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Introduction    
°íÇ°Áú ÆäÀÎÆ® Á¦Ç°ÀÌ µÇ±â À§Çؼ­´Â Á¦Ç°¿¡ ´ÙÀ½°ú °°Àº Çö»óÀÌ ÀϾÁö ¾Ê°Å³ª ÃÖ¼ÒÈ­ µÇ¾î¾ß ÇÑ´Ù.

- Syneresis : liquid dispersion media ÀÇ separation
- Pigment segregation : container ³»¿¡ »ö¼Ò¼ººÐÀÇ º¯È­
- Particle segregation : container ³»¿¡ ÀÔµµ ºÐÆ÷ÀÇ º¯È­

ÀÌ·± Çö»óÀÌ ÀϾÁö ¾Ê°Ô ÇϱâÀ§Çؼ­´Â »õ·Î¿î ÆäÀÎÆ®Á¦Ç° °³¹ß´Ü°è »Ó¸¸ ¾Æ´Ï¶ó Á¦Ç° »ý»ê°úÁ¤¿¡¼­ÀÇ Ç°Áú°ü¸® ´Ü°è¿¡¼­µµ ¸¹Àº °ü½ÉÀÌ ÁÖ¾îÁ®¾ß ÇÑ´Ù. STEP Technology ¸¦ ±â¹ÝÀ¸·Î ÇÏ´Â ºÐ»ê¾ÈÁ¤¼º ºÐ¼®±â¹ýÀ» ÀÌ¿ëÇϸé ÆäÀÎÆ®Á¦Ç°ÀÇ separation stability ¸¦ ½Å¼ÓÇÏ°Ô ÃøÁ¤ÇÒ ¼ö ÀÖÀ¸¸ç ¶ÇÇÑ ÆäÀÎÆ®³»ÀÇ ÀÔµµºÐÆ÷±îÁö Á¤¹ÐÇÏ°Ô ºÐ¼®À» ÇÒ ¼ö ÀÖ´Ù.

 
How does multi-sample analytical centrifugation work?    
 
STEP Technology ´Â ¿ø½É·ÂÇÏ¿¡¼­ tube ³» sample ÀÇ time °ú position ¿¡ µû¸¥ transmission º¯È­¸¦ µ¿½Ã¿¡ ÃøÁ¤ÇÏ¿© sample ÀÇ dispersion stability ¸¦ ºÐ¼®ÇÏ´Â ±â¹ýÀ¸·Î¼­ LUMiFuge ¿Í LUMiSizer Àåºñ¸¦ ÀÌ¿ëÇÑ´Ù. ÃøÁ¤µÈ sample ÀÇ sedimentation profile À» Integral Transmission (clarification speed) ¿Í Front Tracking (separation velocity) ºÐ¼® mode ¸¦ ÀÌ¿ëÇÏ¿© sample ÀÇ separation Ư¼ºÀ» ºñ±³ ºÐ¼®ÇÑ´Ù.
 
Samples vulnerable to syneresis and pigment segregation    
 
Fig.1. Evolution of transmission profiles with time- first recorded profile after 30 seconds lowest (red), last profile after 2 hours uppermost (green), centrifugation of a colorant formulation (exhibiting zone sedimentation and pigment segregation) at 2300x g, 20¡É, above the sample after centrifugation

À§ transmission profiles ÀÇ time line ¿¡¼­ º¼ ¼ö ÀÖµíÀÌ, sample ³» ÀÔÀÚµéÀÇ separation ÀÌ tube bottom À¸·Î sharp ÇÏ°Ô À̵¿ÇÏ°í ÀÖ´Â °ÍÀ» ¾Ë ¼ö ÀÖ´Ù. ÀÌ·± ÇüÅÂÀÇ transmission profile Àº ¸ðµç ÀÔÀÚµéÀÌ ÇÔ²² °°ÀÌ À̵¿ÇÏ´Â °Í, Áï zone sedimentation ¿¡¼­ ³ªÅ¸³­´Ù.

 
Samples vulnerable to particle segregation    
 
Fig. 2. Evolution of transmission profiles with time - first recorded profile after 10 seconds lowest (red), last profile after 15 hours uppermost (green), centrifugation of a latex based paint ar 328 g, 20 ¡É, every 25th profile displayed.

ÀÌ°ÍÀº latex ¸¦ ±â¹ÝÀ¸·Î ÇÏ´Â paint ÀÇ transmission profile À¸·Î¼­ ´Ù¾çÇÑ Å©±âÀÇ ÀÔÀÚµé·Î ÀÌ·ç¾î Áø ¹°ÁúÀÌ Ä§ÀüÇÏ´Â ÇüÅÂ, Áï polydisperse sedimentation À» º¸¿©ÁÖ°í ÀÖ´Ù. transmission ÀÌ Å©°Ô ³ªÅ¸³ª°í ÀÖ´Â 106mm ÁöÁ¡Àº sample ÀÇ filling height À» ÀǹÌÇÑ´Ù. ÀÌ·± ÇüÅÂÀÇ polydisperser sedimentation Àº ÆäÀÎÆ® ÀÔÀÚµéÀÇ Å©±â´Â ´Ù¾çÇÏ°Ô Á¸ÀçÇϳª aggregation Àº ÀϾÁö ¾Ê´Â´Ù´Â °ÍÀ» ÀǹÌÇÑ´Ù.

 
How to compare the quality of different samples / batches    
 
Fig. 3. Separation kinetics of three different batched of a latex paint during prolonged centrifugation at 328 g. Movement of the interface supernantant-dispersion. Comparison witha product of standard quality.

¾ö°ÝÇÑ Ç°Áú °üÁú Ãø¸é¿¡¼­ º»´Ù¸é ¿À·£ ½Ã°£ °­ÇÑ ¿ø½É·ÂÀ» °¡ÇÏ¿©µµ sample Àº transmission ÀÌ º¯È­ÇÏ°Å´Ï ÀÔÀÚ°¡ ħÀüÇÏ´Â Çö»óÀÌ ³ªÅ¸³ª¸é ¾ÈµÈ´Ù. LUMiFuge ¿Í LUMiSizer ¿Í °°Àº STEP Technology ±â¹ÝÀÇ ºÐ»ê¾ÈÁ¤¼º ºÐ¼®Àåºñ´Â µ¿ÀÏÇÑ Á¶°ÇÇÏ¿¡¼­ ÃøÁ¤µÈ °¢±â ´Ù¸¥ sample ÀÇ seperation kinetics ¸¦ ºñ±³ÇÒ ¼ö ÀÖ°Ô ÇÏ¿© ÁØ´Ù.

 
Are results obtained under centrifugal acceleration reliable for evaluation of stability under normal earth gravity?    
 
Newtonian behavior Ư¼ºÀ» °¡Áø ÆäÀÎÆ®ÀÇ separation velocity ´Â °¡ÇØÁö´Â ¿ø½É·ÂÀÇ ¼¼±â¿¡ ºñ·ÊÇÑ´Ù. ±×·¯³ª ÆäÀÎÆ® Á¦Ç°µéÀº ´ë°³ º¹ÀâÇÑ non-Newtonian behavior Ư¼ºÀ» ³ªÅ¸³½´Ù. ÆäÀÎÆ® ¼ººÐ Á¶¼º¿¡ µû¶ó ¿ø½É·ÂÀÌ °¡ÇØ Áú¼ö·Ï separation velocity °¡ »¡¶óÁö´Â shearing thinning Çö»óÀ» ÁÖ·Î º¸ÀδÙ.
±×·¯¹Ç·Î ¿ø½É·Â ÇÏ¿¡¼­ÀÇ separation ÇüŸ¦ º¸°í ¾î¶»°Ô ÀÚ¿¬Áß·Â Çп¡¼­ÀÇ separation ÇüŸ¦ À¯ÃßÇÒ ¼ö ÀÖ´ÂÁö¿¡ ´ëÇÑ Àǹ®ÀÌ »ý±ä´Ù. ±×·¯³ª ÀÌ¿¡ ´ëÇÑ ÇØ´äÀº ¸Å¿ì °£´ÜÇÏ´Ù. sample À» ³·Àº ¿ø½É·Â ÇÏ¿¡¼­ ÃøÁ¤ÇÏ°í ¶Ç ³ôÀº ¿ø½É·Â ÇÏ¿¡¼­ ÃøÁ¤ÇÏ¿© centrifugal separation À» ºÐ¼®ÇÏ´Â °ÍÀÌ´Ù. ÀÌ ¹æ¹ýÀ» ÀÌ¿ëÇϸé Á¤»óÀûÀÎ Áß·Â ÇÏ¿¡¼­ particle and pigment segregation ÀÌ ÀÏ¾î ³ª´ÂÁö ±×¸®°í Áõ°¡ÇÏ´Â ¿ø½É·Â ÇÏ¿¡¼­ separation velocity °¡ ºñ·ÊÀûÀ¸·Î Áõ°¡ÇÏ´ÂÁö¸¦ ¾Ë ¼ö ÀÖ´Ù.

Table 1. Evaluation of separation stability for different batches of a colorant formulation, centrifugation at 328 and 2300 g (14 and 2 hours, respectively), 20 ¡É. (v328 and v2300 - separation velocity at 328 and 2300 g, v/v 2300/328 ? ratio between separation velocity measured at 2300 and 328 g, which should be close to a value of 7 for Newtonian behavior, < 7 indication of shear thickening behavior and > 7 indication of shear thinning behavior.


Table 1 Àº °¢±â ´Ù¸¥ 7°³ÀÇ sample À» 4000 rpm (2300 g, 2 hours) °ú 1500 rpm (328 g, 14 hours) À¸·Î ó¸®ÇÏ¿© ÃøÁ¤ÇÑ °á°úÀÌ´Ù. Newtonian behavior ¸¦ µû¸£´Â sample ÀÎ °æ¿ì¿¡´Â ¿ø½É·Â º¯È­¿¡ µû¶ó separation velocity ¿Í phase separation (supernatant volume / sample volume) µµ µ¿ÀÏÇÏ¿©¾ß ÇÑ´Ù.

Sample A ÀÇ °æ¿ì 2300 g ¿¡¼­´Â pigment segregation ÀÌ ½ÉÇÏ°Ô ÀϾ°í ÀÖÀ¸³ª ³·Àº ¿ø½É·Â ÇÏ¿¡¼­´Â Separation ÀÌ ÀϾÁö ¾ÊÀ¸¹Ç·Î ¸Å¿ì ¾ÈÁ¤ÇÑ »óŶó°í ÇÒ ¼ö ÀÖ´Ù. ¾ÈÁ¤¼º¿¡ ÀÖ¾î °¡Àå ¹®Á¦°¡ ÀÖ´Â sample Àº B, C, G ¶ó ÇÒ ¼ö ÀÖ´Ù. Áï sample B ´Â sample ³»ÀÇ media °¡ separation µÇ°í ÀÖ´Ù´Â °ÍÀ» ¾Ë ¼ö ÀÖÀ¸¸ç, Sample C ´Â pigment °¡ ½ÉÇÏ°Ô ºÐ¸®µÇ°í ÀÖÀ¸¸ç sample C ´Â syneresis Çö»óÀº ³ªÅ¸³ªÁö ¾ÊÀ¸³ª ´ë½Å shear thickening Çö»óÀÌ ³ªÅ¸³ª°í ÀÖ´Ù´Â °ÍÀ» ¾Ë ¼ö ÀÖ´Ù.

 
Conclusions    
 
- STEP Technology ±â¹ÝÀÇ ºÐ»ê ¾ÈÁ¤¼º ºÐ¼® ±â¹ýÀº ÆäÀÎÆ® Á¦Ç°ÀÇ separation stability ¸¦ ºÐ¼®ÇÏ´Â µ¥ °¡Àå È¿°úÀûÀÎ
  ¹æ¹ýÀÌ´Ù.

- syneresis, pigment and particle segregation °ú °°Àº Á¦Ç°ÀÇ ºÐ»ê ¾ÈÁ¤¼ºÀ» È¿°úÀûÀ¸·Î È®ÀÎ °¡´ÉÇÏ¸ç ¶ÇÇÑ Á¤·®È­
  ÇÒ ¼ö ÀÖ´Ù. °¢±â ´Ù¸¥ sample »çÀÌÀÇ Á¦Ç°ÀÇ Ç°ÁúÀ» ªÀº ½Ã°£¿¡ Á÷Á¢ÀûÀ¸·Î ºñ±³ ºÐ¼®ÇÒ ¼ö ÀÖ´Ù.

- »ó´ëÀûÀ¸·Î ³·Àº ¿ø½É·ÂÇÏ¿¡¼­ ±×¸®°í Å« ¿ø½É·ÂÇÏ¿¡¼­ ÃøÁ¤ÇÏ¸é ½ÇÁ¦ÀûÀÎ ÀÚ¿¬ Áß·ÂÇÏ¿¡¼­ ³ªÅ¸³ª´Â ¾ÈÁ¤¼ºÀ» ºÐ¼®ÇÒ ¼ö
  ÀÖ´Ù. ÀÌ »Ó ¾Æ´Ï¶ó ÆäÀÎÆ® ¼ººÐÁ¶¼º¿¡ µû¸¥ rheological behavior ¿¡ ´ëÇÑ µ¥ÀÌÅ͵µ ¾Ë ¼ö ÀÖ´Ù.



 
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