光电直读光谱法测定铸造铝合金中微量钙和钠  被引量:7

Determination of Trace Amounts of Calcium and Sodium in Cast Aluminum Alloys by Photoelectric Direct-Reading Spectrometry

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作  者:兰标景 陆科呈 刘俊生[1] LAN Biaojing, LU Kecheng, LIU Junsheng(ALNAN Aluminium Inc. of Guangxi , Nanning 530031, China)

机构地区:[1]广西南南铝加工有限公司,南宁530031

出  处:《理化检验(化学分册)》2018年第11期1329-1333,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘  要: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0.000 01%和0.000 02%。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%。Photoelectric direct-reading spectrometry was applied to the determination of trace amounts of calcium and sodium in cast aluminum alloys and optimum conditions for the determination were studied. The following requirements should be fulfilled in order to obtain satisfactory analytical results: ① slit of the spectrograph should be adjusted to its best position by integral tracing to have the light with highest intensity passing through; ②sampling should be performed according to the rules described in GB/T 17432--2012, in order to avoid inclusion, crackles, gas holes, greasy dirt, dust, oxides and etc. on the analytical surface of the sample; ③ the prepared sample should have a smooth and clean surface; ④argon of high purity and desirable flow should be used;⑤ type calibration should be performed by analyzing standard sample having its values of contents of calcium and sodium very close to those of the unknown sample. Detection limits (3s) of calcium and sodium were 0.000 01% and 0.000 02% respectively. 5 CRMs of aluminum alloys were analyzed by the proposed method, giving results of calcium and sodium in consistency with the certified values, and another 3 known samples were analyzed duplicately giving values of RSDs (n=ll) in the range of 1.6%-3.9%.

关 键 词:光电直读光谱法 铸造铝合金   

分 类 号:O657.3[理学—分析化学]

 

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