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1、J I S K*O120 86 4933608 0055067 I JIS JAPANESE I NDUSTRIAL STANDARD General Rules for Fluorometric Analysis JIS K o I 20-1986 Translated and Published by Japanese Standards Association Printed in Japan /- I UDC 543.426 9s Copyright Japanese Standards Association Provided by IHS under license with JS
2、ALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 20:01:05 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S K*OL20 86 Y33b08 0055068 3 Translation without guarantee standard in Japanese is to be evidence i n the event of any doubt arising
3、, the original e ,- o e Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 20:01:05 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S K*OL20 Bb m 4933608 0055069
4、5 JAPANESE INDUSTRIAL STANDARD General Rules for Fluorometric Analysis UDC 543.426 J I S K 0120-1986 1. Scope the measurement of fluorescence intensity at the wavelength of 185 to 1200 nm by means of a fluorometric analyzer and thereby the analysis of inorganic and organic substance. This Japanese I
5、ndustrial Standard specified the generals concerning 2. Common Matters Common matters shall be in accordance with JIS K 0050. 3. Definition The definition of the main terms used in this standard, other than those specified in JIS K 0211, JIS K 0212, and JIS Z 8103, the following definitions apply. f
6、luorescence the molecules excited by light into an excited singlet state are transferred to their ground state. In this case, the light (phosphorescence) emitted via an excited triplet state shall be included. The fluorescence means the light emitted when exciting light molecules at ground state to
7、an excited singlet state. The light radiated in order to transfer the fluorophotometer means of a filter at both an exciting light side and a fluorescence side. The apparatus carrying out measurement by spectrophotofluorometer ment by means of a monochrometer for wavelength selection at both an exci
8、ting light side and a fluorescence side. The apparatus carrying out measure- fluorospectrophotometer ment by means of a filter at exciting light side and a monochro- meter at fluorescence side for wavelength selection. apparatus equipped with a monochrometer at exciting light side and a filter at fl
9、uorescence side is also called a fluorospectro- photometer. The apparatus carrying out measure- The Applicable Standards : JIS K 0050-General Rules for Chemical Analysis JIS K 0211-Technical Terms for Analytical Chemistry (General Part) JIS K 0212-Technical Terms for Analytical Chemistry (Optical Pa
10、rt) JIS Z 8103-Glossary of Terms Used in Instrumentation Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 20:01:05 MDTNo reproduction or networking permitted without license from IHS -,-,- J
11、 I S K*O120 86 9 4933608 0055070 L 2 K 0120-1986 quenching (at fluorometric analysis) molecules excited by light may lose their activity to emit fluorescence due to the collision against other molecules or to a chemical reaction. The phenomena that the deoxygenation solvent by the aeration of such g
12、as as nitrogen, argon, and others. - cell (for fluorometric analysis) The cell shall give no, or very weak, fluorescence in the measuring range of light wavelength. The procedure to expel the oxygen dissolved in contrast cell (for fluorometric analysis) that can be used for fluoroscence measuring. T
13、he standard cell cell for sample (for fluorometric analysis) used for measuring the fluorescence of sample in comparison with a contrast cell. The cell that can be 4. Apparatus 4.1 Constitution of Apparatus The constitution of a fluorometric analyzer shall be shown in Fig. 1. Fig, 1. Fluorometric An
14、alyzer (Example) WaveIength selection unit at exciting light side at fluorescence side Wavc !ength selection unit r- 1 r- 1 I I I i Filter Indicatin and recor8ing Photornet Filter Light source unit I device device Monochrometer t I I I I 4 Monochrometer 1 7 L- - - - - 3 - - - - - -I I I I I I I L -
15、-I (1) Light Source Unit source, power source for light, and others. The light source unit is composed of a light (1.1) Light Source The light source shall radiate stably the exciting light (l). Note (l) There are mercury lamp, xenon lamp, deuterium lamp, laser, alkaline halide lamp, incandescent la
16、mp, and the like. (1.2) Power Source for Burning The power source for burning shall have a function to burn the light source and to keep its luminance constant. (2) Wavelength Selection Unit at Exciting Light Side The wave- length selection unit at exciting light is composed of the filter or monochr
17、ometer which selects the exciting light, having the wavelength suitable for analysis, out of the light radiated from a light source. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 20:01:05
18、 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S K*O320 8b 4733608 0055073 3 (3) 3 K 0120-1986 (a) Filter This is any of a coloured glass filter, gelatinous filter, plastic filter, or interference filter, or their combination. (b) Monochrometer This is either or the c
19、ombination of a prism or diffraction grating. Chamber for Sample The chamber for sample has a function, placing the sample in the optical path of exciting light, to introduce the emitted fluorescence to the wavelength selection unit of fluorescence side. This is composed of the cell of liquid, cell
20、for liquid chromatograph, and the holder of these cells or sample. (a) Cell for Liquid This cell shall have a high transparency for exciting light or fluorescence in the range of a wavelength required for analysis, shall give no, or very weak fluorescence, and be composed of the material free from c
21、orrosion by a sample or solvent. (b) Cell for Liquid Chromatograph The cell for a liquid chromatograph, composing a part of flowing channel , shall be free from a leakage of fluid. This shall have a high transparency in the range of a wavelength required for analysis, give no, or very weak, fluoresc
22、ence, and be composed of the,material free from corrosion by sample or eluate. (c) Holder The holder can fasten a cell of various type or sample in the optical path of exciting light, and shall have a structure not to change the intensity of fluorescence emitted from a sample. Wavelength Selection U
23、nit at Fluorescence Side selection unit at fluorescence side is composed of the filter or The wavelength monochrometer which selects the fluorescence , having a wave- length suitable for analysis, out of the fluorescence emitted from a sample. (a) Filter The same one as (2) (a). Monochrometer The sa
24、me one as (2) (b). Photometry Device detector and a signal processing part. The photometry device is composed of a (a) Detector The detector converts proportionally the intensity of fluorescence to the electric signal, and such as a photomultiplier , phototube , photoelectric cell, photocon- ductivi
25、ty cell, or photodiode can be used as a detector. (b) Signal Processing Part The signal processing part has a function to separate and output the signal, which is necessary for measurement, out of the signals from a detector. Copyright Japanese Standards Association Provided by IHS under license wit
26、h JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 20:01:05 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S K*O120 8b q933608 0055072 5 = 4 K 0120-1986 (6) Indicating and Recording Device The indicating and recording device has a func
27、tion to indicate the fluorescence intensity, or the relation between the fluorescence intensity and the wavelength of exciting light or the wavelength of fluorescence. 4.2 Marking Performance of Apparatus The following performance of apparatus shall be marked. . Fluorop hotome t er King of Light Sou
28、rce Marking of Wavelength (a) Exciting-Light Side The kind of a wavelength selection filter, and, centre wavelength and half-width or the wavelength of selected luminance, shall be marked. (b) Fluorescence Side The kind of a wavelength selection filter, and, centre wavelength and half-width, shall b
29、e marked. Stability of Photometry fluorescence intensity per hour under a certain condition This is the fluctuation value of S pect rop hot o fluor omet er Kind of Light Source Accuracy of Wavelength This is the bias represented by wavelength, between the maximum wavelength approx. the monochromatic
30、 light emitted from a monochgometer and the found wavelength on an indicator. Repeatability of Wavelength Setting dispersion on a scale when a certain wavelength is set in order to take out monochromatic light of the same wavelength from a monochrometer. This is represented by the Resolution light e
31、mitted from a monochrometer. This is represented by the spectrum width of the Stray Light of light having Wavelength other than the set one to the light intensity emitted from a wavelength selection unit. The light intensity of the wavelength other than the set wavelength can be obtained by transmit
32、tance of the light through a sample which has tranmissivity small enough for the set wavelength. This is represented by the ratio of total intensity Stability of Photometry fluorescence intensity (including scattering light) per hour under a definite condition, This is the fluctuation value of Fluor
33、osxect roDhotomet er The prescription on a filter is the same as in 4.2.1. The prescription on a monochrometer is the same as in 4.2.2. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 20:01
34、:05 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S K*OL20 Bb = 4933608 0055073 7 E F 5 K 0120-1986 4.3 Attachments The following are available for an attachment, and, as required, they may be attached. (1) Indicator of concentration (2) Indicator of differential phot
35、ometry (3) Automatic sample introducing apparatus (4) Automatic cell exchanging apparatus (5) Thermostatic apparatus for cell (6) Thermostatic apparatus at low temperature for cell (7) Scanner for thin layer chromatograph (8) (9) Apparatus for data processing Measuring apparatus of polarized fluores
36、cence 5. Water and Reagent 5.1 Water The water to be used in this standard shall be distilled .- water, ion-exchanged water, or super-demineralized water, however, in the case of separately specified, the specification shall be followed. Water shall give an electric conductivity of not more than 2 /
37、cm (25OC), have a colour keeping-time (2) not less than 60 min by potassium permanganate, and give no measuring error by fluorescence. This means the time interval, after 02 ml of potassium permanganate solution (0.002 mol/P,) and 2 ml of sulfuric acid (1 + 1) are dissolved in 500 ml of water while
38、mixing with agitating and the solution is allowed to stand, until the colour fades away. Note (2) 5.2 Reagent Reagents shall be in accordance with JIS K 0050. e Remark: Even though solvent has not fluorescence as it is, frequently the impurities contained may give fluorescence, therefore the blank t
39、est shall be carried out without fail. In cases where there is an abstructive fluorescence for measuring, purification or substitution by other reagent should be considered. Specially, in such cases as quenching owing to the oxygen in solvent (including water) and hindrance by photo-oxidation , deoy
40、genation is necessary. 6. Operation 6.1 Installation of Apparatus The condition for apparatus installation shall be as follows: (1) There is no construction nearby such as producing strong magnetic field, electric field, or high frequency. Copyright Japanese Standards Association Provided by IHS und
41、er license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 20:01:05 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S K*OL20 86 m 4933b08 0055074 9 6 K 0120-1986 (2) There is no strong or continuous vibration. (3) The place is not
42、 so dusty and no corrosive gas. (4) There is no direct sunshine. (5) The condition is 15 to 35OC at temperature and 30 to 85 % in relative humidity, and their fluctuation shall be . small, (6) There is a satisfactory ventlation. 6.2 Preparation of Sample The preparation of sample shall be carried ou
43、t according to the method specified in individual standard, however, the Q) I composition and state of a sample, and the concentration and property of the target ingredient shall be considered in order to prevent the target ingredient from the loss owing to evaporation, undissolving, degeneration, a
44、nd others. 6.3 Setting of Apparatus Operating Condition Operating condition on following items shall be set. Fluorop hot ometer Selection of a light source Selection of a filter at exciting light side Selection of quantity of light at exciting light side Selection of a filter at fluorescence side Se
45、lection of the intensity of fluorescence Spect rophotofluorometer Selection of a light source Selection of a photometric mode ( 3 ) Note (3) This is either a fluorescence intensity or excitation intensity. Selection of wavelength of an exciting light and fluorescence Selection of a slit width of a m
46、onochrometer at an exciting light side and fluorescence side Selection of a scanning method of a monochrometer at an exciting light side and fluorescence side Selection of an intensity of exciting light and fluorescence I Fluorospect rophotomet er The description on a filter is same as in 6.3.1. The
47、 description on a monochrometer is same as in 6.3.2. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 20:01:05 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S
48、 K*OL20 86 E 4933608 0055075 O E 7 K 0120-1986 a 7. Measuring of Spectrum 7.1 Measuring of Excitation Spectrum The measuring of excitation spectrum shall be carried out by using a fluorospectrophotometer - (monochrometer and filter method) or a spectrophotometer. 7.1.1 Case of Measuring by Single Beam Method In the case of measuring by using single beam, carry out according to the following procedures : Adjust a wavelength at fluorescence side to the maximum value of the fluorescence or the wavelength suitable for