标准编号:	GB/T 223.54-1987
中文名称:	钢铁及合金化学分析方法 火焰原子吸收分光光度法测定镍量
英文名称:	Methods for chemical analysis of iron, steel and alloy - The flame atomic absorption spectrophotometric method for the determination of nickel content
行业分类:	GB    国家标准
发布机构:	冶金工业部
发布日期:	1987-04-03
实施日期:	1988-3-1
标准状态:	superseded
被新标准替代:	GB/T 223.54-2022 钢铁及合金 镍含量的测定 火焰原子吸收光谱法
被替代日期:	2023-2-1
翻译语言:	英文
文件格式:	PDF
中文字符数:	5000 字
翻译价格(元):	420.0
交付时间:	付款后 1~3 个工作日

UDC 669.14/.15.543.06. NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA 中华人民共和国国家标准 GB 223.54-87 Methods for Chemical Analysis of Iron, Steel and Alloy the Flame Atomic Absorption Spectrophotometric Method for the Determination of Nickel Content 钢铁及合金化学分析方法 火焰原子吸收分光光度法测定镍量 Issued on: April 3, 1987 Implemented on: March 1, 1988 Issued by the Ministry of Metallurgical Industry NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA 中华人民共和国国家标准 GB 223.53-87 Methods for Chemical Analysis of Iron, Steel and Alloy the Flame Atomic Absorption Spectrophotometric Method for the Determination of Nickel Content 钢铁及合金化学分析方法 火焰原子吸收分光光度法测定镍量 This Standard is applicable to the determination of nickel content in cast iron, carbon steel and low alloy steel. The determination range: 0.005~0.50%. This Standard complies with "General Rules and Regulations of the Chemical Analysis Methods for Products of Metallurgical Industries" (GB 1467-78). 1 Principle Decompose the test sample with suitable mixed acid; add perchloric acid; evaporate to smoke; dissolve the salt with water; spray the sample solution into air-acetylene flame; take nickel hollow cathode lamp as light source; measure the absorbance at 232.0 nm wavelength of atomic absorption spectrophotometer. In order to eliminate the effects of matrix, iron with the same quantity as that of the sample solution shall be added when plotting the calibration graph. 2 Reagents 2.1 Perchloric acid (ρ 1.67g/ml). 2.2 Mixed acid of hydrochloric acid-nitric acid: mix one portion of hydrochloric acid (ρ 1.19g/ml), one portion of nitric acid (ρ 1.42g/ml) and two portion of water. Prepare just before use. 2.3 Mixed acid of nitric acid-perchloric acid: mix 100ml of nitric acid (ρ1.42 g/ml) and 800ml of perchloric acid (2.1), dilute to 1L with water and mix. 2.4 Pure iron solution: weigh 10g of pure iron (nickel content < 0.0005 %); place in a 800 ml beaker; add 100ml of mixed acid (2.2) of hydrochloric acid-nitric acid; heat to complete dissolution; add 120 ml of perchloric acid (2.1); evaporate to white smoke of perchloric acid occur and maintain for 1min; cool down; add 100ml of water; heat to dissolve the salt; cool down and transfer to a 250ml volumetric flask; dilute to the mark with water and mix. 2.5 Nickel standard solution 2.5.1 Weigh 1.0000g of metallic nickel (> 99.9 %); place in a 250ml beaker; add 50ml of nitric acid (1+1); heat to dissolve; cool down to room temperature; transfer in a 1000ml volumetric flask; dilute to the mark with water and mix; 1ml of this solution contains 1.0 mg of nickel. 2.5.2 Take 10.00 ml of nickel standard solution (2.5.1); place in a 100ml volumetric flask; dilute to the mark with water and mix; 1ml of this solution contains 100 μg of nickel. 3 Apparatus Atomic absorption spectrophotometer, equipped with an air-acetylene burner and a nickel hollow cathode lamp; air-acetylene shall be pure enough (free of water, oil and nickel) to give a steady clear fuel-lean flame. The atomic fluorescence spectrophotometer used shall reach the following indexes: 3.1 Minimum requirements on precision: absorbance shall be measured with the calibration solution of maximum concentration for ten times, and the standard deviation shall not exceed 1.0% of the mean absorbance. Measure the absorbance for 10 times with the calibration solution of the minimum concentration (not the zero calibration solution), and the standard deviation adopted shall not exceed 0.5 % the mean absorbance of the calibration solution of the maximum concentration. 3.2 Characteristic concentration: the characteristic concentration of nickel shall be less than 0.10 μg nickel/ml (wavelength 232.0 nm) in the solution with the same matrix as the sample solution for final measurement. 3.3 Detection limit: the detection limit of nickel shall be less than 0.15 μg nickel/ml (wavelength 232.0 nm) in the solution with the same matrix as the sample solution for final measurement. 3.4 Linear of calibration graph: the ratio of the slope (expressed as variable quantity) of upper part of calibration graph within the range of 20 % concentration to the slope of lower part of calibration graph within the range of 20 % concentration shall not be less than 0.7. 4 Analytical Procedures 4.1 Sample mass Weigh 1.0000 g of test sample. 4.2 Blank test Carry out blank tests along with the tests on test samples. 4.3 Determination 4.3.1 Place the sample (4.1) in a 400ml beaker; add 15 ml of mixed acid (2.3) of nitric acid-perchloric acid; cover with a watch glass; heat at low temperature to dissolve; evaporate until white smoke of perchloric acid occur and maintain for 1 min; cool down; add 15 ml of water; dissolve the salts at subfebrile temperature; cool down to room temperature; transfer into a 100ml volumetric flask; dilute to the mark with water and mix. In case such precipitates as graphite, silicic acid, tungstic acid, etc. separate out from test solution, dry filtering must be conducted. Note: (1) as for the test sample difficult to dissolve in mixed acid (2.3) of nitric acid-perchloric acid, mixed acid (2.2) of hydrochloric acid-nitric acid may be adopted for dissolving; then add 12 ml of perchloric acid (2.1); evaporate to smoke and maintain for 1 min; the rest operations shall be conducted according to the corresponding procedures specified in (4.3.1). (2) if the nickel content in the sample solution exceeds 1.0 %, the sample solution shall be diluted: take 20ml of sample solution (4.3.1), place in a 100ml volumetric flask; dilute to the mark with water and mix. Dilute the blank solution with the same procedures. 4.3.2 Set the air-acetylene flame to zero with water and measure the absorbance of the sample solution at 232.0 nm wavelength on atomic absorption spectrophotometer; find out the nickel concentration (μg/ml) on the calibration graph according to the absorbance of the sample solution and the absorbance of the accompanied test sample blank solution. 4.4 Plotting the calibration graph 4.4.1 Nickel content < 0.10% Add 25ml of pure iron solution (2.4) into eight 100ml volumetric flasks respectively; then add 0.00 ml, 0.50 ml, 1.00 ml, 2.00 ml, 4.00 ml, 6.00 ml, 8.00 ml and 10.00 ml of nickel standard solution (2.5.2) respectively; dilute to the mark with water and mix. 4.4.2 Nickel content: 0.10~0.50 % Add 5ml of pure iron solution (2.4) into seven 100ml volumetric flasks respectively; then add 0.00 ml, 1.00 ml, 2.00 ml, 4.00 ml, 6.00 ml, 8.00 ml and 10.00 ml of nickel standard solution (2.5.1) respectively; dilute to the mark with water and mix. 4.4.3 Set the air-acetylene flame to zero with water and measure the absorbance of solution (4.4.1) or solution (4.4.2) at 232.0 nm wavelength on the atomic absorption spectrophotometer. The net absorbance of solution in nickel calibration graph series may be obtained by subducting the absorbance of solution with 0 in concentration from the absorbance of each solution in calibration graph series; plot the calibration graph by taking the nickel concentration as the lateral coordinates and the net absorbance as the vertical coordinates. 5 Calculation of Analysis Results Percentage content of nickel shall be calculated according to the following formula: Ni (%) = ×100 Where, C2—Nickel concentration of the sample solution found on the calibration graph, μg/ml; C1—Nickel concentration of the accompanied test sample blank solution found on the calibration graph, μg/ml; f—Dilution ratio. In case the nickel content is less than or equal to 0.10 %, adopt f=1; in case the nickel content is greater than 0.1 %, adopt f=5; V—Volume of tested sample solution, ml; m—Sample mass, g. 6 Precision Precision Table Level (%) (m/m) Repeatability (r) Reproducibility (R) 0.005~0.50 lgr =-1.5732+0.6021lgm lgR=-1.1569+0.6799lgm Repeatability is the maximum difference value of the two independent test results for the same sample with the same apparatus by the same operator in the same laboratory with normal and correct operation of this method at a probability of 95%. Reproducibility refers to the maximum difference value of two independent results of single tests carried out at a probability of 95% with this method and normal and proper operation by two operators in different laboratories for the identical samples. If the difference between the results obtained from the two independent tests exceeds the corresponding repeatability and reproducibility values, the two results are considered as suspicious. _________________________ Additional Explanations: This Standard was proposed by the Ministry of Metallurgical Industry. This Standard is under the jurisdiction of Technology Department of Central Iron and Steel Research Institute, Ministry of Metallurgical Industry. Central Iron and Steel Research Institute, Ministry of Metallurgical Industry is responsible for the drafting of the Standard. This Standard was drafted by Central Iron and Steel Research Institute. Chief drafting staff of this Standard: Xie Ronghou and Xing Rugang. Level mark of this Standard is as GB 223.54-87 I.

中华人民共和国国家标准 UDC 669、14/、15 钢铁及合金化学分析方法 、543、06 GB 223、54—87 火焰原子吸收分光光度法测定镍量 Methods for chemical analysis of iron,steel and alloy The flame atomic absorption speotrophotometric method for the determination of nickel content _______________________________________________________________________________ 本标准适用于铸铁、碳素钢、低合金钢中镍量的测定。测定范围：0.005～0.50%。 本标准遵守GB 1467—78《冶金产品化学分析方法标准的总则及一般规定》。 1 方法提要 试样以适当的混合酸分解，加高氯酸蒸发至冒烟后，以水溶解盐类，试样溶液喷入空气—乙炔火焰中，用镍空心阴极灯作光源，于原子吸收分光光度计波长232.0nm处，测量其吸光度。 为消除基体影响，绘制校准曲线时，应加入与试样溶液相近的铁量。 _______________________________________________________________________________ 冶金工业部1987-04-03批准 1988-03-01实施 2 试剂 2.1 高氯酸（ρ1.67 g/ml）。 2.2 盐酸—硝酸混合酸：将3份盐酸（ρ1.19g/ml）。1份硝酸（ρ1.42g/ml）和2份水相混合，用时配制。 2.3 硝酸—高氯酸混合酸；将100ml硝酸（ρ1.42g/ml）与800ml高氯酸（2.1）混合，用水稀释至1 L，混匀。 2.4 纯铁溶液；称取10g纯铁（镍含量<0.0005%），置于800ml烧杯中，加入100ml盐酸—硝酸混合酸（2.2），加热至全部溶解，加入120ml高氯酸（2.1），蒸发至冒高氯酸白烟，并保持1 min，冷却，加100ml水，加热溶解盐类，冷却后，移入250ml容量瓶中，用水稀释至刻度，混匀。 2.5 镍标准溶液 2.5.1 称取1.0000g金属镍（>99.9%），置于250ml烧杯中，加50ml硝酸（1+1）加热溶解后，冷却至室温，移入1 000ml容量瓶中，用水稀释至刻度，混匀，此溶液1 ml含1.0mg镍。 2.5.2 移取10.00ml镍标准溶液（2.5.1），置于100ml容量瓶中，用水稀释至刻度，混匀，此溶液1 ml含100μg镍。 3 仪器 原子吸收分光光度计，备有空气—乙炔燃烧器，镍空心阴极灯。空气—乙炔要足够纯净（不含水、油及镍），以提供稳定清澈的贫燃火焰。 所用原子吸收分光光度计，均应达到下列指标。 3.1 精密度的最低要求：用最高浓度的校准溶液，测量10次吸光度，其标准偏差，应不超过平均吸光度的1.0%。 用最低浓度的校准溶液（不是零校准溶液），测量10次吸光度，其标准偏差，应不超过最高校准溶液平均吸光度的0.5%。 3.2 特征浓度：在与最终测量样品溶液的基体相一致的溶液中，镍的特征浓度应小于0.10μg镍/ml（波长232.0nm）。 3.3 检出限：在与最终测量样品溶液的基体相一致的溶液中，镍的检出限应小于0.15μg镍/ml（波长232.0nm）。 3.4 校准曲线的线性：校准曲线上部20%浓度范围内的斜率（表示为吸光度的变化量）与下部20%浓度范围内斜率之比值，应不小于0.7。 4 分析步骤 4.1 试样量 称取1.0000g试样。 4.2 空白试验 随同试样做空白试验。 4.3 测定 4.3.1 将试样（4.1）置于400ml烧杯中，加入15ml硝酸-高氯酸混合酸（2.3），盖上表皿，低温加热溶解，蒸发至冒高氯酸白烟，并保持1 min，冷却，加15ml水，微热至盐类溶解，冷却至室温，移入100ml容量瓶中，用水稀释至刻度，混匀。试液中如有石墨、硅酸、钨酸等沉淀物析出，须干过滤。 注：①对于不易溶解于硝酸—高氧酸混台酸（2.3）的试样，可先用盐酸-硝酸混合酸（2.2）溶解，然后加入12ml高氧酸（2.1）,蒸发至冒烟，并保持1 min,以下按（4.3.1）中相应步骤进行。 ②若试样溶液中含镍量超过1.0%，则要进行稀释：移取20ml试样溶液（4.3.1）置于100ml容量瓶中，用水稀释至刻度，混匀。并同样稀释空白溶液。 4.3.2 将试样溶液在原子吸收分光光度计上，于波长232.0nm处，以空气-乙炔火焰，用水调零，测量其吸光度，将试样溶液的吸光度和随同试样空白溶液的吸光度，从校准曲线上查出镍的浓度μg/ml。 4.4 校准曲线的绘制 4.4.1 镍含量<0.10% 于8个100ml容量瓶中，各加入25ml纯铁溶液（2.4），然后分别加入0.00，0.50、1.00、2.00、4.00、6.00、8.00、10.00ml镍标准溶液（2.5.2），用水稀释至刻度，混匀。 4.4.2 镍含量0.10～0.50% 于7个100ml，容量瓶中，各加入5ml纯铁溶液（2.4），然后分别加入0.00、1.00、2.00、4.00、6.00、8.00、10.00 ml镍标准溶液（2.5.1），用水稀释至刻度，混匀。 4.4.3 将溶液（4.4.1）或（4.4.2）在原子吸收分光光度计上，干波长232.0nm处，以空气—乙炔火焰，用水调零，测量其吸光度。 校准曲线系列每一溶液的吸光度去零浓度溶液的吸光度，为镍校准曲线系列溶液的净吸光度，以镍浓度为横坐标，净吸光度为纵坐标绘制校准曲线。 5 分析结果的计算 按下式计算镍的百分含量： Ni（%）= ×100 式中：C2—自校准曲线上查得的试样溶液中镍的浓度，μg/ml； C1—自校准曲线上查得的随同试样空白溶液中镍的浓度，μg/ml； f—稀释倍数。当试样含镍量小于或等于0.10%时，f=1；当试样含镍量大于0.1%时，f=5； V—被测试样溶液的休积，ml； m—试样量，g。 6 精密度 精密度表 水平（%）（m/m） 重 复 性（r） 再 现 性（R） 0.005～0.50 lgr=-1.5732+0.6021lgm lgR=-1.1569+0.6799lgm 重复性是用本方法在正常和正确操作情况下，由同一操作人员，在同一实验室内，使用同一仪器，并在短期内，对相同试样所作两个单次测试结果，在95%概率水平两个独立测试结果的最大差值。 再现性是用本方法在正常和正确操作情况下，由两名操作人员，在不同实验室内，对相同试样各作单次测试结果，在95%概率水平两个独立测试结果的最大差值。 如果两个独立测试结果之间差值超过了相应的重复性和再现性数值，则认为这两个结果是可疑的。 _________________________ 附加说明： 本标准由冶金工业部提出。 本标准由冶金工业部钢铁研究总院技术归口。 本标准由冶金工业部钢铁研究总院负责起草。 本标准由钢铁研究总院起草。 本标准主要起草人谢荣厚、邢如岗。 本标准水平等级标记GB 223.54—87 I。