基于磷钼酸喹啉重量法测定进出口磷铁中磷含量  

Determination of Phosphorus Content in Imported and Exported Ferrophosphorus Based on Quinoline Phosphomolybdate Gravimetric Method

作　　者：曲强 田琼 刘益锋 叶金燕 QU Qiang;TIAN Qiong;LIU Yi-Feng;YE Jin-Yan(Zhanjiang Customs Technology Center,Zhanjiang 524022;Zhongshan Customs Technology Center,Zhongshan 528403)

机构地区：[1]湛江海关技术中心,湛江524022 [2]中山海关技术中心,中山528403

出　　处：《中国口岸科学技术》2025年第3期42-46,共5页China Port Science and Technology

基　　金：湛江市非资助科技攻关计划项目(2024B01085)。

摘　　要：磷铁中磷含量的测定主要标准有YB/T4532-2016《磷铁磷含量的测定酸碱滴定法》,该方法操作步骤较为繁琐,存在一定的系统误差。而波长色散X射线荧光光谱法、电感耦合等离子体发射光谱法以及分光光度法等仪器分析法,则对实验室仪器设备要求较高,在一定程度上增加了检测成本。为此,本研究建立了磷钼酸喹啉重量法测定磷铁中磷含量,用数理统计t值检验法检验两种方法的准确度和两种方法之间是否存在显著性差异,用数理统计F检验法比较两种方法的精密度。结果显示,两种方法均准确可靠,与标准值非常接近;两种方法的结果吻合得很好,不存在显著性差异。但经对比,磷钼酸喹啉重量法的精密度比酸碱滴定法好。用磷钼酸喹啉重量法对标准样品做加标回收试验,回收率在99.29%~100.71%之间;研究测定结果与干燥沉淀时间的关系,干燥沉淀时间分别设为1.0 h、1.5 h、2.0 h、2.5 h进行实验,测定结果无明显差异,为避免其他因素的影响,选择1.5 h较为合适。结果表明,使用磷钼酸喹啉重量法测定磷铁中的磷含量,准确度和精密度都很好,相对标准偏差(Relative Standard Deviation,RSD)为0.25%(n=7),且分析步骤简单,检测人员易于掌握,耗时短,更加适合分析实验室工作的需求。The main reference standard for the determination of phosphorus content in ferrophosphorus is YB/T 4532-2016Ferrophosphorus-Determination of phosphorus content-Acid-base titration method,which has cumbersome operation steps and certain systematic errors.Instrumental analysis methods such as wavelength dispersive X-ray fluorescence,inductively coupled plasma emission spectroscopy,and spectrophotometry have higher requirements for laboratory instruments and equipment,thereby increasing detection costs.This study established a quinoline phosphomolybdate gravimetric method for determining phosphorus content in ferrophosphorus.The accuracy and significant differences between this method and acid-base titration were evaluated using the t-test,while the precision of both methods was compared using the F-test.The results indicate that both methods are accurate and reliable,with values extremely close to the standard values.The results obtained from the two methods are in good agreement,with no significant differences observed.Upon comparison,the quinoline phosphomolybdate gravimetric method demonstrated superior precision to the acid-base titration method.A spike-recovery experiment was conducted using the quinoline phosphomolybdate gravimetric method on standard samples,with the recovery rates ranging from 99.29-100.71%.The relationship between the analytical results and the drying precipitation time was also investigated.Experiments were performed with drying precipitation times set at 1.0 h,1.5 h,2.0 h,and 2.5 h,respectively,and no significant differences were observed in the results.To minimize the influence of other factors,a drying precipitation time of 1.5 h was deemed appropriate.The results indicate that the quinoline phosphomolybdic gravimetric method for determining the phosphorus content in ferrophosphorus exhibits excellent accuracy and precision,with a relative standard deviation(RSD)of 0.25%(n=7).The analytical procedure is simple,easily mastered by laboratory personnel,and time-efficient,making it particu

关 键 词：磷铁 磷 磷钼酸喹啉重量法 酸碱滴定法 

分 类 号：O657.3[理学—分析化学]