Determination of Carbon in Ni-Al Powder by the Pure Chemical Substance Calibration-high Frequency Combustion Infrared Absorption Method
-
摘要: 镍基粉末中碳含量的分析质量直接影响材料的性能，但由于碳含量范围较宽，且测定干扰不同，最佳测量条件不一致，更无国家标准方法。高频燃烧-红外吸收法已广泛用于新型材料（如复合碳硅锰铁）中碳和硫的分析，本文基于前期测定镍基钎料以及镍基自熔合金的研究，采用高频燃烧-红外吸收法测定镍铝粉末中的碳，实验中选择纯铁与钨锡作助熔剂，高温燃烧分解样品，通过优化助熔剂用量及其添加顺序、样品称样量等测定条件，获得了较为准确的结果。该方法用于实际样品中碳的测定，相对标准偏差小于1.2%（RSD，n=11），加标回收率为98.0%~105.0%。本方法采用的助熔剂解决了样品导磁性差、燃烧易飞溅等问题，并且针对新型材料缺少标准样品，根据待测样品含量配制相应浓度的基准物质碳酸钠绘制校准曲线，消除了无标准校正的影响，提高了分析结果的准确性。该方法可分析镍铝粉末中含量在0.005%~0.60%范围的碳，也可为制定镍基粉末中碳的标准分析方法提供依据。
Abstract: The carbon in Ni-based powder directly influences the property of the material. However, there is no national standard method to determine carbon content in Ni-based powder, according to the wide content range of carbon, different interferences and inconsistent optimal measuring conditions. The High Frequency Combustion-Infrared Absorption Method is already widely used to determine carbon and sulfur in new materials (such as carbon ferro-silico-manganese). Based on the preliminary study on Ni-based brazing material and Ni-based self-fluxing alloy, the high frequency combustion infrared absorption method is used to determine carbon content in Ni-Al powder. The sample is burned at high-temperature and decomposed by adding the flux of Fe and W-Sn fluxes. The measurement conditions such as flux adding amounts, sequence and sample weight have been optimized to obtain accurate results. The method has been applied to the determination of practical samples with the relative standard deviation of less than 1.2% and recovery rate of 98.0%-105.0%. The flux used by the method solves the problems of bad conductivity and splashing during burning. As new materials fall short of standard materials, the calibration curve is prepared by standard sodium carbonate relating to the carbon content, which solves the problem of no reference material and also improves the accuracy. The provided analytical method is not only suitable for the analysis of carbon in Ni-Al power within the carbon content range of 0.005%-0.60%, but also provides the basis for the development of a carbon standard analysis method for nickel-based powder. -
-
表 1 助熔剂筛选试验
Table 1 Experiment effect of different flux agents
助熔剂 分次测定值(%) RSD(%) 最大燃烧电流(mA) 燃烧状况 锡 0.4040.400
0.3970.3960.9 390 坩埚有气泡，不光滑 钨 0.3710.364
0.3600.3741.7 200 坩埚有气泡，不光滑 钨锡 0.3960.398
0.3960.3950.3 230 坩埚有气泡，不光滑 铁 0.3880.396
0.3930.3881.0 450 坩埚有气泡，不光滑 铁+钨 0.3930.390
0.3780.3722.6 390 坩埚有少量气泡，较光滑 锡+铁+钨 0.3870.389
0.3950.3910.9 400 坩埚光滑，无气泡 铁+钨锡 0.3940.391
0.3960.3910.6 410 坩埚光滑，无气泡 
下载: 导出CSV
表 2 助熔剂用量及加入方式对碳测定结果的影响
Table 2 Effect of flux agent dosage and adding mode on determination results of carbon
用量与加入方式 分次测定值(%) RSD(%) 燃烧状况 试样+0.3 g铁+1.5 g钨锡 0. 3970.390
0.3990.3931.0 坩埚不光滑，底部有褶皱 试样+0.5 g铁+1.5 g钨锡 0.3940.391
0.3960.3910.6 坩埚光滑，灰尘较少 试样+0.7 g铁+1.5 g钨锡 0.3930.394
0.3960.3980.6 坩埚光滑，灰尘较少 试样+1.0 g铁+1.5 g钨锡 0.3990.401
0.4030.3970.6 坩埚光滑，灰尘较少 试样+0.5 g铁+1.0 g钨锡 0.3910.404
0.3950.3981.4 坩埚光滑，灰尘少 试样+0.5 g铁+1.2 g钨锡 0.3940.396
0.3990.3871.3 坩埚光滑，灰尘少 试样+0.5 g铁+1.7 g钨锡 0.3920.395
0.3890.3981.0 坩埚光滑，灰尘较多 0.5 g铁+试样+1.5 g钨锡 0.3990.395
0.4020.3960.8 坩埚光滑，灰尘较少
下载: 导出CSV
表 3 不同称样量对碳测定结果的影响
Table 3 Effect of sample weight on determination results of carbon
称样量(g) 碳的测定值(%) RSD(%) 分次测定值 平均值 0.10 0. 4000.3870.3880.388 0.391 1.6 0.15 0.3980.4010.3970.409 0.401 1.4 0.20 0.3900.3920.3900.399 0.393 1.1 0.25 0.4020.3980.3950.394 0.397 0.9 0.30 0.4020.4090.3970.398 0.402 1.4
下载: 导出CSV
表 4 方法精密度
Table 4 Precision tests of the method
样品编号 碳的测定值(%) RSD(%) 分次测定值 平均值 镍铝-1 0.4030.4020.4060.401
0.3980.4040.4020.411
0.4090.4110.3960.404 1.2 镍铝-2 0.2990.2940.2930.295
0.2910.2960.2940.301
0.3000.2990.2980.296 1.1
下载: 导出CSV
表 5 加标回收率试验
Table 5 Spiked recovery tests of the method
样品编号 碳的测定值(%) 回收率(%) 本底量 加入量 测得总量 镍铝-1 0.398 0.100 0.517 103.8 0.400 0.100 0.522 104.4 0.400 0.150 0.543 98.7 0.394 0.150 0.572 103.2 0.399 0.200 0.607 101.3 0.407 0.200 0.611 100.6 镍铝-2 0.292 0.100 0.400 102.1 0.294 0.100 0.392 99.6 0.296 0.150 0.457 102.5 0.290 0.150 0.454 103.2 0.293 0.200 0.484 98.2 0.294 0.200 0.492 99.6
下载: 导出CSV
-
胡建华,林冲,张文赜.镍-铝粉末材料的变形致密化研究[J].塑性工程学报,2008,15(4):86-89. http://cdmd.cnki.com.cn/Article/CDMD-10674-2002101939.htm 曹宏燕.冶金材料分析技术与应用[M].北京:冶金工业出版社,2008:40-59. 郭建亭.高温合金材料学(上册)[M].:科学出版社,2008:162. ASTM E1941—2010,Standard Test Method for Determ-ination of Carbon in Refractory and Reactive Metals and Their Alloys[S].
GB/T 223.86—2009,钢铁及合金碳含量的测定——感应炉燃烧后红外吸收法[S]. ASTM E1915—2005,Standard Test Method for Analysis of Metal Bearing Ores and Relative Materials by Combustion Infrared-Absorption Spectrometry[S].
赵淑云,王成,葛钰玮,索金玲,彭秧.高频燃烧-红外碳硫吸收仪测定含铜烧结物料中的高含量硫[J].岩矿测试,2011,30(3):353-356. http://www.cnki.com.cn/Article/CJFDTOTAL-YKCS201103034.htm 王小松,陈曦,王小强,何沙白,杨光宇.高频燃烧-红外吸收光谱法测定钼矿石和镍矿石中的高含量硫[J].岩矿测试,2013,32(4):581-585. http://www.cnki.com.cn/Article/CJFDTOTAL-YKCS201304011.htm 李兰群,尹艳清.高频感应燃烧-红外吸收法测定复合碳硅锰铁中碳和硫[J].冶金分析,2010,30(6):62-65. http://www.cnki.com.cn/Article/CJFDTOTAL-YKCS201404013.htm 郭飞飞,杨植岗,王学华,徐井然,王朝亮,黄小峰,王蓬.高频燃烧红外吸收法测定碳化硼中总碳[J].冶金分析,2012,32(7):38-40. http://www.cnki.com.cn/Article/CJFDTOTAL-YJFX201207007.htm 杨丽,张庸,张继民,刘新,韩树国.高频燃烧-红外吸收法测定钎料中低碳[J].冶金分析,2013,33(9):28-31. http://www.cnki.com.cn/Article/CJFDTOTAL-YJFX201309008.htm 郑立春,张庸,闫秀芬,张继民,杨丽,詹秀嫣,李继超.高频燃烧-红外吸收法测定镍基自熔合金中碳[J].冶金分析,2013,33(11):67-70. http://www.cnki.com.cn/Article/CJFDTOTAL-YJFX201311017.htm YS539—2009,镍基合金粉化学分析方法[S]. 刘英,臧慕文.金属材料分析原理与技术[M].北京:化学工业出版社,2009:550. 张长均,王蓬,张之果.影响高频红外碳硫仪分析结果稳定性的探讨[J].冶金分析,2006,26(6):90-91. http://www.cnki.com.cn/Article/CJFDTOTAL-YJFX200606028.htm 邢华宝,徐汾兰,李锦,曾尊武,陈英颖.钢中超低碳的分析[J].冶金分析,2001,21(2):24-25. http://www.cnki.com.cn/Article/CJFDTOTAL-BXGZ201501004.htm 钟华.纯化学物质校准-高频燃烧红外吸收法测定钛及钛合金中碳[J].冶金分析,2012,32(3):30-34. http://www.cnki.com.cn/Article/CJFDTOTAL-YJFX201203007.htm 任维萍.高频燃烧红外吸收法测定高锰不锈钢中痕量硫的助熔剂选择及其作用机理研究[J].冶金分析,2012,32(11):26-30. doi: 10.3969/j.issn.1000-7571.2012.11.006 张明杰,戴雪峰,陆丁荣,王杰.高频燃烧-红外碳硫仪用于农用地土壤质量调查样品中碳硫的快速测定[J].岩矿测试,2010,29(2):139-142. http://www.cnki.com.cn/Article/CJFDTOTAL-YKCS201002015.htm ASTM E1941—2011,Standard Test Methods for Deter-mination of Carbon, in Refractory and Reactive Metals and Their Alloys[S].
吴永明,陶武,荣金相,张小英.新型W-Fe-Sn复合助熔剂研制、表征及应用[J].冶金分析,2013,33(3):80-84. http://www.cnki.com.cn/Article/CJFDTOTAL-YJFX201303018.htm 张蓉.高频燃烧-红外吸收法分析高碳铬铁中硫[J].冶金分析,2009,29(10):60-62. doi: 10.3969/j.issn.1000-7571.2009.10.014 陈琣榕,李景虹,邓勃.现代仪器分析实验与技术[M].北京:清华大学出版社,2006:21.
计量
- 文章访问数: 892
- HTML全文浏览量: 259
- PDF下载量: 9
京公网安备 11010202008159号