標準編號:	GB/T 223.54-1987
中文名稱:	鋼鐵及合金化學分析方法 火焰原子吸收分光光度法測定鎳量
英文名稱:	Methods for chemical analysis of iron, steel and alloy - The flame atomic absorption spectrophotometric method for the determination of nickel content
行業分類:	GB    國家標準
發布機構:	冶金工業部
發布日期:	1987-04-03
實施日期:	1988-3-1
標準狀態:	superseded
被新標準替代:	GB/T 223.54-2022 鋼鐵及合金 鎳含量的測定 火焰原子吸收光譜法
被替代日期:	2023-2-1
翻譯語言:	英文
文件格式:	PDF
中文字符數:	5000 字
翻譯價格(元):	420.0
交付時間:	付款后 1~3 個工作日

UDC 669.14/.15.543.06. NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA 中華人民共和國國家標準 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 鋼鐵及合金化學分析方法 火焰原子吸收分光光度法測定鎳量 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 中華人民共和國國家標準 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 鋼鐵及合金化學分析方法 火焰原子吸收分光光度法測定鎳量 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.

中華人民共和國國家標準 UDC 669、14/、15 鋼鐵及合金化學分析方法 、543、06 GB 223、54—87 火焰原子吸收分光光度法測定鎳量 Methods for chemical analysis of iron,steel and alloy The flame atomic absorption speotrophotometric method for the determination of nickel content _______________________________________________________________________________ 本標準適用于鑄鐵、碳素鋼、低合金鋼中鎳量的測定。測定范圍：0.005～0.50%。 本標準遵守GB 1467—78《冶金產品化學分析方法標準的總則及一般規定》。 1 方法提要 試樣以適當的混合酸分解，加高氯酸蒸發至冒煙后，以水溶解鹽類，試樣溶液噴入空氣—乙炔火焰中，用鎳空心陰極燈作光源，于原子吸收分光光度計波長232.0nm處，測量其吸光度。 為消除基體影響，繪制校準曲線時，應加入與試樣溶液相近的鐵量。 _______________________________________________________________________________ 冶金工業部1987-04-03批準 1988-03-01實施 2 試劑 2.1 高氯酸（ρ1.67 g/ml）。 2.2 鹽酸—硝酸混合酸：將3份鹽酸（ρ1.19g/ml）。1份硝酸（ρ1.42g/ml）和2份水相混合，用時配制。 2.3 硝酸—高氯酸混合酸；將100ml硝酸（ρ1.42g/ml）與800ml高氯酸（2.1）混合，用水稀釋至1 L，混勻。 2.4 純鐵溶液；稱取10g純鐵（鎳含量<0.0005%），置于800ml燒杯中，加入100ml鹽酸—硝酸混合酸（2.2），加熱至全部溶解，加入120ml高氯酸（2.1），蒸發至冒高氯酸白煙，并保持1 min，冷卻，加100ml水，加熱溶解鹽類，冷卻后，移入250ml容量瓶中，用水稀釋至刻度，混勻。 2.5 鎳標準溶液 2.5.1 稱取1.0000g金屬鎳（>99.9%），置于250ml燒杯中，加50ml硝酸（1+1）加熱溶解后，冷卻至室溫，移入1 000ml容量瓶中，用水稀釋至刻度，混勻，此溶液1 ml含1.0mg鎳。 2.5.2 移取10.00ml鎳標準溶液（2.5.1），置于100ml容量瓶中，用水稀釋至刻度，混勻，此溶液1 ml含100μg鎳。 3 儀器 原子吸收分光光度計，備有空氣—乙炔燃燒器，鎳空心陰極燈。空氣—乙炔要足夠純凈（不含水、油及鎳），以提供穩定清澈的貧燃火焰。 所用原子吸收分光光度計，均應達到下列指標。 3.1 精密度的最低要求：用最高濃度的校準溶液，測量10次吸光度，其標準偏差，應不超過平均吸光度的1.0%。 用最低濃度的校準溶液（不是零校準溶液），測量10次吸光度，其標準偏差，應不超過最高校準溶液平均吸光度的0.5%。 3.2 特征濃度：在與最終測量樣品溶液的基體相一致的溶液中，鎳的特征濃度應小于0.10μg鎳/ml（波長232.0nm）。 3.3 檢出限：在與最終測量樣品溶液的基體相一致的溶液中，鎳的檢出限應小于0.15μg鎳/ml（波長232.0nm）。 3.4 校準曲線的線性：校準曲線上部20%濃度范圍內的斜率（表示為吸光度的變化量）與下部20%濃度范圍內斜率之比值，應不小于0.7。 4 分析步驟 4.1 試樣量 稱取1.0000g試樣。 4.2 空白試驗 隨同試樣做空白試驗。 4.3 測定 4.3.1 將試樣（4.1）置于400ml燒杯中，加入15ml硝酸-高氯酸混合酸（2.3），蓋上表皿，低溫加熱溶解，蒸發至冒高氯酸白煙，并保持1 min，冷卻，加15ml水，微熱至鹽類溶解，冷卻至室溫，移入100ml容量瓶中，用水稀釋至刻度，混勻。試液中如有石墨、硅酸、鎢酸等沉淀物析出，須干過濾。 注：①對于不易溶解于硝酸—高氧酸混臺酸（2.3）的試樣，可先用鹽酸-硝酸混合酸（2.2）溶解，然后加入12ml高氧酸（2.1）,蒸發至冒煙，并保持1 min,以下按（4.3.1）中相應步驟進行。 ②若試樣溶液中含鎳量超過1.0%，則要進行稀釋：移取20ml試樣溶液（4.3.1）置于100ml容量瓶中，用水稀釋至刻度，混勻。并同樣稀釋空白溶液。 4.3.2 將試樣溶液在原子吸收分光光度計上，于波長232.0nm處，以空氣-乙炔火焰，用水調零，測量其吸光度，將試樣溶液的吸光度和隨同試樣空白溶液的吸光度，從校準曲線上查出鎳的濃度μg/ml。 4.4 校準曲線的繪制 4.4.1 鎳含量<0.10% 于8個100ml容量瓶中，各加入25ml純鐵溶液（2.4），然后分別加入0.00，0.50、1.00、2.00、4.00、6.00、8.00、10.00ml鎳標準溶液（2.5.2），用水稀釋至刻度，混勻。 4.4.2 鎳含量0.10～0.50% 于7個100ml，容量瓶中，各加入5ml純鐵溶液（2.4），然后分別加入0.00、1.00、2.00、4.00、6.00、8.00、10.00 ml鎳標準溶液（2.5.1），用水稀釋至刻度，混勻。 4.4.3 將溶液（4.4.1）或（4.4.2）在原子吸收分光光度計上，干波長232.0nm處，以空氣—乙炔火焰，用水調零，測量其吸光度。 校準曲線系列每一溶液的吸光度去零濃度溶液的吸光度，為鎳校準曲線系列溶液的凈吸光度，以鎳濃度為橫坐標，凈吸光度為縱坐標繪制校準曲線。 5 分析結果的計算 按下式計算鎳的百分含量： Ni（%）= ×100 式中：C2—自校準曲線上查得的試樣溶液中鎳的濃度，μg/ml； C1—自校準曲線上查得的隨同試樣空白溶液中鎳的濃度，μg/ml； f—稀釋倍數。當試樣含鎳量小于或等于0.10%時，f=1；當試樣含鎳量大于0.1%時，f=5； V—被測試樣溶液的休積，ml； m—試樣量，g。 6 精密度 精密度表 水平（%）（m/m） 重 復 性（r） 再 現 性（R） 0.005～0.50 lgr=-1.5732+0.6021lgm lgR=-1.1569+0.6799lgm 重復性是用本方法在正常和正確操作情況下，由同一操作人員，在同一實驗室內，使用同一儀器，并在短期內，對相同試樣所作兩個單次測試結果，在95%概率水平兩個獨立測試結果的最大差值。 再現性是用本方法在正常和正確操作情況下，由兩名操作人員，在不同實驗室內，對相同試樣各作單次測試結果，在95%概率水平兩個獨立測試結果的最大差值。 如果兩個獨立測試結果之間差值超過了相應的重復性和再現性數值，則認為這兩個結果是可疑的。 _________________________ 附加說明： 本標準由冶金工業部提出。 本標準由冶金工業部鋼鐵研究總院技術歸口。 本標準由冶金工業部鋼鐵研究總院負責起草。 本標準由鋼鐵研究總院起草。 本標準主要起草人謝榮厚、邢如崗。 本標準水平等級標記GB 223.54—87 I。