新疆烟煤中钠量测定方法的改进  

Improvement of the Determination of Sodium in Bituminite of Xinjiang Origin

作　　者：卢远梅[1] 王维雪[1] 杜晓光[2] 陈红川[1] 邬琦斌[1] 

机构地区：[1]国网新疆电力公司电力科学研究院,乌鲁木齐830011 [2]西安热工研究院有限公司,西安710023

出　　处：《理化检验（化学分册）》2016年第12期1380-1383,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家科技支撑计划项目(2015BAA04B03);电力行业标准制定项目(中电联标准[2014]169号)

摘　　要：称取已粉碎并经空气干燥的煤样1．0000g，加入乙醇3mL及0．005mol·L^-1盐酸溶液100mL，在近沸状态下保持5min，以3000r·min^-1速率离心分离15min，分出并保留提取液，残渣按上述方法再提取一次。合并两次提取液（试液A），供测定可溶性钠。残渣及滤纸一并移入瓷坩埚中，于815℃灰化后转入聚四氟乙烯容器中，加入高氯酸1mL及氢氟酸7mL，消化并蒸发至近干，加入盐酸（1＋3）溶液20mL，加热至近沸，冷却，在塑料容量瓶中定容至100mL，此溶液（试液B）供测定酸不溶性钠。按火焰原子吸收光谱法分别测定上述2种溶液中的钠量，其总和即为煤样中钠量的合理值。钠的线性范围在0．80mg·L^-1以内，方法的检出限（3s）为0．030mg·L^-1。加标回收率在86．4%-108％之间，测得钠量在提取液及残渣消化液中的相对标准偏差（n=10）分别为3．2％，6．6％。The crushed and air-dried coal sample （1. 000 0 g） was extracted with C2H5OH （3 mL） and 0. 005 mol·L^-1 HCl solution （100 mL） for 5 min at near boiling temperature. Extract and the insoluble residue were separated by centrifuging at a rate of 3 000 r·L^-1 for 15 min. The extract was separated and reserved. The residue was extracted again in same way as described above. The extract was combined with the first one and reserved for determination of acid soluble sodium. The residue together with the filter paper was ignited in porcelain crucible at 815℃, and the residue was transferred to a PTFE container and digested with I mL of HC104 and 7 mL of HF. The mixture was then fumed to dryness. The residue was taken up by heating with 20 mL of HCl （1＋3） solution. After cooling, the solution was made up to 100 mL in a plastic volumetric flask and used for determination of acid insoluble sodium. Content of sodium in the 2 solutions was determined by FAAS, and sum of sodium in the 2 solutions gave the rational sodium value in the oil sample. Linearity range of sodium was found within 0.80 mg·L^-1 with detection limit （3s） of 0. 030 mg·L^-1. Values of recovery found by standard addition method were in the range of 86.4%-108%. Values of RSD＇s （n=10） for sodium in the extract and in the residue were found as 3.2% and 6.6% respectively.

关 键 词：钠含量 新疆烟煤 火焰原子吸收光谱法 

分 类 号：O657.31[理学—分析化学]