Abstract：The composition of sintered flux is complex. In addition to some natural minerals such as quartz, fluorite and marble, it also contains metals and their alloys. For the existing detection methods of sintered flux, only the total amount of silicon dioxide in sintered flux was determined, but the content of quartz phase could not be quantitatively analyzed. The selective dissolution tests of the common components in sintered flux were carried out. The results showed that the soluble substances such as magnesia, calcium carbonate, wollastonite, potassium feldspar, iron powder and nickel powder could be fully dissolved with hydrochloric acid and nitric acid. In the presence of fluorite in sintered flux, the addition of boric acid could effectively prevent the corrosion of quartz by F- generated from fluorite under strong acidic conditions. When sintered flux contained ferrosilicon alloy, the ferrosilicon alloy could be fully and selectively dissolved by adding hydrofluoric acid under the protection of boric acid. Nitric acid-phosphoric acid could effectively dissolve the refractory minerals such as corundum. Based on this, a determination method of quartz content in sintered flux was established. Firstly, the system of boric acid, hydrochloric acid, nitric acid hydrofluoric acid was added to dissolve the soluble minerals such as fluorite and marble as well as metals and their alloys, thus the quartz was preliminarily enriched. Then, nitric acid-phosphoric acid was added to dissolve and separate refractory minerals such as corundum, thus realizing the further enrichment of quartz. Finally, nitric acid, hydrofluoric acid and perchloric acid were used to dissolve the quartz after the above two steps of enrichment and vaporize silicon, and the content of quartz after separation and enrichment was determined by subtraction gravimetric method. The contents of quartz in sintered flux samples were determined according to the proposed method. The relative standard deviations (RSD, n=8) of determination results were between 0.46% and 0.93%, and the recoveries were between 99% and 103%.
王吉, 向滢, 彭强, 杨光茜. 重量法测定烧结焊剂中石英[J]. 冶金分析, 2023, 43(6): 55-61.
WANG Ji, XIANG Ying, PENG Qiang, YANG Guangqian. Determination of quartz in sintered flux by gravimetric method. , 2023, 43(6): 55-61.
[1] 孙咸.烧结焊剂的冶金过程及工艺质量控制[J].机械制造文摘(焊接分册),2015(1):1-5. SUN Xian.Metallurgical process and process quality control of sintered flux[J].Welding Digest of Machinery Manufacturing,2015(1):1-5. [2] 程年寿,汪徐春,张雪梅,等.石英砂中二氧化硅含量的红外定量分析[J].硅酸盐通报,2015,34(6):1648-1652. CHENG Nianshou,WANG Xuchun,ZHANG Xuemei,et al.Infrared quantitative analysis of silicon dioxide content in quartz sand[J].Bulletin of The Chinese Ceramic Society,2015,34(6):1648-1652. [3] 张文钺.焊接冶金学(基本原理)[M].北京:机械工业出版社,2014:52-56. [4] 张舒婷.焊剂对焊接接头成型的影响的优化设计[J].山东工业技术,2014(13):22. ZHANG Shuting.Optimization design of the effect of flux on the forming of welded joints[J].Shandong Industrial Technology,2014(13):22. [5] 中华人民共和国工业和信息化部.JB/T 7948.1—2017焊剂化学分析方法 第1部分 二氧化硅含量测定[S].北京:机械工业出版社,2017. [6] 甘肃省机械工程学会.T/GMES005—2018焊剂中多种成分的测定X射线荧光光谱法[S].甘肃:甘肃省机械工程学会,2018. [7] 陶倩.X射线荧光光谱分析烧结焊剂[J].理化检验(化学分册),2007,43(8):684-685. TAO Qian.XRFS analysis of sintered welding powder (CHF301)-Preparation of sample disk by mouldpressing method[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2007,43(8):684-685. [8] 刘攀,常国梁,张欣耀,等.我国焊接药剂化学分析标准体系现状与发展[J].冶金分析,2020,40(11):8-16. LIU Pan,CHANG Guoliang,ZHANG Xinyao,et al.Status and development of standard system for chemical analysis of welding flux in China[J].Metallurgical Analysis,2020,40(11)8-16. [9] 刘攀,李景滨,何鹏飞,等.我国焊接药剂分析方法的应用现状[J].冶金分析,2021,41(7):1-9. LIU Pan,LI Jingbin,HE Pengfei,et al.Application status of analysis methods for welding flux in China[J].Metallurgical Analysis,2021,41(7):1-9. [10] 席进萍,沈燕君,温明慧.岩石矿物及粉尘中游离二氧化硅的测定[J].岩矿测试,2002,21(1):71-73. XI Jinping,SHEN Yanjun,WEN Minghui.The determination of free-SiO2 in rocks,minerals and dusts[J].Rock and Mineral Analysis,2002,21(1):71-73. [11] 牛改玲.磷酸溶解灰岩中游离二氧化硅测试方法的改进与讨论[J].中国非金属矿工业导刊,2017(4):20-21,25. NIU Gailing.Improvement and discussion on the test method of free silica in limestone dissolved by phosphoric acid[J].China Non-Metallic Minerals Industry,2017(4):20-21,25. [12] 龚丽芳.矿石中游离二氧化硅的测定方法研究[J].世界有色金属,2018(4):291-292. GONG Lifang.Study on determination of free silica in ore[J].World Nonferrous Metals,2018(4):291-292. [13] 雷萍,蒲志,陈伟.灰岩中的游离二氧化硅的化学物相分析方法的探讨[J].福建分析测试,2011,20(5):33-35. LEI Ping,PU Zhi,CHEN Wei.Discussion of chemistry phase analytic method of the dissociation silicon dioxide in calcareous rock[J].Fujian Analysis & Testing,2011,20(5):33-35. [14] 郑大中,郑若锋.矿石中游离二氧化硅的快速物相分析[J].四川化工与腐蚀控制,2002,5(3):4-10. ZHENG Dazhong,ZHENG Ruofeng.Rapid phase analysis of free silica in ores[J].Sichuan Chemical Industry,2002,5(3):4-10.
