CN1076473C - Method for determining C60 - Google Patents

Method for determining C60 Download PDF

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Publication number
CN1076473C
CN1076473C CN 95107595 CN95107595A CN1076473C CN 1076473 C CN1076473 C CN 1076473C CN 95107595 CN95107595 CN 95107595 CN 95107595 A CN95107595 A CN 95107595A CN 1076473 C CN1076473 C CN 1076473C
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infrared
carbon
determination
infrared spectrum
determinand
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Expired - Fee Related
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CN 95107595
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CN1141432A (en
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杨爱明
方宝贤
郑如梅
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Yunnan University YNU
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Yunnan University YNU
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Abstract

The present invention relates to a method for determining C60, which belongs to the technical field of spectral analysis. The method incudes a dissolving working procedure, an evaporation working procedure, a tabletting working procedure, and a determination working procedure of an infrared spectrometer. The present invention has the advantages of simplicity, practicality, high speed, accuracy, low cost, etc.

Description

A kind of mensuration carbon 60The method that exists
The present invention relates to a kind of mensuration carbon 60The method that exists belongs to field of spectral analysis technology.
United States Patent (USP): the patent No. is 5,334,837, the date be Augusts 2 in 1994 day, be called force microscopy methods, the sampler tray that is used for force microscopy methods, by using the method for described force microscopy methods detection organic compound, the method that is suitable for the instrument of force microscopy methods and separates micro-working fluid.This method cost height, operation, debugging and maintenance are complicated, and cross pollution can appear in sample, so the accuracy that detects is unreliable.
Infrared spectrometer is touched tool (29 days Augusts nineteen ninety of CN2061282U) and manual fast infrared sample pelleting press (CN93237016.0 March 30 in 1994) with LZ type compressing tablet, uses above-mentioned compressing tablet to touch the tool method therefor and surveys trace carbon 60Sensitivity too low, can not measure carbon 60Characteristic absorption peak.
The objective of the invention is to overcome the deficiency of prior art, and provide a kind of simple and practical, quick and precisely, cheap mensuration carbon 60The method that exists.
The present invention is achieved in that this method is made up of dissolving, evaporation, compressing tablet, determination of infrared spectroscopy step.Wherein, artificial carbon's cage and natural minerals solute and volume of organic solvent ratio are 1: 2 in the dissolving step, and dissolution time is 24 hours, and course of dissolution carries out at normal temperatures and pressures; Evaporation step is earlier with top layer lysate sucking-off, adopts the nature volatilization then or evaporates under infrared lamp, until obtaining Powdered determinand; The compressing tablet step for Powdered potassium bromide and determinand by 700~1000: 1 weight ratio is mixed, and grinds after the mixing, when being ground to 200 orders, obtains a thin slice at 6~9 tons after suppressing 1 minute with hydropress pressure; The determination of infrared spectroscopy step obtains measuring the infrared spectrum of thing for thin slice is put into infrared spectrograph sample bin with the infrared spectrum determination method test; Analyze this infrared spectrogram, when occurring four absorption peaks on the infrared spectrum figure simultaneously and be 525~527cm, 1427~1428cm, 537~577cm, 1180~1183cm, in this material of decidable carbon is arranged 60Exist.
Accompanying drawing 1 is a carbon 60/ carbon 70(content is 98%, wherein carbon 60Be principal ingredient) infrared spectrogram.
Accompanying drawing 2 is a carbon 60The infrared spectrogram of (content is 7%).
Accompanying drawing 3 is the infrared spectrogram of natural minerals.
The present invention is described in further detail below in conjunction with the present invention:
Embodiment 1: qualitative determination content is artificial carbon's cage (carbon of 98% 60/ carbon 70, carbon wherein 60Be principal ingredient)
At first, with carbon 60/ carbon 70Artificial carbon's cage of (content is 98%) is put into organic solvent (as toluene, dimethylbenzene, carbon disulphide etc.), and the volume ratio of carbon cage and solvent is 1: 2, and dissolution time is 24 hours, and course of dissolution carries out at normal temperatures and pressures.Then with top layer lysate sucking-off, adopt the nature volatilization immediately or under infrared lamp, evaporate, until obtaining Powdered determinand; Mix by 1000: 1 weight ratio with determinand with Powdered potassium bromide again, grind after the mixing, when being ground to 200 orders, obtain a thin slice 6 tons of compactings after 1 minute with hydropress pressure; Repressed thin slice is put into infrared spectrograph sample bin, obtains measuring the infrared spectrum (accompanying drawing 2) of thing with the infrared spectrum determination method test; Analyze this infrared spectrogram, when occurring four absorption peaks on the infrared spectrum figure simultaneously and be 525cm, 1428cm, 577cm, 1183cm, in this material of decidable carbon is arranged 60Exist.
Embodiment 2: measure the carbon in the natural minerals (fossil) 60Whether exist.
Method and process are substantially with embodiment 1.Difference is mixed by 700: 1 weight ratio with determinand for potassium bromide in this example, grinds after the mixing, when being ground to 200 orders, obtains a thin slice 9 tons of compactings after 1 minute with hydropress pressure; Repressed thin slice is put into infrared spectrograph sample bin, obtains measuring the infrared spectrum (accompanying drawing 3) of thing with the infrared spectrum determination method test; Analyze this infrared spectrogram, when occurring four absorption peaks on the infrared spectrum figure simultaneously and be 527cm, 1427cm, 573cm, 1181cm, in the decidable natural minerals carbon is arranged 60Exist.
The present invention has simply, the advantage such as practical, quick, accurate, cheap.

Claims (4)

  1. A kind of mensuration carbon 60The method that exists is characterized in that this method is made up of dissolving, evaporation, compressing tablet, determination of infrared spectroscopy step; Wherein:
    (1) artificial carbon's cage and natural minerals solute and volume of organic solvent ratio are 1: 2 in the dissolving step, and dissolution time is 24 hours, and course of dissolution carries out at normal temperatures and pressures;
  2. (2) evaporation step is earlier with top layer lysate sucking-off, adopts the nature volatilization then or evaporates under infrared lamp, until obtaining Powdered determinand;
  3. (3) the compressing tablet step for Powdered potassium bromide and determinand by 700~1000: 1 weight ratio is mixed, and grinds after the mixing, when being ground to 200 orders, obtains a thin slice at 6~9 tons after suppressing 1 minute with hydropress pressure;
  4. (4) the determination of infrared spectroscopy step obtains measuring the infrared spectrum of thing for thin slice is put into infrared spectrograph sample bin with the infrared spectrum determination method test; Analyze this infrared spectrogram, when occurring four absorption peaks on the infrared spectrum figure simultaneously and be 525~527cm, 1427~1428cm, 537~577cm, 1180~1183cm, in this material of decidable carbon is arranged 60Exist.
CN 95107595 1995-07-22 1995-07-22 Method for determining C60 Expired - Fee Related CN1076473C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 95107595 CN1076473C (en) 1995-07-22 1995-07-22 Method for determining C60

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 95107595 CN1076473C (en) 1995-07-22 1995-07-22 Method for determining C60

Publications (2)

Publication Number Publication Date
CN1141432A CN1141432A (en) 1997-01-29
CN1076473C true CN1076473C (en) 2001-12-19

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CN 95107595 Expired - Fee Related CN1076473C (en) 1995-07-22 1995-07-22 Method for determining C60

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Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102944528A (en) * 2012-11-14 2013-02-27 上海交通大学 Method for measuring concentration of C60 nanocrystal particles in water medium
CN102944531B (en) * 2012-12-01 2014-09-17 上海微谱化工技术服务有限公司 Method for determining trace substances on surface of solid

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