| 光谱学与光谱分析 |
|
|
|
|
|
| A Set of Infrared Cells for the Determination of Titanium Oxychloride in Refined Titanium Tetrachloride |
| SONG Guang-lin1,2, LUO Yun-jun1*, LI Jin-qing1, LI Qing2, TAN Hong2 |
1. School of Material Science and Engineering, Beijing Institute of Technology, Beijing 100081, China
2. Guizhou Academy of Testing and Analysis, Guiyang 550002, China |
|
|
|
|
Abstract The content control of the impurities in refined TiCl4 becomes the key part for the quality control of titanium material. Refined TiCl4 is the key procedure in producing titanium sponge. Besides, the content of the impurities in titanium sponge and that of the impurities in refined TiCl4 presents the 4-times enrichment relationship. Therefore, control the content of the oxygen, there is the need to analyze the source of oxygen impurities so that strict control can be conducted over the impurities of refined TiCl4. Determination of TiOCl2 in refined TiCl4 was significant for analysis of its impurities. TiOCl2 could be determined by infrared spectroscopy due to its infrared characteristic spectrum line. However, normal infrared absorption cell was not fit for the sample analysis, because TiCl4 easily reacted with moisture in the air and immediately was hydrolyzed to form highly corrosive hydrochloric acid smoke. According to Lambert-Beer Law, which means the concentration (cx) and absorbance(A)～length (L) curve’s slope have direct ratio. The infrared absorption cell with the window film of ZnSe (10×1 mm, wavenumers: 7 800～440 cm-1) and the glass cell (optical path: 22, 12, 7 and 4 mm) was assembled and utilized in determination of the TiOCl2 in refined TiCl4 by standard addition method. The detection limit of TiOCl2 was 17.8 mg·kg-1, the regression equation was Y=1.011 8X, R=0.996 3; With standard addition method, the regression equation of TiOCl2 was Y=1.940 0X, R=0.997 0, it’s good in linearity relation, the TiOCl2 content in refined TiCl4 is determined to be 833.8 mg·kg-1 and SD up to 40.0 mg·kg-1. RSD of the method precision is between 0.95%～1.94%, while recovery rate is between 88.5%～93.1%. This infrared absorption device was safe, simple and convenient, easily removable and washable, and re-useable. The method could conduct the quantitative analysis over the TiOCl2 content in refined TiCl4 through adding standard sample for one time, it could meet the requirement of determination of TiOCl2 in refined TiCl4.
|
|
Received: 2015-01-05
Accepted: 2015-04-15
|
|
|
|
Corresponding Authors:
LUO Yun-jun
E-mail: yjluo@bit.edu.cn
|
|
[1] PU Xue-wei, CUI Qing-xiong(普学伟, 崔庆雄). Hunan Nonferrous Metals(湖南有色金属)，2012, 28 (1): 31.
[2] LI Shui-e, ZHANG Jin-zhu, LI Rong(李水娥, 张金柱, 李 容). Light Metals (轻金属)，2012(6): 55.
[3] DENG Guo-zhu, WANG Xiang-dong(邓国珠, 王向东). Titanium Industry Progress(钛工业进展), 2007, 24(2): 9.
[4] OUYANG Quan-sheng, ZHAO Zhong-wei, ZHU Yong-hong(欧阳全胜, 赵中伟, 祝永红). Rare Metals and Cemented Carbides(稀有金属与硬质金属), 2004, 32(2): 47.
[5] MO Wei, DENG Guo-zhu, LUO Fang-cheng(莫 畏, 邓国珠, 罗方承). Titanium Alloys(钛冶金). Beijing: Metallurgical Industry Press(北京: 冶金工业出版社)，1998. 135.
[6] YAN Shou-yi(闫守义). Titanium Industry Progress(钛工业进展), 2012, 29(1): 1.
[7] DENG Guo-zhu(邓国珠). Iron Steel Vanadium Titanium(钢铁钒钛), 2011, 32(4): 1.
[8] Sarala Raoot, Desikan N R, Shekhar R, et al. Applied Spectroscopy, 2000, 54(9): 1412.
[9] SONG Yu-ping, TAN Hong, SUN Jun-ping, et al(宋玉萍, 谭 红, 孙军平, 等). Journal of Chongqing University(重庆大学学报), 2007, (Supplement): 88.
[10] WENG Shi-fu(翁诗甫). Analysis of Fourier Transform Infrared Spectroscopy(傅里叶变换红外光谱分析). Beijing: Chemical Industry Press(北京: 化学工业出版社)，2010. 321. |
| [1] |
CHEN Di, SONG Chen, SONG Shan-shan, ZHANG Zhi-jie*, ZHANG Hai-yan. The Dating of 9 Batches of Authentic Os Draconis and the Correlation
Between the Age Range and the Ingredients[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2023, 43(06): 1900-1904. |
| [2] |
HAO Jun1, WANG Yu2, LIU Cong2, WU Zan2, SHAO Peng2, ZU Wen-chuan2*. Application of Solution Cathode Glow Discharge-Atomic Emission Spectrometry for the Rapid Determination of Calcium in Milk[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2022, 42(12): 3797-3801. |
| [3] |
TANG Ju1, 2, DAI Zi-yun2*, LI Xin-yu2, SUN Zheng-hai1*. Investigation and Research on the Characteristics of Heavy Metal Pollution in Children’s Sandpits Based on XRF Detection[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2022, 42(12): 3879-3882. |
| [4] |
WANG Guo-shui1, GUO Ao2, LIU Xiao-nan1, FENG Lei1, CHANG Peng-hao1, ZHANG Li-ming1, LIU Long1, YANG Xiao-tao1*. Simulation and Influencing Factors Analysis of Gas Detection System Based on TDLAS Technology[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2021, 41(10): 3262-3268. |
| [5] |
YANG Hui-qin1, 2, ZHANG Bo1, 2, MA Ling1, 2, SHANG Yi1, 2, GAO Dong-li1, 2*. Extraction and Spectroscopic Analysis of Chlorogenic Acid in Diploid Potato[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2020, 40(12): 3860-3864. |
| [6] |
LI Ling1, 2, 3, NAI Xue-ying1, 2*, CHAI Xiao-li1, 2, 3, LIU Xin1, 2, GAO Dan-dan1, 2, DONG Ya-ping1, 2. Optimization of Determination Method of Lithium in Oil-Field Water Based on DOE[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2020, 40(08): 2617-2621. |
| [7] |
ZHANG Jiu-ming1, 2, ZHOU Bao-ku1, WEI Dan3*, CHI Feng-qin1*, HAO Xiao-yu1, JIN Liang1, KUANG En-jun1. Spectroscopic Characteristics of HA Structure in Black Soil with Organic and Inorganic Fertilizer[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2019, 39(03): 845-850. |
| [8] |
NIE Li-xing, CHANG Yan, DAI Zhong, MA Shuang-cheng*. A New Method for Determination of Polysorbate 80 in Shengmai Injection Based on Absorption Coefficient[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2019, 39(01): 199-203. |
| [9] |
YU Jie1, ZHU Shu-wen1, LU Quan-fang1, 2*, ZHANG Zhi-chao1, ZHANG Xiao-min1, WANG Xing1, YANG Wu1. High Sensitive Determination of Pb and Zn in Refined Copper Ores Samples Using Liquid Cathode Glow Discharge-Atomic Emission Spectrometry[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2018, 38(11): 3550-3557. |
| [10] |
XIE Feng-ying1, LI Feng-feng1, ZHANG Shuang1, BI Wei-wei2, ZHANG Xiu-ling1*, ZHANG Xiao-nan1. Analysis of Acylation Modification of Black Rice Anthocyanins Using Fourier Transform Infrared Spectroscopy (FTIR)[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2018, 38(08): 2386-2389. |
| [11] |
ZHONG Yong-cui1, 3, 4, YANG Li-wei2, QIU Yun-qi2, WANG Shu-mei1,3,4, LIANG Sheng-wang1, 3, 4*. Rapid Determination of Geniposide in Gardenia Jasminoids Ellis in Different Preparations Methods with NIRS[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2017, 37(06): 1771-1777. |
| [12] |
LI Jian-ting1, 2, ZHANG Yi-ming2, DU Mei2, HAO Qian2, LI Jian-qiang1*. Study on the Interferences and Direct Determination of Sc in Metallurgical Tails with Inductively Coupled Plasma Mass Spectrometry[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2017, 37(04): 1259-1263. |
| [13] |
QUAN Chao-ming1, 2, 3, HU Yao-qiang1, 2, 3, LIU Hai-ning1, 2, LI Ming-zhen1, 2, YE Xiu-shen1, 2*, WU Zhi-jian1, 2* . Rapid Determination of Dodecylmorpholine in Aqueous Solutions with UV-Vis Spectrophotometry[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2017, 37(02): 509-512. |
| [14] |
GUO Meng-lin, YANG Hui-qing, HUANG Ping, CHEN Lin, LI Dong-hui* . Application of Cationic Aluminum Phthalocyanine, a Red-Emitting Fluorescent Probe, for Sensitive Quantitative Analysis of RNA at Nanogram Level[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2016, 36(03): 749-754. |
| [15] |
WANG Shu-tao, CHEN Dong-ying*, WANG Xing-long, WEI Meng, WANG Zhi-fang . A New Method for the Determination of Potassium Sorbate Combining Fluorescence Spectra Method with PSO-BP Neural Network[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2015, 35(12): 3549-3554. |
|
|
|
|
