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1、UDC 543.423.5.082.52 JIS JAPANESE I NDUSTRIAL STANDARD General Rules for Photoelectric Emission Spectrochemical Analysis of Metal Materials JIS z 2611-1977 I 1 I standard i n Japanese is to be evidence ! _._ - Translation without guarantee In the event of any doubt arising, the original i I I Transl
2、ated Japanese Standards Association 1-24, Akasaka 4, Minato-ku Tokyo 107 Japan 0 JSA, 1984 PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:37:26 MDTNo reproduction
3、 or networking permitted without license from IHS -,-,- U?C 543.423.5.082.52 JAPANESE INDUSTRIAL STANDARD J I S General Rules for Photoelectric Z 2611-1977 Emission Spectrochemical (Reaffirmed: 1980) Analysis of Metal Materials 1. Scope This Japanese Industrial Standard specifies the following gener
4、al matters concerning the photoelectric emission spectrochemical analysis of metal materials. (1) Apparatus (2) Devices and machinery for sampling and preparing samples (3) Materials ( 4 ) Samples (5) Methods of preparing samples (6) Measuring operation and methods of determination (7) Selection and
5、 installation of apparatus (8) Analysis error and control thereof (9) Safety and sanitation (10) Items to be described in each standard of analysis method 2. Summary In this method, the sample is used as electrodes in the state of the metal solid as it is or being suitable formed, or the sample is m
6、ade a solution and using auxiliary electrodes, and photoelectric emission is produced in the condition adapted to the object of analysis, - 1 - PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie N
7、ot for Resale, 03/13/2007 08:37:26 MDTNo reproduction or networking permitted without license from IHS -,-,- the rays are converted to spectra in a spectroscope, the strength of each analysis line of the element to be determined is measured photoelectrically, and the content of each element in the a
8、nalysis sample is obtained by using the calibration curves that have been prepared preliminarily based on standard samples. 3. Apparatus 3.1 Summary of Apparatus This apparatus consists of an exciting power source, a light source, a condenser, a spectroscope, a light receiver, and photometer. The ex
9、citing power source supply the exciting force for the sample to the light source to cause emission. The condenser condenses and brings the light to the spectroscope. The spectroscope converts the incident light into the spectral lines of the component elements and send them to the light receiver. Th
10、e photometer photoelectrically measures the intensity of the spectral line of each element that has entered the receiver, and indicates or records the results or converts the measured values into element contents and displays them. 3.2 Constitution of Apparatus The apparatus is constituted of the fo
11、llowing units. Fig. 1 shows an example of the constitution. (1) Exciting power source (2) Light source (3) Condenser ( 4 ) Spectroscope (a) Inlet-slit system (b) Spectral system (c) Outlet-slit system - 2 - PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license
12、 with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:37:26 MDTNo reproduction or networking permitted without license from IHS -,-,- (5) Photometer (a) Photomultiplier (b) Integrating unit (c) Recorder, indicator and converter for content (d) Operating circuit
13、Fig. 1 An Example of Constitution of Emission Spectrochemical Analysis Apparatus - 3 - PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:37:26 MDTNo reproduction or
14、networking permitted without license from IHS -,-,- 3.2.1 Exciting Power Source This apparatus includes the sparking power source, arcing power source, low-voltage condenser discharging source, etc. the sample evaporate and vaporize and exciting it to luminescence. Examples of exciting power sources
15、 that are commonly used are described below: These apparatus supply the power source unit for making (1) Sparking Power Source (a) D.C. High-Voltage Sparking (DC HVS) Power Source This apparatus raises the voltage up to about 1 0 kV or over by means of a high-voltage transformer, and rectifies this
16、current with rectifier tubes or rectifiers, charge condensers with the rectified current, and then, make the condensers discharge the electricity in turn with a synchronous rotary interrupter. Fig. 2 shows an example of its main circuit. Fig. 2 Main Circuit Diagram of D.C. High-Voltage Sparking Powe
17、r Source 1. High-voltage transformer: 4 . Synchronous rotary inter- 8 to 15 kV secondary voltage rupter 2. Rectifier tubes 5 . Inductance coil, O to 820 uH 3. Condenser, 0.007 pF 6. Analyzing gap - 4 - PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with
18、 JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:37:26 MDTNo reproduction or networking permitted without license from IHS -,-,- (b) A.C. High-Voltage Sparking (AC HVS) Power Source This apparatus raises the voltage up to about 10 kV or over with a high-voltage
19、transformer, charges a condenser with this electricity, and controls the discharge from the condenser with the controlling gap that is arranged in series or in parallel with the analyzing gap or with a synchronous rotary interrupter that is arranged in series with the analyzing gap. Fig. 3 shows an
20、example of the main circuit of the apparatus. Fig. 3 Main Circuit Diagram of Series-Control-Gap Type A.C. High-Voltage Sparking Power Source 1. 2. 3. 4 . (2) High-voltage transformer: 5. Inductance coil, O to 1 0 to 20 KV secondary voltage 1250 UH Resist er 6. Analyzing gap Condenser, 0.025 to 0.075
21、 UF 7, Air-blower Resister, O to 3 . Q 8. Controlling gap Arcing Power Source The apparatus in this category includes the d.c. arcing power source and the a.c. arcing power source, of which the latter is chiefly used in the photoelectric spectrochemical analysis. The a.c. arc is of either high-volta
22、ge (AC HVC) or low-voltage (AC LVA), and the both are usually ignited by means of high-voltage sparks or high-frequency discharge. In one type of these appara- - 5 - PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/111111100
23、1, User=Wing, Bernie Not for Resale, 03/13/2007 08:37:26 MDTNo reproduction or networking permitted without license from IHS -,-,- tus, the arcing intervals are controlled by the commercial power frequency unit and in the other type by the second uni t. Figs. 4, 5, 6 and 7 show the examples of main
24、circuits of these apparatus. Fig. 4 Main Circuit Diagram of High-Frequency Spark Ignition Type High-Voltage A.C. Arcing Power Source 1. Time switch for high- 5. Tesla coil frequency ignition 2. High-voltage transformer: 6 . Transformer: 2;4 kV 5 kV secondary voltage secondary voltage 3. Ignition gap
25、 7. Resister 4. Condenser 8 . Analyzing gap - 6 - PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:37:26 MDTNo reproduction or networking permitted without license
26、from IHS -,-,- Fig. 5 Main Circuit Diagram of High-Voltage Spark Ignition Type Low-Voltage A.C. Arcing Power Source 1. High-voltage transformer 7. Controliing gap 2. Choke coil 8. Resister, 9.5 to 77 $ 7 3. Condenser, 0,0025 to 9. Transformer: 280 V 0.0075 pF secondary voltage 4. Inductance coil 5.
27、Resister, O to 3 51 6. Blower - 7 - 10. Choke coil 11. Analyzing gap PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:37:26 MDTNo reproduction or networking permitt
28、ed without license from IHS -,-,- Fig. 6. Main Circuit Diagram of High-Voltage Spark Ignition Type Rectified Arcing Power Source 1. High-voltage transformer 7. Controlling gap 2. Choke coil 8. Resister, 9.5 to 77 S i 3. Condenser, 0.0025 to 9. Transformer: 280 V 0.0075 LIF secondary voltage 4. Induc
29、tance coil 10. Rectifier tube 5. Resister, O to 3 52 11. Choke coil -_ - - ._ b. blower 12. Analyzing gap - 8 - PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:37:
30、26 MDTNo reproduction or networking permitted without license from IHS -,-,- Fig. 7. Main Circuit Diagram of Pheilsticker Type Interrupted Arcing Power Source A 1. 2. 3. 4 . 5. (3) Res ist er 6 . Synchronous rotary interrupter Interrupter cam (both inter- 7. Tesla coil rupting ratio and interrupt- i
31、ng cycle are variable) 8. Resister, 1 to 80 $2 High-voltage transformer: 4.5 9. Condenser to 13.5 kV secondary voltage Choke coil 10. Choke coil Condenser, 0.003 t o 0.0066 tiF 11. Analyzing gap Low-Voltage Condenser Discharging Power Source This apparatus is an exciting power source that charges a
32、large capacity condenser up to about 1 kV at most and then, makes ignition with a high-voltage spark. The discharge is controlled by means of a synchronous rotary interrupter, an interrupter with electronic tube circuit, a fixed controll- ing gap, etc. This apparatus can vary the discharge stepwise
33、from that of a d.c. low-voltage spark (DC LVS) t o that of d.c. low-voltage arc (DC LVA). Figs. 8 and 9 show examples of main circuit of this appara- tus. - 9 - PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, Us
34、er=Wing, Bernie Not for Resale, 03/13/2007 08:37:26 MDTNo reproduction or networking permitted without license from IHS -,-,- Fig. 8. Main Circuit Diagram of Hasler Type Low- Voltage Condenser Discharging Power Source 1. High-voltage transformer: 7. Rectifier tube 15 kV secondary voltage 2. High-vol
35、tage rectifier 8. Choke coil tube 3. Condenser 9. Condenser, 2 to 60 J.F 4 . Resister 10. Resister, 2 to 200 Sl 5. Synchronous rotary inter- li. Inductance coil, 50 to rupter 360 1.iH 6. Transformer 1 kV: 12. Analyzing gap secondary voltage - 10 - PROTECTED BY COPYRIGHT Copyright Japanese Standards
36、Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:37:26 MDTNo reproduction or networking permitted without license from IHS -,-,- Fig. 9. Main Circuit Diagram of Fixed Control Gap Type Low-Voltage Condenser Dischargin
37、g Power Source 8 - m I 1 1 2 1. Resister 7. Transformer: 1 kV secondary voltage 2. High-voltage transformer: 8. Rectifier 20 kV secondary voltage 3. High-voltage rectifier 9. Condenser, 1 to 15 UF 4 . Resister 10. Resister, 1 to 50 52 5. Condenser 11. Inductance coil, 50 or 330 VH 6. Controlling gap
38、 12. Aaalyzing gap 3.2.2 Light Source Apparatus This apparatus is an electrode holder for making the sample emission by electric discharge and is designed to be able to hold the flat sample or bar sample electrode, or an auxiliary electrode for sample and the counter electrode to it. Also it is cons
39、tructed so as to use a specific gas as the emissive atmosphere, or is designed to rotate the auxiliary electrode for sample, or is designed to facilitate water-cooling of the sample- electrode holder. - 11 - PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under licens
40、e with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:37:26 MDTNo reproduction or networking permitted without license from IHS -,-,- (1) Electrode Holder for Flat Sample This electrode holder can generally hold a flat sample with not less tan 20 mm diame- ter
41、in the vacuum type spectrometer, or a flat sample with not less than 30 mm diameter in the ordinary pressure type spectrometer. However, it is sometimes designed to be able to hold a bar sample also. argon is generally used for the atmosphere of the light source and its flow rate is controllable wit
42、h a flowmeter and an automatic valve. Fig. 10 shows an example of the light source of the vacuum type spectrometer, and F i g . l l shows an example of the.1ight source of the ordinary pressure type spectrometer. In a vacuum type spectrometer, Fig. 10. Example of Electrode Holder of Vacuum Type Spec
43、trometer 1. Condensing lens 4 . Counter electrode 2. Protector quartz plate 5. Sample 3, Argon inlet 6 . Argon outlet - 12 - PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/1
44、3/2007 08:37:26 MDTNo reproduction or networking permitted without license from IHS -,-,- Fig. 11. Example of Electrode Holder of Ordinary Pressure Type Spectrometer 1. 2. 3 . (2) (3) 3.2.3 6 Il Sample 4 . Counter electrode holder Counter electrode 5. Safety door switch Sample tab 1 e 6 . Exhaust po
45、rt Electrode Holder for Bar Sample generally constructed so as to be able to hold a bar sample with not more than 20 m diameter. Also it is sometimes devised to facilitate the projection of the electrode for its positioning, or devised to facilitate the water-cooling of the electrode holder for prev
46、enting overheating. This electrode holder is Rotary Electrode Holder for Solution Sample holder can rotate the auxiliary electrode for sample around the vertical axis at a speed of 5 to 15 rpm in general. This electrode Condenser This device consists of a system of condenser lenses and is used to co
47、ndense the light from the light source and project it into the spectral system. For the condensing lens system, the collimator imaging method, midway imaging method, cylindrical lens imaging method, etc. are used, and for the spectrometer, the collimator imaging method is generally used. - 13 - PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:37:26 MDTNo reproduction or networking permitted without license from IHS -,-,- (