X射线衍射K值法测定氧化铁皮中游离α-SiO2的含量
防城港出入境检验检疫局, 广西 防城港 538001 |
Determination of Free α-SiO2 Content in Mill Scale by X-ray Diffraction K Value Method
Fangchenggang Entry-Exit Inspection and Quarantine Bureau, Fangchenggang 538001, China |
摘要：目前通常采用焦磷酸法和X射线衍射法测定游离α-SiO2的含量, 其中焦磷酸法不能消除氧化铁皮中FeO、Fe3O4和Fe2O3等焦磷酸难溶物质的影响, 不适合用于测定氧化铁皮中的游离α-SiO2。本文建立了采用X射线衍射K值法测定氧化铁皮中游离α-SiO2含量的方法。以α-Al2O3作为参考物质, 以α-SiO2(101) 衍射峰和α-Al2O3(012) 衍射峰作为测量谱峰, 将α-SiO2和α-Al2O3(质量比1:1) 混合均匀制备成测量K值的试样, 获得K值为7.86, 应用此值分析已知游离α-SiO2含量的氧化铁皮样品, 游离α-SiO2含量的测定值与实际值相符。该方法的测定范围为游离α-SiO2含量≥0.50%, 测量范围宽, 且方便快速, 能够满足进口氧化铁皮检验监管的工作需求。
Determination of Free α-SiO2 Content in Mill Scale by X-ray Diffraction K Value Method
ABSTRACT At present, free α-SiO2 content is often determined by the pyrophosphate method and X-ray Diffraction (XRD) method. However, insoluble materials including FeO, Fe3O4 and Fe2O3 in mill scale cannot be decomposed by pyrophosphate, and thus the pyrophosphate method is not suitable for the determination of free α-SiO2 content in mill scale. A method for detecting free α-SiO2 content in mill scale through X-ray diffraction K value method has been developed. α-Al2O3 was used as the reference material. Diffraction peaks of crystal face (101) for α-SiO2 and crystal face (012) for α-Al2O3 were used for measured diffraction peaks. Samples for detecting K value were prepared by mixing α-SiO2 with α-Al2O3 at a mass ratio of 1:1. The acquired K value is 7.86. The measured K value has been applied to the determination of mill scale samples with known free α-SiO2 content, and the analytical results of free α-SiO2 content are in good agreement with practical values. Detection range of this method is that free α-SiO2 are equal or greater than 0.5%. This method is convenient and rapid, and has a wide detection range and can meet the need of imported mill scale inspection and supervision work.
本文参考文献
| [1] |
韩小红. 粉尘中游离二氧化硅含量测定过程的质量控制[J]. 山西化工, 2011, 31(6): 43-44. Han X H. Quality Control in the Determination of Content of Free Silica in Dust[J]. Shanxi Chemical Industry, 2011, 31(6): 43-44. |
| [2] |
徐彦, 于会明, 于冬雪, 等. 工作场所粉尘中游离二氧化硅含量焦磷酸测定法的影响因素[J]. 工业卫生与职业病, 2012, 38(5): 262-265. Xu Y, Yu H M, Yu D X, et al. Interferences in Determination of Free Silica in Dust of Workplaces with Pyrophosphoric Acid Method[J]. Industrial Health and Occupational Diseases, 2012, 38(5): 262-265. |
| [3] |
李小萍, 麦志丹, 梁德新, 等. X射线衍射里特沃尔德全谱图拟合法与焦磷酸法测定锡冶炼粉尘中游离二氧化硅水平比较[J]. 中国职业医学, 2013, 40(1): 45-46. Li X P, Mai Z D, Liang D X, et al. Comparison between X-ray Diffraction Rietveld Full Spectrum Diagram and Pyrophosphate Methods in Determinaton of Free Silica Content in Tin Smelting Dust[J]. China Occupational Medicine, 2013, 40(1): 45-46. |
| [4] |
赵明琦, 方政, 杨仁江, 等. 用X射线衍射测定呼吸性粉尘中游离α-SiO2[J]. 理化检验(物理分册), 2003, 39(12): 631-635. Zhao M Q, Fang Z, Yang R J, et al. The Determination of α-quartz in Respirable Dust by X-ray Diffraction[J].Physical Testing and Chemical Analysis (Part A:Physical Testing), 2003, 39(12): 631-635. |
| [5] |
吴建鹏, 曹丽云, 张国运, 等. XRD物相定量分析外标法标准曲线库的建立[J]. 分析测试学报, 2006, 25(4): 95-97. Wu J P, Cao L Y, Zhang G Y, et al. Establishment of the Standard Curve Database for XRD Analysis Based on the External Standard Method[J]. Journal of Instrumental Analysis, 2006, 25(4): 95-97. |
| [6] |
袁珂, 廖立兵, 万红波, 等. 膨润土中方石英和α-石英的定量相分析——X射线衍射外标法和K值法的对比[J]. 硅酸盐学报, 2011, 39(2): 377-382. Yuan K, Liao L B, Wan H B, et al. Quantitative Analysis of Cristobalite and α-quartz in Bentonite by X-ray Powder Diffraction—Comparison between External Standard and K-value Method[J].Journal of the Chinese Ceramic Society, 2011, 39(2): 377-382. |
| [7] |
吴建鹏, 黄剑锋, 贺海燕, 等. X射线衍射物相定量分析内标法标准曲线库的建立[J]. 岩矿测试, 2006, 25(3): 215-218. Wu J P, Huang J F, He H Y, et al. Development and Application of a Standard Curve Database in Quantitative Phase Analysis by XRD Based on the Internal Standard Method[J]. Rock and Mineral Analysis, 2006, 25(3): 215-218. |
| [8] |
Al-Jaroudi S S, Ul-Hamid A, Mohammed A I, et al. Use of X-ray Powder Diffraction for Quantitative Analysis of Carbonate Rock Reservoir Samples[J].Powder Technology, 2007, 175: 115-121. doi: 10.1016/j.powtec.2007.01.013 |
| [9] |
房俊卓, 张霞, 徐崇福, 等. 实验条件对X射线衍射物相定量分析结果的影响[J]. 岩矿测试, 2008, 27(1): 60-62. Fang J Z, Zhang X, Xu C F, et al. Effect of Experimental Condi-tions on X-ray Diffractometric Quantitative Phase Analysis[J]. Rock and Mineral Analysis, 2008, 27(1): 60-62. |
| [10] |
Ural S. Quantification of Crystalline (Mineral) Matter in Some Turkish Coals Using Interactive Rietveld-based X-ray Diffractometry[J].International Journal of Coal Geology, 2007, 71: 176-184. doi: 10.1016/j.coal.2006.08.002 |
| [11] |
曾令民, 杨喜英, 王力珩, 等. X射线衍射里特沃尔德全谱图拟合法测定粉尘中游离的SiO2[J]. 分析化学, 2008, 36(5): 599-603. Zeng L M, Yang X Y, Wang L H, et al. Determination of Weight Concentration of Free Silicon Dioxide for Dust Using X-ray Diffraction Technique and Rietveld Refinement Method[J].Chinese Journal of Analytical Chemistry, 2008, 36(5): 599-603. |
| [12] |
李昆, 王文宝. 云母矿粉中游离二氧化硅含量的快速测定[J]. 分析仪器, 2014, (2): 43-46. Li K, Wang W B. Quick Determination of Free Silica in Mica Powder[J]. Analytical Instrumentation, 2014, (2): 43-46. |
| [13] |
晋勇,孙小松,薛屺. X射线衍射分析技术[M] . 北京: 国防工业出版社, 2008 Jin Y,Sun X S,Xue Q. X-ray Diffraction Analysis Technique[M] . Beijing: National Defence Industry Press, 2008 |
| [14] |
于吉顺,雷新荣,张锦化. 矿物X射线粉晶鉴定手册[M] . 武汉: 华中科技大学出版社, 2011 Yu J S,Lei X R,Zhang J H. X-ray Powder Mineral Identification Manual[M] . Wuhan: Huazhong University of Science and Technology Press, 2011 |
| [15] |
迟广成, 张泉, 赵爱林, 等. X射线粉晶衍射仪定量测量海泡石矿样的实验条件[J]. 岩矿测试, 2012, 31(2): 282-286. Chi G C, Zhang Q, Zhao A L, et al. Experimental Conditions of X-ray Powder Diffraction for Sepiolite Measurement[J]. Rock and Mineral Analysis, 2012, 31(2): 282-286. |
相似文献（共20条）
| [1] |
周丹怡, 陈华, 陆太进, 柯捷, 何明跃. 基于拉曼光谱-红外光谱-X射线衍射技术研究斜硅石的相对含量与石英质玉石结晶度的关系. 岩矿测试, 2015, 34(6): 652-658. doi: 10.15898/j.cnki.11-2131/td.2015.06.008 |
| [2] |
黄剑锋, 朱广燕, 吴建鹏, 曹丽云, 贺海燕. 无机材料中24种组分X射线衍射物相定量分析外标法标准曲线库的建立. 岩矿测试, 2007, 26(5): 398-400. |
| [3] |
任叶叶, 张俭, 严俊, 林剑, 陈思杭, 盛嘉伟. 应用X射线衍射-红外光谱等技术研究滑石在机械力研磨中的形貌和晶体结构变化及影响机制. 岩矿测试, 2015, 34(2): 181-186. doi: 10.15898/j.cnki.11-2131/td.2015.02.005 |
| [4] |
徐国栋, 王冠, 程江, 董随亮. 应用能谱扫描电镜与X射线衍射等分析技术研究西藏扎西康铅锌矿中伴生元素锰的赋存状态. 岩矿测试, 2014, 33(6): 808-812. doi: 10.15898/j.cnki.11-2131/td.2014.06.008 |
| [5] |
叶美芳, 刘三, 解古巍, 赵慧博, 周宁超, 魏小燕, 杨建国, 侯弘, 王磊, 王轶. 应用扫描电镜-X射线衍射-电子探针研究北山斑岩铜矿区绢英岩中白色云母的特征. 岩矿测试, 2016, 35(2): 166-177. doi: 10.15898/j.cnki.11-2131/td.2016.02.009 |
| [6] |
周姣花, 汪建宇, 顾茗心, 王真. 利用X射线衍射和岩矿鉴定等技术研究河南汤家坪钼矿区主要矿物标型特征. 岩矿测试, 2015, 34(1): 82-90. doi: 10.15898/j.cnki.11-2131/td.2015.01.011 |
| [7] |
张梅, 高孝礼, 黄光明, 封亚辉. 微量石棉的X射线衍射定量检测. 岩矿测试, 2010, 29(3): 309-312. |
| [8] |
武素茹, 宋义, 谷松海, 郭芬, 孙鑫. X射线荧光光谱-X射线衍射-红外光谱联用技术鉴别锰矿与锰冶炼渣. 岩矿测试, 2015, 34(6): 659-664. doi: 10.15898/j.cnki.11-2131/td.2015.06.009 |
| [9] |
迟广成, 肖刚, 伍月, 陈英丽, 王海娇, 胡建飞. X射线粉晶衍射仪在大理岩鉴定与分类中的应用. 岩矿测试, 2014, 33(5): 698-705. |
| [10] |
解古巍, 叶美芳, 黄静, 王小琳, 南珺祥, 任志鹏, 石小虎, 柳娜. 大颗粒黏土矿物对黏土矿物X射线衍射定量分析的影响. 岩矿测试, 2018, 37(5): 499-506. doi: 10.15898/j.cnki.11-2131/td.201708190131 |
| [11] |
曾蒙秀, 宋友桂. 基于麦夸特算法的X射线衍射物相定量分析的影响因素研究. 岩矿测试, 2012, 31(5): 798-806. |
| [12] |
张妮, 林春明. X射线衍射技术应用于宝石鉴定-合成及晶体结构研究进展. 岩矿测试, 2016, 35(3): 217-228. doi: 10.15898/j.cnki.11-2131/td.2016.03.002 |
| [13] | |
| [14] |
聂轶苗, 牛福生, 刘淑贤, 魏少波. 应用X射线衍射-扫描电镜-光学显微镜鉴定黑龙江石墨尾矿中的绢云母. 岩矿测试, 2015, 34(2): 194-200. doi: 10.15898/j.cnki.11-2131/td.2015.02.007 |
| [15] |
任伟, 汪立今, 李甲平. 电子探针和X射线衍射仪测定新疆祖母绿宝石. 岩矿测试, 2010, 29(2): 179-181. |
| [16] |
胡海祥, 范作鹏, 牛桂强, 刘洪澜, 刘海龙, 王攀志. 焦家金矿选厂旋流器溢流产品工艺矿物学分析. 岩矿测试, 2014, 33(4): 535-544. |
| [17] | |
| [18] |
陈岳, 罗武干, 穆青, 赵学峰, 王昌燧. 河北临漳曹村窑址青釉器物工艺特征研究. 岩矿测试, 2013, 32(1): 64-69. |
| [19] | |
| [20] |
计量
- PDF下载量(1035)
- 文章访问量(1452)
- HTML全文浏览量(38)
- 被引次数(0)