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2 ,E" ",-: 1 "1 ; 6 " "1,89 < 1nm,8 9G# B% 200,() ratio=x>?@a>$ B 1 LM C,JKDC " G#:,E 6!3O # ) OG#:E K" 3 CD E,,34,567 " ",%& Z [1 \P,] + UV E D6 O 1 1 _` R:+ ", ) # H a : (meannormali zation)+1 UV E, E K "1 F 2 F 2O E K" ,1650,1950,2250nm E"./ b E"./ Z%!2, E K"c "1! Z, )!3 3.1?@ O* "21,E 48 1 "UV F 1 F 1 GHI"1 U V6 1100~1200nm E %%CZ! CH 2 J K L X " M N O. /,6 1400~ 1500nm E % NCT NG CH 2 "MN./,6 1650~1750nm E % RDX CH 2 "./,E"./ NC NG CH JKLX" NO./,6 1850~ 2000nm E % NC NG " N O "JKLXM NO. /, 2200~2300nm E % C Z! " CHJKLXTP LX"MNO./ " Q D1,6./ OH ". /, 1400~1450nm E OH" NO./,6 1800~2300nm E OH"./ T, U!"./ V W,X +1!!3,Y " : ) 2 O#Ha : E K" Fig.2 Nearinfraredspectraafterpre processedbymeannor malization 3.2?@$% F&GH ' >? ) " I M (PLS), Z " X R + = R " a'> ) I M (PLS), S + O E K"1 '>!3,G' " Z!" <=>? BR 1 I 1!" <=>? B Table1 The quantitative calibration modelparametersof variouscomponents component RMSEC RMSEP r c r p NC NG RDX water Note:RMSECistherootmeansquarederorofcalibration,RMSEPistheroot meansquarederorofprediction,r c isthecorelationcoeficientofcal ) "UV Fig.1 Raw nearinfraredspectraof48samples 1 "UV, W, *!6 "O ibration,r p isthecorelationcoeficientofprediction. >?" S >?@A,B r c T S # F(RMSEC)+ <=>?", [11] `" >?@A,B r p T # F (RMSEP)+ >? " ChineseJournalofEnergeticMaterials,Vol.24,No.4,2016( ) materials.org.cn
3 345 1 S >?@A,B >?@A,B^CD 0.98, "1,! ' ">?+ 1 " 3.3?@$% FJ K L %& ' "!>?", ) 8.' ">? "21, E, )1!"PQH+ F F, F 3GI F 3a,! NC NG RDX" + F ^ID 1.5%; " + F C, C % 5%,G#H% 1.52%, D,!6./0 "!2 #$, "B P Q 1 6 F F 3b! + F ^ ID 10%,! NC 61,Gc " E,! NG F C% 42.63%,! % FCD 20%# 6! I, +D! NG, ID 6%, )>?+1, F C! RDX6 C D FID 10%,! CD + F ^ID 5%, RDX, F I,!,?&6!, F C, b ^ID 10% HI G' ">?+1,? F C, b " E 3.4?@&K MNO' %! NG 6!61,Gc %& G' >?" ), 1!" #$,, c 68.1, E"1,6, "O,, `1 GR:" / " ) ) 3.2 G ' "! " < = >? + ", `&1 / " H, F 4GI ) 4 1! H"R: Fig.4! Changesinpredictedvaluesofvariouscomponentforsample F 4, V "! HR: C, "R:,!" #$,! " H Da % & D " 1 H PQH"FS, 1! K 5 "G#H %1!" H, H 1 "PQH R 2 2,1! " + F ^ I D 2%,! " + F C,% + F ^ I D 7%,! P Q " RDX@+ F C,% 6.16%, + F F I,% 3.35% I 2 1 H PQH" Table2 Comparisonofthepredictedvaluesandactualones ofvariouscomponentsforsamples b.resultsofrelativeerors ) 3 21,"E Fig.3 Theinternalpredictedresultsofsamplesystems component finalypredicted values/% true values/% absolute erors/% relative erors/% NC NG RDX water
4 346 %& 1!" #$, 1! H " R S, B (CoeficientofVariation, CV) % ],CV D1!"R: `", HRS ",CVH I, 1! #$ GB/T # $ ",CV" $ : S 2 = n i=1 2 ( x i -x ) n-1 (1) CV= S 100% (2) x $,S% F,x i %! H,x %! H"G#H,n% B " B B n=5, I 5 " B % 1! CVH",,B " B, K " B, `1! CVH " R :!" CVH "R: F 5GI m i=1s i MBSD= m,,34,567 (4) $,A ij % j E % i".,a i % ie" n. "G#H,n% B " B B,m % B n=5 m=1201, IB LM " 5 %!3,B 1201!3, )K "!3 )", `&1 / " MBSDH, R: F 6 ) 6 1 MBSD H"R: Fig.6 ChangesinMBSD valuesofsample ) 5! CVH"R: Fig.5 ChangesinCVvaluesofeachcomponent F 5, "R:,!" #$ CVH RI, D 0, R: I O,1, #$ "! H "R: %& D _1 2" #$,)W XY F (MovingBlockStandardDeviation, MBSD)+1 UV E,MBSD D1 "U V ` ", [10], MBSD $ : n i=1(a ij -A i) 2 S i = 槡 n-1 (3) F 6 1 " MBSD H "R : I, Z,6 2.5min K MBSD H ^ID 0.001, ) C"R:, 1!! B <E"FS I,1 #$ 4 C (1) ) NIR : +21, E! ' A, B # C D 0.98,2 1, E,>? F I, "a (2) )' "!>?+ 1 P ", ` /! " X, "1! + F#I D 2%, )! 3 +!"P (3)! ) CVT MBSD Z +1! #$!3,! CVH [! 6 O "R:, MBSD H ChineseJournalofEnergeticMaterials,Vol.24,No.4,2016( ) materials.org.cn
5 347 % _1 2" #$,M )+! #$!3 +: [1]3,,.DNTF + X c " [J].,2010,18(2): LILiang liang,wang Jiang ning,liu Zi ru.efectsofdntf contentsondynamicmechanicalpropertiesofmodifieddouble basepropelant[j].chinesejournalofenergeticmaterials(han nengcailiao),2010,18(2): [2],3,,. ^ +9 " [J].,2013,21(3): QIXiao fei,lijun qiang,zhang Xiao hong,etal.influence ofenergeticpotasium saltaseliminated flameadditiveonper formanceofnitraminemodifieddouble basepropelant[j].chi nesejournalofenergeticmaterials(hannengcailiao),2013,21 (3): [3] L,,.!3 6 O " )[J]. *!,2009(6): JIANG Zhen ming,han Xi,LU Fu jie.applicationofnearin fraredtechnologyinrdxproduction[j].modernscientificin struments,2009(6): [4],,1,.6 0! " )[J].P,2006,23(2): GUO Zhi qiang,ren Qian,HUANG You zhi,etal.applica tionofnearinfrared spectroscopyin determination ofcompo nentsofdetonator[j].chinesejournalofspectroscopylaborato ry,2006,23(2): [5],,,. 0 HMX" [J]. 0,2010,33(3): SU Peng fei,chen Zhi qun,zhou Wen jing,etal.fastdeter minationofthecontentofhmxincompositeexplosivebynear infrareddifusereflectancespectroscopy[j].chinesejournalof Explosives&Propelants,2010,33(3): [6], &!, ",.6 9 #! [J].# $.2012,35(6): ZOU Quan,DENG Guo dong,guo Xiao de,etal.real time detectionofthemainsolidcomponentsconcentrationinrdx CMDBwithNIR spectralanalysis[j].journalofsolid Rocket Technology,2012,35(6): [7]KolerD M,PoschA,H rlg.,etal.continuousquantitative monitoringofpowdermixingdynamicsbynear infraredspectros copy[j].powdertechnology,2011,205: [8]AdityaU Vanarase,MaijuJ rvinen,jannepaaso,etal.devel opmentofamethodologytoestimateerorintheon linemeas urementsofblend uniformity in a continuouspowdermixing process[j].powdertechnology,2013,241: [9] MakotoOtsuka,IkuroYamane.Predictionoftabletproperties Basedonnearinfraredspectraofraw mixedpowdersbychemo metrics:scale upfactorofblendingandtabletingproceses[j]. JournalofPharmaceuticalSciences,2009,98(11): [10]WataruMomose,KeijiImai,ShojiYokota,etal.Procesanalyti caltechnologyappliedforend pointdetectionofpharmaceutical blendingbycombiningtwocalibration freemethods:simultane ouslymonitoringspecificnear infraredpeakintensityandmoving blockstandard deviation[j]. PowderTechnology,2011,210 (2): [11]DongMing gang,wangning.adaptivenetwork basedfuzzyin ferencesystem withleave one outcross validationapproachfor predictionofsurfaceroughness[j].appliedmathematicalmod eling,2011,35(3): RapidTestofModifiedDouble basepropelantcomponentuniformitybynirspectroscopy CHENG Shi chao 1,LIN Xiang yang 1,LIYan 1,JIAN Gui xing 2 (1.SchoolofChemicalEngineering,NanjingUniversityofScienceandTechnology,Nanjing210094,China;2.ShanxiNorthXing anchemicalindustryco. LTD,Taiyuan030008,China) Abstract:Toestablisharapidquantitativetestmethodofblendinguniformityofmodifieddouble basepropelantcomponents,a nearinfrared(nir)spectrometerwasadoptedtotestthedouble baseabsorbedsampleandtoquantitativelyanalyzethecontents ofeachcomponentandtheirdispersionuniformity.firstly,basedonsampletesting,thequantitativecalibrationmodelsofthe components:nitrocelulose(nc),nitroglycerine(ng),cyclotrimethylenetrinitramine(rdx)andwaterwereestablishedandthe corelationcoeficientsofeachcomponentmodelaremorethan0.98,andthemeanvaluesofcomponents absoluteerorsob tainedbyinternalvalidationarelessthan2%.thennirspectraofsamplesintheblendingprocesswerecontinualycolected. Thecomponentcontentsofsamplewerepredictedbytheestablishedmodels.Theabsoluteerorsofthepredictedresultsandthe actualvaluesarelessthan2%.theblendinguniformityofsamplewasanalyzedbycoeficientofvariation(cv)methodforthe contentsofeachcomponentandandmovingblockstandarddeviation(mbsd)methodfortheoriginalspectraofsamples.the CVvaluesofeachcomponentarelessthan1.5%,whileMBSD valueofthesampleislessthan0.001.twokindsofevaluation indexeshavereachedsteadystateafter2.5min,indicatingthatsamplecomponentshaduniform distribution.resultsshow thatit isfeasibletousenearinfrared(nir)spectroscopytotesttheblendinguniformityofmodifieddouble basepropelantcomponents. Keywords:materialtestandanalysis;nearinfrared(NIR);modifieddouble basepropelant;absorbentpowder CLCnumber:TJ55;O65 Documentcode:A DOI: /j.issn
Europa-Universität Viadrina
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