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Á¦¸ñ ICP-OES¸¦ ÀÌ¿ëÇÑ Coal Fly AshÀÇ Dual-View ºÐ¼®
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Teledyne Leeman Labs»ç ICP-OES Prodigy Plus¸¦ ÀÌ¿ëÇÏ¿©

Coal Fly AshÀÇ Dual-View ºÐ¼®

 

 

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Introduction

 

ºñ»êÀç(Coal Fly Ash)´Â ¹Ì¼¼ÇÏ°Ô ºÐ¼âµÈ ¼®ÅºÀ» Å¿ì´Â °úÁ¤¿¡¼­ ¹ß»ýÇÏ´Â ºÎ»ê¹°·Î, ÁÖ¿ä ±¸¼º¹°ÁúÀÌ ½Ç¸®Ä«ÀÎ ¹Ì¼¼ ºÐ¸»Çü ¹°ÁúÀÔ´Ï´Ù. ÁÖ·Î ¼®Åº È­·Â ¹ßÀü¼Ò¿¡¼­ »ý»êµÇ¸ç ¼®Åº ¿¬¼Ò ÀÜ¿©¹° (CCR)·Î ¾Ë·ÁÁø ¼®Åº ¿¬¼Ò ºÎ»ê¹° Áß ÇϳªÀÔ´Ï´Ù. ´Ù¸¥ CCR ¹°Áú¿¡´Â ¹Ù´ÚÀç (Bottom Ash), º¸ÀÏ·¯ ½½·¡±× ¹× ¿¬µµ°¡½º (Flug Gas) ŻȲ ¹°ÁúÀÌ Æ÷ÇԵ˴ϴÙ.

 

2014³â¿¡´Â ¾à 1¾ï 3õ¸¸ÅæÀÇ ¼®ÅºÀÌ ¹Ì±¹¿¡¼­ »ý»êµÇ¾î °¡Àå Å« »ê¾÷ Æó±â¹° À¯Çü Áß Çϳª°¡ µÇ¾ú½À´Ï´Ù. ÀÌ Æó±â¹°ÀÇ ´ëºÎºÐÀº ÀÚ¿ø Àý¾à DÁ¶ÀÇ ¿ä±¸»çÇ׿¡ µû¶ó ¸Å¸³Áö¿¡ ÀúÀåµË´Ï´Ù. ºñ»êÀç´Â ÄÜÅ©¸®Æ®, À¯µ¿¼º ÃæÀüÀç, Ŭ¸µÄ¿(Clinker), °ñÀç ´ëü Àç·á, Åä¾ç °³Á¶/¾ÈÁ¤È­ µîÀÇ ´Ù¾çÇÑ Á¦Ç°°ú Àç·á¿¡µµ »ç¿ëµÉ ¼ö ÀÖ½À´Ï´Ù. ºñ»êÀçÀÇ ÀÌ·¯ÇÑ ¿ëµµ´Â ȯ°æ°ú ¿ì¸®¿¡°Ô ¸Å¿ì ±àÁ¤ÀûÀÎ ¿µÇâÀ» ¹ÌĨ´Ï´Ù.

 

ºñ»êÀçÀÇ ±¸¼ºÀº ¿¬¼Ò¿¡ »ç¿ëµÈ ¼®ÅºÀÇ Æ¯¼º°ú Á÷Á¢ÀûÀ¸·Î °ü·ÃÀֱ⠶§¹®¿¡ Æó±â ¹× Àç»ç¿ë ¸ðµÎ¿¡¼­ ¹Ì·® ¿ø¼Ò³ª ÁÖ¿ä ¿ø¼Ò°¡ ħÃâµÇ¾î È¯°æ À§ÇèÀ» ÃÊ·¡ÇÒ ¼ö ÀÖ½À´Ï´Ù. µû¶ó¼­ ºñ»êÀç´Â ¿ø¼Ò Á¶Á¤À» È®ÀÎÇØ¾ßÇϸç À̸¦ À§ÇØ ±Ý¼Ó °áÁ¤ÀÇ Å×½ºÆ®°¡ ÁøÇàµË´Ï´Ù.

 

 

 

Instrumentation

 

Dual-view ÅäÄ¡¿Í Teledyne CETAC ASX-280 ¿ÀÅä»ùÇ÷¯(120 position, Ohama, NE)°¡ ÀåÂøµÈ Prodigy Plus Inductively Coupled Plasma (ICP) ºÐ±¤°è¸¦ »ç¿ëÇÏ¿© ÀÌ ÀÀ¿ë³ëÆ®ÀÇ µ¥ÀÌÅ͸¦ ºÐ¼®Çß½À´Ï´Ù.

2.PNG

                        ÁÂ) ICP-OES Prodigy Plus    ¿ì) Teledyne CETAC ASX-280 Autosampler

 

 

Prodigy Plus´Â Mega pixelÀÇ ´ëÇü Æ÷¸Ë CMOS (L-CMOS) °ËÃâ±â¿Í 800mm ÃÊÁ¡ °Å¸® Echelle ±¤ÇÐ ½Ã½ºÅÛÀ» °áÇÕ½ÃŲ Ź»óÇü µ¿½Ã ICP-OESÀÔ´Ï´Ù. L-CMOSÀÇ È°¼º ¿µ¿ªÀº 28x28mm·Î ÇöÀç ICP-OES¿¡¼­ »ç¿ëµÇ°í ÀÖ´Â ´Ù¸¥ °íü °ËÃâ±âº¸´Ù ÈξÀ Å®´Ï´Ù. ÀÌ Á¶ÇÕÀ» ÅëÇØ Prodigy Plus´Â ´Ù¸¥ °íü °ËÃâ±â ±â¹Ý ICP ½Ã½ºÅÛº¸´Ù ³ôÀº ±¤ÇÐ ÇØ»óµµ¸¦ ¾òÀ» ¼ö ÀÖ½À´Ï´Ù. °ËÃâ±â´Â 165nm¿¡¼­ 1100nm »çÀÌÀÇ ¿¬¼ÓÀûÀÎ ÆÄÀå ¹üÀ§¸¦ Á¦°øÇÏ¿© ÆÄÀå ¹üÀ§³ª ºÐÇØ´ÉÀÇ ÀúÇϾøÀÌ ÇÑ ¹ø¿¡ Àüü ICP ½ºÆåÆ®·³À» ÃøÁ¤ÇÒ ¼ö ÀÖ½À´Ï´Ù. ¿°¼Ò ¶Ç´Â ºê·Ò ÃøÁ¤ÀÌ ÇÊ¿äÇÑ ÀÀ¿ë ºÐ¾ßÀÇ °æ¿ì, ¼±ÅÃÀû ÇÒ·Î°Õ °ËÃ⠽ýºÅÛÀ» »ç¿ëÇÒ ¼ö ÀÖ¾î ÆÄÀå ¹üÀ§¸¦ 135-1100nm±îÁö È®ÀåÇÒ ¼ö ÀÖ½À´Ï´Ù. ¶ÇÇÑ Ä«¸Þ¶óÀÇ °í¼Ó ÆÇµ¶Àº »ç½Ç»ó °ËÃâ±â ºÎ°¡½Ã°£ (Overhead time)À» Á¦°ÅÇϸç, ÆÇµ¶ ½Ã°£Àº ¾à 1ÃÊÀ̹ǷΠRandom access, ºñÆÄ±« ÆÇµ¶ÀÌ °¡´ÉÇÑ 6ÀÚ¸® ÀÌ»óÀÇ ´ÙÀ̳ª¹Í ·¹ÀÎÁö¸¦ Á¦°øÇÕ´Ï´Ù. Prodigy Plus´Â 40.68MHzÀÇ °­·ÂÇÑ Free-running RF ¹ß»ý±â¸¦ »ç¿ëÇÏ¿© ÀϹÝÀûÀÎ À¯±â ¿ëÁ¦ »Ó ¾Æ´Ï¶ó °¡Àå ¾î·Á¿î ½Ã·á ¸ÅÆ®¸¯½ºµµ ó¸®ÇÒ ¼ö ÀÖ½À´Ï´Ù.

 

 

 

 

Sample Introduction

 

ÀÌ ÀÀ¿ëÀÚ·á¿¡´Â Ryton¢ç Spray Chamber¿Í Hildebrand Grid ³×ºæ¶óÀÌÀú·Î ±¸¼ºµÈ HF¿¡ ³»¼ºÀ» Áö´Ñ ½Ã·á ÁÖÀÔ ½Ã½ºÅÛÀÌ »ç¿ëµÇ¾ú½À´Ï´Ù. (±×¸² 4) Ç¥ÁØ ¼®¿µ ½Ã·á ÁÖÀÔ±â´Â HF ³»¼º ¾Ë·ç¹Ì³ª·Î ±³Ã¼µÇ¾ú½À´Ï´Ù. Hildebrand Grid´Â ¿¹¿ÜÀûÀÎ ´Ù¿ëµµÀÇ ºÐ¹«±â·Î¼­ HF »Ó¸¸ ¾Æ´Ï¶ó ¼ö¼º, À¯±â¹°, °í¿ëÁ¸ °íÇü¹° µî °ÅÀÇ ¸ðµç ¸ÅÆ®¸¯½º¿¡¼­ÀÇ ½Ã·á¿¡ »ç¿ëÇÒ ¼ö ÀÖ½À´Ï´Ù. ÀÌ Á¦Ç°ÀÇ ¼³°è´Â ¿ì¼öÇÑ °ËÃâ ÇѰè¿Í ¿ëÇØµÈ °íÇü¹°¿¡ ÀÇÇÑ ¸·Èû¿¡ ´ëÇØ ³ôÀº È¿À²À» Á¦°øÇÕ´Ï´Ù. Prodigy Plus ÅäÄ¡´Â ½Ã·á À¯ÇüÀÌ ´õ ³ôÀº À¯·®À» ÇÊ¿ä·Î ÇÒ °æ¿ì, ÃÖ´ë 20L/min¿¡¼­ ÀÛµ¿ÇÒ ¼ö ÀÖ´Â ÂøÅ»½Ä, ÀúÀ¯·® ¼³°èÀÔ´Ï´Ù. (±×¸² 4)

ÅäÄ¡ ¼ö¸íÀ» Çâ»ó½ÃŰÀÌ À§ÇØ Prodigy Plus´Â Radial, Axial and Dual view¿Í °°Àº ¸ðµç ±â±¸ ±¸¼º¿¡ ªÀº ¹æ»çÇü ÅäÄ¡¸¦ »ç¿ëÇÕ´Ï´Ù. Viewing ports, slots ¹× È®ÀåµÈ ÅäÄ¡ ±æÀÌ´Â »ç¿ëµÇÁö ¾Ê½À´Ï´Ù.

 


2018-10-19 15;30;48.PNG

                ±×¸² 4. Ryton¢ç Spray Chamber, Hildebrand Grid Nebulizer ¹× Prodigy Plus Torch



Operating Parameters

ÀÌ ¿¬±¸¿¡ »ç¿ëµÈ Prodigy Plus ÀÛµ¿ ÆÄ¶ó¹ÌÅÍ Ç¥ 1¿¡ »ç¿ëµÈ ÆÄÀå ¹× ÇöóÁ view ±¸¼ºÀº Ç¥ 2¿¡ ³ªÅ¸³»¾ú½À´Ï´Ù.

Ç¥1. Instrument Operating Parameters 

Parameter

Setting

RF Power

1.2 kW

Coolant Flow

14 L/min

Auxiliary Flow

0

Torch

Quartz Demountable

Injector

Alumina

Nebulizer Pressure

42 psi

Nebulizer

Hildebrand Grid

Spray Chamber

RytonTM

Sample Uptake Rate

35 rpm

Axial Integration Time

15 s

Radial Integration time

5 s

 

 Ç¥2. Analytical Wavelenghths

Element

Wavelength, nm

View

 

Element

Wavelength, nm

View

Al

308.215

Radial

 

Mn

257.610

Axial

396.152

Radial

 

259.372

Axial

As

189.042

Axial

 

Na

588.995

Radial

193.759

Axial

 

589.592

Radial

Ba

233.527

Radial

 

Ni

231.604

Axial

493.409

Radial

 

232.003

Axial

Ca

315.887

Radial

 

Pb

217.000

Axial

317.933

Radial

 

220.353

Axial

Cr

267.716

Axial

 

Si

251.611

Radial

283.563

Axial

 

288.158

Radial

Cu

324.754

Axial

 

Sr

407.771

Radial

327.396

Axial

 

421.552

Radial

Fe

238.204

Radial

 

Ti

334.941

Radial

259.940

Radial

 

336.122

Radial

K

766.491

Radial

 

V

292.401

Axial

769.897

Radial

 

310.230

Axial

Mg

279.078

Radial

 

Zn

202.548

Axial

285.213

Radial

 

206.200

Axial


 

 

 

 

Sample Preparation

 

NIST SRM 1633C Coal Fly Ash´Â ´ÙÀ½ ÀýÂ÷´ë·Î ÁغñµÇ¾ú½À´Ï´Ù.

 

1. 0.2000gÀÇ ½Ã·á¸¦ Ī·®Çϰí Teflon¢â ºñÀÌÄ¿¿¡ ÷°¡ÇÕ´Ï´Ù.

2. ½Ã·á¸¦ ¿ÏÀüÈ÷ µ¤À»¸¸Å­ dzºÐÇÑ Ãʼø¼ö(DI)¸¦ ÷°¡ÇÕ´Ï´Ù.

3. 5mLÀÇ ¿Õ¼ö (Áú»ê : ¿°»ê = 1 : 3 ºñÀ²)¿Í 2mLÀÇ ºÒ»ê(HF)À» ÷°¡ÇÕ´Ï´Ù.

4. ºñÀÌÄ¿¸¦ Teflon¢â Ä¿¹ö·Î µ¤°í 95~100¡É¿¡¼­ 2½Ã°£µ¿¾È °¡¿­ÇÕ´Ï´Ù. ½Ã·á°¡ »êºÐÇØµÇ¾úÀ¸¸é °¡¿­¿ø¿¡¼­ ºñÀÌÄ¿¸¦ Á¦°ÅÇÏ°í ½Ç¿ÂÀ¸·Î ³Ã°¢ÇÕ´Ï´Ù.

5. Whatman¢ç42 ¿©°úÁö¸¦ »ç¿ëÇÏ¿© ÇÃ¶ó½ºÆ½ 100mL ºÎÇÇ Çöó½ºÅ©¿¡ °É·¯³»°í Ãʼø¼ö¸¦ ÀÌ¿ëÇÏ¿© 100gÀ¸·Î Èñ¼®ÇÕ´Ï´Ù.

 

 

 

Calibration Stansdards

 

±³Á¤ Ç¥Áع°Àº VHG Labs (Manchester, NH)ÀÇ ´ÜÀÏ ¿ø¼Ò Ç¥Áع°À» »ç¿ëÇÏ¿© ÁغñµÇ¾ú½À´Ï´Ù. Ç¥ÁØ ¹°ÁúÀº 5mLÀÇ ¿Õ¼ö¿Í 2mLÀÇ HF¸¦ ÷°¡ÇÑ ´ÙÀ½, Ãʼø¼ö¸¦ ÀÌ¿ëÇØ 100gÀ¸·Î Èñ¼®ÇÏ¿© ½Ã·á¿Í µ¿ÀÏÇÑ ¸ÅÆ®¸¯½º·Î ¸ÂÃè½À´Ï´Ù. ±³Á¤ Ç¥Áع° ³óµµ´Â Ç¥ 3¿¡ ³ªÅ¸³»¾ú½À´Ï´Ù.

 

Ç¥3. Calibration Standard Concentrations, mg/kg

Element

Std0

Std1

Std2

Std3

Al

0

200

400

800

As, Cr, Cu, Mn, Ni, Zn

0

0.20

0.50

1.00

Ba, Sr

0

1.00

2.00

5.00

Ca, K

0

20.0

50.0

100

Fe

0

100

200

400

Mg

0

5.00

10.0

20

Na

0

2.00

5.00

10.0

Pb

0

0.10

0.20

0.50

Si

0

250

500

1000

Ti

0

10.0

20.0

50.0

V

0

0.50

1.00

2.00


 

 

 

 

 

Results and Discussion

 

NIST SRM 1633C Coal Fly Ash ½Ã·á´Â Ç¥ 2¿¡ ³ª¿­µÈ ºÐ¼® ÆÄÀå ¹× ÇöóÁ view ±¸¼º¿¡¼­ Ç¥ 1¿¡ Ç¥½ÃµÈ ÀÛµ¿ ÆÄ¶ó¹ÌÅ͸¦ »ç¿ëÇÏ¿© ºÐ¼®µÇ¾ú½À´Ï´Ù. ºÐ¼® °á°ú´Â Ç¥ 4¿¡ ³ªÅ¸³ÂÀ¸¸ç ÃøÁ¤µÈ °ªÀº ÀÎÁõµÈ NIST °ª°ú °ÅÀÇ ÀÏÄ¡ÇÕ´Ï´Ù. ¶ÇÇÑ 2°³ÀÇ ¼­·Î ´Ù¸¥ ÆÄÀå¿¡¼­ ÃøÁ¤µÈ ¿ø¼Ò´Â °á°ú°£¿¡ ¿ì¼öÇÑ ÀÏÄ¡¸¦ ³ªÅ¸³»¾î ½ºÆåÆ®·³ °£¼·ÀÌ ¾øÀ½À» ³ªÅ¸³À´Ï´Ù. (Both inter-element or intra-order)

 

Ç¥4. NIST SRM 1633 Results

Element

Concentration

SD

RSD

Units

Certified Value

% Recovery

Al 308.215 r

13.08

0.039

0.30

%

13.28

98.5

Al 396.152 r

12.98

0.061

0.47

97.8

As 189.042

186.2

3.347

1.80

mg/kg

186.2

100.0

As 193.759

178.7

1.86

1.04

96.0

Ba 233.527 r

0.111

0

0.20

%

0.1126

98.6

Ba 493.409 r

0.11

0.001

0.59

97.7

Ca 315.887 r

1.348

0.004

0.33

%

1.365

98.8

Ca 317.933 r

1.339

0.005

0.38

98.1

Cr 267.716

272.9

1.326

0.49

mg/kg

258

105.8

Cr 283.563

270.9

0.785

0.29

105.0

Cu 324.754

172.1

0.498

0.29

mg/kg

173.7

99.1

Cu 327.396

169.5

0.786

0.46

97.6

Fe 238.204 r

10.30

0.068

0.66

%

10.49

98.2

Fe 259.940 r

10.28

0.068

0.66

98.0

K 766.491 r

1.754

0.006

0.36

%

1.773

98.9

K 769.897 r

1.733

0.008

0.47

97.7

Mg 279.078 r

0.492

0.002

0.39

%

0.498

98.8

Mg 285.213 r

0.491

0.002

0.33

98.6

Mn 257.610

239.5

0.548

0.23

mg/kg

240.2

99.7

Mn 259.372

239.0

0.605

0.25

99.5

Na 589.592 r

0.163

0.001

0.89

%

0.1707

95.5

Na 588.995 r

0.167

0

0.06

97.8

Ni 231.604

133.0

0.254

0.19

mg/kg

132

100.8

Ni 232.003

130.8

2.129

1.63

99.1

Pb 220.353

94.40

0.803

0.85

mg/kg

95.2

99.2

Pb 217.000

94.29

3.824

4.06

99.0

Si 251.611 r

20.84

0.19

0.91

%

21.3

97.9

Si 288.158 r

20.95

0.133

0.63

98.4

Sr 407.771 r

892.4

2.641

0.30

mg/kg

901

99.0

Sr 421.552 r

889.8

6.791

0.76

98.8

Ti 334.941 r

0.709

0.003

0.45

%

0.724

97.

 

9

Ti 336.122 r

0.703

0.006

0.89

97.1

V 292.401

283.3

0.549

0.19

mg/kg

286.2

99.0

V 310.230

280.6

1.044

0.37

98.1

Zn 202.548

236.1

0.964

0.41

mg/kg

235

100.5

Zn 206.200

235.5

0.727

0.31

100.2

Sr 407.771 r

892.4

2.641

0.30

mg/kg

901

99.0

Sr 421.552 r

889.8

6.791

0.76

98.8

Ti 334.941 r

0.709

0.003

0.45

%

0.724

97.9 

Ti 336.122 r

0.703

0.006

0.89

97.1

V 292.401

283.3

0.549

0.19

mg/kg

286.2

99.0

V 310.230

280.6

1.044

0.37

98.1

Zn 202.548

236.1

0.964

0.41

mg/kg

235

100.5

Zn 206.200

235.5

0.727

0.31

100.2


HF ³»¼º ½Ã·á µµÀÔ ½Ã½ºÅÛÀº ¶Ù¾î³­ °¨µµ¿Í Á¤¹Ðµµ¸¦ Á¦°øÇϺó´Ù. Hildebrand grid ³×ºæ¶óÀÌÀú´Â ´Ù¸¥ ¸¹Àº HF ³»¼º ³×ºæ¶óÀÌÀúº¸´Ù ´õ È¿À²ÀûÀÌ¸ç °ß°íÇÕ´Ï´Ù. Hildebrand grid´Â HF ³»¼º »Ó¸¸ ¾Æ´Ï¶ó ¸·Èû Çö»óÀ̳ª ¾Æ¸£°ï °¡½À±â ¾øÀ̵µ ³ôÀº ¼öÁØÀÇ ¿ëÇØ °íÇü¹° (>10%)À» ó¸®ÇÒ ¼ö ÀÖ½À´Ï´Ù.

 

CMOS °ËÃâ±â´Â ´ÜÀÏ ÆÇµ¶°ª ¹× °¢ ÇöóÁ view ±¸¼º¿¡ ´ëÇØ ¸ðµç ½Ã·áÀÇ ¿ø¼Ò ¹æ»ç ·¹º§À» Æ÷ÂøÇÒ ¼ö ÀÖ¾î ºÐ¼® ½Ã°£À» ´ëÆø ´ÜÃàÇÒ ¼ö ÀÖ¾ú½À´Ï´Ù. ¿ø¼Ò °£ÀÇ °­µµ Â÷ÀÌ¿¡ °ü°è¾ø°í ÇÊ¿äÇÑ °­µµ·Î ÆÄÀåÀ» ºÐ·ùÇϱâ À§ÇÑ »çÀü °Ë»ç¾øÀÌ ÇÑ ¹ø¿¡ ¿©·¯ ÆÄÀåÀ» ÀûºÐÇÒ ¼ö ÀÖ½À´Ï´Ù. °ËÃâ±âÀÇ ³ôÀº ÆÇµ¶ ¼Óµµ´Â 1ÃÊ À̳»¿¡ 150°³ ÀÌ»óÀÇ ÆÄÀåÀ» ¼öÁýÇß½À´Ï´Ù. Prodigy Plus´Â ³·Àº À¯·®ÀÇ ÅäÄ¡¿Í °áÇÕµÈ ÁøÁ¤ÇÑ Àúºñ¿ë ºÐ¼®À» Á¦°øÇÏ¿© ½Ã·á 󸮷®À» ³ôÀ̱â À§ÇØ Àüü ºÐ¼®½Ã°£À» ÁÙ¿©¼­ ¾Æ¸£°ï ¼Òºñ¸¦ ÁÙÀÔ´Ï´Ù. ÀÌ·¯ÇÑ ¸ðµç ¼Ó¼ºµéÀÌ °áÇÕµð¾î Prodigy Plus´Â ³ÐÀº ¹üÀ§ÀÇ ºÐ¼® ³óµµ¸¦ °¡Áø ½Ã·á¸¦ ºÐ¼®ÇÏ´Â ½ÇÇè½Ç¿¡ ÀÌ»óÀûÀÎ ½Ã½ºÅÛÀÔ´Ï´Ù.

 

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