于150mL三角烧瓶或烧杯中,按照7.3步骤将其溶解,冷却至室温,移入6个100mL容量瓶中按表3加入被测元素的标准溶液,用水稀释至刻度,混匀。
7.4.2 校准曲线的绘制于ICP光谱仪上,测量各校准曲线溶液(7.4.1)中锑和锡的光谱强度,每个溶液重复测量2次~3次,计算其平均值。以各光谱强度平均值减去零浓度光谱强度平均值为纵坐标,校准曲线溶液的浓度为横坐标,分别绘制锑和锡的校准曲线。计算校准曲线的相关系数,相关系数应符合5.1.6的要求。
7.5 分析线中干扰线的校正先检查各共存元素对被测元素分析线的光谱干扰。有光谱干扰的情况下,按A.3求出光谱干扰校正系数,即当共存元素质量分数为1%时相当的被测元素的质量分数。
7.6 试料溶液中元素的光谱测量测量试料溶液中锑和锡的光谱强度,每个溶液重复测量2次~3次,计算其平均值。以各光谱强度平均值减去空白溶液(相当于零浓度)光谱强度平均值,得到净光谱强度。
8 结果计算根据校准曲线,将试液中锡和锑的净强度转化为浓度,以μg/mL表示。被测元素的含量以质量分数wM 计,数值以%表示,按式(1)计算:
9 精密度本标准的精密度数据是在2015年由8个实验室对钢铁中锑的6个水平,9个实验室对钢铁中锡的6个水平进行共同试验所确定的。按照GB/T 6379.2的规定的重复性条件下,各实验室对钢铁中锑和锡的每个水平测定3次完成的。共同精密度试验所用样品和精密度结果参见附录B。原始数据按照GB/T 6379.2进行统计分析,精密度见表4。在重复性条件下,获得的两次独立测试结果的绝对差值不大于重复性限r,大于重复性限r的情况以不超过5%为前提;在再现性条件下,获得的两次独立测试结果的绝对差值不大于再现性限R,大于再现性限R 的情况以不超过5%为前提。
10 试验报告试验报告应包括下列内容:
a) 识别样品、实验室和试验日期所需的全部资料;
b) 参考本标准所用的方法;
c) 试验结果及表示;
d) 试验中观察到的异常现象;
e) 任何本标准中未规定的操作,或任何可能影响结果的操作。
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.
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
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
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
(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.
tested element solution by the intensity of water.
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