烟火药剂中高氯酸盐定性检测方法研究.pdf

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1、第25卷第9期化学研究与应用Vo1．25，No．92013年9月ChemicalResearchandApplicationSep．，2013文章编号：1004—1656(2013)09—1325-05烟火药剂中高氯酸盐定性检测方法研究严春，肖焕新(广西出入境检验检疫局烟花爆竹检测中心烟花爆竹国家重点实验室，广西北海536000)摘要：本文提出了一种烟火药剂中高氯酸盐定性检测方法。将中性红用于高氯酸盐的定性检测；根据烟火药剂的组成特点对可能干扰检测结果的化学组分做了详细研究，提出了用0~C的10％KC1溶液洗涤样品排除干扰的步骤；对现有13类

2、烟花爆竹用烟火药剂组成进行分析后，确立了用5％CaC1溶液脱附碳粉中高氯酸盐的前处理步骤。研究结果表明，方法检出限为100ng·g～。与以往的分析方法相比，本方法具有简单、实用、可靠等优点，可发展为烟花爆竹用烟火药剂中高氯酸盐定性检测的技术。关键词：烟火药剂；高氯酸盐；定性检测中图分类号：0652．3文献标志码：AResearchonanovelqualitativedetectionmethodofperchlorateinpyrotechniccompositionYANChun’，XIAOHuan-xin(TheStateKeyLabo

3、ratoryofFireworksandFirecracker，GuangxiEntry—ExitInspectionandQuarantineBureauFireworksandFirecrackerTestingCenter，Beihai536000，China)Abstract：Perchlorateisacommonoxidizingagentusedinfireworksandfirecrackers．Themostpopularwayofqualitativedetectionofperehlorateisconventional

4、chemicalanalysismethod．However，therearefewqualitativedetectionmethodswhicharespecificallymeantforperchloratesorperehlorieaciduptonow．Inthispaper，anovelqualitativedetectionmethodonthe印plicationofperchlo—rateinpyrotechniccompositionisproposed．Thepyrotechniccompositioniswashed

5、withtenpercentpotassiumchloridesolutionatzerocentigradeuntilitbecomescolorlessandbasicallyneutra1．Fivepercentcalciumchloridesolutionisappliedasanextractantandthemixtureisheatedandstirredoveraboilingwaterbathforfiveminutes．Themixtureisfilteredwhenitisstillhot．Afewdropsofcool

6、edfiltrateisappliedtotheneutralredreagent：Abrownprecipitationisformedimmediately，whichisanindicationofthepresenceofperchloratesaltdepositsinthePyrotechniccomposition．Therearethreeinnovationsinthismethod．Firstly，neutralredisusedinthedetectionofporchlorateasaloxidation—reduct

7、ionindicator，whichsignificantlyreducetheanalyticaltimebecauseitselectivelyreactswithperehloratesveryquickly．Secondly，basedonthecharacteristicsofpyrotechniccomposition，anin—depthre-searchonthechemicalcomponentswhichcouldinterferetlltheresulthasbeenmade．andaninterferencesuppr

8、essionsteptocleanthesampleswitllpotassiumchloridesolutionhasbeenproposed．Thirdly．b