Abstract：The sample was put in muffle furnace. After increasing the temperature to 700 ℃, the sample was burned for 30 min to decompose the activated carbon. The residue was reduced with 1 mL of hydrazine hydrate followed by dissolution with 15 mL of hydrochloric acid and 5 mL of nitric acid. Yttrium was added into testing solution as internal standard. Pd 340.458 nm was selected as the analytical line. The instrumental conditions were optimized. The determination method of palladium in palladium-carbon by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The results showed that the trace coexisting elements in palladium-carbon sample had no influence on the determination of palladium. The mass concentration of palladium in range of 50.00-300.00 mg/L was linear to the emission intensity with correlation coefficient of r=0.999 99. The detection limit of palladium in this method was 0.015 mg/L. The proposed method was applied to the determination of palladium in palladium-carbon sample. The relative standard deviations (RSD, n=11) were less than 1%. The found results were consistent with those obtained by dimethylglyoxime precipitation - EDTA complexometric titration method.
马媛, 李青, 杨晓滔, 杨辉, 甘建壮, 韩艳波. 电感耦合等离子体原子发射光谱法测定钯炭中钯[J]. 冶金分析, 2016, 36(8): 69-72.
MA Yuan, LI Qing, YANG Xiao-tao, YANG Hui, GAN Jian-zhuang, HAN Yan-bo. Determination of palladium in palladium-carbon by inductively coupled plasma atomic emission spectrometry. , 2016, 36(8): 69-72.
黄晓维.废钯炭催化剂分析方法研究[J].再生资源与循环经济,2008,1(7):35-37.HUANG Xiao-wei.Study on a analysis method of spend palladium-carbon catalyst[J].Renewable Resources andRecycling Economy,2008,1(7):35-37.
[2]
黄瑶,沙娇,徐莲,等.Pd/C催化剂及其冶金废料分解和测定的研究[J].贵金属,2014,35(1):70-74.HUANG Yao,SHA Jiao,XU Lian,et al.Research on dissolution and determination for Pd/C catalyst and itsmetallurgy wast[J].Precious Metals,2014,35(1):70-74.
[3]
朱良.碳钯催化剂中钯含量分析方法改进[J].山西化工,2010,30(2):47-49.ZHU Liang.Improvement of palladium content analysis method in carbon-palladium catalyst[J].Shanxi ChemicalIndustry,2010,30(2):47-49.
[4]
肖红新,岳伟,庄艾春,等.湿法分解-AAS法测定废钯碳催化剂中的钯[J].材料研究与应用,2013,7(3): 202-204.XIAO Hong-xin,YUE Wei,ZHUANG Ai-chun,et al.Determination of the palladium in the waste palladium on carbon catalyst by wet method[J].Materials Research and Application,2013,7(3): 201-204.
[5]
刘东艳,张园力.等离子发射光谱法测定催化剂中的钯[J].石油化工,2001,30(2):138-140.LIU Dong-yan,ZHANG Yuan-li.Determination of palladium content in catalyst by inductively coupled plasmaatomic emission spectrometry(ICP-AES)[J].Petrochemical Technology,2001,30(2):138-140.
[6]
王铁,刘殿丽,王明刚,等.等离子发射光谱法测定钯炭催化剂中钯含量[J].聚酯工业,2012,25(6):30-32.WANG Tie,LIU Dian-li,WANG Ming-gang,et al.Determination the Pd content in Pd-C catalyst by ICP emissionspectroscopy[J].Polyester Industry,2012,25(6):30-32.
刘伟,蔡文云,马媛,等.新制和失效钯炭催化剂中钯含量的ICP-AES法测定[J].贵金属,2013,34(2):61-63.LIU Wei,CAI Wen-yun,MA Yuan,et al.Determination of palladium in fresh and spend Pd/C catalyst byICP-AES[J].Precious Metals,2013,34(2):61-63.
[9]
臧慕文.ICP-AES法测定钯碳催化剂中钯的不确定度的评定[J].分析试验室,2003,22(6):13-17.ZANG Mu-wen.Evaluation of uncertainty for determination of Pd in palladium carbon catalyst by ICP-AES[J].Chinese Journal of Analysis Laboratory,2003,22(6):13-17.
[10]
魏小娟,刘秋香,谢智平,等.电感耦合等离子体原子发射光谱法测定废钯炭催化剂中钯[J].冶金分析,2014,34(11):32-36.WEI Xiao-juan,LIU Qiu-xiang,XIE Zhi-ping,et al.Determination of palladium in waste palladium-carbon catalyst by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2014,34(11):32-36.
