Determining percent solids in suspension using Raman spectroscopy
IPC분류정보
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
G01J-003/44
G01N-021/65
G01G-009/00
G01N-015/06
출원번호
US-0194630
(2016-06-28)
등록번호
US-9625390
(2017-04-18)
발명자
/ 주소
Antunovich, Jason J.
Hamfeldt, Arthur T.
Woods, Rodney J.
Shum, Sam C.
출원인 / 주소
MannKind Corporation
대리인 / 주소
Wolf, Greenfield & Sacks, P.C.
인용정보
피인용 횟수 :
0인용 특허 :
19
초록▼
Methods and apparatus are provided for determining weight percent of solids in a suspension using Raman spectroscopy. The methods can be utilized to acquire Raman spectral data from the suspension and to determine weight percent of solids in a process being carried out, for example, in a vessel, wit
Methods and apparatus are provided for determining weight percent of solids in a suspension using Raman spectroscopy. The methods can be utilized to acquire Raman spectral data from the suspension and to determine weight percent of solids in a process being carried out, for example, in a vessel, without the need to remove samples for analysis. The weight percent of the solids can be determined with a desired accuracy in a relatively short time, typically 10 minutes or less. The acquired Raman spectral data may be processed by chemometric software using, for example, a partial least squares algorithm and data pretreatment to provide a predicted value of weight percent solids. In some embodiments, the invention is used to determine the weight percent of microparticles of a diketopiperazine in an aqueous solution.
대표청구항▼
1. A method for determining weight percent of solids in a suspension, comprising: mixing the suspension;acquiring Raman spectral data of the solids in the suspension; andprocessing the Raman spectral data to determine weight percent of the solids in the suspension. 2. A method as defined in claim 1,
1. A method for determining weight percent of solids in a suspension, comprising: mixing the suspension;acquiring Raman spectral data of the solids in the suspension; andprocessing the Raman spectral data to determine weight percent of the solids in the suspension. 2. A method as defined in claim 1, wherein the weight percent of the solids in the suspension is in a range of 5% to 20%. 3. A method as defined in claim 1, wherein the solids are microparticles of a diketopiperazine. 4. A method as defined in claim 3, wherein the microparticles have a size in a range of 0.1 to 34 micrometers. 5. A method as defined in claim 3, wherein acquiring Raman spectral data includes acquiring data in a range of 1180 to 1800 cm−1 and a range of 2782 to 3136 cm−1. 6. A method as defined in claim 1, wherein processing the Raman spectral data includes executing a partial least squares algorithm with Savitzky-Golay first derivative data pretreatment. 7. A method as defined in claim 1, wherein processing the Raman spectral data includes executing a Partial Least Squares algorithm using two principal components. 8. A method as defined in claim 1, wherein the Raman spectral data is processed by a computing device executing a partial least squares algorithm with data pretreatment. 9. A method as defined in claim 1, wherein processing the Raman spectral data includes executing a regression algorithm comprising a partial least squares, multiple linear regression, or principal component regression, with or without data pretreatment. 10. A method as defined in claim 9, wherein the data pretreatment is selected from multiplicative and extended multiplicative scatter correction, standard normal variate, various derivatives, and normalizations. 11. Apparatus for determining weight percent of solids in a suspension, comprising: a Raman spectrometer to acquire Raman spectral data of the solids in the suspension; anda computing device including a processor and a computer-readable storage medium, the computer-readable storage medium containing computer instructions that, when executed by the processor, perform a method of processing the Raman spectral data to determine weight percent of the solids in the suspension. 12. Apparatus as defined in claim 11, wherein the Raman spectrometer includes a short focus optical device adapted for immersion in the suspension. 13. Apparatus as defined in claim 12, wherein the Raman spectrometer and the method of processing the Raman spectral data are configured to determine weight percent of microparticles of a diketopiperazine. 14. Apparatus as defined in claim 13, wherein the Raman spectrometer is configured to acquire Raman spectral data in a range of 1180 to 1800 cm−1 and a range of 2782 to 3136 cm−1. 15. Apparatus as defined in claim 11, wherein the Raman spectrometer is configured to acquire Raman spectral data in less than 10 minutes. 16. Apparatus as defined in claim 11, wherein the Raman spectrometer is configured to acquire Raman spectral data for an exposure time of 45 seconds and for 4 accumulations, and to perform cosmic ray filtration. 17. Apparatus as defined in claim 11, wherein the processing of the Raman spectral data includes executing a Partial Least Squares algorithm with Savitzky-Golay first derivative data pretreatment. 18. Apparatus as defined in claim 11, wherein the Raman spectral data is processed by the computing device executing a Partial Least Squares algorithm with data pretreatment. 19. Apparatus as defined in claim 11, wherein processing the Raman spectral data includes executing a regression algorithm comprising a partial least squares, multiple linear regression, or principal component regression, with or without data pretreatment. 20. Apparatus as defined in claim 19, wherein the data pretreatment is selected from multiplicative and extended multiplicative scatter correction, standard normal variate, various derivatives, and normalizations.
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이 특허에 인용된 특허 (19)
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Steiner Solomon S. ; Feldstein Robert ; Lian Huiling ; Rhodes Christopher A. ; Shen Gregory S., Microparticles for lung delivery comprising diketopiperazine.
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