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1、i i .; , e b e , J I S Z*3920 91 4933b08 O533239 T7T IS UDC 621.791 :628.511.122:543 JAPANESE INDUSTRIAL STANDARD Methods for chemical analysis of elements in welding fumes JIS Z 3 9 2 0 - 1 9 9 1 Translated and Published bY Japanese Standards Association Printed in Japan 11 s Copyright Japanese Sta
2、ndards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/16/2007 00:35:36 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S Z*3920 93 4933608 0533240 791 In the event of any doubt arising, the origi
3、nal Standard in Japanese is to be final authority. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/16/2007 00:35:36 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S Z
4、U3920 91 4933608 0513241 628 a P a a a UM: 621.791:628.511.122:543 JAPANESE INDUSTRIAL STANDARD J I S Methods for chemical analysis of elements in welding fumes Z 3920-1991 1 . Scope This Japanese Industrial Standard specifies the methods for analysis of the chemical composition contained in the fum
5、es generated from welding and brazing floating in the air in welding environment. Applicable Standards are as follows: JIS K 0050 JIS K 0115 Remarks: General rules for chemical analysis General rules for molecular absorptiometric analysis General rules for atomic absorption spectrochemical analysis
6、Standard substances for volumetric analysis JIS K 0121 JIS K 8005 JIS Z 3950 Methods of measurement for weld fume concentration JIS Z 8401 Rules for rounding off of numerical values 2. Composition to be analyzed The composition of fumes generated from welding, thermal cutting and brazing to be analy
7、zed shall be as follows: (1) Fume from welding Manganese, copper, nickel, chromium, vanadium, cobalt, lead, zinc, molybdenum, iron, aluminium and fluorine. (2) Fume from brazing Silver, copper, zinc, cadmium, phosphorus and fluorine. 3. General matters The general matters common to chemical analysis
8、 shall comply with JIS K 0050, JIS K 0115 and JIS K 0121. 4. Sampling and handling of samples for analysis The sampling and handling of samples for analysis shall be as follows: Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Win
9、g, Bernie Not for Resale, 03/16/2007 00:35:36 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S ZX3920 93 4933608 0533242 564 2 Z 3920-1991 The sampling of samples for analysis shall be done by the measuring method for total dust mass concentration measuring method as s
10、pecified in 4.2 (measuring method for mass concentration of total dust) of JIS Z 3950. However, filter papers used for the filtering and collecting equipments shall be called filtering materials, and they are low hygroscopic and having a collecting efficiency of not less than 95 % for the particles
11、of 0 . 3 um diameters. And, as a rule, glass fiber filter papers are used for them. The weighing out of samples for analysis shall be done as quickly as possible, to avoid absorption of moisture and mixture of foreign matters. The samples for analysis shall be weighed out by using a chemical balance
12、 and reading to the figure of 0 . 1 mg. 5. Notes on analyzing operation In performing analysis, blank tests shall be made through whole the operations, and the measured values shall be corrected accordingly. 6. Rounding off of analysis values The analysis values shall be expressed in percentages whi
13、ch shall, as a rule, be calculated to three significant figures and rounded off to two figures in accordance with JIS Z 8401. 7 . Methods for chemical analvsis of weld fumes 7 . 1 Classification of methods for chemical analysis The classification of methods for chemical analysis shall be as follows:
14、 (1) Atomic absorption spectrometry This method is used for determination of manganese, copper, nickel, chromium, vanadium, cobalt, lead, zinc, molybdenum, iron and aluminum. (2) Sulphosalicylic acid extraction absorptiometry This method is used for the determination of iron in the sample of iron co
15、ntent 10 wt% or more. (3) Thermal hydrolysis separation - Lanthanum alizarin complexon absorptiometry fluorine. This method is used for the determination of 7 . 2 Atmomic absorption spectrometry 7 . 2 . 1 Summary Put the sample into a platinum crucible together with the filter, decompose it by addin
16、g nitric acid, perchloric acid and hydro- fluoric acid, and concentrate by heating until white smoke arises. hydrochloric acid to it to dissolve salts, and spray into the air-acetylene flame or nitrous oxide-acetylene flame of the atomic absorption spectrometer, and measure the absorbance of it. Add
17、 Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/16/2007 00:35:36 MDTNo reproduction or networking permitted without license from IHS -,-,- (7) (11) 3 Z 3920-1991 Reagents Hydrochloric acid (l+l) R
18、eagents shall be as follows: Nitric acid Perchloric acid Hydrofluoric acid Standard manganese solution (100 ugMn/ml) Weigh out 0 . 1 0 0 g of manganese (not less than 99.9 wt%), decompose it by adding 10 ml of hydrochloric acid (l+l) and heating it, after cooling to the normal temperature, transfer
19、it with water into a 1000 ml volumetric flask and dilute it with water up to the mark line. Standard copper solution (100 UgCulml) Weigh out 0 . 1 0 0 g of copper (not less than 99.96 wt%), decompose it by adding 1 0 ml of nitric acid (l+l) and heating it, after cooling to the normal temperature, tr
20、ansfer it with water into a 1000 ml volumetric flask and dilute it with water up to the mark line. Standard nickel solution (100 LIgNi/ml) Weigh out 0 . 1 0 0 g of nickel (not less than 99.95 wt%), decompose it by adding 10 ml of nitric acid (1+1) and heating it, after cooling to the normal temperat
21、ure, transfer it with water into a 1000 ml volumetric flask and dilute it with water up to the mark line. Standard chromium solution (100 ugCr/ml) Weigh out 0 . 1 0 0 g of chromium (not less than 99.9 wt%), decompose it by adding 10 ml of hydrochloric acid (l+l) and heating it, after cooling to the
22、normal temperature, transfer it with water into a 1000 ml volumetric flask and dilute it with water up to the mark line. Standard vanadium solution (100 ugV/ml) vanadium (not less than 99.9 wt%), decompose it by adding 10 ml of aqua regia (hydrochloric acid 3 + nitric acid i ) and heating it, and ev
23、aporate it to almost dryness. 10 ml of hydrochloric acid (l+i) to this and heating it, after cooling to the normal temperature, transfer it with water into a 1000 ml volumetric flask and dilute it with water up to the mark line. Weigh out 0 . 1 0 0 g of Dissolve salts by adding Standard cobalt solut
24、ion (100 I.igCo/ml) Weigh out 0 . 1 0 0 g of cobalt (not less than 99.9 wt%), decompose it by adding 10 ml of nitric acid (l+l) and heating it, after cooling to the normal temperature, transfer it with water into a 1000 ml volumetric flask and dilute it with water up to the mark line. Standard lead
25、solution (100 ugPb/ml) (not less than 99.99 wt%), decompose it by adding 25 ml of nitric acid (1+4) and heating it, after cooling to the normal tempera- ture, transfer it with water into a 1000 ml volumetric flask and dilute it with water up to the mark line. Weigh out 0 . 1 0 0 g of lead Copyright
26、Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/16/2007 00:35:36 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S Z*3920 91 m 4733608 0533244 337 m 4 Z 3920-1991 (12) Standard
27、zinc solution (100 vgZn/ml) (not less than 99.99 ut%), decompose it by adding 10 m l of hydrochloric acid (l+i) and heating it, after cooling t o the normal temperature, transfer it with water into a 1000 m l volumetric flask and dilute it with water up t o the mark line. Weigh out 0.100 g of zinc (
28、13) Standard molybdenum solution (100 LigMo/ml) Weigh out 0.100 g of molybdenum (not less than 99.9 ut%), decompose it by adding 10 m l of hydrochloric acid (l+i) and a small quantity of nitric acid and heating it, after cooling t o the normal temperature, transfer it with water into a 1000 m l volu
29、metric flask and dilute it with water up t o the mark line. (14) Standard iron solution (100 UgFe/ml) (not less than 99.5 ut%), decompose by adding 10 m l of nitric acid (l+l) and heating it, after cooling to the normal temperature, transfer it with water into a 1000 m l volumetric flask and dilute
30、it with water up to the mark line. Weigh out 0.100 g of iron (15) Standard aluminum solution (100 pgAl/ml) aluminum (not less than 99.9 ut%), decompose it by adding 5 m l of hidrochloric acid (l+i) and 5 m l of nitric acid (l+i) and heating it, purge nitric oxide and others, after cooling t o the no
31、rmal temperature, transfer it with water into a 1000 m l volumetric flask and dilute it with water up t o the mark line. Weigh out 0.100 g of 7.2.3 Quantity of sample to be weighed out Take the difference of the masses of the f i l t e r before and after collecting the weld fumes, as specified in 4
32、. 2 (Measuring method for mass concentration of total dust) of JIS Z 3950 as the quantity of sample t o be weighed out, and accurately weigh out about 10 m g of it. 7.2.4 Operation The operation shall be as follows: (1) Preparing of sample solution The preparing of sample solution shall be performed
33、 by the following procedures: (a) Transfer the sample together with the f i l t e r into a platinum crucible (for example No. 50) or a plutinum dish (for example No. 50). (b) Decompose it by adding 3 m g of nitric acid, 5 m l of perchloric acid and 10 m g of hydrofluoric acid and gently heating it.
34、Further, continue heating until white smoke of perchloric acid arises and evaporate it until it concentrates t o 2 to 3 ml. (c) After allowing the solution t o cool down t o the room tempera- ture, dissolve it by adding 10 mg of hydrochloric acid (l+l (1)(2), after cooling t o the normal temperature
35、, transfer it w i t h water into a 100 m l volumetric flask and, dilute it with water up t o the mark line( 3 ) . Notes (I) In this occasion, i f any insoluble matter such as silicon dioxide is observed, f i l t e r it with a f i l t e r paper (Class 5 A) and wash the residue with water. Copyright J
36、apanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/16/2007 00:35:36 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S Zt3920 93 m 4933b08 0533245 273 m Element Wavelength nm Mangane
37、se 279.5 5 Z 3920-1991 Flame used Air-acetylene ( 2, When the content of aluminum is high and aluminum oxide or the like is likely to remain as insoluble matter, operate as follows : Copper 324.8 Nickel 305.1 or 232.0 Chromium 357.9 Vanad i um 3 1 8 . 4 Filter the sample solution with a filter paper
38、 (Class 5 C ) , wash the residue with warm water and retain the filtrate and washings as the main solution. a platinum crucible (for example No.20) together with the filter paper, dry and ignite them to ashes. Add 1 . 0 g of sodium carbonate (anhydrous) to the ashes, melt them by ignition, and then
39、cool them to the room temperature. Dissolve the molten substance in a little volume of water by heating, add hydrochloric acid (l+l carefully to make the solution slightly acidic and add it to the main solution having been retained. Transfer the residue into Air-acetylene Air-acetylene Nitrous oxide
40、-acetylene Nitrous oxide-acetylene ( 3 When the mass of each element in this sample solution exceeds the following value, separate out to be less than it. Cobalt Lead Zinc Molybdenum Iron Aluminum For manganese, copper, nickel, vanadium, lead, zinc, iron and aluminum, the masses shall be 1000 pg. Fo
41、r chromium, cobalt and molybdenum, they shall be 500 pg. 240.7 Air-acetylene 283.3 Air-acetylene 213 . 9 Air-acetylene 313.3 Nitrous oxide-acetylene 248.3 Air-acetylene 309.3 Nitrous oxide-acetylene Transfer the separated sample solution into a 100 ml volumetric flask, after adjusting the total volu
42、me of hydrochloric acid (l+i) contained in it to be 10 ml, and cooling to the normal temperature, dilute it with water up to the mark line. Measurement of absorbance by ( i ) ( c ) , measure the absorbance of each element, by using an atomic absorption spectrometer zero point of which is adjusted by
43、 water, in accordance with the measuring conditions of Table 1 . With a part of the solution prepared Table 1 . Measuring conditions Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/16/2007 00:35:36
44、 MDTNo reproduction or networking permitted without license from IHS -,-,- 6 Z 3920-1991 Standard element solution Subclause Standard manganese solution i7.2.2 (511 Standard copper solution C 7 . 2 . 2 (611 Standard nickel solution 7.2.2 (711 7 . 2 . 5 Blank test Without a sample, make the same oper
45、ation as make with the sample in parallel, using a filter of the same kind as used in collecting weld fumes. Sample quantity (Corresponding quantity of element) O to 1 0 . 0 ml (as quantity of element O to 1000 ug1 7 . 2 . 6 Preparation of calibration curves The preparation of calibra- tion curves s
46、hall be performed by the following procedures. Standard chromium solution 1 7 . 2 . 2 ( 8 1 1 Standard cobalt solution 7.2.2 ( l o ) Standard molybdenum solution 7.2.2 (1311 (1) Selecting the standard element solutions, corresponding to the kind of the electrodes generating the weld fumes, put the v
47、olumes of them shown in Table 2, in steps on several platinum crusibles or dishes. O to 5.0 ml (as quantity of element O to 500 pg) Table 2 . Sample quantity of standard element solution Standard vanadium solution 7 . 2 . 2 (911 Standard lead solution 17.2.2 ( i l ) Standard zinc solution 7.2.2 (121
48、1 Standard iron solution i7.2.2 ( 1 4 ) Standard aluminium solution i7.2.2 (1511 (2) Operate each of them following the procedures of (b) and (c) in 7.2.4 (ii(41. a 0 a a Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/16/2007 00:35:36 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S Z*3920 91 4933608 0533247 O46 7 Z 3920-1991 (3) With a part of these solutions, make the operation