Comparison of the Reflectance and the Absorption Spectrometries Using the Combined Spectrometer

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(1)Journal of the Korean Chemical Society 2001, Vol. 45, No. 1 Printed in the Republic of Korea.

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(3) (2000. 11. 29 ) †. Comparison of the Reflectance and the Absorption Spectrometries Using the Combined Spectrometer Hoon Hwang* , Sehui Jung, and Kyungsoo Lee† Department of Chemistry, Kangwon National University, Chunchon 200-701, Korea † Bookwon Girls Senior Highschool, Wonjoo 220-100, Korea (Received November 29, 2000). . !" #$%

(4) &'( )* +%,-. Cu ./0123 Co ./01234( 25 67 8 %9, :& ; <= >? @AB :& CD EF GH I? @A J. KL M*N OP. QR ST238 5 8 2.%U V2W X-N 6( YZ%,-. 2+. 2+. ABSTRACT. A combined spectrometer which could function as either the absorption spectrometer or the reflectance spectrometer was built and used for the comparison of the applicabilities of the two types of spectrometers. According to the results the sensitivity of the reflectance spectrometry was found to be useful for the quantitative analysis when the concentration of the analyte was too low or the molar absorptivity of the analyte was too small for one to perform the quantitative analysis using the absorption spectrometry.. KL (absorption spectrometer)4 ? [\8 5 ] (absorption)^:8 _`%

(5) ST a :&8 b5 OPVZ Oc" dMe, f gh8N (radiation source), ij (monochromator), k6(cell compartment), fl mnK(radiation detector) o)* p&&(component)4. qr(configuration)st X-. .N ul @A mnK cell( avM* wx J? y8 z% { qrst XMe, M*h| ST238 } ] a ST238 ~ st N (reflected light). mn K8 ~ H-. [\ 8 . K u8 _`%N ? ^ } * 09. 5 ST4(: , , ., )8 5 8 2s XMe, &. G O5 09( HN 3ST48 5 $ 8N 2s XH I-. fB _8 0 8 %9 3ST8 5 '& . #SsMe, f8 9 Cu ./0123( 25 +67 1.0¡10 M~0.10 M ; ¢z8 )N . 8 +~ £ 2qO. ¤ ¥ " c

(6) } X-. fB f 8) ¦5 &'+ 67 @A 25 4 .8 ^§5 ¨.©4. g% X-. ª, @A 6768) #$5 " 2%,MB, 1. 2. 2+. −4. 45.

(7) . 46. N ^ :VM* #$«¬s X N ‘Spectronic 20’( 2%,-. .N x 4 }®5 p&&4( ¯ mnK) °& . )* GU - ±²³ Ó ¯ 0Sµ¶8. ^§5 ¨. X-N ·( ¸5-. ¹ º»¼ &'+ " z~)N x H 4( ½ J? ¾¿(½ J? &'( À , mnK, fl ²³Ó ¯ 0S )%8) #$~Á 5-N HV. '5 ·.-. Â5, Ã +678)N M* i5 Ä(Å ?j) ]Æ( 2%,MB c- +" z~)N - " K~ Á Ç È®& XN ·.-..

(8) . . 678)N ½J? mnK" É2%

(9) #$5 4. ! (combined spectrometer)" #$%,-(Fig. 1). ! N ST238 ~ ÊsN ] K sN ] K" S8 ÓÇ XMe, ) 5 ¾¿ Ë@8) &'( )* +Ç XU -. &'( OYF ¬i%K z~)N '5 Ì? ]4( M* 2~Á 5-. fB S Í ÎÏ ]4? KÐVM* Å? j DÑ ]4(Å ?j8) ÒÓj) Ô¼ j DÑ ]4(Õ{j8) cj)* pÇ X-. ª, Ö DÑ ]4( 0 Ç XN Å?j Ô¼j ]( gN x H 4Æ( Í×VM* 2%

(10) dtHN 48 _` %

(11) }tÀ &'( ´%

(12) Ø = l Ù( ·.-. ) . 678)N Å?j Ô. ¼j ]( µn%N (high luminescence) -.Ú(light emitting diode, LED)4( M* 2%,-. Â5, Ö LED*h| µnsN ]( 5 µÛM* wÜ S8 Ý? HÞ( À ]ß * àËSá}K z~ LED" Ä.â(pyrex) lb (g@: 5.0 mm, ã.: £ 20 cm) 5y ä gh* åæ%

(13) OSç-. Ä.â lb »èh? é§ êjë.ì* í}t LED*h| µn ]. Êî5 lb gh" HBN ]. ïh* nsN ·( µHð S8 lb gñ8) ±% N ] " òÀSç-. Â5, ïh ]. lb gh* Àæ%N ·( µH%K z~ êj ë.ì óÀ lb ïh" -S 5ô m?j ë.ì* í}-. k õh8N Fig. 18) ö XN ·÷ø lb ï@c- -ù ¥ g@( À m? j b( ú%

(14) LED" ú5 lb4 åæ Zn. '% { Æ4t ÜM*û 4( üU ËÇ XU %,-. b gh* åæ lb äh? k8) £ 1 cmO `l " x z%U se, k 098N HÞ. £ 8 mmO Z ]ß. ýÖM* µ-. mnK *N -.Ú(photodiode)" 2%,Me, ( z~)N k y £ 1 cmO `l 8 þ%,-. . ÿ -.ÚN m?j b gh ä h8 úse, f b? Ã p¾8 O-. 2 mnK*N õ8) %, b ïh ä h8 J? -. Ú" ú%

(15) 2%,-. ST23( N 2K*N Î(quartz)k( 2%

(16) k 8 5 " ù %,-. Fig. 18) ö X. , mnK, fl k. z%N h? m? j : gh8 zSá ïh*h| ]8 5 ÎÛ( µH%,-. mnK48) ±%N ÃKVZ ²³(Ã)4? ¸|(multimeter)* Ó%,-.

(17) . CoCl «6H O(extra pure, Junsei Chemical) CuCl «2H O(extra pure, Junsei Chemical)" ¤ .: O#O Ù. 2%

(18) ; 1.00 MZ Co ./ Cu ./ 01234( #¾ 5 , Ö 0 123( V F > 1.00¡10 , 2.00¡10 , 4.00¡ 10 , 6.00¡10 , 8.00¡10 , 1.00¡10 , 2.00¡10 , 4.00¡10 , 6.00¡10 , 8.00¡10 , 1.00¡10 , 2.00 ¡10 , 4.00¡10 , 6.00¡10 , 8.00¡10 , 0.100 M 2. 2. 2+. 2+. −4. −4. 2. 2. −4. −3. Fig. 1. Schematic diagram of the combined spectrometer.. −2. −4. −4. −3. −3. −2. −3. −3. −2. −2. −2. Journal of the Korean Chemical Society.

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(20) . Z 01234( #¾%,-.. 47. ( c9 1.00¡10 M~0.100 M ; ÎÏ8) Co . / 0123 ; À~8 23 09M* h| sN ] K ùð( ö X-. f B Ê (T) :& ; 8 +%

(21) à %H IN ·÷ø ÏS ; 8 O+%

(22) à %H I( X-. 8)N : & ; à 8 ýÍVM* à%N &\*û ‘A=-logT’* O sN (absorbance, A)" 2 5-. ª, ST238 5 :& ; .8N ýÍVZ bD &%N ·.-(Beer ¶). 8)N ST238 µ ]4 a 23( Ê%

(23) HB ]? #ï% 23 0 98) st N ] K" --. 23( Ê%

(24) HBN ]( #ï5 BH ] a hN 23 098 L%N :&8 ~ -. Æ 23 098) ±%N ] ^:. Beer ¶( ¼-9, 23 098) st N ] K ÏS 23 ; O+bD" B ·.-. -Æ, :& ; 8 O +%

(25) !%N N ul 8) N :& ; à 8 O+%e ù %N ^:. b´stÁ %N ·.-. ) @A8 8 :%N "*# &\( O −4. Ô¼j Co ./ 0123( 25 +6 7.

(26) j( N Co ./ 01234 Ô¼ ] ( 2%

(27) dtÀ Table 18 6X-. k8 m? j G" t1 Ó5 KN 4.24 mV.Me, .N k0 9M*h| st BN ] K.-(Ã 8) 5 » J. m? j : gh09.B k( OSN m? j ¤<cell holder> 09 M*h| st N ] KN =SÇ X -). ) Co ./ 01234 [( 2%

(28) d? K*h| . ( t}9 cO dtÀ -. . cON o%U Co ./ 0123 098 ) st N ] K.-.

(29) K) . (reflectance, R)N - J. O Ç X-. z5 K(cO) $%&' ST238 [8 5 K(cO) 8) N 8) Ê (transmittance, T)8 :%N 2t.-. Table 1 2+. 2+. 2+. 2+. 2+. Table 1. The reflectance(R) and the degree of reflection(r) of the Co2+ standard solutions [Co2+], M. Magnitude of the reflected light Magnitude of the reflected (before correction), mV light (after correction), mV. 0(water) 1.00×10−4 2.00×10−4 4.00×10−4 6.00×10−4 8.00×10−4 1.00×10−3 2.00×10−3 4.00×10−3 6.00×10−3 8.00×10−3 1,00×10−2 2,00×10−2 4,00×10−2 6,00×10−2 8,00×10−2 0.100 black ink 2001, Vol. 45, No. 1. 35.53 35.48 35.40 35.38 35.25 35.16 35.04 34.64 33.86 32.95 32.20 31.54 28.40 23.26 19.60 16.68 14.52 4.24. 31.29 31.24 31.16 31.14 31.01 30.92 30.80 30.40 29.62 28.71 27.96 27.30 24.16 19.02 15.36 12.44 10.28. Reflectance (R). Degree of reflectance (r=1+logR). 1.0000 0.9984 0.9958 0.9952 0.9911 0.9882 0.9843 0.9716 0.9466 0.9175 0.8936 0.8725 0.7721 0.6079 0.4909 0.3976 0.3285. 1 0.9993 0.9982 0.9979 0.9961 0.9948 0.9931 0.9875 0.9762 0.9626 0.9511 0.9408 0.8877 0.7838 0.6910 0.5994 0.5166.

(30) . 48. ~Á Ç È® X , . 8)N - J. O Ç XN "*# 2t" æ% 5-. (degree of reflection) = r = 1 + logR Fig. 28) B( ‘ vs. [Co ]’ plot( c9, Co ./ 0123 ; !ð8 N ` ýÍ* ù%U )( ö X-. -Æ Co ./ 0123 ; ýÍ8) £ *tBN ^:? 23 a8) Co ./. Co ./M* + W X-N 68 KZ%N ·M* ,OÇ X-. Table 2N " 2%

(31) d? " c

(32) } X-. 8) -.H* k8 G" Ó5 Ê KN 0 mV.-.

(33) K) Ê (T) (A)N - J. O 5-. 5 Ê K Ê (T)' ST238 [8 5 Ê K (A)=−log T Table 2( c9, " 2/( ÿ N ul Co ./ 0123 ; 1.00¡10 M. W ÿ0H 23 ; !8 sN ] 8 =1 à Ù( ö X-. .N 2+. 2+. 2+. 2+. 3+. −3. 2+. Table 2. The transmittance and absorbance of the Co2+ stan-. dard solutions [Co2+], M 0(water) 1.00×10−4 2.00×10−4 4.00×10−4 6.00×10−4 8.00×10−4 1.00×10−3 2.00×10−3 4.00×10−3 6.00×10−3 8.00×10−3 1,00×10−2 2,00×10−2 4,00×10−2 6,00×10−2 8,00×10−2 0.100. The intensity of the Transmittance Absorbance tranmitted light, V (T) (A) 0.4253 0.4253 0.4253 0.4253 0.4253 0.4253 0.4253 0.4251 0.4247 0.4241 0.4236 0.4229 0.4198 0.4132 0.4059 0.3968 0.3875. 1.0000 1.0000 1.0000 1.0000 1.0000 1.0000 1.0000 0.9995 0.9986 0.9972 0.9960 0.9944 0.9871 0.9715 0.9544 0.9330 0.9111. 0 0 0 0 0 0 0 2.172×10−4 6.084×10−4 1.218×10−3 1.741×10−3 2.439×10−3 5.639×10−3 0.01256 0.02027 0.03012 0.04043. 8) :& ; } >? @A ± Ç XN VZ ^:.-. 8)N A Í ST238 5 ] Ê " Ó5 f8 _`%

(34) " p5-. ª, õ8) .¸ O 5 » J. ST23( Ê%N ] K(‘x’ %) " o5 [( Ê%N ] K(Table 18) c9 425.3 mV)* B2t Ê " p5-9, mnK8. u%N ] K 425.3 mVZ :38) f c$? (x). BgN +4(x/425.3)( p%U -. f15 ; } >`B :& CD } $? @A8N ST23 ¸5 ; à 8 ±%N Ê Kà (∆x) ÏS ¸% U -. ¹ Ê%N ] Kà " :VM* 0^5-9 ‘∆x/425.3’* B XMe, f ? VZ &' mnK*)N HÇ ÙN O. * $À-. @A [8 ~ sN ] K" K1M* Ö 238 5 " p% e, [8 ~ sN ] KN 8) [( Ê%

(35) mnK8 u%N ] K8 +~ :VM* } $? .-. ª, 8 + ~ :VM* } $? ] K" K1(Table 1( c9 31.29 mV’)M* %

(36) Ö 238 ~ st N ] K(y)" :VM* 0^(y/31.29)%N @A8N ST23 ¸5 ; à 8 ~ ±%N K $? à (∆y/31.29). HÇ XU -. ) @A 8 +~ (sensitivity) 6 ST23 ; <= >`B :& CD < = $ KL 8 ~ OP. t# 8 &7VM* 2W XN ·.-. [8 ST23 ; EF À~H`B :[\ CD +V ¥ @A8N . 5 ©? HU -. Ã 8) #S " c9 ST23 ; !ð8 . N H9VM* !%N 9, à N ¤ . : à%H IU sN H©8 u%N ^:. b´s -. ST23 ; !%9) ù%N ^:? üU ´Ç X-. õ8) 5 » J. 8) " p%K z~ 2%N KÐ ? 31.29 mV. 8) Ê " p%K z~ 2%N KÐ? 425.3 mV.-. x @A wx ST23 ; !8 Journal of the Korean Chemical Society.

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(38) . 238 ~ ±%N ²³(x ÂN y)4. KÐ 4 * _(: x:31.29, : y:. 49. 425.3)U se, @A 8 +~ ¤ ; U < :8 u%N ·.-. Fig. 2 8N (‘ vs. [Co ]’) ¤ t (‘A vs. [Co ]’) 0^st XMe, Co ./ 0123 ; à 8 ¼ . à =. à =8 +~ >? ¤ @( ö X-. Cu . Ô¼j( N Cu ./ 01234 Å?j ( 25 @A8 dtÀ Table 38 6X-. k8 m? j G" t1 Ó5 KN 9.0 mV.-. Cu ./ 0 1234 Å?j ( 25 ÏS 1.00¡10 M~0.100 M ; ÎÏ8) Cu ./ 0123 ; À~8 23 09M *h| sN ] K ùð( c

(39) }e, Fig. 3( c9 Cu ./ 0123 ; 8 ýÍVM* ùð( c

(40) 1-(õ Co ./ 23 N ul Cu ./? + sH I f* L% A* ýÍ( B(-). Table 4N " c

(41) }e, . @A8 k8 G" Ó5 Ê KN 0 mV.-. Co ./ 0123( 25 67 -.H* Cu ./ 0123 2+. 2+. 2+. 2+. 2+. 2+. −4. 2+. 2+. 2+. 2+. 2+. Fig. 2. Plots of absorbance(A) or degree of reflection(r) vs. [Cu2+].. 2+. Table 3. The reflectance(R) and the degree of reflection(r) of the Cu2+ standard solutions [Co2+], M. The intensity of the reflected light The intensity of the reflected light (before correction), mV (after correction), mV. 0(water) 1.00×10-4 2.00×10-4 4.00×10-4 6.00×10-4 8.00×10-4 1.00×10-3 2.00×10-3 4.00×10-3 6.00×10-3 8.00×10-3 1,00×10-2 2,00×10-2 4,00×10-2 6,00×10-2 8,00×10-2 0.100 black ink 2001, Vol. 45, No. 1. 169.45 169.26 169.00 168.37 167.48 166.75 165.99 163.66 158.12 152.97 148.24 143.30 122.32 089.12 065.82 049.12 037.72 009.00. 160.45 160.26 160.00 159.37 158.48 157.75 156.99 154.66 149.12 143.97 139.24 134.30 113.32 080.12 056.82 040.12 028.72. Reflectance (R). Degree of reflection (r=1+logR). 1.0000 0.9988 0.9972 0.9933 0.9877 0.9832 0.9784 0.9639 0.9294 0.8973 0.8678 0.8370 0.7063 0.4993 0.3541 0.2500 0.1790. 1.0000 0.9995 0.9988 0.9971 0.9946 0.9926 0.9905 0.9840 0.9682 0.9529 0.9384 0.9227 0.8490 0.6984 0.5492 0.3980 0.2528.

(42) . 50. Table 4. The transmittance and the absorbance of the Cu2+ standard solutions [Co2+], M. Fig. 3. Plots of absorbance(A) or degree of reflection(r) vs. [Co2+].. ; 1.00¡10 M8 ." ÿ0HN 23 ; ! 8 sN ] 8 ` à Ù( X-. Fig. 3? ‘ vs. [Cu ]’ plot ð B ‘ vs. [Cu ]’ plot( c

(43) } XMe, Co ./ 0123 @A +C%U Cu ./ ;. à 8 ¼ à =. à = 8 +~ >? ¤ @( ö X-. −3. 2+. 2+. 2+. 2+. . p8) #$5 !" 2%

(44) ¦5 &'+ N - J-. AÍ, ? 3 : ST8 5 8 2W X( S 5ô XMe, @A 8) 2sN 8 :%N 2t*û " "DU O %

(45) 2%,-. ª, 8)N 23 ; !8 +%

(46) ýÍV M* ù5-. EF*N, Å?j Ô¼j( BgN 4( 25 .ô 678) ¸ XN 4( d-N 68 _`%

(47) . SÍ Î Ï wR ]48 V2W X. G H-. IF,. The magnitude of Transmittance Absorbance the transmitted (T) (A) light, volt. 0(water) 1.00×10−4 2.00×10−4 4.00×10−4 6.00×10−4 8.00×10−4 1.00×10−3 2.00×10−3 4.00×10−3 6.00×10−3 8.00×10−3 1,00×10−2 2,00×10−2 4,00×10−2 6,00×10−2 8,00×10−2 0.100 black ink. 0.4715 0.4714 0.4714 0.4713 0.4713 0.4713 0.4713 0.4712 0.4709 0.4706 0.4702 0.4699 0.4676 0.4625 0.4574 0.4518 0.4462 0. 1.0000 0.9998 0.9998 0.9996 0.9996 0.9996 0.9996 0.9994 0.9987 0.9981 0.9972 0.9966 0.9917 0.9809 0.9701 0.9582 0.9463. 0 8.687×10−5 8.687×10−5 1.738×10−4 1.738×10−4 1.738×10−4 1.738×10−4 2.607×10−4 5.650×10−4 8.259×10−4 1.218×10−3 1.479×10−3 3.620×10−3 8.375×10−3 0.0131800 0.0185400 0.0239700. N ST23 ; <= J`B :& CD } $ KL *N OP. QR ST238 5 8 2.%U V2W X-N 6( YZ%,-. fB ST23 ; EF À~H`B :V M* ¥ CD" HN :& @A8 N 8 + ~ ¤ J\ X-. fB 3ST8 5 8 b5 c- - 5 p ®p-. 3 8 5 @A 3 098 L%N K? L8) " MN ·M* M X-. ) @A N ul } V? STÆ( È®* %U -N ©( HU sN ·.-. ^: .5 ©8 _`%

(48) ¨ p#N 8 2%N ST 23 ù " z5 µ ( -N 5-.. 1. 1. Surles, T; Erickson, J. O.; Priesner, D. Amer. Lab. 1975, 7, 55. , ; J. Korean Chem. Soc. 2000, 44(4), 316. 2.. . Journal of the Korean Chemical Society.

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Comparison of the Reflectance and the Absorption Spectrometries Using the Combined Spectrometer 

Comparison of the Reflectance and the Absorption Spectrometries Using the Combined Spectrometer