利用PoDFA离线测渣分析方法对7055铝合金熔体中的渣进行检测分析.通过过滤铝合金熔体将夹杂物富集,然后采用物理金相方法对夹杂物进行鉴别分析,建立7055铝合金熔体夹杂物形貌特征与图谱.结果表明7055铝合金熔体主要含有氧化膜、氧化镁、尖晶石、TiB2、耐火材料夹杂.
铝铁中间合金是铝合金生产中的重要原料之一,分析平衡态下金属间化合物的析出特征是很有必要的,可为铸造铝合金或变形铝合金化学成分、组织的调整与控制提供参考依据.通过物理金相方法对入厂原材料AlFe10中间合金进行化合物相分析,用金相显微镜(OM)及配套的ProImaging金相图像分析软件对化合物相的形貌、分布、含量进行检测,用扫描电子显微镜(SEM)及能谱仪(EDS)对化合物相进行微区成分分析.结果表明:AlFe10中间合金含有长条状或小块状FeAl3相,FeAl3相面积约27.6%;脱落部位含有C、O、Al、Si、Cl等元素非金属夹杂,非金属夹杂面积约3.8%;检测区域未能发现单质Fe的存在.
基于标准方法GB/T 20975.25-2020中对铝合金多元素进行测定的方法进行实验验证探讨,具体对铝合金中Si、Fe、Cu、Mn、Mg、Cr、Ni、Zn、Ti、Zr的含量进行测定,用有证标准物质对实验过程进行验证评估,同时采用加标回收验证.实验结果表明:铝合金标样质量浓度在0~20mg/L范围内,工作曲线相关系数r>0.999 9,各元素检出限均低于标准方法检测下限,精密度、准确度均优于标准方法的要求,加标回收率在92.86%~102.70%之间,分析结果准确可靠.通过验证表明,本实验具备使用该方法进行铝合金化学成分分析的技术能力.
为帮助实验室更好地理解和执行新检测标准,以减少检测误差,本文对电感耦合等离子体原子发射光谱法分析铝及铝合金的检测标准进行研究,基于比较法,从测量范围、方法提要、试剂、仪器、分析步骤、试验数据处理、精密度等方面,比较了GB/T 20975.25-2020和GB/T 20975.25-2008的差异,探讨了标准还需要完善的地方.结果表明,新版标准较旧版增加了15个可检测元素,元素含量范围、定容体积和精密度要求有所调整,并增加了一种溶样方法.
为了使直读光谱法检测铝合金中硅、锰、镁、锌的标准曲线适应不同系列铝合金样品,减少测量误差,将仪器预置标准曲线细分至10条,即将1条高含量预置标准曲线细分为7条,将1条低含量预置标准曲线细分为3条.通过检测大量铝合金光谱标准样品,将检测结果与标准值进行线性拟合,得出的截距和斜率分别用于调整细分标准曲线的截距A0和斜率A1,并使用标准样品进行验证.结果表明,标准曲线细分和优化后,硅、锰、镁和锌的检测结果更加接近证书值,测量误差更小,所考察的标准样品中,最低含量的硅、锰、镁、锌的绝对误差分别从0.0026% 降至0.0009%、从0.0010%降至0.0000%、从0.0050%降至0.0002%、从0.0051%降至0.0003%;最高含量的硅、锰、镁、锌的绝对误差分别从0.070%降至0.001%、从0.13%降至0.01%、从0.33%降至0.14%、从0.49%降至0.09%.
阐述直读光谱成分分析、ICP成分分析、固态测氢等铝合金化学成分分析样品的加工方法和过程,结合实际工作经验,提出样品加工过程中需要注意的事项,汇总样品加工过程常见的异常现象及处理方式。
光电直读发射光谱法因具有操作简单、多元素同时分析、分析速率快、准确度高、重现性好、不易受到污染、干扰小和成本低等[1-2]优点,广泛应用于铝及铝合金化学成分分析中.光电直读发射光谱法尤其迎合企业生产过程中炉前、炉后快速化学成分分析和调整的生产需要,光电直读发射光谱仪已经成为铝制造企业不可或缺的检测设备之一.光电直读发射光谱法基本原理是样品被火花光源激发,经入射狭缝到达光栅上色散成光谱,作用在光电倍增管或电荷耦合元件(CCD)检测器上产生光电流(即光能转变为电能).通过检测系统、计算机数模转换,测出特征谱线的强度,然后准确计算出样品中各元素的含量.由计算机程序控制完成分析的全部过程.
为了更好地理解及执行5XXX铝合金晶间腐蚀质量损失试验新版标准ASTM G67-2018,从适用范围、试验装置、试剂浓度、温度要求、取样及试样处理、方法验证、控制样品、报告内容、精密度要求等方面对ASTM G67-13、ASTM G67-2018和GB/T 26491-2011 3份5XXX铝合金晶间腐蚀质量损失试验标准进行差异性分析,重点比对了ASTM G67-13和ASTM G67-2018的差异.
A method for determination of Zr and Ti contents in passivation films on 6061 aluminum alloy by using hand-held X-ray fluorescence spectrometer was established. The square of linear correlation coefficients of the working curves were larger than 0.999. The detection limit was 0.66 mg/m2 for Zr and 1.23 mg/m2 for Ti. The accuracy of the method was evaluated by redetermination of standard samples and interlaboratory comparison. The relative error in redetermination test was within ±4% and the interlaboratory error was better than ±0.50 mg/m2. The repeatability was about 3.5% when the number of repeated samples was 5. The effects of five structures i.e. soft round stool, white computer desk, round woody stool, black test table, and tile floor for supporting the sample as background on the determination result were studied. The results showed that all of them had positive interference on the determination results. The sample to be tested should not be in touch with the support background directly, and the distance between them should be kept at least 30 cm. The method could be used for onsite fast and accurate determination of Zr and Ti contents in passivation films on 6016 aluminum alloy, providing important support to process control in aluminum passivation line.
介绍了使用火花直读发射光谱法测定7050铝合金中锌的测量不确定度评定方法,建立数学模型,分析了检测过程中的不确定度重要来源,包括样品测量过程随机性、类型校准、分析方法、标样定值、数值修约等,根据不确定度传递公式的特点,采用标准不确定度评定各个分量,重点对不确定度B类评定进行了阐述,并对各个不确定度来源对不确定度的贡献进行评价.
以朗伯-比耳定律为定量依据,建立傅立叶变换红外光谱测定铝合金热轧乳液中有效成分的方法.用旋转蒸发法处理热轧乳液样品,提取出油分,以空气为背景检测提取物中非结合酸、总酯、乳化剂和有机皂的含量.非结合酸采用固定峰高定量,总酯、乳化剂和有机皂采用范围峰高定量,波数或波数范围分别为1710,1725~1760,920~980,1510~1620 cm–1.在线性范围内,热粗轧油和热精轧油的工作曲线线性相关系数分别在0.999和0.998以上.用该方法对标准油进行测定,粗轧油测定结果的相对误差在 ±2% 以内,精轧油测定结果的相对误差在 ±3% 以内;粗轧油和精轧油测定结果的相对标准偏差均小于2%(n=5).该法可准确测定铝合金热轧乳液中的有效成分,为热轧生产工艺控制提供依据.
利用电感耦合等离子体原子发射光谱法(ICP-OES)测定5052铝合金中镁元素,分析检测过程中的不确定度来源,包括样品称量、定容、标准曲线拟合等,根据不确定度传递公式的特点,采用相对标准不确定度评定各个分量,重点评定了标准曲线拟合引入的不确定度,并对各个不确定度来源对不确定度的贡献进行评价.经计算得出合成不确定度()(Yuc=0.0257%)和扩展不确定度(U95=0.005%).
Thermal conductivity method was established to determine the hydrogen content in aluminum alloy. The sample was processed into long round sticks by CNC lathe and then cut into small round sticks for analysis. The important parameters of RHEN602 hydrogen determinator were discussed, including analysis parameters, element parameters, electrode furnace parameters, temperature sustain. The outgas circle of crucible was 4. The analysis power of surface hydrogen was 850 W and that of bulk hydrogen was 1 300 W. The integration time of surface hydrogen and bulk hydrogen was 120 and 330 s,respectively. Program steps were used to control the temperature of furnace during ramping analysis. The key factors on hydrogen test result were discussed. The crucible should be tested as blank at least 3 times to reduce the specimen blank on the test result. The purity of carrier gas should be more than 99.999%. The instrument should be operated at least 3 h to get a stable state. The specimen mass should between 2-5 g. The alloy serial of reference sample should be in accordance with specimens and hydrogen content higher than that of specimens. The study showed that this method had good accuracy due to the relative error was 1.39% when used reference sample for verification. The method also exhibited good repeatability with RSD of 12.60% (n=10) when used aviation aluminum alloy 2219 for analysis example, which met the technical requirement for the repeatability test of samples. This method can be used to determine the hydrogen content in aluminum alloy.
采用光电直读光谱法测定铸造铝合金中微量钙和钠,并对其最佳条件进行试验.做到以下几点可获得满意的分析结果:① 用积分描迹调整光谱仪器的狭缝位置,保证了最大强度的光通过;② 严格按照GB/T 17432-2012的规定取样,确保样品的分析面无夹杂、裂纹、气孔、油污、粉尘及氧化物等;③ 样品表面必须光滑、无污染;④ 所用氩气应保证其纯度和流量;⑤ 采用与被分析样品中钙、钠含量非常接近的铝合金标准物质做类型校准.钙、钠的检出限(3s)依次为0.00001%和0.00002%.方法分析了5块铝合金标准物质,测得钙、钠的含量与其认定值一致;另取3块已知样品各重复测定11次,测定值的相对标准偏差为1.6%~3.9%.