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改进了氧弹燃烧分解-原子荧光法快速测定煤中汞含量方法。在之前研究结果的基础上,进一步考察了氧气含量、样品质量对测定结果的影响,以及该方法对不同煤种、不同灰分含量煤炭样品的适应性。结果表明,维持前方法的其他条件不变,通过反复充放氧气提高氧弹内氧气的含量,样品质量可由原来的0.2 g增加至约1.0 g,回收率可达98%以上;当样品中的汞含量较低时,适当减小样品质量仍能获得理想的回收率。经与权威标准方法比对,该方法对无烟煤、烟煤、褐煤都有很好的适应性,灰分含量在9.76%~46.62%(干基)范围内检测结果不受灰分含量影响。经过有证国家标准物质验证,方法准确可靠。改进后的方法可以促进煤炭样品的充分燃烧、煤中汞的释放以及被酸性高锰酸钾溶液转化吸收,克服了原方法对汞含量低的样品回收率低以及由于称样量小而导致的称量误差大、样品代表性差的缺点,同时提高了仪器的响应值,降低了方法检出限,具有更强的实用价值,可用于煤中汞含量的快速检测。
Improved oxygen bomb combustion decomposition - atomic fluorescence method for rapid determination of mercury in coal. Based on the previous research results, the effects of oxygen content, sample quality on the determination results and the adaptability of the method to coal samples with different coal types and different ash contents were further investigated. The results show that the other conditions of the former method are unchanged, and the oxygen content in the bomb can be increased by repeatedly charging and discharging oxygen. The sample mass can be increased from 0.2 g to 1.0 g and the recovery rate can reach over 98% When the mercury content is low, the proper recovery rate can still be obtained by properly reducing the sample quality. Compared with the authoritative standard method, this method has good adaptability to anthracite coal, bituminous coal and lignite. The test results are not affected by ash content in the range of 9.76% ~ 46.62% (dry basis). After certified national standard material verification, the method is accurate and reliable. The improved method can promote the full combustion of the coal sample, the release of mercury in the coal and the absorption and transformation by the acid potassium permanganate solution, which overcomes the low recovery rate of the sample with low mercury content due to the original method and the small sample weight Weighing error, poor sample representative of the shortcomings, while improving the response of the instrument, reducing the detection limit of the method has a stronger practical value, can be used for rapid detection of mercury in coal.