KR810000624B1 - Method of sulfur analysis by x-ray spectro photometer - Google Patents

Method of sulfur analysis by x-ray spectro photometer Download PDF

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KR810000624B1
KR810000624B1 KR1019800000521A KR800000521A KR810000624B1 KR 810000624 B1 KR810000624 B1 KR 810000624B1 KR 1019800000521 A KR1019800000521 A KR 1019800000521A KR 800000521 A KR800000521 A KR 800000521A KR 810000624 B1 KR810000624 B1 KR 810000624B1
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sulfur
ray
filter paper
fuel oil
analysis
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KR1019800000521A
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Korean (ko)
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고덕주
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포항종합제철 주식회사
박태준
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence

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  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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Abstract

Sulfur component in fuel oil can be simply analized by X-ray spectro photometer. Standard fuel oil by sulfur conc. and testing oil is homogeneiously precipitated on filter paper and dried in oven at 105±5≰C for 30mins. So the intensity of precipitated filter paper is compared with that of standard material to give sulfur content.

Description

형광 X선 분광기에 의한 유황(Sulfur) 분석방법Sulfur analysis method by fluorescence X-ray spectroscopy

본 발명은 형광 X선 분광기에 의한 연료유 중의 유황성분을 신속하게 정량 분석하기 위한 방법이다.The present invention is a method for rapidly quantitatively analyzing sulfur components in fuel oil by fluorescent X-ray spectroscopy.

이러한 방법으로 이미 오래 전부터 연료유 중 유황성분을 분석하기 위하여 정유공장등에서 기 사용되어온 X선 설퍼메타(X-Ray Sulfur Meter) 및 온라인 설퍼메타 (On-line Sulfur Meter)에 의한 분석방법과 폴리프로필렌포일(Poly Propylene Foil) 마일러 포일(Mylay Foil) 및 특수 스크린(Screen)을 사용한 리퀴드 샘플 홀더(Liquid Sample Holder)를 이용하여 형광 X선 분광장치에 의한 연료유중의 유황분을 정량 분석하는 방법이 있어 왔다.In this way, polypropylene and analytical methods using X-Ray Sulfur Meter and On-line Sulfur Meter have been used in oil refineries for analyzing sulfur components in fuel oils for a long time. A method of quantitatively analyzing sulfur content in fuel oil by fluorescent X-ray spectroscopy using a liquid sample holder using a poly propylene foil and a mylar foil and a special screen It has been.

그러나 X선 설퍼메타 온라인 설퍼메타 및 특수스크린을 사용한 리퀴드 샘플 홀더에 의한 유황성분의 정량분석 방법은 제작 및 구입비가 엄청날 뿐더러 부속자재의 구입이 어렵고 분석에 장시간을 요하는 등 실용적인 측면에서 많은 문제점을 갖고 있다.However, the method of quantitative analysis of sulfur components by liquid sample holder using X-ray sulfur meta online sulfur meta and special screens is not only expensive to manufacture and purchase but also difficult to purchase accessory materials and requires a long time for analysis. Have

본 발명은 상기한 문제점을 해결하기 위하여 분석에 필요한 특수 스크린 대신에 구입이 수월하고 저렴한 필터 페이퍼(Filter paper)류로 대체시키고 그것에 가장 적합한 분석조건을 부여하여 신속하고 정확하게 설퍼성분의 함량을 구할 수 있는 방법으로 본 발명을 상세히 설명하면 다음과 같다. 분석하고져 하는 미지시료(연료유)와 설퍼농도별 표준시료를 같은 조건하에서 필터페이퍼에 균일하게 침적시키고 침적된 필터페이퍼를 105±5℃ 상태의 드라이오븐(Dry Oven) 속에 넣고 30분 동안 충분히 건조시킨 후 형광 X선 분광장치의 샘플홀더에 맞도록 절단하여, 표준시료가 침적된 필터 페이퍼를 형광 X선 분광장치로 강도를 분석하여 그 결과에 따라 검량선을 작성한다. 이때 같은 방법으로 미지시료가 침적된 필터페이퍼를 형광 X선 분광장치로 강도를 분석하여 표준시료에 의해 작성된 검량선과 비교하여 설퍼함량을 구할 수 있다.In order to solve the above problems, instead of a special screen necessary for analysis, it is easy to purchase and inexpensive filter papers, and it is possible to obtain the content of sulfur components quickly and accurately by giving the most suitable analysis conditions thereto. When explaining the present invention in detail as follows. The unknown sample (fuel oil) and sulfur concentration standard sample to be analyzed are uniformly deposited on the filter paper under the same conditions, and the deposited filter paper is placed in a dry oven at 105 ± 5 ° C and dried for 30 minutes. After cutting, the filter paper is cut to fit the sample holder of the fluorescent X-ray spectrometer and the intensity of the filter paper on which the standard sample is deposited is analyzed by the fluorescent X-ray spectrometer to prepare a calibration curve according to the result. At this time, the strength of the filter paper in which the unknown sample is deposited can be analyzed by fluorescence X-ray spectroscopy, and the sulfur content can be obtained by comparing with the calibration curve prepared by the standard sample.

이와같이 필터 페이퍼류로서 특수스크린을 대체하여 연료유중의 설퍼 함량치를 분석해 낼 수 있는 가장 적합한 분석조건으로는 표 1과 같다.As such, the most suitable analytical conditions for analyzing the sulfur content of fuel oil by replacing the special screen as filter papers are shown in Table 1.

[표 1]TABLE 1

Trget Rh(또는 Cr)Trget Rh (or Cr)

Spectrum S-

Figure kpo00001
Spectrum S-
Figure kpo00001

Voltage 20KV(사용범위내에서 변경가능)Voltage 20K V (can be changed within the range of use)

Current 10mA( " )Current 10mA (")

Detector F-PCDetector F-PC

Crystal Ge(또는 ADP, Nacl, PET, RAP)Crystal Ge (or ADP, Nacl, PET, RAP)

Path VacuumPath vacuum

Measuring Time 40Sec(설정가능범위내에서 변경가능)Measuring Time 40Sec (can be changed within the settable range)

이와 같이 상술한 본 발명은 형광 X선 분광장치를 이용하여 연료유중의 설퍼성분을 분석하기 위한 것으로 가격이 고가인 특수스크린등을 이용한 종래의 방법에 비하여 분석에 필요한 자재를 저렴하고 쉽게 구할 수가 있으며 분석에 따른 소요시간의 단축과 양호한 분석결과를 얻을 수 있는 필터페이퍼류를 침적시켜 설퍼 성분분석에 필요한 시료를 제공하여 형광 X선 분광장치에 의한 연료유중위 유황분을 신속하게 분석하는 방법이다.As described above, the present invention is to analyze sulfur components in fuel oil by using a fluorescent X-ray spectrometer, and it is possible to obtain materials necessary for analysis cheaply and easily as compared to the conventional method using a special screen, which is expensive. In addition, it is a method to rapidly analyze fuel-mediated sulfur content by fluorescence X-ray spectroscopy by providing samples necessary for sulfur component analysis by depositing filter papers which can reduce the time required for analysis and obtain good analysis results.

Claims (1)

필터 페이퍼에 연료유를 균일하게 침적시킨 후 건조시킨 것을 시료로 하여 형광 X선 분광장치에 의하여 설퍼 함량을 분석하는 방법.A method of analyzing sulfur content by fluorescence X-ray spectroscopy with a sample of fuel oil deposited uniformly on a filter paper and then dried.
KR1019800000521A 1980-02-11 1980-02-11 Method of sulfur analysis by x-ray spectro photometer KR810000624B1 (en)

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