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1、 J IS JAPANESE INDUSTRIAL STANDARD Translated and Published by Ja pa nese Standards Association (JAIMA/ JSA) General rules for atomic emission spectrometry ICs 71.040.50 Reference number : JIS K 0116 : 2003 (E) PROTECTED BY COPYRIGHT 24 S -,-,- K 0116 : 2003 Foreword This translation has been made b
2、ased on the original Japanese Industrial Standard revised by the Minister of Economy, Trade and Industry through deliberations at the Japanese Industrial Standards Committee, as the result of proposal for revision of Japanese Industrial Standard submitted by Japan Analytical Instruments Manufacturer
3、s Association (JAIMA) / Japanese Standards Association (JSA) with the draft being attached, based on the provision of Article 12 Clause 1 of the Industrial Standard- ization Law applicable to the case of revision by the provision of Article 1 4 . Consequently JIS K 0116 : 1995 is replaced with this
4、Standard. Date of Establishment: 1965-06-01 Date of Revision: 2003-06-20 Date of Public Notice in Official Gazette: 2003-06-20 Investigated by: Japanese Industrial Standards Committee Standards Board Technical Committee on Chemical Analysis JIS K 0116 : 2003, First English edition published in 2004-
5、05 Translated and published by: Japanese Standards Association 4-1-24, Akasaka, Minato-ku, Tokyo, 107-8440 JAPAN In the event of any doubts arising as to the contents, the original JIS is to be the final authority. O JSA 2004 All rights reserved. Unless otherwise specified, no part of this publicati
6、on may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from the publisher. Printed in Japan PROTECTED BY COPYRIGHT -,-,- Contents K 0116 : 2003 Page 1 2 3 4 5 5.1 5.2 5.3 5.4 5.5 5.6 5.7 5.8 5.9 5.10
7、 5.11 6 6.1 6.2 6.3 6.4 6.5 6.6 6.7 6.8 6.9 Scope Normative references Definitions Classification of analytical method ICP emission spectroscopy . Structure of apparatus . Attachments Additional functions Water. reagents. and gas . Preparation of the sample solution Preparation of the solution for c
8、alibration graph. the solution for correction of calibration graph and the blank solution for calibration graph . Setting of measuring conditions . Installation requirements of the apparatus . Quantitative analysis Safety . Items to be described in the analytical result . Spark source atomic emissio
9、n spectrometry Composition of apparatus Attachment . Addition function . Water, reagents and gas Preparation of sample . Counter electrode and auxiliary electrode Setting of measuring conditions . Quantitative analysis Setting condition of apparatus PROTECTED BY COPYRIGHT 1 1 1 3 4 4 8 8 9 9 13 14 1
10、6 21 22 23 24 24 25 25 26 26 27 27 27 30 K 0116 : 2003 6.10 Safety . 30 6.11 30 Items to be described in the analytical result . 7 The matters to be described by an individual standard 31 Annex 1 (normative) Items for judgment of using inductively coupled plasma atomic emission spectrometer 32 Annex
11、 2 (informative) Analytical method by photographic detection . 36 (ii) PROTECTED BY COPYRIGHT -,-,- JAPANESE INDUSTRIAL STANDARD JIS K 0116 : 2003 General rules for atomic emission spectrometry 1 Scope This Standard provides for general rules when quantitative analysis is carried out with an emissio
12、n spectrophotometer. 2 Normative references The following standards contain provisions which, through reference in this Standard, constitute provisions of this Standard. The most recent editions of the standards (including amendments) indicated below shall be applied. JIS K 0050 General rules for ch
13、emical analysis JIS K 0211 Technical terms for analytical chemistry (general part) JIS K 0212 Technical terms for analytical chemistry (optical part) JIS K 02 15 Technical terms for analytical chemistry (analytical instrument part) JIS K 0553 Testing methods for determination of metallic elements in
14、 highly purified water JIS K 0557 Water used for industrial water and wastewater analysis JIS K 1105 Argon JIS K 8001 General rule for test methods of reagents JIS Z 8402-1 Accuracy (trueness and precision) of measurement methods and re- sults-Part 1 : general principles and definitions IS0 3696 Wat
15、er for analytical laboratory use-Specification and test method 3 Definitions For the purposes of this Standard, the definitions given in JIS K 0050, JIS K 0211, JIS K 0212, JIS K 0215, JIS K 0553, JIS K 0557, JIS K 1105, JIS K $001, JIS Z 8402-1 and IS0 3696, and the following definitions apply: ato
16、mic emission spectrometry Quantitative analysis carried out by mea- suring the emission intensity of the atomic spectral line of the target element of the sample, or qualitative analysis carried out by identifying the wavelength of the target element of the sample, by vaporizing and exciting dischar
17、ge tech- nique such as ICP, spark discharge or arc discharge. photoelectric detection method A method to record the spectrum and measure spectral line intensity by using a photo multiplier or a photo-electric element. photographic detection method A method to identify wavelength and measure blacknes
18、s by photographing spectral line image with photosensitive materials. sequential scanning spectrometer The instrument for measuring the in- tensity of a spectrum or, in sequence, the intensity of spectral lines after sepa- rating the incident light into spectra. simultaneous spectrometer The instrum
19、ent for measuring simultaneous of the intensity of plural spectral lines after separating an incident light into spectra. PROTECTED BY COPYRIGHT -,-,- 2 K 0116 : 2003 integration time gration for a fixed time. The measuring time to measure emission intensity by inte- exposure time The time for keepi
20、ng the detector under an exposure state to measure light emission intensity. It is mainly used for photographic detection method. analytical sample A sample prepared to be measured. sample for calibration graph, solution for calibration graph The sample or solution containing target elements of the
21、known concentration, in order to prepare the calibration graph. sample for correction of calibration graph, solution for correction of calibration graph The sample or solution used for correction of calibration graph for each specific time or in each measurement of the specific number of samples. la
22、boratory reagent blank The signals given by water treated with just the same condition as that for the sample, including contact with glass instruments and apparatus during analytical practices or by matrix without target element for inspection of laboratory environment for target element or for int
23、erference elements and contamination from instruments and reagents. calibration blank The solution whose target element concentration is zero and whose composition is the same as that of the solution for calibration graph. test solution The solution prepared by carrying out the pretreatment of the g
24、aseous, liquid or solid samples so that they can be measured. detection limit The concentration giving a signal of three times the standard deviation of the light emission intensity or background intensity of a blank test solution. instrument limit of detection; ILOD The concentration that gives a s
25、ignal of three times the standard deviation of the signal obtained when measuring the blank solution for calibration graph ten continuous times. method limit of quantification; MLOD The concentration that gives a Sig- nal of 14.1 times the standard deviation of the signal obtained when measuring the
26、 laboratory reagent blank ten times continuously. short term precision Relative standard deviation of emission intensity or intensity ratio when the same sample is measured repeatedly for a short term. long term precision tensity ratio when the same sample is measured repeatedly for a long term. Rel
27、ative standard deviation of emission intensity or in- resolution each other. Ability of spectroscope to separate two spectral lines adjacent to PROTECTED BY COPYRIGHT -,-,- 3 K 0116 : 2003 inductively coupled plasma The plasma to be generated by inductive cou- pling of high frequency power in radio
28、frequency region. ICP is the abbrevia- tion of inductively coupled plasma. torch The tube having the concentric and triple structures used to supply the gas flow necessary for lighting and maintenance of ICP. nebulizer The implement for making the sample solution into fine liquid drops. splay chambe
29、r The implement used to introduce only very fine liquid drops to an emission part by separating and removing large particle size drops. plasma gas, coolant gas The main forming gas of plasma in ICP. It is sup- plied through the most exterior peripheral tube of a torch for the purpose of cooling torc
30、h. It is also called coolant gas. auxiliary gas The gas subsidiarily used for floating plasma upward in ICP. It is supplied through the middle tube of torch. carrier gas The gas used for introduction of a sample into plasma in ICP. It is supplied through the central tube of torch. background equival
31、ent concentration; (BEC) The element concentration giving signal intensity equal to background intensity. electrode The generic term of counter electrode, sample electrode, and auxil- iary electrode for forming the discharging gap of spark discharge and arc dis- charge. atmospheric chamber The instr
32、ument substituting atmospheric gas around the electrode of spark discharge or arc discharge. atmospheric gas The gas flowed around the electrode of spark discharge OF arc discharge for the purposes such as stabilization of discharge, removal of in- fluence owing to sample hysteresis, absorption owin
33、g to oxygen in air, and band spectrum, etc. Argon, nitrogen, oxygen or mixed gas thereof is used according to its pur- pose. preburn time, predischarge time The time set as the period when photom- etry or exposure is not carried out, during the time from start of discharge to stabilization of emissi
34、on intensity in spark discharge atomic emission spectrometry. 4 Classification of analytical method The analytical method is classified into an inductively coupled plasma emission spectroscopy (hereafter referred to as “ICP emission spectroscopy”) and a spark source atomic emission spectrometry. Rem
35、arks 1 The atomic emission spectroscopy that uses the high-voltage spark electrical discharge or the low voltage spark electrical discharge (including the low voltage capacitor electrical discharge) is called a spark source atomic emission spectrometry. PROTECTED BY COPYRIGHT 4 K 0116 : 2003 Emissio
36、n part - Excitation - source part 2 Though there are an arc discharge atomic emission spectrometry, a glow discharge atomic emission spectrometry, and a microwave induction plasma emission spectrometry (MIP emission spectros- copy), etc., those are not specified in this Standard. When it is necessar
37、y to use these analytical methods, they shall be specified by individual standards. 3 The photographic detection method (refer to Annex 2) may be used for qualitative analysis or to adjust the spectroscope. Spectrophotometry - Data processing part part 5 ICP emission spectroscopy 5.1 Structure of ap
38、paratus The ICP emission spectrophotometer shall be com- posed of the excitation source part, sample introduction part, the emission part, the spectrophotometry part, data processing part and the control system part. Fig. 1 shows an example of the basic structure of the instrument. Sample introducti
39、on Control system Fig. 1 Structure of ICP emission spectrophotometer 5.1.1 Excitation source part This part is composed of the electric power source circuit and control circuit to supply and control electric energy in order to maintain the emission part. 5.1.2 Sample introduction part It is the part
40、 introducing the sample into the emission part (Fig. 2) composed of a nebulizer, a spray chamber, and a drain trap. The drain trap shall not allow the carrier gas to flow out. PROTECTED BY COPYRIGHT -,-,- 5 K 0116 : 2003 To a torch T o a drain Fig. 2 Sample induction part (example) 5.1.3 Emission pa
41、rt This is a part where the target element in the sample is excited and emitted and composed of the torch and the induction coil (Fig. 3). The torch usually consists of a threefold tube, and the sample is introduced from the central tube. Argon is used for the gas to form the plasma. Induction Carri
42、er gas + samples Fig. 3 Emission part (example) which are the horizontal observation method and the observation axially method. There are two types of the observation method from the emission part (Fig. 4), PROTECTED BY COPYRIGHT 6 K 0116 : 2003 Spectrophotometry Pad OaO -I_ Spectrophotometry part o
43、00 Horizontal observation method Observation axially method Fig. 4 Observation method of light 5.1.4 Spectrophotometry part The spectrophotometry part is composed of the convergent light system which introduces light radiated from the emission part to a spectral part effectively, a spectral part whi
44、ch separates spectral lines, and a detec- tion part. There are Tselni Turner type spectroscope (Fig. 5), Passhen Runge type spectroscope (Fig. 61, and a Echelle type spectroscope (Fig. 7), etc. in the spectro- scope. The Tselni Turner type spectroscope is used as a sequential spectroscope, and the P
45、asshen Runge type spectroscope and the Echelle type spectroscope are used chiefly as a simultaneous measurement type spectroscope. The detector converts the incident light into an electric signal corresponding to its intensity, and a photo- multiplier or a solid state detector is used. Remarks : For
46、 measuring spectral lines in a vacuum ultraviolet region (wave- length 190 nm or under), the spectroscope shall have a structure for evacuating the convergent light system and the spectroscope, or a structure for substituting air for the argon or nitrogen. n Exit slit n Detector Concave mirror Conca
47、ve mirror Light n system source U Entrance slit Fig. 5 Spectrophotometry part with Tselni Turner type spectroscope PROTECTED BY COPYRIGHT -,-,- 7 K 0116 : 2003 Detector Fig. 6 Spectrophotometry part with Passhen Runge type spectroscope Entrance Convergent dit system Light Concave mirror Concave mirr
48、or J Detector Fig. 7 Spectrophotometry part with Echelle type spectroscope (an example) 5.1.5 Data processing part After data processing(l), the calibration graph and the measurement result, etc. are showed by using CRT and the printer, etc. Note (1) In order to improve accuracy of processing data, some data processing parts have functions of background correction, the spectral interfer- ence correction, correction by an internal standard element, etc. 5.1.6 Control system part For using the apparatus under the optimum condi- tions, this part controls the gas flows, and torc